CN114644550A - Reaction system and process for preparing acetic acid by methanol carbonylation - Google Patents
Reaction system and process for preparing acetic acid by methanol carbonylation Download PDFInfo
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- CN114644550A CN114644550A CN202011520544.2A CN202011520544A CN114644550A CN 114644550 A CN114644550 A CN 114644550A CN 202011520544 A CN202011520544 A CN 202011520544A CN 114644550 A CN114644550 A CN 114644550A
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 title claims abstract description 182
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 title claims abstract description 147
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 86
- 238000005810 carbonylation reaction Methods 0.000 title claims abstract description 34
- 230000006315 carbonylation Effects 0.000 title claims abstract description 30
- 238000004519 manufacturing process Methods 0.000 title abstract description 12
- 239000000376 reactant Substances 0.000 claims abstract description 8
- 239000007791 liquid phase Substances 0.000 claims description 33
- 238000000034 method Methods 0.000 claims description 23
- 239000012263 liquid product Substances 0.000 claims description 18
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 17
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 17
- 230000008569 process Effects 0.000 claims description 17
- 239000003054 catalyst Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 13
- 238000000926 separation method Methods 0.000 claims description 13
- 230000009471 action Effects 0.000 claims description 10
- 230000000903 blocking effect Effects 0.000 claims description 10
- 239000012071 phase Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 230000003014 reinforcing effect Effects 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 claims description 4
- 238000004891 communication Methods 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims description 2
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 claims 1
- 238000007789 sealing Methods 0.000 abstract description 12
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 239000003973 paint Substances 0.000 abstract description 2
- 230000000737 periodic effect Effects 0.000 abstract 1
- 150000001299 aldehydes Chemical class 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 229920001744 Polyaldehyde Polymers 0.000 description 3
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 3
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 239000013064 chemical raw material Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052703 rhodium Inorganic materials 0.000 description 2
- 239000010948 rhodium Substances 0.000 description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- 229920006221 acetate fiber Polymers 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000010420 art technique Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 description 1
- 229940106681 chloroacetic acid Drugs 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/10—Preparation of carboxylic acids or their salts, halides or anhydrides by reaction with carbon monoxide
- C07C51/12—Preparation of carboxylic acids or their salts, halides or anhydrides by reaction with carbon monoxide on an oxygen-containing group in organic compounds, e.g. alcohols
-
- 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
- B01D3/06—Flash distillation
-
- 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
- B01J19/0053—Details of the reactor
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a reaction system and a process for preparing acetic acid by methanol carbonylation, which comprises the following steps: a reaction vessel, a vessel shell, a vessel liner and the like. Set up reaction vessel into the structure that vessel shell and container inner bag combine, reaction vessel includes vessel shell, container inner bag and container closing cap, the container inner bag is located vessel shell, the inner wall of container inner bag replaces vessel shell and reactant contact, the container closing cap is used for sealing reaction vessel's open end, the coating has anticorrosive paint on the lateral wall of container inner bag, the setting of container inner bag can replace vessel shell and reactant contact, consequently, only need carry out periodic replacement to the container inner bag and can reach and need not to change the holistic purpose of reaction vessel, thereby effective less equipment cost.
Description
Technical Field
The invention relates to the technical field of acetic acid preparation, in particular to a reaction system and a process for preparing acetic acid by methanol carbonylation.
Background
Acetic acid is an important basic organic chemical raw material, and main raw materials such as chloroacetic acid, vinyl acetate monomers, polyvinyl alcohol, terephthalic acid, acetate fibers, metal acetate and the like are synthesized by acetic acid, so that the acetic acid has wide application in various aspects such as pesticides, medicines, dyes, adhesives, organic solvents and the like along with scientific development.
As an important chemical raw material with wide application, the synthesis method of acetic acid mainly comprises the methods of fermentation of carbohydrate, oxidation of naphtha or n-butane, oxidation of ethylene or acetaldehyde and carbonylation of methanol, wherein the methanol carbonylation method accounts for 60% of the production of acetic acid in the world at present, and the methanol carbonylation method takes methanol and carbon monoxide as raw materials and synthesizes the acetic acid through carbonylation. The low pressure method in the methanol carbonylation method is to synthesize the acetic acid by carbonylation reaction by taking rhodium as a main catalyst and iodide as a catalyst promoter under the conditions that the temperature is 150-200 ℃ and the pressure is 3-6Mpa, and a large amount of water is usually added into the system in order to avoid the precipitation of the rhodium catalyst and improve the reaction rate.
The methanol carbonylation process has inherent defects, one is that the existence of the catalyst promoter iodide can cause serious corrosion to equipment, so that the whole equipment is frequently replaced, the investment cost is high, and the other is that a large amount of water in the system causes difficult product separation, so that the product purity is low.
Disclosure of Invention
Therefore, the invention provides a reaction system and a process for preparing acetic acid by methanol carbonylation, which are used for overcoming the problems that in the prior art, the existence of a catalyst promoter iodide can cause serious corrosion to equipment, and simultaneously, a large amount of water in a system for preparing acetic acid by a methanol carbonylation method causes difficult product separation and low product purity.
The invention provides a reaction system for preparing acetic acid by methanol carbonylation, which comprises:
the reactor comprises a reactor shell, a reactor liner and a reactor closing cover, wherein the reactor shell is arranged in the reactor shell, the inner wall of the reactor liner replaces the reactor shell to contact with reactants, and the reactor closing cover is used for closing the opening end of the reactor;
the bottom wall of the container liner is in a convex shape along the vertical upward direction, a reserved cavity is formed between the bottom wall of the container liner and the bottom wall of the container shell, and a fixing component for fixing the container liner is arranged in the reserved cavity;
the flash tank is communicated with the reaction container and is used for carrying out flash separation on products in the reaction container;
a cooler in communication with said reaction vessel and said flash tank for condensing gas discharged from the top of said reaction vessel and gas discharged from said flash tank;
and the evaporator is communicated with the flash tank and the cooler and is used for purifying the liquid product discharged by the flash tank and the liquid product discharged by the cooler.
Preferably, fixed subassembly includes the compensating plate, the both sides wall of symmetry is cambered surface lateral wall and plane lateral wall respectively on the compensating plate, the cambered surface lateral wall of compensating plate with the diapire fixed connection of container inner bag, on the plane lateral wall of compensating plate with first spread groove and the second spread groove that equal fixedly connected with used of mutually supporting on the diapire in the container casing, the one end of fixed connection spring in the second spread groove, the other end of spring with first spread groove joint.
Preferably, the lower end of the container closing cover is fixedly connected with an annular clamping groove used for fixing the container inner container.
Preferably, an annular compensation strip equal to the height difference between the container inner container and the container outer shell is arranged in the annular clamping groove.
Preferably, a locking assembly for fixing the container closing cover is arranged on the side wall of the annular clamping groove.
Preferably, the locking assembly comprises connecting blocks which are symmetrically arranged, a locking plate is rotatably connected to the connecting blocks, locking holes are formed in the locking plate and the side wall of the reaction container, and a locking bolt penetrates through the locking plate.
Preferably, the inside of the container closing cover is of a cavity structure, and a reinforcing rib is arranged inside the container closing cover.
Preferably, the material conveying pipe and the gas discharge pipe are both arranged on the container closing cover.
Preferably, the main part of evaporimeter is square jar of body, the inside of evaporimeter evenly is provided with the choked flow board group, the choked flow board group comprises two inclined panel that set up in vertical direction, the inclined panel is square panel, the one end of inclined panel with the inside wall fixed connection of evaporimeter, the free end of inclined panel is located the upside of stiff end.
The invention provides a reaction process for preparing acetic acid by methanol carbonylation, which comprises the following steps:
step 1: catalyst solution is conveyed into the reaction container through a material conveying pipe arranged on the container closing cover, gaseous carbon monoxide and gaseous methanol are conveyed into the reaction container through the material conveying pipe arranged on the container closing cover, the carbon monoxide and the gaseous methanol are subjected to methanol carbonylation reaction under the action of a catalyst to synthesize acetic acid and multi-element aldehyde, and the container inner container in the reaction container is periodically replaced;
step 2: liquid products in the reaction container enter the flash tank under the action of pump force, gas in the reaction container is discharged into the cooler along the top, after the liquid products in the flash tank are flashed, a gas phase part comprising a small amount of acetic acid, water, a small amount of catalyst components and polyaldehyde is discharged into the cooler from the top of the flash tank, a liquid phase part enters the evaporator to be purified by the acetic acid, after the gas in the cooler is cooled, condensable liquid flows to the evaporator, non-condensable gas is discharged to an external absorption process, and the flash tank and the cooler finish primary separation of the products;
and step 3: the liquid phase part from the flash tank and the cooler enters from the upper part of the evaporator, the liquid phase part is uniformly provided with a flow blocking plate group along the inside of the evaporator and flows from top to bottom, the internal temperature of the evaporator is controlled at 105 ℃, the water and the multi-element aldehyde part in the liquid phase part are gradually evaporated to be in a gas phase and are discharged to an external collecting tank along the top of the evaporator, and the residual liquid phase part is acetic acid and is discharged along the bottom of the evaporator.
Compared with the prior art, the reaction container has the beneficial effects that the reaction container is arranged into a structure combining the container shell and the container liner, the reaction container comprises the container shell, the container liner and the container closing cover, the container liner is positioned in the container shell, the inner wall of the container liner replaces the container shell to be in contact with a reactant, the container closing cover is used for closing the opening end of the reaction container, the anticorrosive coating is coated on the side wall of the container liner, the container liner can replace the container shell to be in contact with the reactant, and therefore the purpose of not replacing the whole reaction container can be achieved only by replacing the container liner regularly, so that the equipment cost is effectively reduced;
the bottom wall of the container liner is convex in the vertical upward direction, a reserved cavity is formed between the bottom wall of the container liner and the bottom wall of the container shell, a fixing component for fixing the container liner is arranged in the reserved cavity, and the reserved cavity is used for providing an installation space for the fixing component, so that the fixing component can stably fix the container liner in the container shell, and the aim of easy replacement is fulfilled;
the flash tank is communicated with the reaction container and is used for carrying out flash separation on products in the reaction container, and liquid products in the reaction container enter the flash tank under the action of pump force to carry out gas-liquid flash separation;
the cooler is communicated with the reaction container and the flash tank and is used for condensing gas discharged from the top of the reaction container and gas discharged from the flash tank, after liquid products in the flash tank are flashed, a gas phase part comprises a small amount of acetic acid, water, a small amount of catalyst components and multi-aldehyde and is discharged into the cooler from the top of the flash tank, after the gas in the cooler 7 is cooled, condensable liquid flows to the evaporator, non-condensable gas is discharged to an external absorption process, and the flash tank and the cooler finish primary separation of the products;
the evaporator is communicated with the flash tank and the cooler and used for purifying the liquid product discharged from the flash tank and the liquid product discharged from the cooler, the liquid phase parts of the flash tank and the cooler enter the evaporator to be purified by acetic acid, the liquid phase parts uniformly are provided with the flow blocking plate groups along the inside of the evaporator and flow from top to bottom, the internal temperature control of the evaporator is controlled at 100-105 ℃, the water and the multi-element aldehyde parts in the liquid phase parts are gradually evaporated to be gas phase and are discharged to the external collecting tank along the top of the evaporator, and the residual liquid phase parts are acetic acid and are discharged along the bottom of the evaporator.
Furthermore, the fixing component comprises a compensating plate, two symmetrical side walls on the compensating plate are respectively an arc side wall and a plane side wall, the arc side wall of the compensating plate is fixedly connected with the bottom wall of the container liner, the plane side wall of the compensating plate and the bottom wall of the container shell are fixedly connected with a first connecting groove and a second connecting groove which are matched with each other for use, one end of a spring is fixedly connected in the second connecting groove, the other end of the spring is clamped with the first connecting groove, the compensating plate is arranged for compensating the arc bottom wall of the container liner, so that a flat connecting plane is formed, the connection of the first connecting groove is convenient, when the container liner is positioned in the container shell, the spring has certain vertical upward acting force on the container liner, the container liner is clamped between the container closing cover and the fixing component, and therefore, the container liner is in a fixed state in the container shell under the condition that the container closing cover is kept in a closed state, when the container inner container needs to be replaced, the container inner container is taken out only by opening the container closing cover, and the fixing assembly realizes that the container inner container is stably fixed in the container shell, and meanwhile, the purpose of easy replacement is achieved.
Furthermore, the lower end of the container sealing cover is fixedly connected with an annular clamping groove used for fixing the container liner, when the container sealing cover is in a closed state, the upper ends of the container shell and the container liner are both located in the annular clamping groove, and therefore the annular clamping groove plays a role in fixing the upper end of the container liner.
Furthermore, an annular compensation strip which is equal to the height difference value between the container inner container and the container outer shell is arranged in the annular clamping groove. The height of container inner bag is less than container shell's height, and the setting of annular compensation strip is used for compensating the difference in height between the two, further carries out the omnidirectional to container inner bag 3's upper end and fixes.
Furthermore, the side wall of the ring-shaped clamping groove is provided with a locking assembly for fixing the container closing cover, and the container closing cover is locked at the opening at the upper end of the reaction container by the locking assembly, so that the reaction container is closed.
Further, the lock catch assembly comprises connecting blocks which are symmetrically arranged, a locking plate is rotatably connected to the connecting blocks, locking holes are formed in the locking plate and the side wall of the reaction container, a lock bolt penetrates through the locking plate, the locking plate can rotate under the action of external force, the lock bolt is fixed in the locking plate and the locking holes formed in the side wall of the reaction container, so that the locking plate is fixed, the container sealing cover is locked at the opening at the upper end of the reaction container, and the reaction container is sealed.
Furthermore, the inside of the container closing cover is of a cavity structure, reinforcing ribs are arranged inside the container closing cover, the weight of the container closing cover is reduced to a certain extent due to the cavity structure inside the container closing cover, the container liner inside the container closing cover is further convenient to replace, and the reinforcing ribs are arranged to strengthen the strength of the container closing cover.
Furthermore, the main body part of the evaporator is a square tank body, a flow blocking plate group is uniformly arranged in the evaporator, the flow blocking plate group is composed of two inclined panels arranged in the vertical direction, each inclined panel is a square panel, one end of each inclined panel is fixedly connected with the inner side wall of the evaporator, the free end of each inclined panel is located on the upper side of the fixed end, the flow blocking plate group is uniformly arranged in the liquid phase part along the evaporator from top to bottom, the liquid phase part flows along the inclined panels layer by layer, and the free end of each inclined panel is located on the upper side of the fixed end, so that the liquid phase part needs to flow from bottom to top under the subsequent fluid accumulation effect when passing through each inclined panel, the circulation time of the liquid phase part in the evaporator is effectively prolonged, the water and the multi-element aldehyde part in the liquid phase part are completely evaporated, and the purity of acetic acid is improved.
Drawings
FIG. 1 is a schematic diagram of the configuration of a reaction system for the carbonylation of methanol to produce acetic acid in accordance with the present invention;
FIG. 2 is an enlarged view taken at A in FIG. 1 according to the present invention;
FIG. 3 is an enlarged view of the invention at B of FIG. 1;
fig. 4 is a top cross-sectional view of an evaporator and an inclined panel of the present invention.
In the figure: 1-reaction vessel, 2-vessel shell, 3-vessel liner, 4-vessel closing cap, 5-fixed component, 501-compensation plate, 502-first connecting groove, 503-second connecting groove, 504-spring, 6-flash tank, 7-cooler, 8-evaporator, 9-ring clamping groove, 10-ring compensation strip, 11-locking component, 111-connecting block, 112-locking plate, 113-locking bolt, 12-reinforcing rib, 13-inclined panel and 14-reserved cavity.
Detailed Description
Preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only for explaining the technical principle of the present invention, and do not limit the scope of the present invention.
Referring to fig. 1, which is a schematic structural diagram of a reaction system for preparing acetic acid by methanol carbonylation according to the present invention, a reaction system for preparing acetic acid by methanol carbonylation includes:
the reactor comprises a reaction vessel 1, a vessel liner 3 and a vessel closing cover 4, wherein the vessel liner 3 is positioned in the vessel shell 2, the inner wall of the vessel liner 3 replaces the vessel shell 2 to be in contact with reactants, the vessel closing cover 4 is used for closing the opening end of the reaction vessel 1, the side wall of the vessel liner 3 is coated with anticorrosive paint, and the vessel liner 3 can replace the vessel shell 2 to be in contact with the reactants, so that the whole reaction vessel can be replaced only by replacing the vessel liner 3 regularly, and the equipment cost is effectively reduced;
the bottom wall of the container liner 3 is convex in the vertical upward direction, a reserved cavity 14 is formed between the bottom wall of the container liner 3 and the bottom wall of the container shell 2, a fixing component 5 for fixing the container liner 3 is arranged in the reserved cavity 14, and the reserved cavity 14 is used for providing an installation space for the fixing component 5, so that the fixing component 5 can firmly fix the container liner 3 in the container shell 2, and the aim of easy replacement is fulfilled;
the flash tank 6 is communicated with the reaction container 1 and is used for carrying out flash separation on products in the reaction container 1, and liquid products in the reaction container 1 enter the flash tank 6 under the action of pump force to carry out gas-liquid flash separation;
a cooler 7, which is communicated with the reaction vessel 1 and the flash tank 6, and is used for condensing the gas discharged from the top of the reaction vessel 1 and the gas discharged from the flash tank 6, after the liquid product in the flash tank 6 is flashed, a gas phase part comprising a small amount of acetic acid, water, a small amount of catalyst components and polyaldehydes is discharged from the top of the flash tank 6 to the cooler 7, after the gas in the cooler 7 is cooled, a condensable liquid flows to the evaporator 8, and a non-condensable gas is discharged to an external absorption process, and the flash tank 6 and the cooler 7 complete the primary separation of the product;
and the evaporator 8 is communicated with the flash tank 6 and the cooler 7 and is used for purifying the liquid product discharged from the flash tank 6 and the liquid product discharged from the cooler 7, liquid phase parts of the flash tank 6 and the cooler 7 enter the evaporator 8 to be purified by acetic acid, flow blocking plate groups are uniformly arranged in the liquid phase part along the inside of the evaporator 8 from top to bottom, the temperature control in the evaporator 8 is controlled at 100-105 ℃, water and multi-element aldehyde parts in the liquid phase part are gradually evaporated to be in a gas phase and are discharged to an external collecting tank along the top of the evaporator 8, and the residual liquid phase part is acetic acid and is discharged along the bottom of the evaporator 8.
Referring to fig. 3, specifically, the fixing assembly 5 includes a compensating plate 501, two symmetrical sidewalls of the compensating plate 501 are an arc sidewall and a planar sidewall, the arc sidewall of the compensating plate 501 is fixedly connected to the bottom wall of the container liner 3, the planar sidewall of the compensating plate 501 and the inner bottom wall of the container casing 2 are both fixedly connected to a first connecting groove 502 and a second connecting groove 503 that are used in cooperation with each other, one end of a spring 504 is fixedly connected to the second connecting groove 503, the other end of the spring 504 is clamped to the first connecting groove 502, the compensating plate 501 is configured to compensate the arc bottom wall of the container liner 3, so as to form a straight connecting plane, which facilitates connection of the first connecting groove 502, when the container liner 3 is located inside the container casing 2, the spring 504 has a certain vertically upward acting force on the container liner, the container liner 3 is clamped between the container closing cover 4 and the fixing component 5, so that the container liner 3 is in a fixed state in the container shell 2 under the condition that the container closing cover 4 keeps a closed state, when the container liner 3 needs to be replaced, the container closing cover 4 is only required to be opened, the container liner 3 is taken out, and the fixing component 5 realizes that the container liner 3 is stably fixed in the container shell 2 and simultaneously achieves the purpose of easy replacement.
Referring to fig. 2, specifically, a ring-shaped clamping groove 9 for fixing the container liner 3 is fixedly connected to a lower end of the container sealing cover 4, and when the container sealing cover 4 is in a closed state, upper ends of the container outer shell 2 and the container liner 3 are both located in the ring-shaped clamping groove 9, so that the ring-shaped clamping groove 9 fixes an upper end of the container liner 3.
Referring to fig. 2, specifically, an annular compensating strip 10 equal to the height difference between the container inner container 3 and the container outer shell 2 is disposed inside the annular clamping groove 9. The height of the container inner container 3 is smaller than that of the container outer shell 2, the annular compensation strip 10 is arranged to compensate for the height difference between the two, and the upper end of the container inner container 3 is further fixed in an all-around mode.
Referring to fig. 2, specifically, a locking assembly 11 for fixing the vessel closing cap 4 is disposed on a side wall of the ring-shaped clamping groove 9, and the vessel closing cap 4 is locked at an upper end opening of the reaction vessel 1 by the locking assembly 11, so as to seal the reaction vessel 1.
Referring to fig. 2, specifically, the locking assembly 11 includes connecting blocks 111 that are symmetrically arranged, a locking plate 112 is rotatably connected to the connecting blocks 111, locking holes are formed in the locking plate 112 and the side wall of the reaction vessel 1, a locking bolt 113 penetrates through the locking plate 112, the locking plate 112 can rotate under the action of an external force, and the locking bolt 113 is fixed to the locking plate 112 and the locking holes formed in the side wall of the reaction vessel 1, so as to fix the locking plate 112, so that the vessel sealing cover 4 is locked at the opening at the upper end of the reaction vessel 1, and the reaction vessel 1 is sealed.
Referring to fig. 2, specifically, the inside of the container sealing cover 4 is of a cavity structure, a reinforcing rib 12 is arranged inside the container sealing cover 4, the weight of the container sealing cover 4 is reduced to a certain extent due to the cavity structure inside the container sealing cover 4, the replacement of the container liner 3 inside is further facilitated, and the reinforcing rib 12 is arranged to reinforce the strength of the container sealing cover 4.
Referring to fig. 1, in particular, a material delivery pipe and a gas discharge pipe are provided on the container closure 4.
Referring to fig. 1 and 4, specifically, the main portion of the evaporator 8 is a square tank, a choke plate group is uniformly arranged inside the evaporator 8, the choke plate group is composed of two inclined panels 13 arranged in the vertical direction, the inclined panels 13 are square panels, one end of each inclined panel 13 is fixedly connected to the inner side wall of the evaporator 8, the free end of each inclined panel 13 is located above the fixed end, the liquid phase portion uniformly provided with the choke plate group along the inside of the evaporator 8 flows from top to bottom, the liquid phase portion flows along the inclined panels 13 layer by layer, because the free end of each inclined panel 13 is located above the fixed end, the liquid phase portion needs to flow from bottom to top under the subsequent fluid accumulation effect when passing through one inclined panel 13, and the flow time of the liquid phase portion in the evaporator 8 is effectively increased, ensure that the water and the polyaldehyde in the liquid phase part are completely evaporated, and improve the purity of the acetic acid.
Referring to fig. 1, a process for preparing acetic acid by carbonylation of methanol includes the following steps:
step 1: catalyst solution is conveyed into the reaction vessel 1 through a material conveying pipe arranged on the vessel closing cover 4, then gaseous carbon monoxide and gaseous methanol are conveyed into the reaction vessel 1 through the material conveying pipe arranged on the vessel closing cover 4, the carbon monoxide and the gaseous methanol are subjected to methanol carbonylation reaction under the action of a catalyst to synthesize acetic acid and multi-aldehyde, and the vessel inner container 3 in the reaction vessel 1 is periodically replaced;
step 2: the liquid product in the reaction container 1 enters the flash tank 6 under the action of pump force, the gas in the reaction container 1 is discharged into the cooler 7 along the top, after the liquid product in the flash tank 6 is flashed, a gas phase part comprising a small amount of acetic acid, water, a small amount of catalyst components and multi-aldehyde is discharged into the cooler 7 from the top of the flash tank, a liquid phase part enters the evaporator 8 for acetic acid purification treatment, after the gas in the cooler 7 is cooled, a condensable liquid flows to the evaporator 8, a non-condensable gas is discharged to an external absorption process, and the flash tank 6 and the cooler 7 finish primary separation of the product;
and 3, step 3: the liquid phase part from the flash tank 6 and the cooler 7 enters from the upper part of the evaporator 8, the liquid phase part is uniformly provided with a flow blocking plate group along the inside of the evaporator 8 and flows from top to bottom, the temperature control inside the evaporator 8 is controlled at 100 ℃ and 105 ℃, the water and the multi-aldehyde part in the liquid phase part are gradually evaporated to be gas phase and are discharged to an external collecting tank along the top of the evaporator 8, and the residual liquid phase part is acetic acid and is discharged along the bottom of the evaporator 8.
In order that the objects and advantages of the invention will be more clearly understood, the invention is further described below with reference to examples; it should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
Acetic acid production is carried out using the above system and process, wherein:
the inlet air temperature of the methanol and the carbon monoxide is 160 ℃, the inlet air pressure is 3.5Mpa, the temperature in the reactor is 170 ℃, the pressure is 3.8Mpa, and the ratio of the inlet air quantity of the methanol and the carbon monoxide is 1: 1.
The temperature in the evaporator was 102 ℃.
After the system and the process are used, the purity of the prepared acetic acid is detected to be 94%.
Example 2
Acetic acid production is carried out using the above system and process, wherein:
the inlet air temperature of the methanol and the carbon monoxide is 160 ℃, the inlet air pressure is 3.5Mpa, the temperature in the reactor is 170 ℃, the pressure is 3.8Mpa, and the ratio of the inlet air quantity of the methanol and the carbon monoxide is 1: 1.
The temperature in the evaporator was 104 ℃.
After the system and the process are used, the purity of the prepared acetic acid is detected to be 94%.
Example 3
Acetic acid production is carried out using the above system and process, wherein:
the inlet air temperature of the methanol and the carbon monoxide is 160 ℃, the inlet air pressure is 3.5Mpa, the temperature in the reactor is 170 ℃, the pressure is 3.8Mpa, and the ratio of the inlet air quantity of the methanol and the carbon monoxide is 1: 1.
The temperature in the evaporator was 100 ℃.
After the system and the process are used, the purity of the prepared acetic acid is 93 percent through detection.
Example 4
Acetic acid production is carried out using the above system and process, wherein:
the inlet air temperature of the methanol and the carbon monoxide is 160 ℃, the inlet air pressure is 3.5Mpa, the temperature in the reactor is 170 ℃, the pressure is 3.8Mpa, and the ratio of the inlet air quantity of the methanol and the carbon monoxide is 1: 1.
The temperature in the evaporator was 101 ℃.
After the system and the process are used, the purity of the prepared acetic acid is 93 percent through detection.
Example 5
Acetic acid production is performed using the above system and process, wherein:
the inlet air temperature of the methanol and the carbon monoxide is 160 ℃, the inlet air pressure is 3.5Mpa, the temperature in the reactor is 170 ℃, the pressure is 3.8Mpa, and the ratio of the inlet air quantity of the methanol and the carbon monoxide is 1: 1.
The temperature in the evaporator was 105 ℃.
After the system and the process are used, the purity of the prepared acetic acid is 95 percent through detection.
Comparative example
The carbonylation of methanol to produce acetic acid was carried out using the prior art technique, wherein the process parameters were selected to be the same as those in the above examples (excluding the evaporator section).
The purity of the finally prepared acetic acid is 83 percent through detection.
So far, the technical solutions of the present invention have been described in connection with the preferred embodiments shown in the drawings, but it is easily understood by those skilled in the art that the scope of the present invention is obviously not limited to these specific embodiments. Equivalent changes or substitutions of related technical features can be made by those skilled in the art without departing from the principle of the invention, and the technical scheme after the changes or substitutions can fall into the protection scope of the invention.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention; various modifications and alterations to this invention will become apparent to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A reaction system for the carbonylation of methanol to produce acetic acid comprising:
the reactor comprises a reaction vessel (1) for providing a reaction site for the carbonylation of methanol, wherein the reaction vessel (1) comprises a vessel outer shell (2), a vessel inner container (3) and a vessel closing cap (4), the vessel inner container (3) is positioned in the vessel outer shell (2), the inner wall of the vessel inner container (3) replaces the vessel outer shell (2) to be in contact with reactants, and the vessel closing cap (4) is used for closing the opening end of the reaction vessel (1);
the bottom wall of the container inner container (3) is in a convex shape along the vertical upward direction, a reserved cavity (14) is formed between the bottom wall of the container inner container (3) and the bottom wall of the container shell (2), and a fixing component (5) for fixing the container inner container (3) is arranged in the reserved cavity (14);
a flash tank (6) which is communicated with the reaction vessel (1) and is used for carrying out flash separation on products in the reaction vessel (1);
a cooler (7) in communication with said reaction vessel (1) and said flash tank (6) for condensing gas exiting the top of said reaction vessel (1) and gas exiting said flash tank (6);
an evaporator (8) in communication with the flash tank (6) and the cooler (7) for purifying the liquid product discharged from the flash tank (6) and the liquid product discharged from the cooler (7).
2. The reaction system for preparing acetic acid through methanol carbonylation according to claim 1, wherein the fixing component (5) comprises a compensation plate (501), the two symmetrical side walls of the compensation plate (501) are respectively an arc side wall and a plane side wall, the arc side wall of the compensation plate (501) is fixedly connected with the bottom wall of the container liner (3), the plane side wall of the compensation plate (501) and the inner bottom wall of the container shell (2) are fixedly connected with a first connecting groove (502) and a second connecting groove (503) which are mutually matched, the second connecting groove (503) is fixedly connected with one end of a spring (504), and the other end of the spring (504) is clamped with the first connecting groove (502).
3. The reaction system for preparing acetic acid by carbonylation of methanol according to claim 2, wherein the lower end of the container closing cap (4) is fixedly connected with a ring-shaped clamping groove (9) for fixing the container inner container (3).
4. A reaction system for preparing acetic acid through methanol carbonylation according to claim 3, wherein the inside of the ring-shaped clamping groove (9) is provided with a ring-shaped compensation strip (10) which is equal to the height difference between the container inner container (3) and the container outer shell (2).
5. A reaction system for the carbonylation of methanol to produce acetic acid as claimed in claim 3 wherein the side wall of the ring groove (9) is provided with a locking assembly (11) for securing the closure (4) to the vessel.
6. The reaction system for preparing acetic acid through methanol carbonylation according to claim 5, wherein the locking assembly (11) comprises symmetrically arranged connecting blocks (111), a locking plate (112) is rotatably connected to the connecting blocks (111), locking holes are formed in the locking plate (112) and the side wall of the reaction vessel (1), and a locking bolt (113) penetrates through the locking plate (112).
7. A reaction system for preparing acetic acid by carbonylation of methanol according to any one of claims 1-6, wherein the inside of the container closure (4) has a cavity structure, and the inside of the container closure (4) is provided with a reinforcing rib (12).
8. A reaction system for the carbonylation of methanol to produce acetic acid according to claim 7 wherein the feed line and the gas withdrawal line are both located in the closure (4) of the vessel.
9. The reaction system for preparing acetic acid through carbonylation of methanol according to claim 2, wherein the main body of the evaporator (8) is a square tank, the inside of the evaporator (8) is uniformly provided with a flow blocking plate group, the flow blocking plate group is composed of two inclined panels (13) arranged in the vertical direction, the inclined panels (13) are square panels, one end of each inclined panel (13) is fixedly connected with the inner side wall of the evaporator (8), and the free end of each inclined panel (13) is positioned at the upper side of the fixed end.
10. A reaction process for preparing acetic acid by methanol carbonylation is characterized by comprising the following steps:
step 1: catalyst solution is conveyed into the reaction container (1) through a material conveying pipe arranged on the container closing cover (4), then gaseous carbon monoxide and gaseous methanol are conveyed into the reaction container (1) through the material conveying pipe arranged on the container closing cover (4), the carbon monoxide and the gaseous methanol are subjected to methanol carbonylation reaction under the action of a catalyst to synthesize acetic acid and multi-element aldehyde, and the container inner container (3) in the reaction container (1) is periodically replaced;
step 2: the liquid product in the reaction container (1) enters the flash tank (6) under the action of pump force, the gas in the reaction container (1) is discharged into the cooler (7) along the top, after the liquid product in the flash tank (6) is flashed, a gas phase part comprising a small amount of acetic acid, water, a small amount of catalyst components and multi-aldehyde is discharged into the cooler (7) from the top of the flash tank, a liquid phase part enters the evaporator (8) for acetic acid purification treatment, after the gas in the cooler (7) is cooled, a condensable liquid flows to the evaporator (8), a non-condensable gas is discharged to an external absorption process, and the flash tank (6) and the cooler (7) finish primary separation of the product;
and 3, step 3: the liquid phase part from the flash tank (6) and the cooler (7) enters from the upper part of the evaporator (8), the liquid phase part is uniformly provided with a flow blocking plate group along the inside of the evaporator (8) and flows from top to bottom, the internal temperature of the evaporator (8) is controlled at 100 ℃ and 105 ℃, the water and the multi-aldehyde part in the liquid phase part are gradually evaporated to be in a gas phase and are discharged to an external collecting tank along the top of the evaporator (8), and the residual liquid phase part is acetic acid and is discharged along the bottom of the evaporator (8).
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