CN111943141A - Hydrochloric acid analysis device with negative pressure dehydration function and analysis process - Google Patents
Hydrochloric acid analysis device with negative pressure dehydration function and analysis process Download PDFInfo
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- CN111943141A CN111943141A CN202010909509.3A CN202010909509A CN111943141A CN 111943141 A CN111943141 A CN 111943141A CN 202010909509 A CN202010909509 A CN 202010909509A CN 111943141 A CN111943141 A CN 111943141A
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 262
- 230000018044 dehydration Effects 0.000 title claims abstract description 174
- 238000006297 dehydration reaction Methods 0.000 title claims abstract description 174
- 238000000034 method Methods 0.000 title claims abstract description 64
- 238000003795 desorption Methods 0.000 claims abstract description 164
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 85
- 239000002253 acid Substances 0.000 claims abstract description 73
- 239000007853 buffer solution Substances 0.000 claims abstract description 41
- 239000007789 gas Substances 0.000 claims description 54
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 36
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 36
- 239000000872 buffer Substances 0.000 claims description 34
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 25
- 239000002918 waste heat Substances 0.000 claims description 22
- 239000000835 fiber Substances 0.000 claims description 20
- 238000012546 transfer Methods 0.000 claims description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 17
- 229910000831 Steel Inorganic materials 0.000 claims description 17
- 239000002131 composite material Substances 0.000 claims description 17
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- 210000003298 dental enamel Anatomy 0.000 claims description 9
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- 229920000049 Carbon (fiber) Polymers 0.000 claims description 6
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- 229920002748 Basalt fiber Polymers 0.000 claims description 5
- UMVBXBACMIOFDO-UHFFFAOYSA-N [N].[Si] Chemical compound [N].[Si] UMVBXBACMIOFDO-UHFFFAOYSA-N 0.000 claims description 5
- 229920006231 aramid fiber Polymers 0.000 claims description 5
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 229920000570 polyether Polymers 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 3
- 239000005416 organic matter Substances 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- 229920006122 polyamide resin Polymers 0.000 claims description 3
- 229920001721 polyimide Polymers 0.000 claims description 3
- 239000009719 polyimide resin Substances 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 3
- 238000007751 thermal spraying Methods 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims 6
- 239000012535 impurity Substances 0.000 abstract description 9
- 238000013461 design Methods 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000000945 filler Substances 0.000 description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 18
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 12
- 239000001110 calcium chloride Substances 0.000 description 12
- 229910001628 calcium chloride Inorganic materials 0.000 description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 10
- 230000000694 effects Effects 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 6
- 238000009833 condensation Methods 0.000 description 6
- 230000005494 condensation Effects 0.000 description 6
- 239000012071 phase Substances 0.000 description 5
- 238000010992 reflux Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 2
- 239000004760 aramid Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000000895 extractive distillation Methods 0.000 description 2
- 239000007849 furan resin Substances 0.000 description 2
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- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000003044 adaptive effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
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- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
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- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
- C01B7/0712—Purification ; Separation of hydrogen chloride by distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Drying Of Gases (AREA)
Abstract
The invention provides a hydrochloric acid analysis device with a negative pressure dehydration function and an analysis process, and the hydrochloric acid analysis device comprises an analysis device and a negative pressure dehydration device, wherein the analysis device comprises an analysis tower, a three-stage preheater, an analysis tower condenser, a demister, an analysis tower reboiling device and an analysis tower dilute acid buffer tank; the negative pressure dehydration device is communicated with the dilute acid buffer tank of the desorption tower through a pipeline and comprises a negative pressure dehydration tower, a dilute acid buffer tank of the dehydration tower, a condenser of the dehydration tower, a vacuum unit, a dilute acid water tank and a dehydration reboiling device. According to the hydrochloric acid analysis device with the negative pressure dehydration function and the analysis process, the negative pressure dehydration process and the hydrochloric acid analysis process are combined, so that the equipment investment and the operation cost can be greatly reduced compared with the traditional split process design, meanwhile, the energy utilization rate can be improved through reasonable design, the hydrochloric acid analysis process is not influenced by impurities in the raw material hydrochloric acid to be treated, and the comprehensive energy consumption is saved by 15-50% compared with the existing split design.
Description
Technical Field
The invention relates to the technical field of hydrochloric acid analysis, in particular to a hydrochloric acid analysis device with a negative pressure dehydration function and an analysis process.
Background
In industrial production, concentrated hydrochloric acid is often required to be resolved to produce HCL gas, and then the resolved diluted hydrochloric acid is returned to the production process to absorb HCL to generate concentrated hydrochloric acid so as to maintain the production balance of a factory, and when the balance does not contain other impurities (including organic matters, metal ions, water and the like), the material balance of a production system can be maintained through conventional resolution. However, in the actual plant production, when hydrochloric acid after being used and analyzed is returned to the production process to absorb tail gas containing HCL, the tail gas often contains water and is absorbed together during absorption, and at this time, redundant water needs to be removed synchronously.
Dilute hydrochloric acid may also be used directly in some manufacturing processes as a solvent or feedstock, where acidic waste water containing numerous impurities may be produced, and excess water may be removed to maintain manufacturing balance.
The conventional hydrochloric acid can only resolve part of HCL in the concentrated hydrochloric acid by normal resolution, and meanwhile, the azeotropic acid is a byproduct. The removal of the excess water in hydrochloric acid in industrial production requires deep analysis, which is generally divided into an extractive distillation method and a pressure difference method. The extractive distillation methods are divided into calcium chloride and sulfuric acid methods. Because the sulfuric acid has strong corrosivity and great difficulty in transportation, storage and operation, the sulfuric acid method has few application examples; calcium chloride is low in price and easy to obtain, so that the calcium chloride is relatively common in application, the calcium chloride is easy to crystallize due to too high concentration control, pipelines can be blocked in actual production due to improper operation, and if impurities (such as sulfate radicals, silicon dioxide and the like) are contained in hydrochloric acid, precipitates or deterioration can be generated, so that the calcium chloride is frequently replaced or supplemented after being recycled for a certain time, and waste is generated; the application case of the differential pressure method is general, although the analysis effect is good, the energy consumption is high, the investment is large, and the material balance control requirement of the device operation is high.
At present, an industrial device is generally independently arranged for normal analysis and deep analysis, the amount of the normal analysis of certain hydrochloric acid is large, and a factory with small removal amount of redundant water can increase investment, improve maintenance and operation cost and form energy waste if the normal analysis and the deep analysis are independently arranged, and particularly, the hydrochloric acid to be treated contains impurities such as lower alcohol, calcium, silicon dioxide and the like, is not suitable for the conditions of selecting a calcium chloride (or magnesium chloride) and a sulfuric acid method, and has very obvious energy-saving effect.
Similar plants include, but are not limited to: the industries of synthesizing polyvinyl chloride, gas-phase white carbon black, burning of chlorine-containing tail gas, certain pharmaceutical and pesticide intermediates and the like have the conditions of large hydrochloric acid desorption amount and small water removal amount, and the hydrochloric acid contains some impurities which are deeply desorbed and sensitive by adopting a common calcium chloride and sulfuric acid method. How to remove a certain amount of water by optimizing and utilizing the conditions of a hydrochloric acid normal-resolution device through a process and recover low-boiling-point organic matters, and meanwhile, the aim of saving more energy than the prior art is needed, which is the problem to be solved by the research of the invention.
Disclosure of Invention
In order to solve the problems, the invention provides a hydrochloric acid analysis device with a negative pressure dehydration function and an analysis process, wherein the negative pressure dehydration process and the hydrochloric acid analysis process are combined, redundant water is removed in the hydrochloric acid analysis process, the equipment investment and the operation cost can be greatly reduced compared with the traditional split process design, the utilization rate of energy can be improved through reasonable design, the hydrochloric acid analysis process is not influenced by impurities in the raw material hydrochloric acid to be treated, and the comprehensive energy consumption is saved by 15-50% compared with the existing split design.
In order to achieve the above purpose, the invention adopts a technical scheme that:
a hydrochloric acid desorption device with a negative pressure dehydration function comprises a desorption device and a negative pressure dehydration device, wherein the desorption device comprises a desorption tower, a desorption tower condenser, a demister, a desorption tower reboiling device and a desorption tower diluted acid buffer tank, the top of the desorption tower condenser is communicated with the top of the desorption tower through a pipeline, the lower part of the demister is communicated with the desorption tower condenser through a pipeline, dried hydrogen chloride gas is output through the pipeline at the top of the demister, the bottom of the desorption condenser and the lower part of the demister are communicated with the upper part of the desorption tower through pipelines, the top of the desorption tower reboiling device is communicated with the lower part of the desorption tower through a pipeline, and the upper part of the desorption tower diluted acid buffer tank is communicated with the lower part of the desorption tower and the bottom of the desorption tower through a pipeline; the negative pressure dewatering device passes through the pipeline with the bottom intercommunication of analysis tower diluted acid buffer tank, the negative pressure dewatering device include negative pressure dehydration tower, dehydration tower diluted acid buffer tank, dehydration tower condenser, vacuum unit, diluted acid water pitcher and dehydration reboiling device, the upper portion of negative pressure dehydration tower pass through the pipeline with the bottom intercommunication of analysis tower diluted acid buffer tank, the lower part of dehydration tower diluted acid buffer tank with the bottom intercommunication of negative pressure dehydration tower, the top of dehydration tower condenser pass through the pipeline with the top intercommunication of negative pressure dehydration tower, the vacuum unit pass through the pipeline with the lower part intercommunication of dehydration tower condenser, the diluted acid water pitcher pass through the pipeline with the bottom intercommunication of dehydration tower condenser, the dehydration reboiling device pass through the pipeline with the lower part and the bottom intercommunication of negative pressure dehydration tower.
Further, still include waste heat recovery device, including one-level pre-heater, second grade pre-heater and tertiary pre-heater, dilute acid in the dehydration tower dilute acid buffer tank is in after the heat transfer in the one-level pre-heater pass through the dilute acid cooler of analytic tower exports to hydrogen chloride absorption process, one-level pre-heater pass through the pipeline with the bottom intercommunication of second grade pre-heater, low-temperature steam condensate water in the low pressure steam condensate water buffer tank is in export outside to steam water tank after the heat transfer in the second grade pre-heater, the top of second grade pre-heater pass through the pipeline with the lower part intercommunication of tertiary pre-heater, concentrated hydrochloric acid in the second grade pre-heater passes through after the heat transfer of tertiary heat exchanger export to the upper portion of analytic tower, the top of tertiary pre-heater pass through the pipeline with the top intercommunication of analytic tower, the upper portion of tertiary pre-heater, The bottom of the analysis tower condenser is communicated with the bottom of the demister, and the lower part of the tertiary preheater is communicated with the lower part of the analysis tower condenser through a pipeline.
Further, the analysis tower condenser comprises an analysis tower first-stage condenser, an analysis tower second-stage condenser and an analysis tower third-stage condenser, and the demister comprises a first-stage demister and a second-stage demister; the top of the first-stage condenser of the desorption tower is communicated with the lower part of the third-stage preheater through a pipeline; the top of the second-stage condenser of the desorption tower is communicated with the lower part of the first-stage condenser of the desorption tower through a pipeline; the lower part of the first-stage demister is communicated with the lower part of the second-stage condenser of the desorption tower through a pipeline; the top of the third-stage condenser of the desorption tower is communicated with the top of the first-stage demister through a pipeline; the lower part of the second-stage demister is communicated with the lower part of the third-stage condenser of the desorption tower through a pipeline, and the dried hydrogen chloride gas is output through a pipeline at the top of the second-stage demister; the bottom of the first-stage condenser of the desorption tower, the second-stage condenser of the desorption tower, the third-stage condenser of the desorption tower, the first-stage demister and the second-stage demister is communicated with the upper parts of the desorption tower and the third-stage preheater through pipelines.
Further, the reboiler of the desorption tower comprises a reboiler of the desorption tower, a medium-pressure steam condensate buffer tank and a low-pressure steam flash tank, the top of the reboiler of the desorption tower is communicated with the lower part of the desorption tower through a pipeline, the medium-pressure steam is output to the upper part of the reboiler of the desorption tower, the top of the medium-pressure steam condensate buffer tank and the low-pressure steam flash tank through pipelines, the lower part of the medium-pressure steam condensate buffer tank is communicated with the lower part of the desorption tower reboiler through a pipeline, the bottom of the reboiler of the desorption tower is communicated with the bottom of the desorption tower through a pipeline, the bottom of the medium-pressure steam condensate buffer tank is communicated with the low-pressure steam flash tank through a pipeline, the bottom of the low-pressure steam flash tank outputs low-pressure steam condensate water to the secondary preheater through a condensate water delivery pump, and the top of the low-pressure steam flash tank outputs the low-pressure steam condensate water to a dehydrating tower reboiler; the dehydration reboiling device comprises the dehydration tower reboiler and a low-pressure steam condensate buffer tank, the top of the dehydration tower reboiler is communicated with the lower part of the negative-pressure dehydration tower through a pipeline, the lower part of the dehydration tower reboiler is communicated with the bottom of the negative-pressure dehydration tower through a pipeline, the top of the low-pressure steam condensate buffer tank is communicated with the low-pressure steam flash tank and the upper part of the dehydration tower reboiler through a pipeline, the bottom of the low-pressure steam condensate buffer tank outputs low-pressure steam condensate to the secondary preheater, and the lower part of the low-pressure steam condensate buffer tank is communicated with the lower part of the dehydration tower reboiler through a pipeline; the upper portion of secondary heater lets in low pressure steam condensate buffer tank and the low pressure steam condensate water in the low pressure steam flash tank, the lower part of secondary heater exports to the steam basin, treats that analytic concentrated hydrochloric acid exports through the primary heater to the bottom of secondary heater.
Further, a part of the dilute acid in the dilute acid water tank is output to a sewage treatment station through a dilute acid water delivery pump, the other part of the dilute acid in the dilute acid water tank is output to the upper part of the negative pressure dehydration tower, and the upper part of the negative pressure dehydration tower is connected with the dehydration tower condenser through a pipeline; and the dilute acid in the dilute acid buffer tank of the dehydration tower is sequentially output to the first-stage preheater and the dilute acid cooler of the desorption tower through a dilute hydrochloric acid delivery pump to the hydrogen chloride absorption process.
Further, a main cylinder of the analysis tower is made of high-strength fiber composite reinforced graphite, the main cylinder is connected with a steel flange, the main cylinder is connected with the steel flange through high-strength fiber composite, and the high-strength fiber is at least one of glass fiber, basalt fiber, aramid fiber, carbon fiber, silicon carbide fiber and silicon nitride fiber; the negative pressure dehydration tower adopts a steel composite enamel component coating, the component material of the steel composite enamel component coating is at least one of silicon dioxide, aluminum oxide, zirconium oxide, a binder, polyamide resin, polyimide resin, polytetrafluoroethylene resin, silicon nitrogen resin and polyether resin, and the steel composite enamel component coating is prepared by adopting a thermal spraying process.
Furthermore, the analysis tower and the negative pressure dehydration tower adopt high-efficiency corrosion-resistant fillers, and the high-efficiency corrosion-resistant fillers are at least one of porous graphite Raschig rings, porous graphite spherical fillers, porous ceramic fillers, tetrafluoro fiber fillers and tetrafluoro regular fillers.
The invention also provides a hydrochloric acid analysis process based on any hydrochloric acid analysis device with the negative pressure dehydration function, which comprises the following steps: s10 concentrated hydrochloric acid is pumped to the top of the desorption tower, and the concentrated hydrochloric acid and mixed steam generated by the reboiler of the desorption tower perform mass transfer and heat transfer in the desorption tower to generate mixed gas and dilute acid; s20, allowing the mixed gas to escape from the top of the desorption tower to the three-stage preheater, and allowing the mixed gas to pass through a desorption tower condenser and the demister in sequence to remove redundant moisture and low-boiling-point organic matters to obtain hydrogen chloride gas for later use; and S30, conveying the dilute acid from the lower part of the desorption tower to the dilute acid buffer tank of the desorption tower, and pumping the dilute acid from the dilute acid buffer tank of the desorption tower to the negative pressure dehydration device to separate out the dilute acid water containing trace hydrogen chloride to a sewage treatment station.
Further, concentrated hydrochloric acid to be analyzed sequentially passes through the first-stage preheater, the second-stage preheater and the third-stage preheater, and is output to the analysis tower after waste heat is recovered step by step.
Further, the mixed gas comprises hydrogen chloride gas, low-boiling-point organic matters and a small amount of water vapor, the pressure operation range of the desorption tower is 0-1.0 MPa, and the operation pressure range of the negative pressure dehydration tower is-0.1-0 MPa.
Compared with the prior art, the technical scheme of the invention has the following advantages:
(1) according to the hydrochloric acid analysis device with the negative pressure dehydration function and the analysis process, the negative pressure dehydration process and the hydrochloric acid analysis process are combined, redundant water is removed in the hydrochloric acid analysis process, the equipment investment and the operation cost can be greatly reduced compared with the traditional split process design, and meanwhile, the utilization rate of energy can be improved through reasonable design.
(2) The hydrochloric acid analysis device with the negative pressure dehydration function and the analysis process are provided with a waste heat recovery device, concentrated hydrochloric acid to be analyzed sequentially passes through the primary preheater, the secondary preheater and the tertiary preheater to be subjected to waste heat recovery step by step, namely, waste heat of the concentrated hydrochloric acid to be analyzed and hydrochloric acid in a dilute acid buffer tank of the dehydration tower, waste heat of dilute hydrochloric acid which does not enter the negative pressure dehydration tower in the analysis tower, waste heat of low-pressure steam condensate water in a low-pressure steam flash tank, waste heat of steam condensate water in the low-pressure steam condensate water buffer tank and waste heat of mixed gas at the top of the analysis tower are subjected to waste heat recovery step by step and then enter the analysis tower, the waste heat is fully utilized to achieve the energy-saving effect, the end point temperature of the concentrated hydrochloric acid to be analyzed for the waste heat recovery is controlled to be 80-120 ℃, and the preferred.
(3) According to the hydrochloric acid analysis device with the negative pressure dehydration function and the analysis process, steam condensate water of the analysis tower reboiler enters the dehydration reboiler for waste heat secondary utilization through secondary steam generated by the low-pressure steam flash tank, so that the energy-saving effect is achieved, and the analysis tower and the negative pressure dehydration tower both adopt special high-efficiency anticorrosive fillers, so that the high separation efficiency is achieved, and the energy-saving effect is achieved.
Drawings
The technical solutions and advantages of the present invention will become apparent from the following detailed description of specific embodiments of the present invention with reference to the accompanying drawings.
FIG. 1 is a schematic diagram of a hydrochloric acid analyzer with negative pressure dehydration function according to an embodiment of the present invention;
fig. 2 is a flow chart illustrating an analyzing process of a hydrochloric acid analyzer with negative pressure dehydration function according to an embodiment of the present invention.
Reference numbers in the figures:
11 analytic tower, 12 tertiary preheaters, 13 analytic tower first grade condenser, 14 analytic tower second grade condenser, 15 analytic tower third grade condenser, 16 first grade defroster, 17 second grade defroster, 18 analytic tower dilute acid buffer tank, 21 negative pressure dehydration tower, 22 dehydration tower dilute acid buffer tank, 23 dehydration tower condenser, 24 vacuum unit, 25 dilute acid water tank, 26 dilute acid water delivery pump, 27 dilute hydrochloric acid delivery pump, 28 analytic tower dilute acid cooler, 31 analytic tower reboiler, 32 medium pressure steam condensate buffer tank, 33 low pressure steam flash tank, 34 condensate water delivery pump, 41 dehydration tower reboiler, 42 low pressure steam condensate buffer tank, 5 secondary preheaters, 6 primary preheaters.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The present embodiment provides a hydrochloric acid analyzer having a negative pressure dehydration function, as shown in fig. 1, including: the device comprises an analysis device, a negative pressure dehydration device and a waste heat recovery device, wherein the negative pressure dehydration device is communicated with the analysis device through a pipeline, and the waste heat recovery device is communicated with the analysis device and the negative pressure dehydration device through a pipeline.
The analysis device comprises an analysis tower 11, an analysis tower condenser, a demister, an analysis tower reboiling device and an analysis tower dilute acid buffer tank 18, wherein concentrated hydrochloric acid is conveyed to the top of the analysis tower 11 through a pump, mass transfer and heat transfer are carried out on mixed steam generated by heating the analysis tower reboiling device in the analysis tower 11, mixed gas obtained by escaping from the top of the analysis tower to the analysis tower condenser is obtained, and the mixed gas comprises hydrogen chloride gas, low-boiling-point organic matters and a small amount of water vapor. The operating pressure adaptive range of the analysis tower 11 is wide, the requirements for pressure resistance, temperature resistance, corrosion resistance and leakage resistance are high, and in order to overcome the use defects of pressure resistance, large thermal expansion coefficient, high leakage failure rate and the like of conventional anticorrosion equipment, a main cylinder body of the analysis tower 11 is made of high-strength fiber composite reinforced graphite, the main cylinder body is connected with a steel flange, the main cylinder body is connected with the steel flange and is made of high-strength fiber composite, and the high-strength fiber is at least one of glass fiber, basalt fiber, aramid fiber, carbon fiber, silicon carbide fiber and silicon nitride fiber. The desorption tower 11 adopts high-efficiency corrosion-resistant filler, and the high-efficiency corrosion-resistant filler is at least one of porous graphite Raschig rings, porous graphite spherical filler, porous ceramic filler, tetrafluoro fiber filler and tetrafluoro regular filler. The types of binder substrates used in the material compounding process include, but are not limited to: one or more of furan resin, phenolic resin, silicon resin, epoxy resin, silicon carbon resin and silicon nitrogen resin. The top of the analysis tower condenser is communicated with the top of the analysis tower 11 through a pipeline, the lower part of the demister is communicated with the analysis tower condenser through a pipeline, dried hydrogen chloride gas is output through the top pipeline of the demister, and the mixed gas passes through the analysis tower condenser and the demister to remove moisture and low-boiling-point organic matters, so that the hydrogen chloride gas with high purity is obtained.
The bottom of the analysis condenser and the lower part of the demister are communicated with the analysis tower 11 through pipelines, and the analysis tower condenser and concentrated hydrochloric acid which is used for removing part of high-concentration organic matters behind the demister return to the analysis tower 11 to continue analysis. The top of the reboiler of the desorption tower is communicated with the lower part of the desorption tower 11 through a pipeline, so that the mixed steam generated by heating is conveniently conveyed to the desorption tower 11 to transfer heat and mass with concentrated hydrochloric acid. The upper part of the dilute acid buffer tank 18 of the desorption tower is communicated with the lower part of the desorption tower 11 and the bottom of the desorption tower 11 through pipelines, so that the dilute acid in the desorption tower 11 is conveniently conveyed to the dilute acid buffer tank 18 of the desorption tower so as to enter a negative pressure dehydration process.
The negative pressure dehydration device is communicated with the bottom of the dilute acid buffer tank 18 of the desorption tower through a pipeline, the negative pressure dehydration device comprises a negative pressure dehydration tower 21, a dehydration tower dilute acid buffer tank 22, a dehydration tower condenser 23, a vacuum unit 24, a dilute acid water tank 25 and a dehydration reboiling device, the upper part of the negative pressure dehydration tower 21 is communicated with the bottom of the dilute acid buffer tank 18 of the desorption tower through a pipeline, the lower part of the dehydration tower dilute acid buffer tank 22 is communicated with the bottom of the negative pressure dehydration tower 21, the top of the dehydration tower condenser 23 is communicated with the top of the negative pressure dehydration tower 21 through a pipeline, the constant boiling dilute hydrochloric acid coming out of the kettle of the desorption tower 11 enters the negative pressure dehydration tower 21 according to the size of the dehydration water quantity, the constant boiling dilute hydrochloric acid enters the negative pressure dehydration tower 21 to be subjected to hydrochloric acid flash evaporation cooling, and steam generated by heating of the kettle of the negative pressure dehydration tower 21 and reflux acid water at the top are subjected to heat transfer in the tower of, And (4) transferring mass and separating out acid water containing trace hydrogen chloride. The dilute hydrochloric acid which does not enter the negative pressure dehydration tower and the raw material hydrochloric acid which enters the desorption tower exchange heat in a two-phase mode and then enter other working procedures of a factory to continuously absorb the hydrogen chloride. The vacuum unit 24 is communicated with the lower part of the dehydrating tower condenser 23 through a pipeline, and the dilute acid water tank 25 is communicated with the bottom of the dehydrating tower condenser 23 through a pipeline. A part of dilute acid in the dilute acid water tank 25 is output to a sewage treatment station through a dilute acid water delivery pump 26, the other part of dilute acid in the dilute acid water tank 25 is delivered to the upper part of the negative pressure dehydration tower 21 as a reflux liquid of the dehydration tower, and the upper part of the negative pressure dehydration tower 21 is connected with the dehydration tower condenser 23 through a pipeline. And water drops of the water vapor at the upper part of the negative pressure dehydration tower 21 under the action of gravity are output to the sewage treatment station through a pipeline. The dehydration reboiling device is communicated with the lower part and the bottom of the negative pressure dehydration tower 21 through pipelines. The negative pressure dehydration tower 21 needs to be resistant to negative pressure, corrosion and leakage and overcomes the defects of conventional materials, the negative pressure dehydration tower 21 adopts a steel composite enamel component coating, the component material of the steel composite enamel component coating is at least one of silicon dioxide, aluminum oxide, zirconium oxide, a binder, polyamide resin, polyimide resin, polytetrafluoroethylene resin, silicon nitrogen resin and polyether resin, and the steel composite enamel component coating is prepared by adopting a thermal spraying process. The negative pressure dehydration tower 21 adopts high-efficiency corrosion-resistant filler, the high-efficiency corrosion-resistant filler is at least one of porous graphite Raschig rings, porous graphite spherical filler, porous ceramic filler, tetrafluoro fiber filler and tetrafluoro regular filler, and the types of the used binder base materials include but are not limited to: one or more of furan resin, phenolic resin, silicon resin, epoxy resin, silicon carbon resin and silicon nitrogen resin. The negative pressure dehydration tower 21 adopts high-efficiency corrosion-resistant filler, so that the number of theoretical plates of the filler per meter can be increased, the separation efficiency is also increased, the reflux ratio can be reduced by 10-30%, and the energy-saving effect is achieved.
The waste heat recovery device comprises a primary preheater 6, a secondary preheater 5 and a tertiary preheater 12, the dilute acid in the dilute acid buffer tank 22 of the dehydration tower exchanges heat in the first-stage preheater 6 and then is output to the hydrogen chloride absorption process through the dilute acid cooler 28 of the desorption tower, the primary preheater 6 is communicated with the bottom of the secondary preheater 5 through a pipeline, the low-temperature steam condensate in the low-pressure steam condensate buffer tank 42 is subjected to heat exchange in the secondary preheater 5 and then is output to an outdoor steam water tank, the top of the secondary preheater 5 is communicated with the lower part of the tertiary preheater 12 through a pipe, concentrated hydrochloric acid in the secondary preheater 5 is output to the upper part of the desorption tower 11 after heat exchange by the tertiary heat exchanger 12, the top of the third-stage preheater 12 is communicated with the top of the desorption tower 11 through a pipeline, and the lower part of the third-stage preheater 12 is communicated with the lower part of the desorption tower condenser through a pipeline. The upper part of the tertiary preheater 12 is communicated with the upper part of the desorption tower 11, the bottom of the desorption tower condenser and the bottom of the demister through pipelines.
The analysis tower condenser comprises an analysis tower first-stage condenser 13, an analysis tower second-stage condenser 14 and an analysis tower third-stage condenser 15, and the demister comprises a first-stage demister 16 and a second-stage demister 17. The top of the analysis tower first-stage condenser 13 is communicated with the lower part of the third-stage preheater 12 through a pipeline, the top of the analysis tower second-stage condenser 14 is communicated with the lower part of the analysis tower first-stage condenser 13 through a pipeline, the lower part of the first-stage demister 16 is communicated with the lower part of the analysis tower second-stage condenser 14 through a pipeline, the top of the analysis tower third-stage condenser 15 is communicated with the top of the first-stage demister 16 through a pipeline, the lower part of the second-stage demister 17 is communicated with the lower part of the analysis tower third-stage condenser 15 through a pipeline, and dried hydrogen chloride gas passes through the pipeline at the top of the second-stage demister 17 to. The bottoms of the desorption tower first-stage condenser 13, the desorption tower second-stage condenser 14, the desorption tower third-stage condenser 15, the first-stage demister 16, and the second-stage demister 17 are communicated with the upper portions of the desorption tower 11 and the third-stage preheater 12 through pipes. If the hydrochloric acid to be treated contains low-boiling-point organic matters, controlling different condensation temperatures of the mixed gas escaped from the top of the desorption tower 11, intermittently discharging concentrated hydrochloric acid solution containing the low-boiling-point organic matters through a sectional condensation method, returning the concentrated hydrochloric acid solution to a user process, and finally, freezing, separating and drying the hydrogen chloride gas to obtain the product. And controlling the system pressure of the desorption tower 11 to be an optimal value, obtaining constant boiling acid with a certain concentration at the tower kettle, and forming a linear relation between the acid outlet concentration of the constant boiling acid and the working pressure of the desorption tower. The concentrated hydrochloric acid to be analyzed contains lower alcohol or other low-boiling point organic matters, calcium ions, sulfate ions, silicon dioxide, other heavy metal ions, high-boiling point organic matters, organic sulfonate and other impurities. The optimal sectional condensation temperature of the lower alcohol or the low-boiling-point organic matter is determined according to the type and the content of the lower alcohol or the low-boiling-point organic matter, and the optimal condensation temperature range is calculated according to the boiling point of the mixed gas component at the top of the desorption tower under normal pressure as follows: the preferable discharge positions of concentrated hydrochloric acid containing low-boiling point organic matters are that: after the secondary condenser 14.
The reboiler of the desorption tower comprises a reboiler 31 of the desorption tower, a medium pressure steam condensate buffer tank 32 and a low pressure steam flash tank 33, wherein the top of the reboiler 31 of the desorption tower is communicated with the lower part of the desorption tower 11 through a pipeline, medium pressure steam is output to the upper part of the reboiler 31 of the desorption tower, the top of the medium pressure steam condensate buffer tank 32 and the low pressure steam flash tank 33 through a pipeline, the lower part of the medium pressure steam condensate buffer tank 32 is communicated with the lower part of the reboiler 31 of the desorption tower through a pipeline, the bottom of the reboiler 31 of the desorption tower is communicated with the bottom of the desorption tower 11 through a pipeline, the bottom of the medium pressure steam condensate buffer tank 32 is communicated with the low pressure steam flash tank 33 through a pipeline, and the bottom of the low pressure steam flash tank 33 outputs low pressure steam condensate to the secondary preheater 5 through a condensate transfer pump 34, the overhead vapor of the low pressure steam flash drum 33 is output to a dehydration column reboiler 41.
The dehydration reboiling device comprises a dehydration tower reboiler 41 and a low-pressure steam condensate buffer tank 42, the top of the dehydration tower reboiler 41 is communicated with the lower part of the negative pressure dehydration tower 21 through a pipeline, the lower part of the dehydration tower reboiler is communicated with the bottom of the negative pressure dehydration tower through a pipeline, the top of the low-pressure steam condensate buffer tank 42 is communicated with the low-pressure steam flash tank 33 and the upper part of the dehydration tower reboiler 41 through a pipeline, low-pressure steam condensate water is output to the secondary preheater 5 from the bottom of the low-pressure steam condensate buffer tank 42, and the lower part of the low-pressure steam condensate buffer tank 42 is communicated with the lower part of the dehydration tower reboiler 41 through a pipeline. The upper portion of secondary preheater 5 lets in low pressure steam condensate buffer tank 42 and the low pressure steam condensate water in the low pressure steam flash tank 33, the lower part of secondary preheater 5 is exported to the steam basin, waits to resolve concentrated hydrochloric acid and exports to the bottom of secondary preheater 5 through one-level preheater 6. The dilute acid in the dilute acid buffer tank 22 of the dehydration tower is sequentially output to the first-stage preheater 6 and the dilute acid cooler 28 of the desorption tower through a dilute hydrochloric acid delivery pump 27 to the hydrogen chloride absorption process.
As shown in fig. 2, the present invention further provides a hydrochloric acid desorption process of a hydrochloric acid desorption device with a negative pressure dehydration function based on any one of the above processes, comprising the following steps: s10 concentrated hydrochloric acid is pumped to the top of the desorber 11 where it undergoes mass and heat transfer with the mixed vapor produced by the desorber reboiling equipment to produce a mixed gas and dilute acid. And S20, allowing the mixed gas to escape from the top of the desorption tower 11 to the tertiary preheater 12, and allowing the mixed gas to pass through a desorption tower condenser and the demister in sequence to remove redundant moisture and low-boiling-point organic matters to obtain hydrogen chloride gas for later use. S30 the dilute acid is transported to the dilute acid buffer tank 18 from the lower part of the desorption tower 11, and is pumped to the negative pressure dehydration device by the dilute acid buffer tank 18 to separate the dilute acid water containing trace hydrogen chloride to a sewage treatment station. The pressure operation range of the desorption tower 11 is 0-1.0 Mpa, and the operation pressure range of the negative pressure dehydration tower 21 is-0.1-0 Mpa.
The method does not aim at completely separating hydrogen chloride and water in the concentrated hydrochloric acid to be analyzed, but removes a proper amount of water based on the normal analysis of the hydrochloric acid, wherein the water removal amount is 0-30% of the flow of dilute hydrochloric acid at the bottom of the analysis tower.
The S10 concentrated hydrochloric acid is pumped to the top of the desorber 11 where it undergoes mass and heat transfer with the mixed vapor produced by the desorber reboiling equipment to produce a mixed gas and dilute acid.
The process for preparing the dry hydrogen chloride gas by using the S20 mixed gas comprises the following steps:
the mixed gas sequentially passes through the top of the analysis tower 11, the third-stage preheater 12, the first-stage condenser 13 of the analysis tower, the second-stage condenser 14 of the analysis tower, the first-stage demister 16, the third-stage condenser 15 of the analysis tower and the second-stage demister 17 to obtain dry hydrogen chloride gas. Part of the liquid water carried by the mixed gas when entering the tertiary preheater 12 is returned to the desorption tower 11 through a pipeline. The third-stage preheater 12, the first-stage condenser 13 of the desorption tower, the second-stage condenser 14 of the desorption tower, the first-stage demister 16, the third-stage condenser 15 of the desorption tower and the concentrated hydrochloric acid solution containing a small amount of organic matters, which is separated in the drying process of the second-stage demister 17, are returned to the desorption tower 11 through a pipeline. The condensate of the second-stage condenser 14 or the third-stage condenser 15 of the desorption tower is subjected to condensation temperature control according to the boiling point of organic matters contained in the mixed gas, and the condensate is discharged from the clearance.
In the S30, the pressure operation range of the desorption tower 11 is preferably 0.2 to 0.6MPa, and the operation pressure range of the negative pressure dehydration tower 21 is preferably-0.09 to-0.07 MPa.
The dehydration process of the negative pressure dehydration device in the step S30 is as follows:
the dilute acid in the desorption tower 11 is output to the dilute acid buffer tank 18 of the desorption tower, the dilute acid in the dilute acid buffer tank 18 of the desorption tower is pumped to the upper part of the negative pressure dehydration tower 21, the dilute acid in the negative pressure dehydration tower 21 and the mixed steam generated by the reboiling device of the dehydration tower perform mass transfer and heat transfer to generate a second mixed gas carrying water vapor, the second mixed gas enters the dilute acid water tank 25 after being cooled by the dehydration tower condenser 23, because the concentration of the hydrochloric acid in the dilute acid water tank 25 is very low, a part of the dilute acid in the dilute acid water tank 25 is output to a sewage treatment station through the dilute acid water delivery pump 26, and the other part of the dilute acid in the dilute acid water tank 25 is delivered to the upper part of the negative pressure dehydration tower 21 as the dehydration tower dehydration liquid. The dilute acid output from the bottom of the negative pressure dehydration tower 21 enters the dehydration tower dilute acid buffer tank 22, is pumped to the primary preheater 6 for waste heat recovery, is cooled by the desorption tower dilute acid cooler 28 after heat transfer, and is output to the hydrogen chloride absorption process.
The process for recovering the waste heat by using the waste heat recovery device comprises the following steps:
and recovering the residual heat of the hydrochloric acid in the dilute acid buffer tank 22 of the dehydrating tower and the residual heat of the dilute hydrochloric acid which does not enter the negative pressure dehydrating tower 21 by the desorption tower through the primary preheater 6, recovering the residual heat of the low-pressure steam condensate water in the low-pressure steam flash tank 33 and the residual heat of the steam condensate water in the low-pressure steam condensate water buffer tank 42 in the secondary preheater 5, then entering the tertiary preheater 12, and recovering the residual heat of the tower top mixed gas of the desorption tower 11 in the tertiary preheater 12 to form a steam-liquid mixture or a high-temperature liquid-phase material. The material after waste heat recovery returns to the desorption tower 11 through a pipeline, vapor-liquid separation is carried out in the desorption tower, the formed mixed gas and the mixed gas in the desorption tower 11 enter a three-stage preheater 12, and liquid flows downwards in the desorption tower 11 to continuously carry out mass transfer and heat transfer.
Example 1
The concentrated hydrochloric acid with 31 percent of ethanol to be treated contains 0.1 percent of ethanol, the treatment capacity is 20t/h, the hydrogen chloride gas is required to be analyzed by adopting the conventional analysis, the redundant water is removed at the same time for 1t/h, a water station is decontaminated, and about 20 percent of diluted hydrochloric acid after the analysis is returned to other working procedures of a factory.
In the embodiment, the hydrochloric acid to be treated contains ethanol, and the ethanol reacts with the entrainer for conventional deep analysis such as calcium chloride and magnesium chloride, so that the hydrochloric acid is not suitable for removing excessive water by the conventional calcium chloride method, the hydrochloric acid is treated by the calcium chloride method, and the comprehensive steam consumption is about 5.7 t/h; the excess water is removed by deep analysis by adopting a differential pressure method, the investment is large, the operation cost is high, and the comprehensive steam consumption is about 7.5 t/h.
The hydrochloric acid analysis device with the negative pressure dehydration function is adopted for analysis, hydrochloric acid to be treated enters the analysis tower 11, the hydrochloric acid is insensitive to ethanol impurities due to no entrainer, mixed gas of hydrogen chloride, water and ethanol escapes from the top of the analysis tower 11, the operation pressure of the analysis tower 11 is controlled to be 0.3MPa (G), about 18.5 percent of dilute hydrochloric acid at the tower bottom of the analysis tower 11 enters the negative pressure dehydration tower 21 at a rate of 16t/h, the rest of the dilute hydrochloric acid and the diluted acid at the tower bottom of the negative pressure dehydration tower 21 enter the primary preheater 6, the operation pressure of the negative pressure dehydration tower 21 is-0.085 MPa (G), the fillers of the analysis tower 11 and the negative pressure dehydration tower 21 adopt the combination of porous graphite spherical filler and tetrafluoro regular filler, the reflux ratio of the negative pressure tower 21 is 0.9, the distilled water at the top of the tower top is 1t/h, the tower bottom outlet acid concentration of the negative pressure dehydration tower 21 is 19.7%, the comprehensive steam consumption is 4.7 t/h. The comprehensive energy-saving efficiency reaches more than 20 percent.
The hydrochloric acid from the primary preheater 6 enters the secondary preheater 5 for double-effect heat exchange with the low-pressure steam condensate water, the hydrochloric acid after heat exchange continues to enter the tertiary preheater 12 for double-effect heat exchange with the gas phase at the top of the desorption tower 11 and then enters the desorption tower 11, and the preheated end point temperature is controlled to be about 98 ℃.
Controlling the temperature of the gas phase at the top of the desorption tower at 45 ℃ in the first-stage condenser 13, controlling the temperature of the second-stage condenser 14 of the desorption tower at-6 ℃, and extracting concentrated hydrochloric acid containing ethanol from a liquid phase outlet of a gas-liquid separator 14 of the second-stage condenser of the desorption tower.
The graphite cylinder body of the desorption tower 11 is reinforced by compounding carbon fibers, the aramid fibers are firstly compounded at the connecting part of the cylinder body connecting flange, then the carbon fibers are integrally compounded, and the carbon fibers, the aramid fibers, the steel flange and the graphite are bonded into a whole by using the modified phenolic resin as a base material.
The negative pressure dehydration tower 21 adopts an enamel-like component composite coating, and comprises the following components: silica, a binder, zirconia, and polytetrafluoroethylene resin.
Example 2
The concentration of concentrated hydrochloric acid to be treated is 28%, a small amount of silicon dioxide is contained, the treatment capacity is 36.4t/h, hydrochloric acid is normally analyzed, hydrogen chloride gas reaches the use point, meanwhile, 3t/h of material balance excess water is evaporated, and dilute hydrochloric acid returns to other procedures to absorb hydrogen chloride, so that a closed cycle is formed.
The concentrated hydrochloric acid to be treated in the embodiment contains silicon dioxide, and calcium chloride or magnesium chloride and other azeotrope breaking agents are adopted for deep analysis, so that the silicon dioxide can generate silicate precipitates and accumulate in the environment of the concentrated hydrochloric acid, and serious influence is caused on long-period production.
When equal amount of hydrogen chloride is analyzed and equal amount of water is removed, the calcium chloride method is adopted for treatment, the comprehensive steam consumption is about 11t/h, and the differential pressure method is adopted for treatment, the comprehensive steam consumption is about 15 t/h.
The hydrochloric acid analysis device with the negative pressure dehydration function is adopted for analysis, concentrated hydrochloric acid to be treated enters the analysis tower 11, a small amount of silicon dioxide cannot be deposited in a system due to no entrainer, mixed gas of hydrogen chloride and water escapes from the top of the tower and is subjected to multi-stage condensation drying, the operation pressure of the analysis tower 11 is controlled to be 0.7MPa (G), about 31.2t/h of dilute hydrochloric acid at the tower bottom of the analysis tower 11 is about 16.1 percent and enters the negative pressure dehydration tower 21, the rest of the dilute hydrochloric acid and tower bottom dilute acid of the negative pressure dehydration tower 21 enter the primary preheater 6, the operation pressure of the negative pressure dehydration tower 21 is-0.085 MPa (G), the fillers of the analysis tower 11 and the negative pressure dehydration tower 21 are regularly combined by adopting porous tetrafluoro fibers, porous graphite Raschig rings and tetrafluoro fillers, the reflux ratio of the negative pressure dehydration tower 21 is 0.7, and the top of the distilled water is 3t/h, the concentration of the acid discharged from the tower bottom is about 17.8 percent, the acid is converted into the equivalent hydrogen chloride and the equivalent water removal, and the comprehensive steam consumption is about 8.0 t/h. The comprehensive energy-saving efficiency reaches more than 37.5 percent. The pressure of the analytical tower is improved and the energy-saving effect is linear and obvious.
The hydrochloric acid from the primary preheater 6 enters the secondary preheater 5 for double-effect heat exchange with the low-pressure steam condensate water, the hydrochloric acid after heat exchange continues to enter the tertiary preheater 12 for double-effect heat exchange with the top gas phase of the desorption tower 11 and then enters the desorption tower 11, and the preheated end point temperature is controlled to be about 90 ℃.
The graphite cylinder of the desorption tower 11 is reinforced by compounding glass fibers, the basalt fibers are firstly compounded locally at the connection part of the cylinder connection flange, then the glass fibers are compounded integrally, and the glass fibers, the basalt fibers, the steel flange and the graphite are bonded into a whole by using epoxy resin as a base material as a binder.
The negative pressure dehydration tower 21 adopts an enamel-like component composite coating, and comprises the following components: silicon dioxide, a binder, aluminum oxide and polyether resin.
The above description is only an exemplary embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent structures or equivalent processes that are transformed by the content of the present specification and the attached drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. A hydrochloric acid analysis device with negative pressure dehydration function is characterized by comprising an analysis device and a negative pressure dehydration device,
the analysis device comprises an analysis tower, an analysis tower condenser, a demister, an analysis tower reboiling device and an analysis tower dilute acid buffer tank, wherein the top of the analysis tower condenser is communicated with the top of the analysis tower through a pipeline, the lower part of the demister is communicated with the analysis tower condenser through a pipeline, dried hydrogen chloride gas is output through a top pipeline of the demister, the bottom of the analysis condenser and the lower part of the demister are communicated with the upper part of the analysis tower through pipelines, the top of the analysis tower reboiling device is communicated with the lower part of the analysis tower through a pipeline, and the upper part of the analysis tower dilute acid buffer tank is communicated with the lower part of the analysis tower and the bottom of the analysis tower through a pipeline;
the negative pressure dewatering device passes through the pipeline with the bottom intercommunication of analysis tower diluted acid buffer tank, the negative pressure dewatering device include negative pressure dehydration tower, dehydration tower diluted acid buffer tank, dehydration tower condenser, vacuum unit, diluted acid water pitcher and dehydration reboiling device, the upper portion of negative pressure dehydration tower pass through the pipeline with the bottom intercommunication of analysis tower diluted acid buffer tank, the lower part of dehydration tower diluted acid buffer tank with the bottom intercommunication of negative pressure dehydration tower, the top of dehydration tower condenser pass through the pipeline with the top intercommunication of negative pressure dehydration tower, the vacuum unit pass through the pipeline with the lower part intercommunication of dehydration tower condenser, the diluted acid water pitcher pass through the pipeline with the bottom intercommunication of dehydration tower condenser, the dehydration reboiling device pass through the pipeline with the lower part and the bottom intercommunication of negative pressure dehydration tower.
2. The hydrochloric acid desorption device with the negative pressure dehydration function as claimed in claim 1, further comprising a waste heat recovery device comprising a primary preheater, a secondary preheater and a tertiary preheater, wherein the dilute acid in the dilute acid buffer tank of the dehydration tower is subjected to heat exchange in the primary preheater and then is output to a hydrogen chloride absorption process through the dilute acid cooler of the desorption tower, the primary preheater is communicated with the bottom of the secondary preheater through a pipeline, the low-temperature steam condensate in the low-pressure steam condensate buffer tank is subjected to heat exchange in the secondary preheater and then is output to an outdoor steam water tank, the top of the secondary preheater is communicated with the lower part of the tertiary preheater through a pipeline, the concentrated hydrochloric acid in the secondary preheater is subjected to heat exchange in the tertiary preheater and then is output to the upper part of the desorption tower, and the top of the tertiary preheater is communicated with the top of the desorption tower through a pipeline, the upper part of the third-stage preheater is communicated with the upper part of the analysis tower, the bottom of the analysis tower condenser and the bottom of the demister through pipelines, and the lower part of the third-stage preheater is communicated with the lower part of the analysis tower condenser through pipelines.
3. The hydrochloric acid desorption device with negative pressure dehydration function as claimed in claim 1, wherein the desorption tower condenser comprises a desorption tower first-stage condenser, a desorption tower second-stage condenser and a desorption tower third-stage condenser, and the demister comprises a first demister and a second demister;
the top of the first-stage condenser of the desorption tower is communicated with the lower part of the third-stage preheater through a pipeline;
the top of the second-stage condenser of the desorption tower is communicated with the lower part of the first-stage condenser of the desorption tower through a pipeline;
the lower part of the first-stage demister is communicated with the lower part of the second-stage condenser of the desorption tower through a pipeline;
the top of the third-stage condenser of the desorption tower is communicated with the top of the first-stage demister through a pipeline;
the lower part of the second-stage demister is communicated with the lower part of the third-stage condenser of the desorption tower through a pipeline, and the dried hydrogen chloride gas is output through a pipeline at the top of the second-stage demister;
the bottom of the first-stage condenser of the desorption tower, the second-stage condenser of the desorption tower, the third-stage condenser of the desorption tower, the first-stage demister and the second-stage demister is communicated with the upper parts of the desorption tower and the third-stage preheater through pipelines.
4. The hydrochloric acid desorption device with negative pressure dehydration function as claimed in claim 1,
the reboiling device of the desorption tower comprises a desorption tower reboiler, a medium-pressure steam condensate buffer tank and a low-pressure steam flash tank, the top of the reboiler of the desorption tower is communicated with the lower part of the desorption tower through a pipeline, the medium-pressure steam is output to the upper part of the reboiler of the desorption tower, the top of the medium-pressure steam condensate buffer tank and the low-pressure steam flash tank through pipelines, the lower part of the medium-pressure steam condensate buffer tank is communicated with the lower part of the desorption tower reboiler through a pipeline, the bottom of the reboiler of the desorption tower is communicated with the bottom of the desorption tower through a pipeline, the bottom of the medium-pressure steam condensate buffer tank is communicated with the low-pressure steam flash tank through a pipeline, the bottom of the low-pressure steam flash tank outputs low-pressure steam condensate water to the secondary preheater through a condensate water delivery pump, and the top of the low-pressure steam flash tank outputs the low-pressure steam condensate water to a dehydrating tower reboiler;
the dehydration reboiling device comprises the dehydration tower reboiler and a low-pressure steam condensate buffer tank, the top of the dehydration tower reboiler is communicated with the lower part of the negative-pressure dehydration tower through a pipeline, the lower part of the dehydration tower reboiler is communicated with the bottom of the negative-pressure dehydration tower through a pipeline, the top of the low-pressure steam condensate buffer tank is communicated with the low-pressure steam flash tank and the upper part of the dehydration tower reboiler through a pipeline, the bottom of the low-pressure steam condensate buffer tank outputs low-pressure steam condensate to the secondary preheater, and the lower part of the low-pressure steam condensate buffer tank is communicated with the lower part of the dehydration tower reboiler through a pipeline;
the upper portion of secondary heater lets in low pressure steam condensate buffer tank and the low pressure steam condensate water in the low pressure steam flash tank, the lower part of secondary heater exports to the steam basin, treats that analytic concentrated hydrochloric acid exports through the primary heater to the bottom of secondary heater.
5. The hydrochloric acid desorption device with negative pressure dehydration function as claimed in claim 2,
a part of dilute acid in the dilute acid water tank is output to a sewage treatment station through a dilute acid water delivery pump, the other part of dilute acid in the dilute acid water tank is output to the upper part of the negative pressure dehydration tower, and the upper part of the negative pressure dehydration tower is connected with a dehydration tower condenser through a pipeline;
and the dilute acid in the dilute acid buffer tank of the dehydration tower is sequentially output to the first-stage preheater and the dilute acid cooler of the desorption tower through a dilute hydrochloric acid delivery pump to the hydrogen chloride absorption process.
6. The hydrochloric acid desorption device with negative pressure dehydration function as claimed in claim 1,
the main cylinder body of the analysis tower is made of high-strength fiber composite reinforced graphite, the main cylinder body is connected with a steel flange, the main cylinder body is connected with the steel flange through high-strength fiber composite, and the high-strength fiber is at least one of glass fiber, basalt fiber, aramid fiber, carbon fiber, silicon carbide fiber and silicon nitride fiber;
the negative pressure dehydration tower adopts a steel composite enamel component coating, the component material of the steel composite enamel component coating is at least one of silicon dioxide, aluminum oxide, zirconium oxide, a binder, polyamide resin, polyimide resin, polytetrafluoroethylene resin, silicon nitrogen resin and polyether resin, and the steel composite enamel component coating is prepared by adopting a thermal spraying process.
7. The hydrochloric acid desorption device with the negative pressure dehydration function as claimed in claim 1, wherein the desorption tower and the negative pressure dehydration tower adopt high-efficiency corrosion-resistant packing, and the high-efficiency corrosion-resistant packing is at least one of porous graphite Raschig rings, porous graphite spherical packing, porous ceramic packing, tetrafluoro fiber packing and tetrafluoro regular packing.
8. A hydrochloric acid desorption process based on the hydrochloric acid desorption device with the negative pressure dehydration function as claimed in any one of claims 1 to 7, which is characterized by comprising the following steps:
s10 concentrated hydrochloric acid is pumped to the top of the desorption tower, and the concentrated hydrochloric acid and mixed steam generated by the reboiler of the desorption tower perform mass transfer and heat transfer in the desorption tower to generate mixed gas and dilute acid;
s20, allowing the mixed gas to escape from the top of the desorption tower to the three-stage preheater, and allowing the mixed gas to pass through a desorption tower condenser and the demister in sequence to remove redundant moisture and low-boiling-point organic matters to obtain hydrogen chloride gas for later use;
and S30, conveying the dilute acid from the lower part of the desorption tower to the dilute acid buffer tank of the desorption tower, and pumping the dilute acid from the dilute acid buffer tank of the desorption tower to the negative pressure dehydration device to separate out the dilute acid water containing trace hydrogen chloride to a sewage treatment station.
9. The hydrochloric acid desorption process of the hydrochloric acid desorption device with the negative pressure dehydration function as claimed in claim 8, wherein concentrated hydrochloric acid to be desorbed is sequentially subjected to the primary preheater, the secondary preheater and the tertiary preheater for gradual waste heat recovery and then output to the desorption tower.
10. The hydrochloric acid desorption process of a hydrochloric acid desorption device with a negative pressure dehydration function as claimed in claim 8, wherein the mixed gas comprises hydrogen chloride gas, low boiling point organic matter and a small amount of water vapor, the pressure operation range of the desorption tower is 0-1.0 Mpa, and the operation pressure range of the negative pressure dehydration tower is-0.1-0 Mpa.
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