CN115350679B - Device and method for preparing dimethyl carbonate by high-speed jet impact on tubular reactor - Google Patents
Device and method for preparing dimethyl carbonate by high-speed jet impact on tubular reactor Download PDFInfo
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- CN115350679B CN115350679B CN202210985228.5A CN202210985228A CN115350679B CN 115350679 B CN115350679 B CN 115350679B CN 202210985228 A CN202210985228 A CN 202210985228A CN 115350679 B CN115350679 B CN 115350679B
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- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 title claims abstract description 218
- 238000000034 method Methods 0.000 title claims abstract description 23
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 774
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 511
- 239000007788 liquid Substances 0.000 claims abstract description 359
- 238000000926 separation method Methods 0.000 claims abstract description 186
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 71
- 238000002156 mixing Methods 0.000 claims abstract description 65
- 239000000463 material Substances 0.000 claims abstract description 46
- 238000006243 chemical reaction Methods 0.000 claims abstract description 35
- 238000005809 transesterification reaction Methods 0.000 claims description 71
- 229910000831 Steel Inorganic materials 0.000 claims description 66
- 238000012856 packing Methods 0.000 claims description 66
- 239000010959 steel Substances 0.000 claims description 66
- 238000010992 reflux Methods 0.000 claims description 65
- 239000012530 fluid Substances 0.000 claims description 42
- 238000010438 heat treatment Methods 0.000 claims description 34
- 239000006200 vaporizer Substances 0.000 claims description 29
- 238000003860 storage Methods 0.000 claims description 26
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims description 22
- 239000003054 catalyst Substances 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 18
- 239000011259 mixed solution Substances 0.000 claims description 15
- 230000003116 impacting effect Effects 0.000 claims description 13
- 230000014759 maintenance of location Effects 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 8
- CXHHBNMLPJOKQD-UHFFFAOYSA-M methyl carbonate Chemical compound COC([O-])=O CXHHBNMLPJOKQD-UHFFFAOYSA-M 0.000 claims description 6
- 238000005086 pumping Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 238000009826 distribution Methods 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 description 6
- 150000002148 esters Chemical group 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 4
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000005381 potential energy Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 1
- 230000000739 chaotic effect Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/26—Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/128—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by alcoholysis
- C07C29/1285—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by alcoholysis of esters of organic acids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C68/00—Preparation of esters of carbonic or haloformic acids
- C07C68/06—Preparation of esters of carbonic or haloformic acids from organic carbonates
- C07C68/065—Preparation of esters of carbonic or haloformic acids from organic carbonates from alkylene carbonates
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C68/00—Preparation of esters of carbonic or haloformic acids
- C07C68/08—Purification; Separation; Stabilisation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a device and a method for preparing dimethyl carbonate by a high-speed jet impact tubular reactor, wherein the device comprises a material mixing tank, a first high-speed jet impact tubular reactor, a vapor-liquid separation tank, a second high-speed jet impact tubular reactor, a curing tank, a light component separation tower system, a methanol rectifying tower system and a dimethyl carbonate rectifying tower system which are sequentially communicated; meanwhile, the material distribution tank is communicated with the glycol rectifying tower system, the methanol rectifying tower system is respectively communicated with the first high-speed jet impact tubular reactor and the second high-speed jet impact tubular reactor, the vapor-liquid separation tank is communicated with the light component separating tower system, and the light component separating tower system is communicated with the glycol rectifying tower system. The device and the method solve the problems of low heat and mass transfer efficiency, long reaction period, high energy consumption, low reaction rate, low product yield and the like of the traditional equipment and process for preparing the dimethyl carbonate.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a device and a method for preparing dimethyl carbonate by impacting a tubular reactor through high-speed jet flow.
Background
The dimethyl carbonate production process is generally phosgene process, methanol oxidative carbosylation process and transesterification process. Since the phosgene method uses highly toxic phosgene as a main raw material, the two other methods become main methods for synthesizing DMC. The technology of synthesizing DMC by transesterification with co-production of ethylene glycol has been developed rapidly in recent years. The preparation process of the dimethyl carbonate generally adopts a kettle-type reactor and mechanical stirring, and the preparation equipment has the defects of low heat and mass transfer efficiency, long reaction period, high energy consumption and cost rise caused by the increase of the energy consumption, and is not beneficial to industrial production.
The technology and equipment for preparing the dimethyl carbonate with low energy consumption and environmental friendliness are eagerly sought in the field so as to overcome the technical problems.
Disclosure of Invention
The invention provides a device and a method for preparing dimethyl carbonate by impacting a tubular reactor through high-speed jet flow, and aims to solve the problems of low heat and mass transfer efficiency, long reaction period, high energy consumption, low reaction rate, low product yield and the like of the existing equipment and process for preparing the dimethyl carbonate.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
The device comprises a material mixing tank, a first high-speed jet impact tubular reactor, a vapor-liquid separation tank, a second high-speed jet impact tubular reactor, a curing tank, a light component separation tower system, a methanol rectifying tower system and a dimethyl carbonate rectifying tower system which are communicated in sequence; meanwhile, the material distribution tank is communicated with the glycol rectifying tower system, the methanol rectifying tower system is respectively communicated with the first high-speed jet impact tubular reactor and the second high-speed jet impact tubular reactor, the vapor-liquid separation tank is communicated with the light component separating tower system, and the light component separating tower system is communicated with the glycol rectifying tower system.
Furthermore, the structure of the material mixing tank, the vapor-liquid separation tank and the curing tank is consistent, and the material mixing tank, the vapor-liquid separation tank and the curing tank are all tank structures with heating mediums arranged on the periphery and mechanical stirrers arranged inside; the liquid inlet at the top of the batching tank is connected with the outlet end of the bottom pump of the glycol rectifying tower system; a liquid outlet at the bottom of the batching tank is communicated with the nozzles of two first Laval nozzles of the first high-speed jet impact tubular reactor through a first power fluid pump;
The inlet end of the upper end of the vapor-liquid separation tank is communicated with the outlet end of the first tubular reactor of the first high-speed jet impact tubular reactor, the vapor outlet end of the upper end of the vapor-liquid separation tank is communicated with the vapor inlet end of the light component separation tower system through a separation tank condenser, and the outlet end of the bottom end of the vapor-liquid separation tank is communicated with the pipe orifices of two second Laval nozzles of the second high-speed jet impact tubular reactor through a second power fluid pump;
the top liquid inlet of the curing tank is connected with the outlet end of the second tubular reactor of the second high-speed jet impact tubular reactor, and the upper overflow port of the curing tank is connected with the top liquid inlet of the light component separation tower kettle of the light component separation tower system.
Further, the first high-speed jet impact tubular reactor is consistent with the second high-speed jet impact tubular reactor in structure, and comprises a first Laval nozzle, a first mixing cavity, a first high-speed jet impact cavity, a first tubular reactor and a first heater; the first Laval nozzles, the first mixing cavity, the first high-speed jet impact cavity and the first tubular reactor are all arranged in the first heater, the two first Laval nozzles are oppositely arranged and communicated, a cavity formed in the middle of the first mixing cavity is the first mixing cavity, the first high-speed jet impact cavity is communicated in the vertical direction of the middle of the first mixing cavity, the first high-speed jet impact cavity is communicated with one end of the first tubular reactor, the other end of the first tubular reactor is communicated with a liquid inlet at the top of the vapor-liquid separation tank, steam inlets are formed in the pipe openings of the two first Laval nozzles, and the steam inlets are communicated with the outlet end of the methanol vaporizer of the methanol rectifying tower system;
the second high-speed jet impact tubular reactor comprises a second Laval nozzle, a second mixing cavity, a second high-speed jet impact cavity, a second tubular reactor and a second heater; the second Laval nozzles, the second mixing cavity, the second high-speed jet impact cavity and the second tubular reactor are all arranged in the second heater, the two second Laval nozzles are oppositely arranged and communicated, the cavity formed by the middle communicating part is the second mixing cavity, the second high-speed jet impact cavity is communicated in the vertical direction of the middle part of the second mixing cavity, the second high-speed jet impact cavity is communicated with one end of the second tubular reactor, and the other end of the second tubular reactor is communicated with a liquid inlet at the top of the curing tank; the orifices of the two second Laval nozzles are communicated with the liquid outlet at the bottom of the vapor-liquid separation tank through a second power fluid pump, and vapor inlets are formed in the orifices of the two second Laval nozzles and are communicated with the outlet end of the methanol vaporizer of the methanol rectifying tower system. Further, the first tubular reactor aspect ratio was 1000 and the second tubular reactor aspect ratio was 1000.
Further, the light component separation tower system comprises a light component separation tower kettle, a light component white steel structured packing tower, a light component condenser, a light component receiving tank, a light component liquid pump and a light component separation tower bottom pump; the light component separation tower kettle is of a structure that a heating medium is arranged on the periphery, a liquid inlet at the top of the light component separation tower kettle is communicated with an upper overflow port of the curing tank, a liquid outlet at the bottom of the light component separation tower kettle is communicated with a liquid inlet of a light component separation tower bottom pump, an outlet of the light component separation tower bottom pump is communicated with a liquid reflux inlet of a light component separation tower kettle, and an outlet end of the light component separation tower bottom pump is connected with a liquid inlet of a glycol rectifying tower system; the upper end of the light component separation tower kettle is communicated with the light component white steel structured packing tower and is integrally arranged, the steam inlet end of the light component white steel structured packing tower is communicated with the outlet end of the separation tank condenser, the steam outlet end of the light component white steel structured packing tower is communicated with the inlet end of the light component condenser, the outlet end of the light component condenser is communicated with the inlet end of the light component receiving tank, the outlet end of the light component receiving tank is communicated with the outlet end of the light component liquid pump, the outlet end of the light component liquid pump is communicated with the reflux inlet at the upper part of the light component white steel structured packing tower, and the outlet end of the light component liquid pump is also communicated with the inlet of the methanol rectifying tower system.
Further, the methanol rectifying tower system comprises a methanol rectifying tower reboiler, a methanol rectifying tower white steel structured packing tower, a methanol rectifying tower condenser, a methanol rectifying tower azeotropic liquid receiving tank, a methanol rectifying tower azeotropic liquid pump, a methanol vaporizer and a methanol rectifying tower bottom pump; the middle liquid inlet of the methanol rectifying tower system is communicated with the outlet end of a light component liquid pump of the light component separating tower system and is also communicated with the outlet end of an azeotropic liquid pump of a dimethyl carbonate rectifying tower of the dimethyl carbonate rectifying tower system; the steam outlet at the top of the white steel structured packing tower of the methanol rectifying tower is communicated with the inlet end of the condenser of the methanol rectifying tower, the outlet end of the condenser of the methanol rectifying tower is communicated with the inlet end at the top of the azeotropic liquid receiving tank of the methanol rectifying tower, the outlet end at the bottom of the azeotropic liquid receiving tank of the methanol rectifying tower is communicated with the inlet end of the azeotropic liquid pump of the methanol rectifying tower, the outlet end of the azeotropic liquid pump of the methanol rectifying tower is communicated with the reflux liquid inlet at the upper part of the white steel structured packing tower of the methanol rectifying tower and is also communicated with the liquid inlet at the middle part of the dimethyl carbonate rectifying tower system; the outlet of the bottom of the white steel structured packing tower of the methanol rectifying tower is communicated with the inlet end of a pump at the bottom of the methanol rectifying tower, the outlet end of the pump at the bottom of the methanol rectifying tower is communicated with the inlet end of a reboiler of the methanol rectifying tower, the reboiler of the methanol rectifying tower is of a structure provided with heating medium, and the outlet end of the reboiler of the methanol rectifying tower is communicated with a reboiling liquid reflux port of the white steel structured packing tower of the methanol rectifying tower; the outlet end of the bottom pump of the methanol rectifying tower is also communicated with the inlet end of the methanol vaporizer, the inlet end of the methanol vaporizer is also communicated with the inlet end of fresh methanol, and the outlet end of the methanol vaporizer is respectively communicated with the steam inlets of the first Laval nozzle and the second Laval nozzle.
Further, the dimethyl carbonate rectifying tower system comprises a dimethyl carbonate rectifying tower reboiler, a dimethyl carbonate rectifying tower white steel structured packing tower, a dimethyl carbonate rectifying tower condenser, a dimethyl carbonate rectifying tower azeotropic liquid receiving tank, a dimethyl carbonate rectifying tower azeotropic liquid pump, a dimethyl carbonate storage tank and a dimethyl carbonate rectifying tower bottom pump; the liquid inlet in the middle of the white steel structured packing tower of the dimethyl carbonate rectifying tower is communicated with the outlet end of the azeotropic liquid pump of the methanol rectifying tower; the steam outlet at the top of the white steel structured packing tower of the dimethyl carbonate rectifying tower is communicated with the inlet end of the condenser of the dimethyl carbonate rectifying tower, the outlet end of the condenser of the dimethyl carbonate rectifying tower is connected with the inlet end at the top of the azeotropic liquid receiving tank of the dimethyl carbonate rectifying tower, the outlet end at the bottom of the azeotropic liquid receiving tank of the dimethyl carbonate rectifying tower is communicated with the inlet end of the azeotropic liquid pump of the dimethyl carbonate rectifying tower, the outlet end of the azeotropic liquid pump of the dimethyl carbonate rectifying tower is communicated with the reflux liquid inlet at the upper part of the white steel structured packing tower of the dimethyl carbonate rectifying tower, and the outlet end of the azeotropic liquid pump of the dimethyl carbonate rectifying tower is also communicated with the liquid inlet at the middle part of the methanol rectifying tower system; the outlet of the bottom of the white steel structured packing tower of the dimethyl carbonate rectifying tower is communicated with the inlet end of a pump at the bottom of the dimethyl carbonate rectifying tower, the outlet end of the pump at the bottom of the dimethyl carbonate rectifying tower is communicated with the inlet end of a reboiler of the dimethyl carbonate rectifying tower, the reboiler of the dimethyl carbonate rectifying tower is of a structure provided with heating medium, and the outlet end of the reboiler of the dimethyl carbonate rectifying tower is communicated with a reboiling liquid reflux port of the white steel structured packing tower of the dimethyl carbonate rectifying tower; the outlet end of the bottom pump of the dimethyl carbonate rectifying tower is also connected with the inlet end of the top of the dimethyl carbonate storage tank.
Further, the ethylene glycol rectifying tower system comprises an ethylene glycol rectifying tower reboiler, an ethylene glycol rectifying tower white steel structured packing tower, an ethylene glycol rectifying tower condenser, an ethylene glycol receiving tank, an ethylene glycol pump, an ethylene glycol storage tank and an ethylene glycol rectifying tower bottom pump; the middle liquid inlet of the glycol rectifying tower system is communicated with the outlet end of the bottom pump of the light component separating tower; the steam outlet at the top of the white steel structured packing tower of the ethylene glycol rectifying tower is communicated with the inlet end of the condenser of the ethylene glycol rectifying tower, the outlet end of the condenser of the ethylene glycol rectifying tower is communicated with the inlet end at the top of the ethylene glycol receiving tank, the outlet end at the bottom of the ethylene glycol receiving tank is communicated with the inlet end of the ethylene glycol pump, the outlet end of the ethylene glycol pump is communicated with the reflux liquid inlet at the upper part of the white steel structured packing tower of the ethylene glycol rectifying tower, and the outlet end of the ethylene glycol pump is also communicated with the inlet end at the top of the ethylene glycol storage tank; the outlet of the reboiler of the ethylene glycol rectifying tower is communicated with the reboiling liquid return port of the white steel structured packing tower of the ethylene glycol rectifying tower; the outlet end of the bottom pump of the glycol rectifying tower is also communicated with the inlet end of the top of the material mixing tank.
The method for preparing the dimethyl carbonate by using the device for preparing the dimethyl carbonate by impacting the tubular reactor through high-speed jet flow specifically comprises the following steps of:
Step 1, raw material ethylene carbonate and a catalyst enter a batching tank to be stirred and mixed uniformly to obtain a mixed solution, wherein the dosage of the catalyst is 0.15-0.25% of the mass of the ethylene carbonate; the mixed solution reaches the reaction temperature under the heating of a heating medium, and continuously enters a first high-speed jet flow impact tubular reactor through a first power fluid pump;
Step 2, pumping the mixed solution of the material mixing tank into two opposite first Laval nozzles through a power fluid pump, and sucking methanol steam at the same time, wherein the molar ratio of the methanol to the ethylene carbonate is 4-4.4: 1, two high-speed jet flows ejected from a first Laval pipe are mutually impacted in a high-speed jet flow impact cavity, then enter a first tubular reactor for transesterification reaction to obtain dimethyl carbonate steam and transesterification liquid, and methanol steam and dimethyl carbonate steam and transesterification liquid generated by the reaction continuously enter a vapor-liquid separation tank;
Step 3, separating the methanol steam, the dimethyl carbonate steam generated by the reaction and the transesterification liquid in a vapor-liquid separation tank, and enabling the separated methanol steam and the dimethyl carbonate steam generated by the reaction to enter a light component separation tower system; continuously feeding the transesterification liquid separated from the light components into a second high-speed jet flow impact tubular reactor through a second power fluid pump;
Pumping the transesterification liquid in the vapor-liquid separation tank into two opposite second Laval nozzles through a second power fluid pump, sucking methanol vapor at the same time, wherein the addition amount of the methanol is consistent with that in the step 2, two high-speed jet streams ejected from the second Laval nozzles are mutually impacted in a high-speed jet stream impact cavity, then the two high-speed jet streams enter a second tubular reactor for transesterification reaction, and the methanol vapor from the second high-speed jet stream impact tubular reactor, and methyl carbonate vapor generated by the reaction and the transesterification liquid continuously enter a curing tank;
Step 5, continuously carrying out supplementary transesterification reaction on the transesterification liquid in a curing tank; the curing liquid overflowed from the curing tank enters a light component separation tower system;
Step 6, continuously feeding methanol steam from a vapor-liquid separation tank and dimethyl carbonate steam generated by reaction and curing liquid from a curing tank into a light component separation tower system, condensing light component gas separated by the light component separation tower system into a light component liquid receiving tank through a condenser, taking part of light component liquid separated by the light component separation tower system as reflux of the light component separation tower system, and feeding part of the light component liquid into a methanol rectifying tower system; the tower bottom liquid of the light component separation tower system continuously enters the glycol rectifying tower system through a pump at the bottom of the separation tower;
step 7, continuously feeding the light component liquid from the light component separation tower system and the azeotropic liquid from the azeotropic liquid receiving tank of the dimethyl carbonate rectifying tower into the methanol rectifying tower system, condensing the azeotropic mixture steam separated from the top of the methanol rectifying tower system by a condenser of the methanol rectifying tower, feeding the azeotropic mixture steam into the azeotropic liquid receiving tank to obtain azeotropic liquid, and feeding part of the azeotropic mixture steam serving as reflux of the methanol rectifying tower system and part of the azeotropic mixture steam into the dimethyl carbonate rectifying tower system; the tower bottom liquid of the methanol rectifying tower system enters a methanol vaporizer through a pump at the bottom of the methanol rectifying tower, and vaporized methanol is continuously used for transesterification;
Step 8, continuously feeding the azeotropic liquid from the azeotropic liquid receiving tank of the methanol rectifying tower system into the dimethyl carbonate rectifying tower system, condensing the azeotropic mixture steam separated from the top of the dimethyl carbonate rectifying tower system through a dimethyl carbonate rectifying tower condenser, feeding the azeotropic mixture steam into the azeotropic liquid receiving tank of the dimethyl carbonate rectifying tower to obtain azeotropic liquid, partially taking the azeotropic liquid as reflux of the dimethyl carbonate rectifying tower system, and partially taking the azeotropic liquid as feed to return to the methanol rectifying tower system; the tower bottom liquid of the dimethyl carbonate rectifying tower system enters a dimethyl carbonate storage tank through a pump at the bottom of the dimethyl carbonate rectifying tower;
Step 9, continuously feeding tower bottom liquid from the light component separation tower system into an ethylene glycol rectifying tower system, condensing ethylene glycol steam separated from the tower top of the ethylene glycol rectifying tower system through an ethylene glycol rectifying tower condenser, feeding the condensed ethylene glycol steam into an ethylene glycol receiving tank to obtain ethylene glycol, partially serving as reflux of the ethylene glycol rectifying tower system, and partially feeding the fed ethylene glycol into an ethylene glycol storage tank; and (3) the tower bottom liquid of the glycol rectifying tower system enters a glycol rectifying tower reboiler through a part of a pump at the bottom of the glycol rectifying tower to be heated, and then returns to the glycol rectifying tower system, and part of the tower bottom liquid is used as a recovered catalyst to continuously enter a batching tank.
Further, in the step 1, the temperature in the material mixing tank is 70-75 ℃, the pressure is normal pressure, and the retention time of the materials is 0.5-0.75 h;
in the step 2, the temperature in the first high-speed jet impact tubular reactor is 80-85 ℃ and the pressure is 0.2-0.25 MPa;
In the step 3, the temperature in the vapor-liquid separation tank is 70-75 ℃, the pressure is normal pressure, and the retention time of the materials is 0.5-0.75 h;
in the step 4, the temperature in the second high-speed jet impact tubular reactor is 80-85 ℃ and the pressure is 0.2-0.25 MPa:
In the step 5, the temperature in the curing tank is 80-85 ℃, the pressure is 0.2-0.25 MPa, and the retention time of the materials is 1.5-2 h;
in the step 6, the temperature of the tower bottom of the light component separation tower system is 75-78 ℃, the temperature of the tower top is 64-66 ℃, the reflux ratio is 3-4, and the pressure is normal pressure;
In the step 7, the bottom temperature of the methanol rectifying tower system is 70 ℃, and the bottom pressure is 0.13MPa; the temperature of the tower top is 64 ℃, the pressure of the tower top is normal pressure, and the reflux ratio is 2;
in the step 8, the bottom temperature of the dimethyl carbonate rectifying tower system is 183 ℃ and the bottom pressure is 1.33MPa; the temperature of the tower top is 147 ℃, the pressure of the tower top is 1.30MPa, and the reflux ratio is 1.2;
In the step 9, the temperature of the top of the glycol rectifying tower system is 150 ℃, and the pressure of the top of the tower is 0.02MPa; the bottom temperature was 178℃and the reflux ratio was 1.5.
Compared with the prior art, the device and the method for preparing the dimethyl carbonate by impacting the tubular reactor by the high-speed jet flow have the beneficial effects that:
1. The high-speed jet impact tubular reactor is adopted to carry out transesterification, two heterogeneous fluids flow in opposite directions at high speed, a highly turbulent impact area is formed by impact, the impact flow effectively improves the mixing and mass transfer effects in the reactor, and the reaction rate and the product yield are improved;
2. the reaction time is shortened, the energy is saved, the production efficiency is improved, and the method is environment-friendly;
3. the device produces the byproduct ethylene glycol while producing the dimethyl carbonate, so that the economic benefit of the device is improved;
4. the yield of the dimethyl carbonate is more than 95 percent, and the quality of the dimethyl carbonate is superior to the industrial national standard; the invention has mature process, advanced equipment, continuous operation and high automation degree.
Drawings
FIG. 1 is a schematic diagram of an apparatus for preparing dimethyl carbonate using a high-velocity jet impingement tube reactor according to the present invention;
Reference numerals: 1. 1-1 parts of a proportioning tank, 1-2 parts of a mechanical stirrer and a first power fluid pump; 2. the first high-speed jet stream impacts the tubular reactor, 2-1, the first Laval nozzle, 2-2, the mixing cavity, 2-3, the first high-speed jet stream impacts the cavity, 2-4, the first tubular reactor, 2-5, the first heater; 3. 3-1 parts of a vapor-liquid separation tank, 3-2 parts of a mechanical stirrer of the separation tank, 3-3 parts of a condenser of the separation tank and 3-3 parts of a second power fluid pump; 4. the second high-speed jet stream impacts the tubular reactor, 4-1, the second Laval nozzle, 4-2, the mixing cavity, 4-3, the second high-speed jet stream impacts the cavity, 4-4, the second tubular reactor, 4-5, the second heater; 5. 5-1 parts of a curing tank and a mechanical stirrer of the curing tank; 6. the device comprises a light component separation tower, 6-1 parts of a light component separation tower, 6-2 parts of a light component white steel structured packing, 6-3 parts of a light component condenser, 6-4 parts of a light component receiving tank, 6-5 parts of a light component liquid pump, and 6-6 parts of a light component separation tower bottom pump; 7. 7-1 parts of methanol rectifying tower, 7-1 parts of methanol rectifying tower reboiler, 7-2 parts of methanol rectifying tower white steel structured packing, 7-3 parts of methanol rectifying tower condenser, 7-4 parts of methanol rectifying tower azeotropic liquid receiving tank, 7-5 parts of methanol rectifying tower azeotropic liquid pump, 7-6 parts of methanol vaporizer, 7-7 parts of methanol rectifying tower bottom pump; 8. 8-1 parts of dimethyl carbonate rectifying tower, 8-2 parts of dimethyl carbonate rectifying tower reboiler, 8-3 parts of dimethyl carbonate rectifying tower white steel structured packing, 8-4 parts of dimethyl carbonate rectifying tower condenser, 8-5 parts of dimethyl carbonate rectifying tower azeotropic liquid receiving tank, 8-6 parts of dimethyl carbonate rectifying tower azeotropic liquid pump, 8-7 parts of dimethyl carbonate storage tank and 8-7 parts of dimethyl carbonate rectifying tower bottom pump; 9. 9-1 parts of ethylene glycol rectifying tower, 9-1 parts of ethylene glycol rectifying tower reboiler, 9-2 parts of ethylene glycol rectifying tower white steel structured packing, 9-3 parts of ethylene glycol rectifying tower condenser, 9-4 parts of ethylene glycol receiving tank, 9-5 parts of ethylene glycol pump, 9-6 parts of ethylene glycol storage tank, 9-7 parts of ethylene glycol rectifying tower bottom pump.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Aiming at engineering problems and market demands, the invention provides a method which has the advantages of mature process, continuous operation, high degree of automation, advanced reactor technology, high reaction efficiency, energy conservation and environmental protection; the advanced high-speed jet flow is adopted to strike the tubular reactor for transesterification reaction, and as the mixed liquid is sprayed out at high speed through the Laval pipe, a negative pressure area is generated at a gas suction inlet, so that the gas is sucked, rapidly expands in the negative pressure area and is beaten into tiny bubbles by a power fluid, and enters a mixing cavity; at this time, in the mixing cavity, the gas and the liquid are fully mixed in the mixing cavity, and the discharge is accelerated due to energy exchange, the speed can reach the sonic speed, the potential energy of the mixed liquid is increased to the maximum, and the effects of mass transfer and heat transfer are stronger; the two fluids flow at a high speed in opposite directions, and a highly turbulent impact area is formed by impact, so that the heat and mass transfer of the process is greatly enhanced; the strong microscopic mixing and pressure fluctuation characteristics of the impinging stream can enable the chemical reaction to be fast carried out, and the effective and uniform supersaturation degree is generated instantaneously; and because of the chaos flow state, the mixing scale is reduced rapidly, the turbulence intensity and the energy diffusion are enhanced by the eddies with different scales and the folding collision with each other, the molecules are promoted to reach more effective high-level collision when the chemical reaction occurs, the impinging stream enhances the heat transfer and the mass transfer, the reaction rate and the product yield are improved, the quality of the prepared dimethyl carbonate is higher than that of the industrial national standard, and the reaction rate and the product yield are improved.
As shown in fig. 1, the device for preparing the dimethyl carbonate by using the high-speed jet impact tubular reactor comprises a material mixing tank 1, a first high-speed jet impact tubular reactor 2, a vapor-liquid separation tank 3, a second high-speed jet impact tubular reactor 4, a curing tank 5, a light component separation tower system 6, a methanol rectifying tower system 7 and a dimethyl carbonate rectifying tower system 8 which are sequentially communicated; meanwhile, the material mixing tank 1 is also communicated with an ethylene glycol rectifying tower system 9, the methanol rectifying tower system 7 is also respectively communicated with the first high-speed jet impact tubular reactor 2 and the second high-speed jet impact tubular reactor 4, the vapor-liquid separation tank 3 is also communicated with a light component separating tower system 6, and the light component separating tower system 6 is also communicated with the ethylene glycol rectifying tower system 9.
The material mixing tank 1 is a tank body structure with a heating medium arranged on the periphery and a mechanical stirrer 1-1 arranged inside, the top of the material mixing tank 1 is provided with a catalyst and ethylene carbonate liquid inlet, and the liquid inlet at the top of the material mixing tank 1 is connected with the outlet end of a pump 9-7 at the bottom of a glycol rectifying tower of the glycol rectifying tower system 9; the liquid outlet at the bottom of the material mixing tank 1 is connected with the inlet end of a first power fluid pump 1-2, and the outlet end of the first power fluid pump 1-2 is connected with the liquid inlet end of a first Laval nozzle 2-1 of a first high-speed jet impact tubular reactor 2; the material mixing tank 1 is used for mixing ethylene carbonate and a catalyst, and uniformly mixing the ethylene carbonate and the catalyst under the stirring action; the mixed solution reaches the reaction temperature under the heating of the heating medium, and enters the first high-speed jet flow impact tubular reactor 2 through the power fluid pump 1-2.
The first high-speed jet impact tubular reactor 2 comprises a first Laval nozzle 2-1, a first mixing cavity 2-2, a first high-speed jet impact cavity 2-3, a first tubular reactor 2-4 and a first heater 2-5; the first Laval nozzle 2-1, the first mixing cavity 2-2, the first high-speed jet impact cavity 2-3 and the first tubular reactor 2-4 are arranged inside the first heater 2-5, the two first Laval nozzles 2-1 are oppositely arranged and communicated, the cavity formed by the middle communicating part is the first mixing cavity 2-2, the first high-speed jet impact cavity 2-3 is communicated in the vertical direction of the middle part of the first mixing cavity 2-2, the first high-speed jet impact cavity 2-3 is communicated with one end of the first tubular reactor 2-4, the other end of the first tubular reactor 2-4 is communicated with the liquid inlet at the top of the vapor-liquid separation tank 3, the first tubular reactor 2-4 is a pipe with the length-diameter ratio of more than 1000, can be phi 75mm or phi 100mm, and can be arranged as a reciprocating type or spring type.
The pipe orifices of the two first Laval nozzles 2-1 are provided with steam inlets which are communicated with the outlet ends of the methanol vaporizer 7-6 of the methanol rectifying tower system 7. The first high-speed jet stream impinges on the tubular reactor 2 for transesterification; the two opposite first Laval nozzles 2-1 are communicated with the material distribution tank 1 through a first power fluid pump 1-2 and are communicated with the outlet end of a methanol vaporizer 7-6 of a methanol rectifying tower system 7, the mixed liquid of the material distribution tank 1 is pumped into the two opposite first Laval nozzles 2-1 through the first power fluid pump 1-2, the air inlets of the two opposite first Laval nozzles 2-1 simultaneously suck the vaporized methanol vapor at the outlet end of the methanol vaporizer 7-6 of the methanol rectifying tower system 7, two high-speed jet streams (mixed liquid of the material distribution tank 1 and methanol vapor of the methanol rectifying tower system 7) ejected from the first Laval nozzles 2-1 are mutually impacted in the high-speed jet impact cavity 2-3 through the first mixing cavity 2-2, then enter the first tubular reactor 2-4 for transesterification, and the transesterification liquid continuously enters the vapor-liquid separation tank 3.
Specifically, as the raw material mixed liquid of the material mixing tank 1 is sprayed out at a high speed through the first Laval nozzle 2-1, a negative pressure area is generated at the steam inlet of the first Laval nozzle 2-1, so that the methanol steam of the methanol rectifying tower system 7 is sucked in, rapidly expands in the negative pressure area and is beaten into tiny bubbles by a power fluid, and enters the first mixing cavity 2-2 of the first Laval nozzle 2-1; at this time, in the first mixing cavity 2-2, the methanol vapor and the mixed liquid are fully mixed, and are accelerated to be discharged due to energy exchange, the speed can reach the sonic velocity, and the potential energy of the mixed liquid is increased to the maximum through the first mixing cavity 2-2 of the first Laval nozzle 2-1, so that the effects of mass transfer and heat transfer are stronger; two streams of fluid from the first Laval nozzle 2-1 flow at opposite high speed, and form a highly turbulent impact area through impact, so that the heat and mass transfer of the process is greatly enhanced; the strong microscopic mixing and pressure fluctuation characteristics of the impinging stream can enable the chemical reaction to be fast carried out, and the effective and uniform supersaturation degree is generated instantaneously; and because the chaotic flow state enables the mixing scale to be rapidly reduced, the vortex with different scales and mutually folded collision enhance the turbulence intensity and the energy diffusion, so that molecules are caused to achieve more effective high-level collision when chemical reaction occurs, the mixing and mass transfer effects in the reactor are effectively improved by the impinging stream, and the reaction rate and the product yield are improved.
The gas-liquid separation tank 3 is a tank body structure with a heat medium arranged on the outer periphery and a separation tank mechanical stirrer 3-1 arranged inside, the inlet end of the upper end of the gas-liquid separation tank 3 is communicated with the outlet end of the first tubular reactor 2-4, the gas outlet end of the upper end of the gas-liquid separation tank 3 is communicated with the gas inlet end of the light component separation tower system 6 through a separation tank condenser 3-2, and the outlet end of the bottom end of the gas-liquid separation tank 3 is communicated with two second Laval nozzles 4-1 of the second high-speed jet impact tubular reactor 4 through a second power fluid pump 3-3. The vapor-liquid separation tank 3 is used for separating methanol vapor and dimethyl carbonate vapor generated by the reaction from transesterification liquid; the transesterification liquid from the first high-speed jet impact tubular reactor 2 continuously enters a liquid inlet at the upper end of a vapor-liquid separation tank 3, the vapor-liquid separation tank 3 separates methanol vapor, dimethyl carbonate vapor generated by reaction and the transesterification liquid, the separated vapor enters a light component separation tower system 6 through a separation tank condenser 3-2, and the transesterification liquid from which light components are separated enters a second high-speed jet impact tubular reactor 4 through a power fluid pump 3-3.
The structure of the second high-speed jet impact tubular reactor 4 is consistent with that of the first high-speed jet impact tubular reactor 2, and the second high-speed jet impact tubular reactor 4 comprises a second Laval nozzle 4-1, a second mixing cavity 4-2, a second high-speed jet impact cavity 4-3, a second tubular reactor 4-4 and a second heater 4-5; the second Laval nozzle 4-1, the second mixing cavity 4-2, the second high-speed jet impact cavity 4-3 and the second tubular reactor 4-4 are arranged inside the second heater 4-5, the two second Laval nozzles 4-1 are oppositely arranged and communicated, the cavity formed by the middle communicating part is the second mixing cavity 4-2, the second high-speed jet impact cavity 4-3 is communicated in the vertical direction of the middle part of the second mixing cavity 4-2, the second high-speed jet impact cavity 4-3 is communicated with one end of the second tubular reactor 4-4, and the other end of the second tubular reactor 4-4 is communicated with a liquid inlet at the top of the curing tank 5. The pipe orifices of the two second Laval nozzles 4-1 are communicated with the liquid outlet at the bottom of the vapor-liquid separation tank 3 through a second power fluid pump 3-3, the pipe orifices of the two second Laval nozzles 4-1 are provided with steam inlets, and the steam inlets are communicated with the outlet end of the methanol vaporizer 7-6 of the methanol rectifying tower system 7. The second high-velocity jet stream impinges on the tubular reactor 4 for transesterification reactions.
The two second Laval nozzles 4-1 are communicated with a liquid outlet at the bottom of the vapor-liquid separation tank 3 through a second power fluid pump 3-3, and are communicated with an outlet end of a methanol vaporizer 7-6 of the methanol rectifying tower system 7, the mixed liquid of the vapor-liquid separation tank 3 is pumped into the two opposite second Laval nozzles 4-1 through the second power fluid pump 3-3, vapor inlets of the two opposite second Laval nozzles 4-1 simultaneously suck the vaporized methanol vapor at the outlet end of the methanol vaporizer 7-6 of the methanol rectifying tower system 7, two high-speed jet streams (the transesterification liquid of the vapor-liquid separation tank 3 and the methanol vapor of the methanol rectifying tower system 7) are ejected from the second Laval nozzles 4-1, and are mutually impacted in the high-speed jet stream impact cavity 4-3 through the second mixing cavity 4-2, then enter the second tubular reactor 4-4 for transesterification, and the transesterification liquid continuously enters the curing tank 5.
The curing tank 5 is of a tank body structure with a heating medium arranged on the periphery and a mechanical stirrer 5-1 arranged in the curing tank; the top liquid inlet of the curing tank 5 is connected with the outlet end of the second tubular reactor 4-4 of the second high-speed jet impact tubular reactor 4, and the upper overflow port of the curing tank 5 is connected with the top liquid inlet of the light component separation tower kettle 6-1; the curing tank 5 is used for continuing the supplementary transesterification reaction; the transesterification liquid from the second high-speed jet stream impacting the tubular reactor 4 continuously enters the curing tank 5, and the supplementary transesterification reaction is continuously carried out in the curing tank 5; the transesterification material overflowed from the curing tank 5 enters the tower kettle of the light component separation tower system 6.
The light component separation tower system 6 comprises a light component separation tower kettle 6-1, a light component white steel structured packing tower 6-2, a light component condenser 6-3, a light component receiving tank 6-4, a light component liquid pump 6-5 and a light component separation tower bottom pump 6-6; the light component separation tower kettle 6-1 is of a structure that a heating medium is arranged on the periphery, a liquid inlet at the top of the light component separation tower kettle 6-1 is communicated with an upper overflow port of the curing tank 5, a liquid outlet at the bottom of the light component separation tower kettle 6-1 is communicated with a liquid inlet of a light component separation tower bottom pump 6-6, an outlet of the light component separation tower bottom pump 6-6 is communicated with a liquid backflow liquid inlet of the light component separation tower kettle 6-1, and an outlet end of the light component separation tower bottom pump 6-6 is connected with a liquid inlet of the ethylene glycol rectifying tower system 9; the upper end of the light component separation tower kettle 6-1 is integrally communicated with the light component white steel structured packing tower 6-2, the steam inlet end of the light component white steel structured packing tower 6-2 is communicated with the outlet end of the separation tank condenser 3-2, the steam outlet end of the light component white steel structured packing tower 6-2 is communicated with the inlet end of the light component condenser 6-3, the outlet end of the light component condenser 6-3 is communicated with the inlet end of the light component receiving tank 6-4, the outlet end of the light component receiving tank 6-4 is communicated with the outlet end of the light component liquid pump 6-5, the outlet end of the light component liquid pump 6-5 is communicated with the reflux inlet at the upper part of the light component white steel structured packing tower 6-2, and the outlet end of the light component liquid pump 6-5 is also communicated with the inlet of the methanol rectifying tower system 7. The light component separation tower system 6 is used for separating the light components of the ester exchange liquid in the vapor-liquid separation tank 3 and the curing tank 5; the light component gas separated by the light component separation tower system 6 is condensed by a condenser 6-3 and enters a light component liquid receiving tank 6-4, part of the light component gas is used as reflux of the light component separation tower system 6, and the other part of the light component gas enters a methanol rectifying tower system 7; the tower bottom liquid of the light component separation tower system 6 continuously enters the glycol rectifying tower system 9 through the tower bottom pump 6-6 of the light component separation tower.
The methanol rectifying tower system 7 comprises a methanol rectifying tower reboiler 7-1, a methanol rectifying tower white steel structured packing tower 7-2, a methanol rectifying tower condenser 7-3, a methanol rectifying tower azeotropic liquid receiving tank 7-4, a methanol rectifying tower azeotropic liquid pump 7-5, a methanol vaporizer 7-6 and a methanol rectifying tower bottom pump 7-7; the middle liquid inlet of the methanol rectifying tower system 7 is communicated with the outlet end of a light component liquid pump 6-5 of a light component separating tower system 6 and is also communicated with the outlet end of a dimethyl carbonate rectifying tower azeotropic liquid pump 8-5 of a dimethyl carbonate rectifying tower system 8; the steam outlet at the top of the white steel structured packing tower 7-2 of the methanol rectifying tower is communicated with the inlet end of the condenser 7-3 of the methanol rectifying tower, the outlet end of the condenser 7-3 of the methanol rectifying tower is communicated with the inlet end at the top of the azeotropic liquid receiving tank 7-4 of the methanol rectifying tower, the outlet end at the bottom of the azeotropic liquid receiving tank 7-4 of the methanol rectifying tower is communicated with the inlet end of the azeotropic liquid pump 7-5 of the methanol rectifying tower, the outlet end of the azeotropic liquid pump 7-5 of the methanol rectifying tower is communicated with the inlet of reflux liquid at the upper part of the white steel structured packing tower 7-2 of the methanol rectifying tower and is also connected with the inlet at the middle part of the dimethyl carbonate rectifying tower system 8; the liquid outlet at the bottom of the white steel structured packing tower 7-2 of the methanol rectifying tower is connected with the inlet end of a pump 7-7 at the bottom of the methanol rectifying tower, the outlet end of the pump 7-7 at the bottom of the methanol rectifying tower is connected with the inlet end of a reboiler 7-1 of the methanol rectifying tower, the reboiler 7-1 of the methanol rectifying tower is of a structure provided with heating medium, and the outlet end of the reboiler 7-1 of the methanol rectifying tower is connected with a reboiling liquid reflux port of the white steel structured packing tower 7-2 of the methanol rectifying tower; the outlet end of the bottom pump 7-7 of the methanol rectifying tower is also connected with the inlet end of the methanol vaporizer 7-6, the inlet end of the methanol vaporizer 7-6 is also connected with the inlet end of fresh methanol, and the outlet end of the methanol vaporizer 7-6 is respectively connected with the gas inlet ends of the first Laval nozzle 2-1 and the second Laval nozzle 4-1; the methanol rectifying tower system 7 is used for rectifying methanol from azeotropic liquid; the azeotrope steam separated from the top of the methanol rectifying tower system 7 is condensed by a methanol rectifying tower condenser 7-3 and enters a methanol rectifying tower azeotropic liquid receiving tank 7-4, part of the azeotrope steam is used as reflux of the methanol rectifying tower system 7, and the part of the azeotrope steam enters a dimethyl carbonate rectifying tower system 8; the tower bottom liquid of the methanol rectifying tower system 7 enters a methanol vaporizer 7-6 through a methanol rectifying tower bottom pump 7-7, and vaporized methanol is continuously used for transesterification reaction of the first high-speed jet impact tubular reactor 2 and the second high-speed jet impact tubular reactor 4.
The dimethyl carbonate rectifying tower system 8 comprises a dimethyl carbonate rectifying tower reboiler 8-1, a dimethyl carbonate rectifying tower white steel structured packing tower 8-2, a dimethyl carbonate rectifying tower condenser 8-3, a dimethyl carbonate rectifying tower azeotropic liquid receiving tank 8-4, a dimethyl carbonate rectifying tower azeotropic liquid pump 8-5, a dimethyl carbonate storage tank 8-6 and a dimethyl carbonate rectifying tower bottom pump 8-7; the middle liquid inlet of the white steel structured packing tower 8-2 of the dimethyl carbonate rectifying tower is communicated with the outlet end of the azeotropic liquid pump 7-5 of the methanol rectifying tower; the steam outlet at the top of the dimethyl carbonate rectifying tower white steel structured packing tower 8-2 is communicated with the inlet end of a dimethyl carbonate rectifying tower condenser 8-3, the outlet end of the dimethyl carbonate rectifying tower condenser 8-3 is connected with the inlet end at the top of a dimethyl carbonate rectifying tower azeotropic liquid receiving tank 8-4, the outlet end at the bottom of the dimethyl carbonate rectifying tower azeotropic liquid receiving tank 8-4 is communicated with the inlet end of a dimethyl carbonate rectifying tower azeotropic liquid pump 8-5, the outlet end of the dimethyl carbonate rectifying tower azeotropic liquid pump 8-5 is communicated with the reflux liquid inlet at the upper part of the dimethyl carbonate rectifying tower white steel structured packing tower 8-2, and the outlet end of the dimethyl carbonate rectifying tower azeotropic liquid pump 8-5 is also communicated with the liquid inlet at the middle part of a methanol rectifying tower system 7; the liquid outlet at the bottom of the white steel structured packing tower 8-2 of the dimethyl carbonate rectifying tower is communicated with the inlet end of a pump 8-7 at the bottom of the dimethyl carbonate rectifying tower, the outlet end of the pump 8-7 at the bottom of the dimethyl carbonate rectifying tower is communicated with the inlet end of a reboiler 8-1 of the dimethyl carbonate rectifying tower, the reboiler 8-1 of the dimethyl carbonate rectifying tower is of a structure provided with heating medium, and the outlet end of the reboiler 8-1 of the dimethyl carbonate rectifying tower is communicated with a reboiling liquid reflux port of the white steel structured packing tower 8-2 of the dimethyl carbonate rectifying tower; the outlet end of the bottom pump 8-7 of the dimethyl carbonate rectifying tower is also connected with the inlet end of the top of the dimethyl carbonate storage tank 8-6; the dimethyl carbonate rectifying tower system 8 is used for rectifying dimethyl carbonate from azeotropic liquid; the azeotrope steam separated from the top of the dimethyl carbonate rectifying tower system 8 is condensed by a dimethyl carbonate rectifying tower condenser 8-3 and enters a dimethyl carbonate rectifying tower azeotropic liquid receiving tank 8-4, part of the azeotrope steam is used as reflux of the dimethyl carbonate rectifying tower system 8, and the other part of the azeotrope steam is used as feed and returns to the methanol rectifying tower system 7; and the bottom liquid of the methyl carbonate rectifying tower system 8 enters a methyl carbonate storage tank 8-6 through a bottom pump 8-7 of the methyl carbonate rectifying tower.
The ethylene glycol rectifying tower system 9 comprises an ethylene glycol rectifying tower reboiler 9-1, an ethylene glycol rectifying tower white steel structured packing tower 9-2, an ethylene glycol rectifying tower condenser 9-3, an ethylene glycol receiving tank 9-4, an ethylene glycol pump 9-5, an ethylene glycol storage tank 9-6 and an ethylene glycol rectifying tower bottom pump 9-7. The middle liquid inlet of the glycol rectifying tower system 9 is communicated with the outlet end of the light component separating tower bottom pump 6-6; the steam outlet at the top of the ethylene glycol rectifying tower white steel structured packing tower 9-2 is communicated with the inlet end of the ethylene glycol rectifying tower condenser 9-3, the outlet end of the ethylene glycol rectifying tower condenser 9-3 is communicated with the inlet end at the top of the ethylene glycol receiving tank 9-4, the outlet end at the bottom of the ethylene glycol receiving tank 9-4 is communicated with the inlet end of the ethylene glycol pump 9-5, the outlet end of the ethylene glycol pump 9-5 is communicated with the reflux liquid inlet at the upper part of the ethylene glycol rectifying tower white steel structured packing tower 9-2, and the outlet end of the ethylene glycol pump 9-5 is also communicated with the inlet end at the top of the ethylene glycol storage tank 9-6; the liquid outlet at the bottom of the ethylene glycol rectifying tower white steel structured packing tower 9-2 is communicated with the inlet end of an ethylene glycol rectifying tower bottom pump 9-7, the outlet end of the ethylene glycol rectifying tower bottom pump 9-7 is communicated with the inlet end of an ethylene glycol rectifying tower reboiler 9-1, the ethylene glycol rectifying tower reboiler 9-1 is of a structure provided with heating medium, and the outlet end of the ethylene glycol rectifying tower reboiler 9-1 is communicated with a reboiling liquid reflux port of the ethylene glycol rectifying tower white steel structured packing tower 9-2; the outlet end of the tower bottom pump 9-7 of the glycol rectifying tower is also communicated with the inlet end of the top of the material mixing tank 1; the glycol rectifying tower system 9 is used for rectifying glycol from tower bottoms of the light component separating tower system 6; the tower bottom liquid of the light component separation tower system 6 is continuously pumped into an ethylene glycol rectifying tower system 9 through a light component separation tower bottom pump 6-6, ethylene glycol steam separated from the tower top of the ethylene glycol rectifying tower system 9 is condensed by an ethylene glycol rectifying tower condenser 9-3 and enters an ethylene glycol receiving tank 9-4, part of the ethylene glycol steam is used as reflux of the ethylene glycol rectifying tower system 9, and part of the ethylene glycol steam is fed into an ethylene glycol storage tank 9-6; and part of tower bottom liquid of the glycol rectifying tower system 9 enters the glycol rectifying tower reboiler 9-1 through the pump 9-7 at the bottom of the glycol rectifying tower to be heated and then returns to the glycol rectifying tower system 9, and part of tower bottom liquid is used as a recovered catalyst to continuously enter the batching tank 1.
The raw materials adopted by the invention are industrial ethylene carbonate (the mass content is more than 99.5 percent), industrial methanol (the mass content is more than 99.5 percent), catalyst and the like; the utility steam is 0.4MPa, and the temperature of the super-heated steam is 290 ℃; the public engineering water vapor mainly provides heat sources for heating media of a batching tank 1, a first heater 2-5 of a first high-speed jet stream impinging on a tubular reactor 2, heating media of a vapor-liquid separation tank 3, a second heater 4-5 of a second high-speed jet stream impinging on a tubular reactor 4, heating media of a curing tank 5, heating media of a light component separation tower system 6, heating media of a methanol rectifying tower system 7, heating media of a dimethyl carbonate rectifying tower system 8 and heating media of a glycol rectifying tower system 9; the devices of the device are connected through corresponding pipelines, and when the pipelines in the figure 1 are crossed on the figure and are not crossed in practice, the pipelines are drawn according to the principle of continuous vertical and horizontal cutting. The heat medium structure is an existing jacket structure; the heat medium structure of the tower kettle is the existing reboiler structure.
The dimethyl carbonate production method based on the device specifically comprises the following steps:
(1) Raw materials of ethylene carbonate and a catalyst are filled into a batching tank 1, the temperature in the batching tank 1 is 70-75 ℃, the pressure is normal pressure, and simultaneously the ethylene carbonate and the catalyst are uniformly mixed under the stirring action of a mechanical stirrer 1-1 to obtain a mixed solution; the mixed solution reaches the reaction temperature under the heating of the heating medium, and the retention time of the materials is 0.5 to 0.75h; continuously entering a first high-speed jet stream by a power fluid pump 1-2 to strike a tubular reactor 2;
(2) The mixed liquid in the material mixing tank 1 is pumped into two opposite first Laval nozzles 2-1 through a power fluid pump 1-2, the steam inlet of the first Laval nozzles 2-1 simultaneously sucks methanol steam of a methanol rectifying tower system 7, two high-speed jet streams ejected from the first Laval nozzles 2-1 collide with each other in a high-speed jet stream collision cavity, then enter a tubular reactor 2-4 for transesterification reaction to obtain transesterification liquid, and the transesterification liquid continuously enters a vapor-liquid separation tank 3; the temperature in the first high-speed jet impact tubular reactor 2 is 80-85 ℃ and the pressure is 0.2-0.25 MPa;
(3) The vapor-liquid separation tank 3 separates unreacted methanol vapor and dimethyl carbonate vapor generated by the reaction from ester exchange liquid, and the separated vapor enters a light component separation tower system 6; the transesterification liquid from which the light components are separated continuously enters a second high-speed jet stream to strike two opposite second Laval nozzles 4-1 of the tubular reactor 4 through a second power fluid pump 3-3; the temperature in the gas-liquid separation tank 3 is 70-75 ℃, the pressure is normal pressure, and the retention time of the materials is 0.5-0.75 h;
(4) The steam inlet of the second Laval nozzle 4-1 simultaneously sucks the methanol steam of the methanol rectifying tower system 7, two high-speed jet streams sprayed out of the second Laval nozzle 4-1 collide with each other in a high-speed jet stream collision cavity, then enter the second tubular reactor 4-4 for transesterification, and the transesterification liquid discharged from the second high-speed jet stream collision tubular reactor 4 continuously enters the curing tank 5; the temperature in the second high-speed jet impact tubular reactor 4 is 80-85 ℃, and the pressure is 0.2-0.25 MPa:
(5) The transesterification liquid is continuously subjected to the supplementary transesterification reaction in a curing tank 5; the curing liquid overflowed from the curing tank 5 enters the tower kettle of the light component separation tower system 6; the temperature in the curing tank 5 is 80-85 ℃, the pressure is 0.2-0.25 MPa, and the retention time of the materials is 1.5-2 h;
(6) The materials from the vapor-liquid separation tank 3 and the curing tank 5 continuously enter a light component separation tower system 6, light component vapor separated by the light component separation tower system 6 is condensed by a condenser 6-3 and enters a light component liquid receiving tank 6-4, and the obtained light component liquid is respectively used as reflux of the light component separation tower system 6 and enters a methanol rectifying tower system 7; the tower bottom liquid of the light component separation tower system 6 continuously enters the glycol rectifying tower system 9 through a pump 6-6 at the bottom of the light component separation tower; the temperature of the tower bottom of the light component separation tower system 6 is 75-78 ℃, the temperature of the tower top is 64-66 ℃, the reflux ratio is 3-4, and the pressure is normal pressure;
(7) Continuously introducing light component liquid from a light component separation tower system 6 into a methanol rectifying tower system 7, condensing azeotrope steam separated from the top of the methanol rectifying tower system 7 by a methanol rectifying tower condenser 7-3, introducing the azeotrope steam into a methanol rectifying tower azeotropic liquid receiving tank 7-4, and respectively taking the obtained azeotropic liquid as reflux of the methanol rectifying tower system 7 and introducing the azeotropic liquid into a dimethyl carbonate rectifying tower system 8; the tower bottom liquid of the methanol rectifying tower system 7 enters a methanol vaporizer 7-6 through a methanol rectifying tower bottom pump 7-7, and vaporized methanol respectively enters a gas inlet of a first Laval nozzle 2-1 and a gas inlet of a second Laval nozzle 4-1 to be continuously used for transesterification reaction; the temperature of the bottom of the methanol rectifying tower system 7 is 70 ℃ and the pressure of the bottom is 0.13MPa; the temperature of the tower top is 64 ℃, the pressure of the tower top is normal pressure, and the reflux ratio is 2;
(8) Continuously feeding the azeotropic liquid from the methanol rectifying tower system 7 into a dimethyl carbonate rectifying tower system 8, condensing the azeotropic mixture steam separated from the top of the dimethyl carbonate rectifying tower system 8 by a dimethyl carbonate rectifying tower condenser 8-3, feeding the azeotropic mixture into a dimethyl carbonate rectifying tower azeotropic liquid receiving tank 8-4, and respectively returning the obtained azeotropic liquid as reflux of the dimethyl carbonate rectifying tower system 8 and as feed to the methanol rectifying tower system 7; the bottom liquid of the dimethyl carbonate rectifying tower system 8 enters a dimethyl carbonate storage tank 8-6 through a pump 8-7 at the bottom of the dimethyl carbonate rectifying tower; the bottom temperature of the dimethyl carbonate rectifying tower system 8 is 183 ℃, and the bottom pressure is 1.33MPa; the temperature of the tower top is 147 ℃, the pressure of the tower top is 1.30MPa, and the reflux ratio is 1.2;
(9) The tower bottom liquid from the light component separation tower system 6 continuously enters an ethylene glycol rectifying tower system 9, ethylene glycol steam separated from the tower top of the ethylene glycol rectifying tower system 9 is condensed by an ethylene glycol rectifying tower condenser 9-3 and enters an ethylene glycol receiving tank 9-4, and the obtained ethylene glycol is respectively used as reflux of the ethylene glycol rectifying tower system 9 and fed into an ethylene glycol storage tank 9-6; the tower bottom liquid of the glycol rectifying tower system 9 is respectively fed into a glycol rectifying tower reboiler 9-1 through a glycol rectifying tower bottom pump 9-7 to be heated and then returned to the glycol rectifying tower system 9, and is continuously fed into the batching tank 1 as a recovered catalyst. The temperature of the top of the glycol rectifying tower system 9 is 150 ℃, and the pressure of the top of the tower is 0.02MPa; the bottom temperature was 178℃and the reflux ratio was 1.5.
Example 1
A method for producing dimethyl carbonate based on a device for preparing dimethyl carbonate by high-speed jet impact pipe type reactor comprises the following steps:
176kg/h of industrial grade ethylene carbonate (the mass content is more than 99.5%) serving as a raw material and 0.44kg/h of catalyst are fed into the batching tank 1, and the ethylene carbonate and the catalyst are uniformly mixed under the stirring effect; the mixed solution reaches the reaction temperature under the heating of the heating medium, and enters a first high-speed jet flow impact tubular reactor 2 through a first power fluid pump 1-2; the temperature in the batching tank 1 is 70 ℃, the pressure is normal pressure, the catalyst dosage is 0.25% of the mass of ethylene carbonate, and the material residence time is 0.75h;
The mixed liquid from the material mixing tank 1 in the step (2) continuously enters a first high-speed jet flow to impact the tubular reactor 2; the mixed solution of the material mixing tank 1 is pumped into two opposite first Laval nozzles 2-1 through a first power fluid pump 1-2, methanol (the mass content is more than 99.5%) steam is sucked into a steam inlet at the same time, two high-speed jet flows ejected from the Laval pipes are impacted mutually in a high-speed jet flow impact cavity, then the mixed solution enters a first tubular reactor 2-4 for transesterification, and the transesterification solution continuously enters a steam-liquid separation tank 3; the temperature in the first high-speed jet impact tubular reactor 2 is 80 ℃, the pressure is 0.2MPa, the length-diameter ratio of the first tubular reactor 2-4 is 1000, and the ethylene carbonate: methanol is 1:4.4 (molar ratio), 282kg/h of methanol;
The step (3) is that the ester exchange liquid from the first high-speed jet flow impact tubular reactor 2 continuously enters a vapor-liquid separation tank 3, the vapor-liquid separation tank 3 separates methanol vapor and dimethyl carbonate vapor generated by reaction from the ester exchange liquid, and the separated vapor enters a light component separation tower system 6; the transesterification liquid from which the light components are separated enters a second high-speed jet stream to strike the tubular reactor 4 through a second power fluid pump 3-3; the temperature in the vapor-liquid separation tank 3 is 70 ℃, the pressure is normal pressure, and the retention time of the materials is 0.75h;
The step (4) is that the transesterification liquid from which the light components are separated by the vapor-liquid separation tank 3 continuously enters a second high-speed jet flow impact tubular reactor 4; pumping the transesterification liquid after separating the gas in the gas-liquid separation tank 3 into two opposite second Laval nozzles 4-1 through a second power fluid pump 3-3, sucking methanol steam at the same time through a steam inlet, mutually impacting two high-speed jet streams ejected from the second Laval pipes 4-1 in a high-speed jet stream impacting cavity, then entering a second tubular reactor 4-4 for transesterification reaction, and continuously entering a curing tank 5 from the transesterification liquid ejected from the second high-speed jet stream impacting the tubular reactor 4; the temperature in the second high-speed jet impact tubular reactor 4 is 80 ℃, the pressure is 0.2MPa, the length-diameter ratio of the second tubular reactor 4-4 is 1000, and the ethylene carbonate: methanol is 1:4.4 (molar ratio), 282kg/h of methanol;
The step (5) is that the transesterification liquid from the second high-speed jet stream impinging on the tubular reactor 4 continuously enters the curing tank 5, and the supplementary transesterification reaction is continuously carried out in the curing tank 5; the curing liquid overflowed from the curing tank 5 enters the tower kettle of the light component separation tower system 6; the temperature in the curing tank 5 is 80 ℃, the pressure is 0.2MPa, and the retention time of the materials is 2h;
The materials from the gas-liquid separation tank 3 and the curing tank 5 in the step (6) continuously enter a light component separation tower system 6, light component vapor separated by the light component separation tower system 6 is condensed by a light component condenser 6-3 and enters a light component liquid receiving tank 6-4, part of the light component vapor is used as reflux of the light component separation tower system 6, and the rest of the light component vapor enters a methanol rectifying tower system 7; the tower bottom liquid of the light component separation tower system 6 continuously enters the glycol rectifying tower system 9 through a pump 6-6 at the bottom of the light component separation tower; the temperature of the tower bottom of the light component separation tower system 6 is 75 ℃, the temperature of the tower top is 64 ℃, the reflux ratio is 3, and the pressure is normal pressure;
Continuously introducing the azeotropic liquid from the light component separation tower system 6 into the methanol rectifying tower system 7, condensing the azeotropic mixture steam separated from the top of the methanol rectifying tower system 7 by the methanol rectifying tower condenser 7-3, introducing the azeotropic mixture steam into the methanol rectifying tower azeotropic liquid receiving tank 7-4, partially taking the azeotropic mixture as reflux of the methanol rectifying tower system 7, and partially introducing the azeotropic mixture steam into the dimethyl carbonate rectifying tower system 8; the tower bottom liquid of the methanol rectifying tower system 7 enters a methanol vaporizer 7-6 through a pump 7-7 at the bottom of the methanol rectifying tower, and vaporized methanol is continuously used for transesterification; the temperature of the bottom of the methanol rectifying tower system 7 is 70 ℃ and the pressure of the bottom is 0.13MPa; the temperature of the tower top is 64 ℃, the pressure of the tower top is normal pressure, and the reflux ratio is 2;
The azeotropic liquid from the methanol rectifying tower system 7 continuously enters the dimethyl carbonate rectifying tower system 8, azeotrope steam separated from the top of the dimethyl carbonate rectifying tower system 8 is condensed by a dimethyl carbonate rectifying tower condenser 8-3 and enters a dimethyl carbonate rectifying tower azeotropic liquid receiving tank 8-4, part of the azeotropic liquid is used as reflux of the dimethyl carbonate rectifying tower system 8, and the other part of the azeotropic liquid is used as feed and returns to the methanol rectifying tower system 7; the bottom liquid of the dimethyl carbonate rectifying tower system 8 enters a dimethyl carbonate storage tank 8-6 through a pump 8-7 at the bottom of the dimethyl carbonate rectifying tower; the bottom temperature of the dimethyl carbonate rectifying tower system 8 is 183 ℃, and the bottom pressure is 1.33MPa; the temperature of the tower top is 147 ℃, the pressure of the tower top is 1.30MPa, and the reflux ratio is 1.2; 172kg/h of dimethyl carbonate are extracted;
The tower bottom liquid from the light component separation tower system 6 in the step (9) continuously enters the glycol rectifying tower system 9, glycol steam separated from the tower top of the glycol rectifying tower system 9 is condensed by the condenser 9-3 and enters the glycol receiving tank 9-4, part of the glycol steam is used as reflux of the glycol rectifying tower system 9, and part of the glycol steam enters the glycol storage tank 9-6; the tower bottom liquid of the glycol rectifying tower system 9 enters a glycol rectifying tower reboiler 9-1 through a part of a glycol rectifying tower bottom pump 9-7 to be heated and then returns to the glycol rectifying tower system 9, and part of the tower bottom liquid is used as a recovered catalyst to continuously enter a batching tank 1; the temperature of the top of the glycol rectifying tower system 9 is 150 ℃, and the pressure of the top of the tower is 0.02MPa; the bottom temperature was 178℃and the reflux ratio was 1.5.
The yield of dimethyl carbonate in this example 1 was greater than 95%.
Example 2
The method for producing the dimethyl carbonate based on the device for preparing the dimethyl carbonate by the high-speed jet impact tubular reactor comprises the following steps of:
176kg/h of industrial grade ethylene carbonate (the mass content is more than 99.5%) serving as a raw material and 0.27kg/h of catalyst are fed into a batching tank 1, and the ethylene carbonate and the catalyst are uniformly mixed under the stirring effect; the mixed solution reaches the reaction temperature under the heating of the heating medium, and enters a first high-speed jet flow impact tubular reactor 2 through a first power fluid pump 1-2; the temperature in the batching tank 1 is 75 ℃, the pressure is normal pressure, the catalyst dosage is 0.15% of the mass of ethylene carbonate, and the material residence time is 0.5h;
The mixed liquid from the material mixing tank 1 in the step (2) continuously enters a first high-speed jet flow to impact the tubular reactor 2; the mixed solution of the material mixing tank 1 is pumped into two opposite first Laval nozzles 2-1 through a first power fluid pump 1-2, methanol (the mass content is more than 99.5%) steam is sucked at the same time, two high-speed jet flows ejected from the first Laval nozzles 2-1 are mutually impacted in an impact cavity of the high-speed jet flows, then the mixed solution enters a first tubular reactor 2-4 for transesterification, and the transesterification solution continuously enters a vapor-liquid separation tank 3; the temperature in the first high-speed jet impact tubular reactor 2 is 85 ℃, the pressure is 0.25MPa, the length-diameter ratio of the first tubular reactor 2-4 is 1000, and the ethylene carbonate: methanol is 1:4 (molar ratio), methanol 256kg/h;
The step (3) is that the ester exchange liquid from the first high-speed jet flow impact tubular reactor 2 continuously enters a vapor-liquid separation tank 3, the vapor-liquid separation tank 3 separates methanol vapor and dimethyl carbonate vapor generated by reaction from the ester exchange liquid, and the separated vapor enters a light component separation tower system 6; the transesterification liquid from which the light components are separated enters a second high-speed jet stream to strike the tubular reactor 4 through a second power fluid pump 3-3; the temperature in the vapor-liquid separation tank 3 is 75 ℃, the pressure is normal pressure, and the retention time of the materials is 0.5h;
The step (4) is that the transesterification liquid from which the light components are separated by the vapor-liquid separation tank 3 continuously enters a second high-speed jet flow impact tubular reactor 4; pumping the transesterification liquid after gas separation in the gas-liquid separation tank 3 into two opposite second Laval nozzles 4-1 through a second power fluid pump 3-3, sucking methanol vapor at the same time, mutually impacting two high-speed jet streams ejected from the second Laval nozzles 4-1 in a high-speed jet stream impacting cavity, then entering a second tubular reactor 4-4 for transesterification reaction, and continuously entering a curing tank 5 from the transesterification liquid ejected from the second high-speed jet stream impacting the tubular reactor 4; the temperature in the second high-speed jet impact tubular reactor 4 is 85 ℃, the pressure is 0.25MPa, the length-diameter ratio of the second tubular reactor 4-4 is 1000, and the ethylene carbonate: methanol is 1:4 (molar ratio), methanol 256kg/h;
The step (5) is that the transesterification liquid from the second high-speed jet stream impinging on the tubular reactor 4 continuously enters the curing tank 5, and the supplementary transesterification reaction is continuously carried out in the curing tank 5; the curing liquid overflowed from the curing tank 5 enters the tower kettle of the light component separation tower system 6; the temperature in the curing tank 5 is 85 ℃, the pressure is 0.25MPa, and the retention time of the materials is 1.5h;
The materials from the vapor-liquid separation tank 3 and the curing tank 5 in the step (6) continuously enter a light component separation tower system 6, light component vapor separated by the light component separation tower system 6 is condensed by a light component condenser 6-3 and enters a light component receiving tank 6-4, part of the light component vapor is used as reflux of the light component separation tower system 6, and the rest of the light component vapor enters a methanol rectifying tower system 7; the tower bottom liquid of the light component separation tower system 6 continuously enters the glycol rectifying tower system 9 through a pump at the bottom of the separation tower; the temperature of the tower bottom of the light component separation tower system 6 is 78 ℃, the temperature of the tower top is 66 ℃, the reflux ratio is 4, and the pressure is normal pressure;
Continuously introducing the azeotropic liquid from the light component separation tower system 6 into the methanol rectifying tower system 7, condensing the azeotropic mixture steam separated from the top of the methanol rectifying tower system 7 by the methanol rectifying tower condenser 7-3, introducing the azeotropic mixture steam into the methanol rectifying tower azeotropic liquid receiving tank 7-4, partially taking the azeotropic mixture as reflux of the methanol rectifying tower system 7, and partially introducing the azeotropic mixture steam into the dimethyl carbonate rectifying tower system 8; the tower bottom liquid of the methanol rectifying tower system 7 enters a methanol vaporizer through a pump 7-7 at the bottom of the methanol rectifying tower, and vaporized methanol is continuously used for transesterification; the temperature of the bottom of the methanol rectifying tower system 7 is 70 ℃ and the pressure of the bottom is 0.13MPa; the temperature of the tower top is 64 ℃, the pressure of the tower top is normal pressure, and the reflux ratio is 2;
The azeotropic liquid from the methanol rectifying tower system 7 continuously enters the dimethyl carbonate rectifying tower system 8, azeotrope steam separated from the top of the dimethyl carbonate rectifying tower system 8 is condensed by a dimethyl carbonate rectifying tower condenser 8-3 and enters a dimethyl carbonate rectifying tower azeotropic liquid receiving tank 8-4, part of the azeotropic liquid is used as reflux of the dimethyl carbonate rectifying tower system 8, and the other part of the azeotropic liquid is used as feed and returns to the methanol rectifying tower system 7; the bottom liquid of the dimethyl carbonate rectifying tower system 8 enters a dimethyl carbonate storage tank 8-6 through a pump 8-7 at the bottom of the dimethyl carbonate rectifying tower; the bottom temperature of the dimethyl carbonate rectifying tower system 8 is 183 ℃, and the bottom pressure is 1.33MPa; the temperature of the tower top is 147 ℃, the pressure of the tower top is 1.30MPa, and the reflux ratio is 1.2; the extraction rate of the dimethyl carbonate is 171.5kg/h;
The tower bottom liquid from the light component separation tower system 6 in the step (9) continuously enters the glycol rectifying tower system 9, glycol steam separated from the tower top of the glycol rectifying tower system 9 is condensed by the glycol rectifying tower condenser 9-3 and enters the glycol receiving tank 9-4, part of the glycol steam is used as reflux of the glycol rectifying tower system 9, and part of the glycol steam enters the glycol storage tank 9-6; the tower bottom liquid of the glycol rectifying tower system 9 enters a glycol rectifying tower reboiler 9-1 through a part of a glycol rectifying tower bottom pump 9-7 to be heated and then returns to the glycol rectifying tower system 9, and part of the tower bottom liquid is used as a recovered catalyst to continuously enter a batching tank 1; the temperature of the top of the glycol rectifying tower system 9 is 150 ℃, and the pressure of the top of the tower is 0.02MPa; the bottom temperature was 178℃and the reflux ratio was 1.5.
The yield of dimethyl carbonate in this example was greater than 95%.
The invention relates to a production method for preparing dimethyl carbonate by high-speed jet impact pipe type reactor; the quality of the dimethyl carbonate is higher than that of HG/T5391-2018 industrial grade dimethyl carbonate.
The technical scheme of the invention is explained in the technical scheme, the protection scope of the invention cannot be limited by the technical scheme, and any changes and modifications to the technical scheme according to the technical substance of the invention belong to the protection scope of the technical scheme of the invention.
Claims (8)
1. The device for preparing the dimethyl carbonate by high-speed jet impact on the tubular reactor is characterized in that: the device comprises a batching tank (1), a first high-speed jet impact tubular reactor (2), a vapor-liquid separation tank (3), a second high-speed jet impact tubular reactor (4), a curing tank (5), a light component separation tower system (6), a methanol rectifying tower system (7) and a dimethyl carbonate rectifying tower system (8) which are sequentially communicated; meanwhile, the batching tank (1) is communicated with the ethylene glycol rectifying tower system (9), the methanol rectifying tower system (7) is respectively communicated with the first high-speed jet impact tubular reactor (2) and the second high-speed jet impact tubular reactor (4), the vapor-liquid separation tank (3) is communicated with the light component separating tower system (6), and the light component separating tower system (6) is communicated with the ethylene glycol rectifying tower system (9);
the batching tank (1), the vapor-liquid separation tank (3) and the curing tank (5) are identical in structure, and are all tank structures with heating mediums arranged on the periphery and mechanical stirrers arranged inside; the liquid inlet at the top of the batching tank (1) is connected with the outlet end of a glycol rectifying tower bottom pump (9-7) of a glycol rectifying tower system (9); a liquid outlet at the bottom of the batching tank (1) is communicated with the nozzles of two first Laval nozzles (2-1) of the first high-speed jet impact tubular reactor (2) through a first power fluid pump (1-2);
The inlet end of the upper end of the vapor-liquid separation tank (3) is communicated with the outlet end of a first tubular reactor (2-4) of the first high-speed jet impact tubular reactor (2), the vapor outlet end of the upper end of the vapor-liquid separation tank (3) is communicated with the vapor inlet end of the light component separation tower system (6) through a separation tank condenser (3-2), and the outlet end of the bottom end of the vapor-liquid separation tank (3) is communicated with the pipe orifices of two second Laval nozzles (4-1) of the second high-speed jet impact tubular reactor (4) through a second power fluid pump (3-3);
The top liquid inlet of the curing tank (5) is connected with the outlet end of the second tubular reactor (4-4) of the second high-speed jet impact tubular reactor (4), and the upper overflow port of the curing tank (5) is connected with the top liquid inlet of the light component separation tower kettle (6-1) of the light component separation tower system (6);
The first high-speed jet impact tubular reactor (2) is consistent with the second high-speed jet impact tubular reactor (4) in structure, and the first high-speed jet impact tubular reactor (2) comprises a first Laval nozzle (2-1), a first mixing cavity (2-2), a first high-speed jet impact cavity (2-3), a first tubular reactor (2-4) and a first heater (2-5); the first Laval nozzles (2-1), the first mixing cavity (2-2), the first high-speed jet impact cavity (2-3) and the first tubular reactor (2-4) are all arranged inside the first heater (2-5), the two first Laval nozzles (2-1) are oppositely arranged and communicated, a cavity formed by the middle communicating part is the first mixing cavity (2-2), the first high-speed jet impact cavity (2-3) is communicated in the vertical direction of the middle part of the first mixing cavity (2-2), the first high-speed jet impact cavity (2-3) is communicated with one end of the first tubular reactor (2-4), the other end of the first tubular reactor (2-4) is communicated with a liquid inlet at the top of the vapor-liquid separation tank (3), a vapor inlet is formed at the pipe orifice of the two first Laval nozzles (2-1), and the vapor inlet is communicated with the outlet end of the methanol vaporizer (7-6) of the methanol rectifying tower system (7);
The second high-speed jet impact tubular reactor (4) comprises a second Laval nozzle (4-1), a second mixing cavity (4-2), a second high-speed jet impact cavity (4-3), a second tubular reactor (4-4) and a second heater (4-5); the second Laval nozzle (4-1), the second mixing cavity (4-2), the second high-speed jet impact cavity (4-3) and the second tubular reactor (4-4) are arranged inside the second heater (4-5), the two second Laval nozzles (4-1) are oppositely arranged and communicated, a cavity formed by the middle communicating part is the second mixing cavity (4-2), the second high-speed jet impact cavity (4-3) is communicated in the vertical direction of the middle part of the second mixing cavity (4-2), the second high-speed jet impact cavity (4-3) is communicated with one end of the second tubular reactor (4-4), and the other end of the second tubular reactor (4-4) is communicated with a liquid inlet at the top of the curing tank (5); the pipe orifices of the two second Laval nozzles (4-1) are communicated with the liquid outlet at the bottom of the vapor-liquid separation tank (3) through a second power fluid pump (3-3), the pipe orifices of the two second Laval nozzles (4-1) are provided with vapor inlets, and the vapor inlets are communicated with the outlet end of a methanol vaporizer (7-6) of the methanol rectifying tower system (7).
2. The apparatus for preparing dimethyl carbonate by high-speed jet impact tube reactor according to claim 1, wherein:
the length-diameter ratio of the first tubular reactor (2-4) is 1000, and the length-diameter ratio of the second tubular reactor (4-4) is 1000.
3. The apparatus for preparing dimethyl carbonate by high-speed jet impact tube reactor according to claim 1, wherein:
The light component separation tower system (6) comprises a light component separation tower kettle (6-1), a light component white steel structured packing tower (6-2), a light component condenser (6-3), a light component receiving tank (6-4), a light component liquid pump (6-5) and a light component separation tower bottom pump (6-6); the light component separation tower kettle (6-1) is of a structure that a heating medium is arranged on the periphery, a liquid inlet at the top of the light component separation tower kettle (6-1) is communicated with an upper overflow port of the curing tank (5), a liquid outlet at the bottom of the light component separation tower kettle (6-1) is communicated with a liquid inlet of a light component separation tower bottom pump (6-6), an outlet of the light component separation tower bottom pump (6-6) is communicated with a liquid backflow liquid inlet of the light component separation tower kettle (6-1), and an outlet end of the light component separation tower bottom pump (6-6) is connected with a liquid inlet of the ethylene glycol rectifying tower system (9); the upper end of a light component separation tower kettle (6-1) is communicated with a light component white steel structured packing tower (6-2) and is integrally arranged, the steam inlet end of the light component white steel structured packing tower (6-2) is communicated with the outlet end of a separation tank condenser (3-2), the steam outlet end of the light component white steel structured packing tower (6-2) is communicated with the inlet end of the light component condenser (6-3), the outlet end of the light component condenser (6-3) is communicated with the inlet end of a light component receiving tank (6-4), the outlet end of the light component receiving tank (6-4) is communicated with the outlet end of a light component liquid pump (6-5), the outlet end of the light component liquid pump (6-5) is communicated with the reflux inlet at the upper part of the light component white steel structured packing tower (6-2), and the outlet end of the light component liquid pump (6-5) is also communicated with the inlet of a methanol rectifying tower system (7).
4. A high velocity jet impingement tube reactor apparatus for producing dimethyl carbonate as defined in claim 3, wherein: the methanol rectifying tower system (7) comprises a methanol rectifying tower reboiler (7-1), a methanol rectifying tower white steel structured packing tower (7-2), a methanol rectifying tower condenser (7-3), a methanol rectifying tower azeotropic liquid receiving tank (7-4), a methanol rectifying tower azeotropic liquid pump (7-5), a methanol vaporizer (7-6) and a methanol rectifying tower bottom pump (7-7); the middle liquid inlet of the methanol rectifying tower system (7) is communicated with the outlet end of a light component liquid pump (6-5) of the light component separating tower system (6) and is also communicated with the outlet end of a dimethyl carbonate rectifying tower azeotropic liquid pump (8-5) of a dimethyl carbonate rectifying tower system (8); the steam outlet at the top of the methanol rectifying tower white steel structured packing tower (7-2) is communicated with the inlet end of a methanol rectifying tower condenser (7-3), the outlet end of the methanol rectifying tower condenser (7-3) is communicated with the inlet end at the top of a methanol rectifying tower azeotropic liquid receiving tank (7-4), the outlet end at the bottom of the methanol rectifying tower azeotropic liquid receiving tank (7-4) is communicated with the inlet end of a methanol rectifying tower azeotropic liquid pump (7-5), the outlet end of the methanol rectifying tower azeotropic liquid pump (7-5) is communicated with the inlet of the middle part of a methyl carbonate rectifying tower system (8), and the reflux liquid inlet at the upper part of the methanol rectifying tower white steel structured packing tower (7-2) is also communicated with the inlet of the methyl carbonate rectifying tower system (8); the bottom liquid outlet of the methanol rectifying tower white steel structured packing tower (7-2) is communicated with the inlet end of a methanol rectifying tower bottom pump (7-7), the outlet end of the methanol rectifying tower bottom pump (7-7) is communicated with the inlet end of a methanol rectifying tower reboiler (7-1), the methanol rectifying tower reboiler (7-1) is of a structure provided with a heating medium, and the outlet end of the methanol rectifying tower reboiler (7-1) is communicated with a reboiling liquid reflux port of the methanol rectifying tower white steel structured packing tower (7-2); the outlet end of the bottom pump (7-7) of the methanol rectifying tower is also communicated with the inlet end of the methanol vaporizer (7-6), the inlet end of the methanol vaporizer (7-6) is also communicated with the inlet end of fresh methanol, and the outlet end of the methanol vaporizer (7-6) is respectively communicated with the steam inlets of the first Laval nozzle (2-1) and the second Laval nozzle (4-1).
5. The apparatus for preparing dimethyl carbonate by high-speed jet impact tube reactor according to claim 4, wherein:
The dimethyl carbonate rectifying tower system (8) comprises a dimethyl carbonate rectifying tower reboiler (8-1), a dimethyl carbonate rectifying tower white steel structured packing tower (8-2), a dimethyl carbonate rectifying tower condenser (8-3), a dimethyl carbonate rectifying tower azeotropic liquid receiving tank (8-4), a dimethyl carbonate rectifying tower azeotropic liquid pump (8-5), a dimethyl carbonate storage tank (8-6) and a dimethyl carbonate rectifying tower bottom pump (8-7); the middle liquid inlet of the white steel structured packing tower (8-2) of the dimethyl carbonate rectifying tower is communicated with the outlet end of an azeotropic liquid pump (7-5) of the methanol rectifying tower; the steam outlet at the top of the dimethyl carbonate rectifying tower white steel structured packing tower (8-2) is communicated with the inlet end of a dimethyl carbonate rectifying tower condenser (8-3), the outlet end of the dimethyl carbonate rectifying tower condenser (8-3) is connected with the inlet end at the top of a dimethyl carbonate rectifying tower azeotropic liquid receiving tank (8-4), the outlet end at the bottom of the dimethyl carbonate rectifying tower azeotropic liquid receiving tank (8-4) is communicated with the inlet end of a dimethyl carbonate rectifying tower azeotropic liquid pump (8-5), the outlet end of the dimethyl carbonate rectifying tower azeotropic liquid pump (8-5) is communicated with the reflux inlet at the upper part of the dimethyl carbonate rectifying tower white steel structured packing tower (8-2), and the outlet end of the dimethyl carbonate rectifying tower azeotropic liquid pump (8-5) is also communicated with the inlet at the middle part of a methanol rectifying tower system (7); the bottom liquid outlet of the dimethyl carbonate rectifying tower white steel structured packing tower (8-2) is communicated with the inlet end of a dimethyl carbonate rectifying tower bottom pump (8-7), the outlet end of the dimethyl carbonate rectifying tower bottom pump (8-7) is communicated with the inlet end of a dimethyl carbonate rectifying tower reboiler (8-1), the dimethyl carbonate rectifying tower reboiler (8-1) is of a structure provided with heating medium, and the outlet end of the dimethyl carbonate rectifying tower reboiler (8-1) is communicated with a reboiling liquid reflux port of the dimethyl carbonate rectifying tower white steel structured packing tower (8-2); the outlet end of the bottom pump (8-7) of the dimethyl carbonate rectifying tower is also connected with the inlet end of the top of the dimethyl carbonate storage tank (8-6).
6. A high velocity jet impingement tube reactor apparatus for producing dimethyl carbonate as defined in claim 3, wherein: the ethylene glycol rectifying tower system (9) comprises an ethylene glycol rectifying tower reboiler (9-1), an ethylene glycol rectifying tower white steel structured packing tower (9-2), an ethylene glycol rectifying tower condenser (9-3), an ethylene glycol receiving tank (9-4), an ethylene glycol pump (9-5), an ethylene glycol storage tank (9-6) and an ethylene glycol rectifying tower bottom pump (9-7); the middle liquid inlet of the glycol rectifying tower system (9) is communicated with the outlet end of a light component separating tower bottom pump (6-6); the top steam outlet of the ethylene glycol rectifying tower white steel structured packing tower (9-2) is communicated with the inlet end of the ethylene glycol rectifying tower condenser (9-3), the outlet end of the ethylene glycol rectifying tower condenser (9-3) is communicated with the inlet end of the top of the ethylene glycol receiving tank (9-4), the outlet end of the bottom of the ethylene glycol receiving tank (9-4) is communicated with the inlet end of the ethylene glycol pump (9-5), the outlet end of the ethylene glycol pump (9-5) is communicated with the reflux liquid inlet at the upper part of the ethylene glycol rectifying tower white steel structured packing tower (9-2), and the outlet end of the ethylene glycol pump (9-5) is also communicated with the inlet end at the top of the ethylene glycol storage tank (9-6); the bottom liquid outlet of the ethylene glycol rectifying tower white steel structured packing tower (9-2) is communicated with the inlet end of an ethylene glycol rectifying tower bottom pump (9-7), the outlet end of the ethylene glycol rectifying tower bottom pump (9-7) is communicated with the inlet end of an ethylene glycol rectifying tower reboiler (9-1), the ethylene glycol rectifying tower reboiler (9-1) is of a structure provided with heating medium, and the outlet end of the ethylene glycol rectifying tower reboiler (9-1) is communicated with a reboiling liquid reflux port of the ethylene glycol rectifying tower white steel structured packing tower (9-2); the outlet end of the tower bottom pump (9-7) of the glycol rectifying tower is also communicated with the inlet end of the top of the material mixing tank (1).
7. A method of preparing dimethyl carbonate using a high velocity jet impingement tube reactor as defined in claim 1, wherein: the method specifically comprises the following steps:
Step 1, raw material ethylene carbonate and a catalyst enter a batching tank (1) to be stirred and mixed uniformly to obtain a mixed solution, wherein the dosage of the catalyst is 0.15-0.25% of the mass of the ethylene carbonate; the mixed solution reaches the reaction temperature under the heating of a heating medium, and continuously enters a first high-speed jet flow impact pipe type reactor (2) through a first power fluid pump (1-2);
Step 2, pumping the mixed solution of the batching tank (1) into two opposite first Laval nozzles (2-1) through a first power fluid pump (1-2), and simultaneously sucking methanol steam, wherein the molar ratio of methanol to ethylene carbonate is (4-4.4): 1, two high-speed jet flows sprayed from a first Laval nozzle (2-1), mutually impacting in a first high-speed jet flow impacting cavity (2-3), then entering a first tubular reactor (2-4) for transesterification reaction to obtain dimethyl carbonate steam and transesterification liquid, and continuously entering a vapor-liquid separation tank (3) from methanol steam and the dimethyl carbonate steam and transesterification liquid generated by the reaction;
Step 3, separating the methanol steam, the dimethyl carbonate steam generated by the reaction and the transesterification liquid in a gas-liquid separation tank (3), and enabling the separated methanol steam and the dimethyl carbonate steam generated by the reaction to enter a light component separation tower system (6); continuously feeding the transesterification liquid from which the light components are separated into a second high-speed jet impact tubular reactor (4) through a second power fluid pump (3-3);
Step 4, pumping the transesterification liquid in the vapor-liquid separation tank (3) into two opposite second Laval nozzles (4-1) through a second power fluid pump (3-3), simultaneously sucking methanol vapor, wherein the addition amount of the methanol is consistent with that in the step 2, two high-speed jet streams sprayed out of the second Laval nozzles (4-1) mutually collide in a second high-speed jet stream collision cavity (4-3), then enter a second tubular reactor (4-4) for transesterification reaction, and the methanol vapor discharged from the second high-speed jet stream collision tubular reactor (4), and dimethyl carbonate vapor generated by reaction and the transesterification liquid continuously enter a curing tank (5);
step 5, continuously carrying out supplementary transesterification reaction on the transesterification liquid in a curing tank (5); the curing liquid overflowed from the curing tank (5) enters a light component separation tower system (6);
Step 6, continuously feeding methanol steam from a gas-liquid separation tank (3) and dimethyl carbonate steam generated by reaction and curing liquid from a curing tank (5) into a light component separation tower system (6), condensing light component gas separated by the light component separation tower system (6) through a condenser (6-3) and feeding the condensed light component gas into a light component receiving tank (6-4), wherein a light component liquid part separated by the light component separation tower system (6) is used as reflux of the light component separation tower system (6), and a part of the light component gas enters a methanol rectifying tower system (7); the tower bottom liquid of the light component separation tower system (6) continuously enters the glycol rectifying tower system (9) through a pump at the bottom of the separation tower;
Step 7, continuously feeding the light component liquid from the light component separation tower system (6) and the azeotropic liquid from the dimethyl carbonate rectifying tower azeotropic liquid receiving tank 8-4 into the methanol rectifying tower system (7), condensing the azeotrope steam separated from the top of the methanol rectifying tower system (7) through the methanol rectifying tower condenser (7-3) and feeding the azeotrope steam into the azeotropic liquid receiving tank (7-4) to obtain azeotropic liquid, wherein part of the azeotropic liquid is used as reflux of the methanol rectifying tower system (7), and the part of the azeotropic liquid is fed into the dimethyl carbonate rectifying tower system (8); the tower bottom liquid of the methanol rectifying tower system (7) enters a methanol vaporizer (7-6) through a pump (7-7) at the bottom of the methanol rectifying tower, and vaporized methanol is continuously used for transesterification;
Step 8, continuously feeding the azeotropic liquid from the azeotropic liquid receiving tank (7-4) of the methanol rectifying tower system into the dimethyl carbonate rectifying tower system (8), condensing the azeotropic mixture steam separated from the top of the dimethyl carbonate rectifying tower system (8) by a dimethyl carbonate rectifying tower condenser (8-3) and feeding the azeotropic mixture steam into the azeotropic liquid receiving tank (8-4) of the dimethyl carbonate rectifying tower to obtain the azeotropic liquid, wherein part of the azeotropic liquid is used as reflux of the dimethyl carbonate rectifying tower system (8), and the other part of the azeotropic liquid is used as feed and returns to the methanol rectifying tower system (7); the tower bottom liquid of the dimethyl carbonate rectifying tower system (8) enters a dimethyl carbonate storage tank (8-6) through a pump (8-7) at the bottom of the dimethyl carbonate rectifying tower;
Step 9, continuously feeding tower bottom liquid from the light component separation tower system (6) into an ethylene glycol rectifying tower system (9), condensing ethylene glycol steam separated from the tower top of the ethylene glycol rectifying tower system (9) through an ethylene glycol rectifying tower condenser (9-3) and feeding the condensed ethylene glycol steam into an ethylene glycol receiving tank (9-4) to obtain ethylene glycol, wherein part of the ethylene glycol is used as reflux of the ethylene glycol rectifying tower system (9), and part of feed enters an ethylene glycol storage tank (9-6); the tower bottom liquid of the glycol rectifying tower system (9) enters a glycol rectifying tower reboiler (9-1) through a part of a glycol rectifying tower bottom pump (9-7) and returns to the glycol rectifying tower system (9) after being heated, and part of the tower bottom liquid is used as a recovered catalyst and continuously enters a batching tank (1).
8. The method for preparing dimethyl carbonate by high-speed jet impact pipe reactor according to claim 7, wherein:
In the step 1, the temperature in the batching tank (1) is 70-75 ℃, the pressure is normal pressure, and the retention time of the materials is 0.5-0.75 h;
In the step 2, the temperature in the first high-speed jet impact tubular reactor (2) is 80-85 ℃ and the pressure is 0.2-0.25 MPa;
In the step 3, the temperature in the vapor-liquid separation tank (3) is 70-75 ℃, the pressure is normal pressure, and the retention time of the materials is 0.5-0.75 h;
In the step 4, the temperature in the second high-speed jet impact tubular reactor (4) is 80-85 ℃ and the pressure is 0.2-0.25 MPa:
in the step 5, the temperature in the curing tank (5) is 80-85 ℃, the pressure is 0.2-0.25 MPa, and the retention time of the materials is 1.5-2 h;
in the step 6, the temperature of the tower bottom of the light component separation tower system (6) is 75-78 ℃, the temperature of the tower top is 64-66 ℃, the reflux ratio is 3-4, and the pressure is normal pressure;
in the step 7, the bottom temperature of the methanol rectifying tower system (7) is 70 ℃ and the bottom pressure is 0.13MPa; the temperature of the tower top is 64 ℃, the pressure of the tower top is normal pressure, and the reflux ratio is 2;
In the step 8, the bottom temperature of the dimethyl carbonate rectifying tower system (8) is 183 ℃, and the bottom pressure is 1.33MPa; the temperature of the tower top is 147 ℃, the pressure of the tower top is 1.30MPa, and the reflux ratio is 1.2;
in the step 9, the temperature of the top of the glycol rectifying tower system (9) is 150 ℃, and the pressure of the top of the tower is 0.02MPa; the bottom temperature was 178℃and the reflux ratio was 1.5.
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