CN106390692A - Recycling device of acyl chloride tail gas - Google Patents

Recycling device of acyl chloride tail gas Download PDF

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Publication number
CN106390692A
CN106390692A CN201611049110.2A CN201611049110A CN106390692A CN 106390692 A CN106390692 A CN 106390692A CN 201611049110 A CN201611049110 A CN 201611049110A CN 106390692 A CN106390692 A CN 106390692A
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China
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tail gas
hydrochloric acid
tower
condenser
falling
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CN201611049110.2A
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Chinese (zh)
Inventor
陈仁
邹远龙
刘文清
商雷
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HUBEI BIOCHEM PHARMACEUTICAL TECHNOLOGY Co Ltd
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HUBEI BIOCHEM PHARMACEUTICAL TECHNOLOGY Co Ltd
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Priority to CN201611049110.2A priority Critical patent/CN106390692A/en
Publication of CN106390692A publication Critical patent/CN106390692A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
    • B01D5/0033—Other features
    • B01D5/0036—Multiple-effect condensation; Fractional condensation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
    • B01D5/0057—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/1406—Multiple stage absorption
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/1418—Recovery of products
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/1456—Removing acid components
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/1493—Selection of liquid materials for use as absorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/18—Absorbing units; Liquid distributors therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
    • B01D53/225—Multiple stage diffusion
    • B01D53/226—Multiple stage diffusion in serial connexion
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
    • B01D53/229—Integrated processes (Diffusion and at least one other process, e.g. adsorption, absorption)
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08—Materials not undergoing a change of physical state when used
    • C09K5/10—Liquid materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
    • B01D2053/221—Devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
    • B01D2252/10—Inorganic absorbents
    • B01D2252/103—Water
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/20—Halogens or halogen compounds
    • B01D2257/204—Inorganic halogen compounds
    • B01D2257/2045—Hydrochloric acid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/02—Other waste gases

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Physics & Mathematics (AREA)
  • Combustion & Propulsion (AREA)
  • Thermal Sciences (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Gas Separation By Absorption (AREA)

Abstract

The invention provides a recycling device of acyl chloride tail gas. Hydrogen chloride gas in the acyl chloride tail gas is recycled, and a hydrochloric acid solution in a cryohydrate system is prepared through taking hydrochloric acid and calcium carbonate to react, so that the tail gas is reutilized and the tail gas reaches emission requirements. The recycling device of the acyl chloride tail gas is simple in structure and ingenious in design and is used for recycling the hydrogen chloride gas in the acyl chloride tail gas; after the hydrogen chloride is absorbed through a three-grade falling film tower and is further absorbed through increasing an absorption area by a packed column to obtain the hydrochloric acid solution with the concentration of about 30 percent; the generated hydrochloric acid reacts with the calcium carbonate and a generated calcium carbonate solution is used as a cooling agent in the cryohydrate system, so that the safety is guaranteed; meanwhile, the hydrogen chloride gas in the tail gas is treated and can meet environment-friendly requirements; the production efficiency is improved and the production cost is reduced at the same time.

Description

A kind of recycle device of acyl chlorides tail gas
Technical field
The present invention relates to chemical industry tail gas processing technology field, specifically a kind of recycle device of acyl chlorides tail gas.
Background technology
Acyl chlorides is a kind of important carboxylic acid derivates, suffers from important application at aspects such as organic synthesis, pharmaceutical synthesis. At present, preparing acyl chlorides most common method has thionyl chloride, phosphorus trichloride, phosphorus pentachloride and triphosgene etc., due to thionyl chloride Synthesis acyl chlorides has the advantages of reaction condition is gentle, at normal temperatures or heating slightly can be reacted, and purity is good, yield is high, wide Large enterprises widely use.But there is also problem during thionyl chloride synthesis acyl chlorides, during thionyl chloride synthesis acyl chlorides Unavoidably create hydrogen chloride gas, result in vent gas treatment costly.Hydrogen chloride and vapor in the atmosphere combine shape The hydrochloric acid mist aerosol becoming, has severe corrosive, corrodes metal, corrodes construction material, damages the art work, so that material is faded, Cause economy, property loss.Human contact, to hydrogen chloride gas, has strong impulse, can corrode skin and mucous membrane, lead to sound Sound is hoarse, schneiderian membrane ulcer, and cornea is muddy, and chest is had a pain, and has sensation of asphyxia, until spitting blood, pulmonary edema in severe patient for cough So that it is dead.Slow poisoning can cause respiratory inflammation, tooth acid corrosion, rhinitis, the illness such as perforation of nasal septum and stomach, enteritis.
At present, process the hydrogen chloride gas producing in acyl chlorides production process and mainly absorbed using water and obtain hydrochloric acid, more right Hydrochloric acid carries out subsequent treatment, and used in cryosel system, cooling agent is mainly purchase calcium chloride or ethylene glycol, due to hydrochloric acid Subsequent treatment and purchase refrigerant are required to put into substantial amounts of fund, and because ethylene glycol is poisonous, thus when using, ethylene glycol exists Safety problem.Therefore, research and develop a kind of recycle device of acyl chlorides tail gas to have great importance.
Content of the invention
Present invention aim to solving existing acyl chlorides vent gas treatment have such problems as that high cost, security are poor, carry For a kind of recycle device of acyl chlorides tail gas.
The concrete scheme of the present invention is：Including falling-film tower, packed tower, condensing tower, air-introduced machine, hydrochloric acid tank, reactor, ice Salt system, rectifying still, the first condenser pipe, the second condenser and reception tank, described acyl chlorides tail gas sequentially passes through three series connection and fills The stage falling-film tower of water, two grades of falling-film towers and three-level falling-film tower, the hydrogen chloride gas in acyl chlorides tail gas are in three falling-film towers Water absorb after obtain hydrochloric acid solution, the offgas outlet of described three-level falling-film tower bottom is connected with the bottom of described filler tower, institute The entrance at the top and condensing tower of stating packed tower connects, and the outlet of condensing tower is connected with described air-introduced machine, and remaining tail gas passes through Air-introduced machine is discharged after extracting out, hydrochloric acid solution through being pumped into described hydrochloric acid tank, the outlet of hydrochloric acid tank and described reaction One dog-house connection of kettle, calcium carbonate puts into from another dog-house of reactor, and hydrochloric acid solution is generated with calcium carbonate reaction Calcium chloride solution enter described cryosel system from the bottom of reactor, the outlet of described acyl chlorides rectifying still and the first condenser Connection, the first condenser is connected with described second condenser, and the bottom of the second condenser is connected with the entrance receiving tank, described ice Salt system is connected with the entrance of the second condenser pipe cooling agent by pump, the outlet of described second condenser pipe cooling agent and cryosel system Connection.
Heretofore described air-introduced machine is polypropylene air-introduced machine.
The operation principle of the present invention is：Described acyl chlorides tail gas sequentially pass through three series connection fill the stage falling-film tower of water, two Level falling-film tower and three-level falling-film tower, the hydrogen chloride gas in acyl chlorides tail gas obtain hydrochloric acid after the water in three falling-film towers absorbs Solution, the offgas outlet of three-level falling-film tower bottom is connected with the bottom of described filler tower, and acyl chlorides tail gas is further through packed tower After absorption, remaining tail gas enters condensing tower from the top of packed tower, then discharges after air-introduced machine is extracted out, hydrochloric acid solution warp Cross and be pumped in hydrochloric acid tank, described hydrochloric acid tank is connected with a dog-house of reactor, and described calcium carbonate is from reactor Another dog-house puts into, and the calcium chloride solution that hydrochloric acid solution is generated with calcium carbonate reaction enters in cryosel system by pipeline, In acyl chlorides rectifying still, rectifying acyl chlorides out enters after passing sequentially through two condensing tube condensations connected and receives in tank, described cryosel Cryosel solution in system is passed through in the second condenser pipe by pump and recycles.
Present configuration is simple, and design is ingenious, recycles the hydrogen chloride gas in acyl chlorides tail gas, hydrogen chloride is through three-level After falling-film tower absorbs, after packed tower increase absorption area absorbs further, obtain 30% about hydrochloric acid solution, using life The hydrochloric acid becoming and calcium carbonate reaction, as the cooling agent in cryosel system, security is ensured the calcium chloride solution of generation, Hydrogen chloride gas in tail gas disclosure satisfy that environmental requirement after treatment simultaneously, reduces production while improve production efficiency Cost.
Brief description
Fig. 1 is the structural representation of the present invention；
Wherein：1- first falling-film tower, 2- second falling-film tower, 3- the 3rd falling-film tower, 4- packed tower, 5- condensing tower, 6- air-introduced machine, 7- Hydrochloric acid tank, 8- reactor, 9- cryosel system, 10- rectifying still, 11- first condenser pipe, 12- second condenser pipe, 13- receives tank.
Specific embodiment
Referring to Fig. 1, a kind of recycle device of acyl chlorides tail gas of the present embodiment, including falling-film tower, packed tower 4, condensation Tower 5, air-introduced machine 6, hydrochloric acid tank 7, reactor 8, cryosel system 9, rectifying still 10, the first condenser pipe 11, the second condenser 12 and Receive tank 13, described acyl chlorides tail gas sequentially passes through 1, two grades of falling-film towers 2 of stage falling-film tower and the three-level fall that three series connection fill water Film tower 3, the hydrogen chloride gas in acyl chlorides tail gas obtain hydrochloric acid solution after the water in three falling-film towers absorbs, described three-level fall The offgas outlet of film tower 3 bottom is connected with the bottom of described filler tower 4, and the top of described filler tower 4 is connected with the entrance of condensing tower 5 Logical, the outlet of condensing tower 5 is connected with described air-introduced machine 6, and remaining tail gas is discharged after air-introduced machine 6 extraction, hydrochloric acid solution warp Cross and be pumped into described hydrochloric acid tank 7, the outlet of hydrochloric acid tank 7 is connected with a dog-house of described reactor 8, calcium carbonate Put into from another dog-house of reactor 8, the calcium chloride solution that hydrochloric acid solution is generated with calcium carbonate reaction is from the bottom of reactor 8 Portion enters in described cryosel system 9, and the outlet of described acyl chlorides rectifying still 10 connects with the first condenser 11, the first condenser 11 and Described second condenser 12 is connected, and the bottom of the second condenser 12 is connected with the entrance receiving tank 13, and described cryosel system 9 is passed through Pump is connected with the entrance of the second condenser pipe 12 cooling agent, and the outlet of described second condenser pipe 12 cooling agent is connected with cryosel system 9.
Air-introduced machine 6 described in the present embodiment is polypropylene air-introduced machine.

Claims (2)

1. a kind of recycle device of acyl chlorides tail gas, including falling-film tower, packed tower, condensing tower, air-introduced machine, hydrochloric acid tank, anti- Answer kettle, cryosel system, rectifying still, the first condenser pipe, the second condenser and receive tank, it is characterized in that：Described acyl chlorides tail gas is successively Fill stage falling-film tower, two grades of falling-film towers and the three-level falling-film tower of water, the hydrogen chloride gas in acyl chlorides tail gas through three series connection Obtain hydrochloric acid solution, the offgas outlet of described three-level falling-film tower bottom and described filler after the water in three falling-film towers absorbs The bottom connection of tower, the top of packed tower is connected with the entrance of condensing tower, and the outlet of condensing tower is connected with described air-introduced machine, remaining Tail gas discharge after air-introduced machine extraction, hydrochloric acid solution through being pumped into described hydrochloric acid tank, the outlet of hydrochloric acid tank Connect with a dog-house of described reactor, calcium carbonate is from another dog-house input, hydrochloric acid solution and the carbonic acid of reactor Calcium reaction generate calcium chloride solution from the bottom of reactor enter described cryosel system, the outlet of described acyl chlorides rectifying still with First condenser connection, the first condenser is connected with described second condenser, the entrance of the bottom of the second condenser and reception tank It is connected, described cryosel system is connected with the entrance of the second condenser pipe cooling agent by pump, the going out of described second condenser pipe cooling agent Mouth and cryosel system connectivity.
2. a kind of recycle device of acyl chlorides tail gas according to claim 1, is characterized in that：Described air-introduced machine is poly- third Alkene air-introduced machine.
CN201611049110.2A 2016-11-25 2016-11-25 Recycling device of acyl chloride tail gas Pending CN106390692A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107930366A (en) * 2017-11-30 2018-04-20 山东凯盛新材料股份有限公司 The technique that thionyl chloride integrates treating tail gas
CN107983090A (en) * 2017-11-30 2018-05-04 山东凯盛新材料股份有限公司 The technique of the acyl chlorides tail gas comprehensive regulation
CN107998857A (en) * 2017-11-30 2018-05-08 山东凯盛新材料股份有限公司 The technique of the thionyl chloride tail gas comprehensive regulation
CN109368601A (en) * 2018-11-23 2019-02-22 山东凯盛新材料股份有限公司 Between/device and method of paraphthaloyl chloride End gas production chlorosulfonic acid
CN110508092A (en) * 2019-09-27 2019-11-29 唐山三友氯碱有限责任公司 Tai gas of rectifying processing system and its automatic running pattern in production of vinyl chloride by calcium carbide method production technology
CN112370942A (en) * 2020-11-02 2021-02-19 江苏春江润田农化有限公司 Hydrogen chloride and sulfur dioxide mixed tail gas separation device

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN200964388Y (en) * 2006-10-28 2007-10-24 周烜 Preparation device for acetyl chloride cogeneration hydroxyl ethidene diphosphoric acid
CN202569628U (en) * 2012-04-01 2012-12-05 东力（南通）化工有限公司 High safety rectification condensing unit
CN102989265A (en) * 2012-12-13 2013-03-27 烟台泰和新材料股份有限公司 Treatment method of acyl chloride production tail gas
CN204824150U (en) * 2015-07-15 2015-12-02 陕西天宏硅材料有限责任公司 A continuous recovery processing device that is arranged in polycrystalline silicon production hydrogen chloride
CN206184224U (en) * 2016-11-25 2017-05-24 湖北博凯医药科技有限公司 Recycle device of acyl chlorides tail gas

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN200964388Y (en) * 2006-10-28 2007-10-24 周烜 Preparation device for acetyl chloride cogeneration hydroxyl ethidene diphosphoric acid
CN202569628U (en) * 2012-04-01 2012-12-05 东力（南通）化工有限公司 High safety rectification condensing unit
CN102989265A (en) * 2012-12-13 2013-03-27 烟台泰和新材料股份有限公司 Treatment method of acyl chloride production tail gas
CN204824150U (en) * 2015-07-15 2015-12-02 陕西天宏硅材料有限责任公司 A continuous recovery processing device that is arranged in polycrystalline silicon production hydrogen chloride
CN206184224U (en) * 2016-11-25 2017-05-24 湖北博凯医药科技有限公司 Recycle device of acyl chlorides tail gas

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107930366A (en) * 2017-11-30 2018-04-20 山东凯盛新材料股份有限公司 The technique that thionyl chloride integrates treating tail gas
CN107983090A (en) * 2017-11-30 2018-05-04 山东凯盛新材料股份有限公司 The technique of the acyl chlorides tail gas comprehensive regulation
CN107998857A (en) * 2017-11-30 2018-05-08 山东凯盛新材料股份有限公司 The technique of the thionyl chloride tail gas comprehensive regulation
CN109368601A (en) * 2018-11-23 2019-02-22 山东凯盛新材料股份有限公司 Between/device and method of paraphthaloyl chloride End gas production chlorosulfonic acid
CN109368601B (en) * 2018-11-23 2023-08-01 山东凯盛新材料股份有限公司 Device and method for producing chlorosulfonic acid from m/p-phthaloyl chloride tail gas
CN110508092A (en) * 2019-09-27 2019-11-29 唐山三友氯碱有限责任公司 Tai gas of rectifying processing system and its automatic running pattern in production of vinyl chloride by calcium carbide method production technology
CN110508092B (en) * 2019-09-27 2021-05-28 唐山三友氯碱有限责任公司 Rectification tail gas treatment system in calcium carbide method chloroethylene production process and automatic operation mode thereof
CN112370942A (en) * 2020-11-02 2021-02-19 江苏春江润田农化有限公司 Hydrogen chloride and sulfur dioxide mixed tail gas separation device

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