CN114777421B - System and method for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas - Google Patents
System and method for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas Download PDFInfo
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- CN114777421B CN114777421B CN202210330291.5A CN202210330291A CN114777421B CN 114777421 B CN114777421 B CN 114777421B CN 202210330291 A CN202210330291 A CN 202210330291A CN 114777421 B CN114777421 B CN 114777421B
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2205/00—Processes or apparatus using other separation and/or other processing means
- F25J2205/40—Processes or apparatus using other separation and/or other processing means using hybrid system, i.e. combining cryogenic and non-cryogenic separation techniques
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The system and the method for purifying the hydrogen chloride from the chloroacetic acid or chloroacetyl chloride synthesis tail gas, disclosed by the invention, comprise the following steps of: a heat exchanger; a rectifying tower for separating heavy components from the tail gas; the sulfur dioxide product tower is connected with the rectifying tower through a pipeline; the dechlorination tower is connected with the sulfur dioxide product tower through a pipeline; the hydrogen chloride purifying tower is connected with the dechlorination tower through a pipeline. The method for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas comprises the following steps: cooling the tail gas; liquefying and separating the cooled tail gas; separating sulfur dioxide from the tail gas; separating the tail gas to obtain chlorine-rich gas; the tail gas is separated to obtain hydrogen chloride. The technical scheme of the invention has the advantages that: the method can purify hydrogen chloride from chloroacetic acid (or chloroacetyl chloride) synthesis tail gas and combine sulfur dioxide, has simple process flow and easy operation, solves the problem of exhaust emission, and simultaneously recovers the effective components in the tail gas.
Description
Technical Field
The invention relates to chemical gas purification, in particular to a system and a method for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas.
Background
Chloroacetic acid and chloroacetyl chloride are widely used as intermediates in the pharmaceutical and pesticide industries. During the production of chloroacetic acid (or chloroacetyl chloride), a large amount of synthesis off-gas is produced, with hydrogen chloride, sulfur dioxide and chlorine being the dominant. The traditional synthetic tail gas treatment mode is condensation recovery, then three-stage falling film is rich in hydrochloric acid, and finally the synthetic tail gas is discharged after water washing and alkali washing.
The traditional treatment mode has the defects that the impurity of the hydrochloric acid which is rich in production is more, the recycling value is low, the waste acid treatment is troublesome, and meanwhile, sulfur dioxide and chlorine in tail gas cannot be recycled, so that certain resource waste is caused.
Disclosure of Invention
The invention aims to provide a system and a method for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas, which can recycle chloroacetic acid or chloroacetyl chloride synthesis tail gas.
The system for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas comprises:
a heat exchanger for cooling the tail gas;
The rectifying tower is used for liquefying and separating the cooled tail gas to separate heavy components from the tail gas, and is connected with the heat exchanger through a pipeline;
the sulfur dioxide product tower is used for separating sulfur dioxide from the tail gas and is connected with the rectifying tower through a pipeline;
The dechlorination tower is used for separating the tail gas into chlorine-rich gas and is connected with the sulfur dioxide product tower through a pipeline;
And the hydrogen chloride purifying tower is used for separating hydrogen chloride from the tail gas and is connected with the dechlorination tower through a pipeline.
The system for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas further comprises a buffer gas tank, an adsorption device and a compressor, wherein an air inlet of the buffer gas tank is connected with an air source of the tail gas through a pipeline, an air outlet of the buffer gas tank is connected with an air inlet of the adsorption device through a pipeline, an air outlet of the adsorption device is connected with an air inlet of the compressor through a pipeline, and an air outlet of the compressor is connected with an air inlet of a heat exchanger through a pipeline, so that the tail gas is compressed to 2bar after being dried and dehydrated through the adsorption device and then cooled by the heat exchanger.
The invention relates to a system for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas, wherein the bottom of a hydrogen chloride purifying tower is connected with a hydrogen chloride output pipe, and the hydrogen chloride output pipe passes through a heat exchanger so as to rewarming liquid hydrogen chloride in the hydrogen chloride output pipe through the heat exchanger to obtain hydrogen chloride gas.
The system for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas is characterized in that the top of a hydrogen chloride purifying tower is connected with a hydrogen chloride gas output pipe, and the hydrogen chloride gas output pipe passes through a heat exchanger so that gaseous hydrogen chloride in the hydrogen chloride gas output pipe is rewarmed through the heat exchanger.
The system for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas further comprises two sets of refrigeration systems, wherein the refrigeration systems comprise a mixed refrigerant compressor and a throttle valve, the mixed refrigerant compressor conveys compressed gas-phase refrigerant to the throttle valve through a first pipeline, the gas-phase refrigerant returns to the mixed refrigerant compressor through a second pipeline after being throttled and cooled by the throttle valve, the gas-phase refrigerant circulates between the mixed refrigerant compressor and the throttle valve through the first pipeline and the second pipeline, the first pipeline passes through a heat exchanger, the second pipeline passes through the heat exchanger, the refrigerant in the first pipeline is cooled in the heat exchanger, and the refrigerant in the second pipeline provides cold energy in the heat exchanger.
The method for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas comprises the following steps:
Cooling the tail gas;
liquefying and separating the cooled tail gas to separate heavy components from the tail gas;
Separating sulfur dioxide from the tail gas;
Separating the tail gas to obtain chlorine-rich gas;
The tail gas is separated to obtain hydrogen chloride.
The invention discloses a method for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas, which comprises the following steps: the tail gas is dried and dehydrated by an adsorption device, compressed to 2bar and cooled by a heat exchanger.
The invention relates to a method for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas, which further comprises the following steps:
the heavy components separated from the tail gas are returned to the reaction kettle after being rewarmed by the heat exchanger;
The chlorine-rich liquid phase separated from the tail gas is sent to a synthesis kettle to be used as a synthesis raw material of chloracetyl chloride after being rewarmed by a heat exchanger;
And (3) re-heating the gas phase of hydrogen chloride separated from the tail gas by a heat exchanger to obtain raw materials for producing methyl chloride, and re-heating the liquid phase of hydrogen chloride separated from the tail gas by the heat exchanger to obtain industrial-grade or electronic-grade hydrogen chloride gas.
The technical scheme of the invention has the advantages that: the method can purify hydrogen chloride from chloroacetic acid (or chloroacetyl chloride) synthesis tail gas and combine sulfur dioxide, has simple process flow and easy operation, solves the problem of exhaust emission, recovers the effective components in the tail gas, increases the added value of the product, and realizes the purpose of turning harm into benefit and changing waste into valuables. The technical scheme of the invention has great significance for sustainable development of economy, ecological environment and society.
Drawings
FIG. 1 is a schematic diagram of the system for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas according to the present invention.
Detailed Description
As shown in fig. 1, the system for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas according to the present invention comprises:
a heat exchanger 10 for cooling the tail gas;
The rectifying tower 11 is used for liquefying and separating the cooled tail gas to separate heavy components from the tail gas, and is connected with the heat exchanger through a pipeline;
a sulfur dioxide product tower 12 for separating sulfur dioxide from the tail gas, which is connected with the rectifying tower through a pipeline;
The dechlorination tower 13 is used for separating the tail gas into chlorine-rich gas and is connected with the sulfur dioxide product tower through a pipeline;
A hydrogen chloride purification column 14 for separating hydrogen chloride from the tail gas is connected to the dechlorination column through a pipeline.
The system for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas further comprises a buffer gas tank 15, an adsorption device 16 and a compressor 17, wherein an air inlet of the buffer gas tank is connected with an air source of the tail gas through a pipeline, an air outlet of the buffer gas tank is connected with an air inlet of the adsorption device through a pipeline, an air outlet of the adsorption device is connected with an air inlet of the compressor through a pipeline, and an air outlet of the compressor is connected with an air inlet of a heat exchanger through a pipeline, so that the tail gas is compressed to 2bar after being dried and dehydrated through the adsorption device and then cooled by the heat exchanger.
The invention relates to a system for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas, wherein the bottom of a hydrogen chloride purifying tower is connected with a hydrogen chloride output pipe 101, and the hydrogen chloride output pipe passes through a heat exchanger so as to rewarming liquid hydrogen chloride in the hydrogen chloride output pipe through the heat exchanger to obtain hydrogen chloride gas.
The system for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas is characterized in that the top of a hydrogen chloride purifying tower is connected with a hydrogen chloride gas output pipe 102, and the hydrogen chloride gas output pipe passes through a heat exchanger so that gaseous hydrogen chloride in the hydrogen chloride gas output pipe is rewarmed through the heat exchanger.
The system for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas further comprises two sets of refrigeration systems, wherein the refrigeration systems comprise a mixed refrigerant compressor 31 and a throttle valve 32, the mixed refrigerant compressor conveys compressed gas-phase refrigerant to the throttle valve through a first pipeline, the gas-phase refrigerant returns to the mixed refrigerant compressor through a second pipeline after being throttled and cooled by the throttle valve, the gas-phase refrigerant circulates between the mixed refrigerant compressor and the throttle valve through the first pipeline and the second pipeline, the first pipeline passes through a heat exchanger, the second pipeline passes through the heat exchanger, the refrigerant in the first pipeline is cooled in the heat exchanger, and the refrigerant in the second pipeline provides cold energy in the heat exchanger.
The method for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas comprises the following steps:
Cooling the tail gas;
liquefying and separating the cooled tail gas to separate heavy components from the tail gas;
Separating sulfur dioxide from the tail gas;
Separating the tail gas to obtain chlorine-rich gas;
The tail gas is separated to obtain hydrogen chloride.
The invention discloses a method for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas, which comprises the following steps: the tail gas is dried and dehydrated by an adsorption device, compressed to 2bar and cooled by a heat exchanger.
The invention relates to a method for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas, which further comprises the following steps:
the heavy components separated from the tail gas are returned to the reaction kettle after being rewarmed by the heat exchanger;
The chlorine-rich liquid phase separated from the tail gas is sent to a synthesis kettle to be used as a synthesis raw material of chloracetyl chloride after being rewarmed by a heat exchanger;
And (3) re-heating the gas phase of hydrogen chloride separated from the tail gas by a heat exchanger to obtain raw materials for producing methyl chloride, and re-heating the liquid phase of hydrogen chloride separated from the tail gas by the heat exchanger to obtain industrial-grade or electronic-grade hydrogen chloride gas.
The invention provides a system and a method for purifying hydrogen chloride from chloroacetic acid (or chloroacetyl chloride) synthesis tail gas.
The method for purifying the hydrogen chloride from the tail gas of chloroacetic acid or chloroacetyl chloride synthesis comprises the following steps of: (1) drying; (2) compressing; (3) liquefying and separating.
The synthesis tail gas of acetic acid (or chloracetyl chloride) firstly enters into a drying process to dehydrate trace water in the tail gas, then enters into a compression process to be compressed, and then enters into a liquefaction and separation process to separate hydrogen chloride, sulfur dioxide and chlorine-rich gas. The liquefaction separation process provides refrigeration by a refrigeration system.
The technical scheme of the invention purifies the hydrogen chloride from the synthesis tail gas of chloroacetic acid (or chloroacetyl chloride), and the prepared product has high purity, simple and reliable process flow, low energy consumption and easy operation of the device. The method for purifying the hydrogen chloride from the tail gas generated in the synthesis of the chloroacetic acid or the chloroacetyl chloride has the characteristics of energy conservation, emission reduction and environmental protection.
And (3) dehydrating chloroacetic acid (or chloroacetyl chloride) synthesis tail gas through a drying process, then, compressing the tail gas to 2-15 bara in a compression process, then, entering a liquefaction and separation process, removing heavy components in the tail gas in the liquefaction and separation process, and then, sequentially separating sulfur dioxide, chlorine-rich gas and hydrogen chloride gas. Sulfur dioxide and hydrogen chloride are directly used as products, chlorine-rich gas returns to the reaction kettle to be used as reaction materials, and the cold energy of the liquefaction and separation process is provided by a refrigerating system.
The main components of the tail gas are as follows: hydrogen chloride, sulfur dioxide, chlorine, air, carbon dioxide, acetic acid, chloroacetic acid and the like.
The drying method includes a low-temperature separation method, a solution absorption method and a solid adsorption method.
The separation method is rectification separation, and the inner part of the rectifying tower is a filler or a tray.
The cold energy of the liquefaction and separation process is provided by a refrigeration cycle system and can be mixed refrigerant refrigeration, expander refrigeration and cascade refrigeration. The refrigerating temperature is 40 ℃ to minus 100 ℃.
The invention provides a system and a method for purifying hydrogen chloride from chloroacetic acid (or chloroacetyl chloride) synthesis tail gas, wherein the method takes chloroacetic acid (or chloroacetyl chloride) synthesis tail gas as a raw material, and the hydrogen chloride, sulfur dioxide and chlorine in the tail gas are recovered through drying, compressing, liquefying and separating and matched refrigeration cycle procedures, so that the emission and waste of active ingredients in the tail gas are reduced, and the added value of products is increased.
The technical scheme of the invention has the advantages that: the method can purify hydrogen chloride from chloroacetic acid (or chloroacetyl chloride) synthesis tail gas and combine sulfur dioxide, has simple process flow and easy operation, solves the problem of exhaust emission, recovers the effective components in the tail gas, increases the added value of the product, and realizes the purpose of turning harm into benefit and changing waste into valuables. The technical scheme of the invention has great significance for sustainable development of economy, ecological environment and society.
The tail gas components of this example are: air 0.16%, carbon dioxide 0.07%, hydrogen chloride 67.47%, chlorine 4.24%, and sulfur dioxide 28.06%.
The synthesis tail gas pressure from chloroacetic acid (or chloracetyl chloride) synthesis kettle is about 10kpa, after drying and dewatering by a drying tower, the synthesis tail gas enters a compression process to be compressed to 2bar, enters a cold box to be cooled to about-10 ℃, enters a separator to separate heavy components, and returns to the reaction kettle after re-heating by a heat exchanger. The separator here may also be a rectifying column. The gas phase of the separator enters a sulfur dioxide product tower, qualified sulfur dioxide products are produced at the bottom of the tower, the gas phase at the top of the tower enters a dechlorination tower, the bottom of the dechlorination tower is a liquid phase which mainly contains chlorine and contains a small amount of hydrogen chloride, and the liquid phase is sent to a synthesis kettle to be used as a synthesis raw material of chloroacetyl chloride after being rewarmed by a heat exchanger. The top of the dechlorination tower is a gas phase which takes hydrogen chloride as a main component and contains trace air, the gas phase enters a hydrogen chloride purification tower, hydrogen chloride is purified in the purification tower, industrial grade or electronic grade hydrogen chloride liquid is taken as a tower bottom, industrial grade or electronic grade hydrogen chloride gas is obtained after the temperature is recovered by a heat exchanger, and the top of the dechlorination tower is the hydrogen chloride gas containing trace air and can be used as a raw material for producing chloromethane after the temperature is recovered by the heat exchanger.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (5)
1. A system for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas, comprising:
a heat exchanger for cooling the tail gas;
The rectifying tower is used for liquefying and separating the cooled tail gas to separate heavy components from the tail gas, and is connected with the heat exchanger through a pipeline;
the sulfur dioxide product tower is used for separating sulfur dioxide from the tail gas and is connected with the rectifying tower through a pipeline;
The dechlorination tower is used for separating the tail gas into chlorine-rich gas and is connected with the sulfur dioxide product tower through a pipeline;
And the hydrogen chloride purifying tower is used for separating hydrogen chloride from the tail gas and is connected with the dechlorination tower through a pipeline.
2. The system for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas according to claim 1, further comprising a buffer gas tank, an adsorption device and a compressor, wherein an air inlet of the buffer gas tank is connected with an air source of the tail gas through a pipeline, an air outlet of the buffer gas tank is connected with an air inlet of the adsorption device through a pipeline, an air outlet of the adsorption device is connected with an air inlet of the compressor through a pipeline, and an air outlet of the compressor is connected with an air inlet of the heat exchanger through a pipeline, so that the tail gas is compressed to 2bar after being dried and dehydrated through the adsorption device and then cooled by the heat exchanger.
3. The system for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas according to claim 2, wherein the bottom of the hydrogen chloride purifying tower is connected with a hydrogen chloride output pipe, and the hydrogen chloride output pipe passes through a heat exchanger, so that liquid hydrogen chloride in the hydrogen chloride output pipe is reheated by the heat exchanger to obtain hydrogen chloride gas.
4. A system for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas according to claim 3, wherein the top of the hydrogen chloride purifying column is connected to a hydrogen chloride gas output pipe, and the hydrogen chloride gas output pipe passes through a heat exchanger, so that gaseous hydrogen chloride in the hydrogen chloride gas output pipe is re-warmed by the heat exchanger.
5. The system for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas of claim 4, further comprising two refrigeration systems, wherein the refrigeration systems comprise a mixed refrigerant compressor and a throttle valve, the mixed refrigerant compressor delivers compressed gas-phase refrigerant to the throttle valve through a first pipeline, the gas-phase refrigerant is throttled by the throttle valve and returns to the mixed refrigerant compressor through a second pipeline after being cooled, the gas-phase refrigerant circulates between the mixed refrigerant compressor and the throttle valve through the first pipeline and the second pipeline, the first pipeline passes through a heat exchanger, the second pipeline passes through the heat exchanger, the refrigerant in the first pipeline is cooled in the heat exchanger, and the refrigerant in the second pipeline provides cold in the heat exchanger.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210330291.5A CN114777421B (en) | 2022-03-31 | 2022-03-31 | System and method for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas |
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| CN202210330291.5A CN114777421B (en) | 2022-03-31 | 2022-03-31 | System and method for purifying hydrogen chloride from chloroacetic acid or chloroacetyl chloride synthesis tail gas |
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| CN114777421B true CN114777421B (en) | 2024-08-02 |
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Citations (2)
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| CN217330414U (en) * | 2022-03-31 | 2022-08-30 | 中科瑞奥能源科技股份有限公司 | System for purify hydrogen chloride in synthetic tail gas of follow chloroacetic acid or chloroacetyl chloride |
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| DE725703C (en) * | 1939-11-22 | 1942-09-29 | Ig Farbenindustrie Ag | Separation of hydrogen chloride and sulfur dioxide in gas mixtures |
| DE1618543A1 (en) * | 1967-03-31 | 1970-10-29 | Industrieforschungszentrum Che | Process for the removal of hydrogen chloride and secondary constituents that boil higher than vinyl chloride from vinyl chloride |
| DE2405813A1 (en) * | 1974-02-07 | 1975-09-04 | Basf Ag | PROCESS FOR THE SIMULTANEOUS REMOVAL OF HYDROGEN CHLORINE AND SULFUR DIOXIDE FROM GASES CONTAINING SUCH COMPOUNDS, IN PARTICULAR AIR |
| JP2726771B2 (en) * | 1991-06-06 | 1998-03-11 | 三井東圧化学株式会社 | Industrial production method of chlorine |
| US6896865B2 (en) * | 2000-04-28 | 2005-05-24 | Tosoh Corporation | Method for recovering hydrogen chloride from chlorine based waste and use of recovered hydrogen chloride |
| CN101968298B (en) * | 2010-09-27 | 2013-10-02 | 开封空分集团有限公司 | Separation and recovery device and method for argon and methane in synthetic ammonia relief gas |
| KR20130039249A (en) * | 2011-10-11 | 2013-04-19 | 홍인화학 주식회사 | A production method and production system for high purity hydrogen chloride |
| JP5906074B2 (en) * | 2011-12-08 | 2016-04-20 | 川崎重工業株式会社 | Hydrogen production system |
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| CN208911798U (en) * | 2018-09-27 | 2019-05-31 | 河北东华舰化工有限公司 | A kind of production of chloroacetic acid reduce hydrochloric acid, in acetic acid by-product sulfuric acid content device |
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| CN105148710A (en) * | 2015-09-10 | 2015-12-16 | 山东谦诚工贸科技有限公司 | Absorption method of tail gas produced in production of trichloroacetyl chloride by means of chlorination process |
| CN217330414U (en) * | 2022-03-31 | 2022-08-30 | 中科瑞奥能源科技股份有限公司 | System for purify hydrogen chloride in synthetic tail gas of follow chloroacetic acid or chloroacetyl chloride |
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