WO2018188375A1 - Procédé de récupération de dichlorométhane dans un gaz résiduaire - Google Patents

Procédé de récupération de dichlorométhane dans un gaz résiduaire Download PDF

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Publication number
WO2018188375A1
WO2018188375A1 PCT/CN2017/118042 CN2017118042W WO2018188375A1 WO 2018188375 A1 WO2018188375 A1 WO 2018188375A1 CN 2017118042 W CN2017118042 W CN 2017118042W WO 2018188375 A1 WO2018188375 A1 WO 2018188375A1
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WO
WIPO (PCT)
Prior art keywords
column
white oil
dichloromethane
tower
desorption
Prior art date
Application number
PCT/CN2017/118042
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English (en)
Chinese (zh)
Inventor
项威
来庆发
王庆云
宋兴豪
陈干英
姚红果
丁少峰
陈学青
张伟
Original Assignee
山东爱地高分子材料有限公司
石家庄工大化工设备有限公司
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Application filed by 山东爱地高分子材料有限公司, 石家庄工大化工设备有限公司 filed Critical 山东爱地高分子材料有限公司
Priority to CN201780089545.6A priority Critical patent/CN110545895A/zh
Publication of WO2018188375A1 publication Critical patent/WO2018188375A1/fr

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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
    • B01D53/14—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
    • B01D53/1487—Removing organic compounds
    • 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
    • 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
    • B01D53/1425—Regeneration of liquid absorbents
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C19/00—Acyclic saturated compounds containing halogen atoms
    • C07C19/01—Acyclic saturated compounds containing halogen atoms containing chlorine
    • C07C19/03—Chloromethanes

Definitions

  • the invention relates to a process for recovering methylene chloride in exhaust gas.
  • Dichloromethane is a commonly used organic extractant in conventional chemical extraction processes.
  • Dichloromethane has a very low boiling point of 39.8 ° C, high volatility, toxicity, and is harmful to the human central nervous system and respiratory system, and its solution is also corrosive.
  • Direct discharge of methylene chloride exhaust gas will cause greater pollution to the atmosphere, damage the operator's body and affect the environment of the surrounding residents.
  • the recovery process absorbs the methylene chloride in the exhaust gas by using a poor white oil through a dichloromethane absorption tower, and obtains an exhaust gas which can be directly discharged to the atmosphere at the top of the tower, and the absorbed white oil enters the desorption after heat exchange in the heat exchanger.
  • the tower is desorbed, and the gas phase at the top of the column is condensed to obtain a methylene chloride liquid with higher purity.
  • the depleted white oil desorbed in the bottom of the tower is preheated by the heat exchanger to the white oil and then returned to the absorption tower through the cooler.
  • the exhaust gas containing methylene chloride is introduced into the bottom of the dichloromethane absorption tower, and the lean white oil is sent to the top of the dichloromethane absorption tower.
  • the tail gas is exhausted to the atmosphere.
  • the rich white oil is sent to the desorption tower;
  • the first step of the white-rich oil is introduced into the upper part of the desorption column, and the steam at the top of the desorption column is withdrawn by a dry vacuum pump and condensed, and then refluxed, and a dichloromethane liquid is taken out, and the analyzed white oil is used.
  • the bottom of the column is recovered and then returned to the dichloromethane absorption column for reuse; the liquid feed position of the desorber is at the upper middle position of the desorption column.
  • the dichloromethane absorption column has 3-7 theoretical plates; preferably 5 theoretical plates.
  • the lean white oil has a temperature of 15-25 ° C, preferably 20 ° C; the exhaust gas has an inlet temperature of 15-25 ° C, preferably 20 ° C; and the white rich oil temperature is about 20-30 ° C, preferably 24 ° C.
  • the operating pressure of the absorption tower is atmospheric pressure.
  • the dichloromethane analytical column has 3-7 theoretical plates; preferably 5 theoretical plates.
  • the analytical column has a column temperature of 170 to 175 °C.
  • the analytical column has an operating pressure of 10 kPa.
  • the lean white oil produced from the analytical column is exchanged with the white oil before returning to the absorption tower, and the temperature of the poor white oil after heat exchange is 15-25 ° C, preferably 20 ° C.
  • Figure 1 is a flow chart showing the recovery process of methylene chloride in the unorganized exhaust gas of the present invention.
  • 1-exhaust gas 2-absorption tower gas phase cooler, 3-absorption tower, 4-rich white oil, 5-tail gas, 6-stage heat exchanger, 7-secondary heat exchanger, 8-desorption tower , 9-dry vacuum pump, 10-dichloromethane condenser, 11-dichloromethane, 12-lean white oil, 13-desorbed column cooler, 14-absorbent liquid cooler.
  • the exhaust gas containing methylene chloride is introduced into the bottom of the dichloromethane absorption tower through a Roots blower, and the lean white oil with higher purity is sent to the top of the dichloromethane absorption tower, and the two phases are countercurrently contacted in the column, and the exhaust gas is exhausted.
  • the methylene chloride is absorbed by the white oil, the exhaust gas is discharged into the atmosphere, and the white oil in the tower is sent to the desorption column.
  • the absorption efficiency of the dichloromethane in this step is about 90%.
  • the dichloromethane absorption tower has a total of five theoretical trays, the operating pressure is normal pressure, the temperature of the absorbent white oil is about 20 ° C, the inlet temperature of the exhaust gas is about 20 ° C, and the temperature of the absorption liquid of the tower is about 24 ° C.
  • the steam at the top of the desorbing tower is extracted by a dry vacuum pump and condensed, and then a dichloromethane liquid is taken out, and the (white oil) of the tower is used for methylene chloride.
  • the absorption tower bottom liquid (white oil) is preheated and then cooled to 20 ° C and returned to the dichloromethane absorption tower for reuse.
  • the desorption tower has a total of 5 theoretical trays, the operating pressure is about 10 kPa, and the liquid feed position of the desorption column is at the upper middle position of the entire desorption column, and the pot temperature is 170-175 ° C.
  • the exhaust gas 1 from the workshop is cooled by the absorption tower vapor cooler 2 and then enters the bottom of the absorption tower 3.
  • the depleted white oil 12 desorbed by the desorption column 8 enters the top of the absorption tower 3, and the two-phase stream is countercurrently contacted in the absorption tower 3.
  • the methylene chloride is absorbed by the absorption liquid white oil to form a white oil 4, and the absorbed tail gas 5 can be discharged into the atmosphere.
  • the white oil 4 is heated by the primary heat exchanger 6 and the secondary heat exchanger 7 to enter the upper middle portion of the desorption column 8, and the gas phase at the top of the desorption column 8 is withdrawn by a dry vacuum pump 9 and then condensed by dichloromethane.
  • the condensate 11 is condensed, and the obtained condensate 11 is a recovered dichloromethane solution; a part of the tower liquid of the desorbing tower 8 is heated to be vaporized by the reboiler and returned to the tower of the desorbing tower 8, and another part of the high temperature lean white oil 12 is passed through two.
  • the heat exchanger 7 and the first-stage heat exchanger 6 exchange heat with the tower liquid-rich white oil 4 of the absorption tower 3, and are cooled as an absorption liquid after being cooled by the analytical tower cooler 13 and the absorption tower liquid-cooler 14.
  • Tower 3 is again absorbed.
  • the entire system absorbs liquid to form a circulation, which minimizes the consumption of the absorption liquid.
  • the main substances in the exhaust gas in the present invention are dichloromethane, air, traces of water vapor and the like.
  • the equipment used in the recycling process of the invention adopts an advanced thermal coupling process, has low energy consumption, high recovery rate, low pollution, and the absorbent can be recycled and used, thereby reducing economic costs.
  • the concentration of methylene chloride in the exhaust gas 1 was 0.35 mg/ml, and the rest was air; the mass percentage of the white oil in the absorbent white oil 12 was 99.9%, and the percentage of dichloromethane was 0.1%.
  • the exhaust gas 1 is sent to the bottom of the absorption tower 3, and the poor white oil 12 is sent to the top of the absorption tower 3, and the two phases are absorbed by countercurrent contact in the column.
  • tail gas 5 having a methylene chloride concentration of less than 0.035 mg/ml was obtained, and in the column, a tower liquid white oil 4 having a mass percentage of dichloromethane of 2.2% was obtained, and the white oil 4 was sent to the desorption column 8.
  • the white oil 4 is exchanged with the secondary heat exchanger 7 through the primary heat exchanger 6 and sent to the upper part of the desorption column 8, and is sucked into the dichlorobenzene by the dry vacuum pump 9 at the top of the desorption column 8.
  • the methane condenser 10 was condensed to give a mass percentage of 99.9% of methylene chloride 11.
  • an absorbent lean white oil 12 having a mass percentage of 99.9% was obtained.
  • the poor white oil 12 exchanges the white oil 4 and then enters the bottom of the absorption tower 3 again to form a cycle.
  • the absorption tower 3 has a diameter of 600 mm, a total of five theoretical trays, and is operated at atmospheric pressure.
  • the feed position of the absorbing liquid lean white oil 12 is in the first theoretical tray, the feed temperature is 20 ° C, and the exhaust gas 1
  • the feed position is in the tower, and the inlet temperature is about 20 °C.
  • the temperature at the top of the column is 20 ° C, and the temperature in the column is about 23 ° C.
  • the absorption efficiency of the absorption tower 3 is 90%.
  • the desorption column 8 has a diameter of 400 mm, a total of 5 theoretical plates, a reduced pressure operation, an operating pressure of -0.09 MPa, a liquid feed position in the first theoretical plate, a liquid feed temperature of 120 ° C, and a column top temperature of 50 ° C.
  • the temperature of the column was 170 °C.
  • the mass percentage of methylene chloride at the top of the column was 99.9%, and the mass percentage of the lean white oil in the column was 99.9%.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Treating Waste Gases (AREA)
  • Gas Separation By Absorption (AREA)

Abstract

L'invention concerne un processus de récupération de dichlorométhane dans un gaz résiduaire, comprenant les étapes spécifiques de : étape I, du gaz résiduaire contenant du dichlorométhane (1) est introduit dans le fond d'une tour d'absorption de dichlorométhane (3), une huile blanche appauvrie (12) est envoyée au sommet de la tour d'absorption de dichlorométhane (3), après un contact à contre-courant des deux phases dans la tour, un gaz d'échappement (5) provenant du sommet de la tour est déchargé vers l'atmosphère, et de l'huile blanche enrichie (4) est envoyée dans une tour de désorption (8); étape II, l'huile blanche enrichie (4) issue de l'étape I est introduite dans la partie supérieure de la tour de désorption (8), de la vapeur dans la partie supérieure de la tour de désorption (8) est retirée par une pompe à vide sèche (9) et chauffé au reflux après condensation, et un liquide de dichlorométhane (11) est récupéré, l'huile blanche appauvrie désorbée (12) est utilisée pour préchauffer l'huile blanche enrichie (4), puis refroidie à 20 °C et renvoyée à la tour d'absorption de dichlorométhane (3) à recycler.
PCT/CN2017/118042 2017-04-14 2017-12-22 Procédé de récupération de dichlorométhane dans un gaz résiduaire WO2018188375A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201780089545.6A CN110545895A (zh) 2017-04-14 2017-12-22 一种废气中二氯甲烷的回收工艺

Applications Claiming Priority (2)

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CN201710247188.3 2017-04-14
CN201710247188 2017-04-14

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Cited By (2)

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CN114225652A (zh) * 2021-12-08 2022-03-25 华南理工大学 一种无补充吸收剂的石油吸收稳定工艺及石油炼化设备
CN115382352A (zh) * 2021-05-25 2022-11-25 浙江毅聚新材料有限公司 含二氯甲烷废气的二氯甲烷回收工艺和回收系统

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CN111689834A (zh) * 2020-07-06 2020-09-22 中材锂膜有限公司 一种湿法锂电池隔膜萃取液分离节能装置
CN114225651A (zh) * 2021-11-23 2022-03-25 安徽金禾实业股份有限公司 一种三氯蔗糖酯化溶剂环己烷回收装置及方法
CN115501723B (zh) * 2022-09-29 2023-11-03 山东海科创新研究院有限公司 一种一氯甲烷废气的回收方法
CN116392931A (zh) * 2023-05-15 2023-07-07 盐城优和博新材料有限公司 一种超高强度聚乙烯纤维生产尾气处理系统及方法

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CN204121940U (zh) * 2014-11-07 2015-01-28 清本环保工程(杭州)有限公司 感光膜印刷中气体处理系统
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CN1962028A (zh) * 2006-10-26 2007-05-16 清华大学 一种废气中二氯甲烷的回收方法
CN203556260U (zh) * 2013-10-28 2014-04-23 张桂华 废水或废气中易挥发有机溶剂的回收装置
JP2015112561A (ja) * 2013-12-12 2015-06-22 学校法人慶應義塾 Ｖｏｃ除去装置、ｖｏｃ除去システム、ｖｏｃ除去方法およびｖｏｃ除去用除去液
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115382352A (zh) * 2021-05-25 2022-11-25 浙江毅聚新材料有限公司 含二氯甲烷废气的二氯甲烷回收工艺和回收系统
CN114225652A (zh) * 2021-12-08 2022-03-25 华南理工大学 一种无补充吸收剂的石油吸收稳定工艺及石油炼化设备
CN114225652B (zh) * 2021-12-08 2022-10-25 华南理工大学 一种无补充吸收剂的石油吸收稳定工艺及石油炼化设备

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CN108722117A (zh) 2018-11-02

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