WO2022016631A1 - D-d混剂精馏分离工艺 - Google Patents

D-d混剂精馏分离工艺 Download PDF

Info

Publication number
WO2022016631A1
WO2022016631A1 PCT/CN2020/108858 CN2020108858W WO2022016631A1 WO 2022016631 A1 WO2022016631 A1 WO 2022016631A1 CN 2020108858 W CN2020108858 W CN 2020108858W WO 2022016631 A1 WO2022016631 A1 WO 2022016631A1
Authority
WO
WIPO (PCT)
Prior art keywords
tower
light
dichloropropene
finished product
sent
Prior art date
Application number
PCT/CN2020/108858
Other languages
English (en)
French (fr)
Inventor
薄纯金
宋朋斌
张延军
王国力
Original Assignee
山东海益化工科技有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 山东海益化工科技有限公司 filed Critical 山东海益化工科技有限公司
Publication of WO2022016631A1 publication Critical patent/WO2022016631A1/zh

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C17/00Preparation of halogenated hydrocarbons
    • C07C17/38Separation; Purification; Stabilisation; Use of additives
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C17/00Preparation of halogenated hydrocarbons
    • C07C17/38Separation; Purification; Stabilisation; Use of additives
    • C07C17/383Separation; Purification; Stabilisation; Use of additives by distillation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07BGENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
    • C07B2200/00Indexing scheme relating to specific properties of organic compounds
    • C07B2200/07Optical isomers

Definitions

  • the invention relates to the technical field of chemical rectification and separation processes, in particular to a D-D mixture rectification and separation process.
  • propylene and chlorine are generally reacted to produce propylene chloride.
  • the main product is propylene chloride, and by-products DD mixture and hydrochloric acid are also produced.
  • DD mixture is directly sold as a by-product, and the product value is not Therefore, how to carry out rectification and separation of DD mixture to obtain a usable product with higher value and purity has become a technical problem to be solved urgently.
  • the present invention aims to solve at least one of the technical problems existing in the prior art or related technologies.
  • the object of the present invention is to provide a kind of DD mixture rectification and separation process, can separate the by-product DD mixture obtained from the bottom of the propylene chloride refining process tower, so that 1,2-dichloropropane and light components can be mixed and recovered.
  • the product purity of cis-1,3-dichloropropene, trans-1,3-dichloropropene, cis-1,3-dichloropropene and trans-1,3-dichloropropene can reach more than 95%, and in trans-1,3-dichloropropene
  • the content of cis-1,3-dichloropropene in the product of formula 1,3-dichloropropene is not more than 0.5%.
  • the technical scheme of the present invention provides a D-D mixture rectification separation process, comprising the following steps:
  • the process mother liquor DD mixture obtained from the column bottom of the purification process of allyl chloride is sent to the weight-removing tower, heated by steam in the reboiler at the bottom of the tower, and the easily carbonized heavy components in the process mother liquor DD mixture are lighter than their light weight.
  • the components are separated by mass transfer in the weight-removing tower;
  • the vapor phase of dichloropropene and light components is controlled to flow back through the partial condenser at the top of the tower, and the non-condensable gas phase is directly sent to the light-removing tower, and the heavy components at the bottom of the weight-removing tower are sent to the rear section for processing;
  • the non-condensable gas phase at the top of the weight-removing tower is fed into the light-removing tower, heated by steam in the bottom reboiler of the weight-removing tower, and the dichloropropane and light components are mixed with dichloropropane.
  • Propylene chloride is mass-transferred and separated in the light-removing tower;
  • Dichloropropane and light component evaporated gas phase arrive at the top of the light-removing tower and are cooled by the condenser, and the condensate enters the reflux tank, and part of it is sent to the tower for reflux, and part is sent to the warehouse for storage after cooling.
  • the material is sent to the finished tower;
  • the bottom material of the delight tower is sent to the finished product tower, and after the bottom reboiler of the finished product tower is heated by steam, cis and trans 1,3 dichloropropenes are stored in the finished product tower.
  • Mass transfer separation the vapor phase of cis-1,3-dichloropropene reaches the top of the finished product tower and is cooled by the condenser, the condensate enters the cis-tank, part of it is sent to the tower for reflux, and part of it is continuously distilled from the top of the tower.
  • the trans-1,3-dichloropropene is extracted from the lower side line of the finished product tower, sent to the trans-type tank after cooling, and then sent to the trans-type finished product tank for storage.
  • the heavy component residue at the bottom of the finished tower is intermittently discharged to Residual tank.
  • the temperature at the bottom of the weight removal tower is 108°C
  • the temperature at the top of the tower is 70.5°C
  • the pressure at the bottom of the tower is 45KPa
  • the pressure at the top of the tower is 35KPa.
  • the temperature at the bottom of the light stripping tower is 81°C
  • the temperature at the top of the tower is 59.1°C
  • the pressure at the bottom of the tower is 44KPa
  • the pressure at the top of the tower is 32KPa.
  • the temperature at the bottom of the finished tower is 80°C
  • the temperature at the top of the tower is 64°C
  • the pressure at the bottom of the tower is 37KPa
  • the pressure at the top of the tower is 25KPa.
  • the process mother liquor D-D mixture is heated by a preheater with system waste heat and then sent to the weight removal tower.
  • the bottom reboilers of the weight removal tower, the light removal tower and the finished product tower are heated by steam PID automatic temperature control, and the heating medium is saturated steam with a pressure of 0.7 MPa.
  • the cooling medium is demineralized water at 30°C, and the water supply pressure is 0.4-0.6 MPa.
  • the DD mixture rectification separation process adopts three-column continuous, pressure-changing operation and side extraction, which not only has high product purity, but also is more energy-saving.
  • the tower can make full use of the thermal energy of the existing production system, which not only further saves energy, but also improves the separation efficiency of the process mother liquor DD mixture in the weight removal tower.
  • the invention discloses a D-D mixture rectification separation process, and those skilled in the art can learn from the content of this article and appropriately improve the process parameters to achieve. It should be particularly pointed out that all similar substitutions and modifications are obvious to those skilled in the art, and they are deemed to be included in the present invention.
  • the method and application of the present invention have been described through the preferred embodiments, and it is obvious that relevant persons can make changes or appropriate changes and combinations of the methods and applications described herein without departing from the content, spirit and scope of the present invention to achieve and Apply the technology of the present invention.
  • the main product is chloropropene, and by-products DD mixture and hydrochloric acid will also be produced.
  • the components of the process mother liquor DD mixture are generally: light component + dichloropropane 50.9%, cis-1,3-dichloropropene 19.5%, anti-1 , 3 dichloropropene 19%, heavy components 10.6%.
  • the process mother liquor DD mixture obtained from the column bottom of the chloropropene purification process is sent to the weight-removing tower, and the reboiler steam heating at the bottom of the tower is carried out, and the easily carbonized heavy components in the process mother liquor DD mixture Mass transfer and separation of its light components in the weight removal tower;
  • the flow rate of the process mother liquor DD mixture is 2100kg/h
  • the components are generally: light components + dichloropropane 50.9%, cis-1,3-dichloropropene 19.5%, trans-1,3-dichloropropene 19%, recombination 10.6%;
  • the tower top pressure of the weight-removing tower is 35KPa, the tower bottom pressure is 45KPa, the tower top temperature is 70.5°C, and the tower bottom temperature is 108°C.
  • the non-condensable gas phase at the top of the weight-removing tower is directly sent to the light-removing tower, and the gas phase separation condensation technology is adopted, which is more energy-saving and can save energy by more than 20%.
  • the top temperature was 59.1°C and the column bottom temperature was 81°C.
  • the condensers there are two condensers, part of the condensate entering the reflux tank is cooled by the cooler and then sent to the warehouse for storage, and the flow rate of dichloropropane and light components distilled from the top of the delight tower is 1070kg/h, and the composition includes Light components + dichloropropane 99.5%, cis 1,3 dichloropropene 0.5%.
  • the bottom material of the light-removing tower is sent to the finished product tower, and after the bottom reboiler of the finished product tower is heated by steam, cis- and trans-1,3-dichloropropene is mass-transferred in the finished product tower Separation, the vapor phase of cis 1,3 dichloropropene reaches the top of the finished tower and is cooled by the condenser, the condensate enters the cis tank, part of it is sent to the tower for reflux, and part is continuously distilled from the top of the tower. After cooling, it is sent to the cis tank. Storage of finished cans;
  • the condensers there are two condensers. Part of the condensate entering the cis tank is cooled by the cooler and sent to the cis finished product tank for storage.
  • the top pressure of the finished tower is 25KPa
  • the bottom pressure is 37KPa
  • the top temperature is 64°C
  • the temperature at the bottom of the tower is 80°C
  • the flow rate of the cis-products distilled from the top of the finished tower is 409kg/h
  • the composition includes light components + dichloropropane 2.5%, cis-1,3-dichloropropene 95.5%, trans- 1,3 Dichloropropene 2%.
  • S112 extract the trans-1,3-dichloropropene from the lower side line of the finished product tower, send it to the trans-type tank after cooling, and then send it to the trans-type finished product tank for storage, and the residual liquid of the heavy components at the bottom of the finished product tower is intermittently discharged to the residual liquid Can.
  • the cooler is used to cool down, and the flow rate of the trans-finished product from the side line at the lower part of the finished product tower is 385kg/h, and the composition includes cis-1,3-dichloropropene 0.5%, trans-1,3-dichloropropene 98%, and heavy components 1.5%,
  • the flow rate of the residual liquid of the heavy component at the bottom of the tower is 236 kg/h, and the composition includes 5% of trans-1,3 dichloropropene and 95% of the heavy component.
  • the heavy components in the process mother liquor DD mixture are first removed by the weight removal tower, and then the dichloropropane and light component impurities are separated from the top through the light removal tower, which can be recycled, and the materials at the bottom of the light removal tower enter the
  • the finished tower carries out mass transfer separation to obtain cis-1,3-dichloropropene and trans-1,3-dichloropropene, the product purity of which can reach more than 95%, and the cis-1,3-dichloropropene in the trans-1,3-dichloropropene product
  • the content of formula 1,3 dichloropropene is not more than 0.5%, which improves the product value.
  • the D-D mixture rectification separation process adopts three-column continuous, pressure swing operation and side extraction, which not only has high product purity, but also is more energy-saving.
  • process mother liquor D-D mixture is heated by the system waste heat by the preheater and then sent to the weight-removing tower.
  • the bottom reboilers of the weight-removing tower, the light-removing tower and the finished product tower are heated by steam PID automatic temperature control, and the heating medium is saturated steam with a pressure of 0.7MPa.
  • the cooling medium is demineralized water at 30°C, and the water supply pressure is 0.4-0.6MPa.
  • the process mother liquor DD mixture is heated by the preheater and then sent to the weight removal tower, making full use of the thermal energy of the existing production system, which not only further saves energy, but also improves the separation of the process mother liquor DD mixture in the weight removal tower. efficient.
  • the temperature control is more accurate and energy saving.
  • Two condensers are set up to further ensure the condensation effect. On the whole, the rectification separation effect is further improved and energy is saved.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

一种D-D混剂精馏分离工艺,包括以下步骤:工艺母液D-D混剂中的易碳化重组分与其轻组分在脱重塔内传质分离;二氯丙烯及轻组分蒸发气相经塔顶分凝器控制回流,不凝气相直接送入脱轻塔;二氯丙烷及轻组分与二氯丙烯在脱轻塔内传质分离;二氯丙烷及轻组分蒸发气相到达脱轻塔的塔顶被冷却,脱轻塔的塔底物料送入成品塔;将脱轻塔的的塔底物料送入成品塔,顺、反式1,3二氯丙烯在成品塔内传质分离,顺式1,3二氯丙烯蒸发气相到达成品塔的塔顶被冷却进入顺式罐;从成品塔下部侧线采出反式1,3二氯丙烯。该工艺采用三塔连续、变压操作以及侧线采出,产品纯度高,更加节能,顺式和反式1,3二氯丙烯产品纯度均可达到95%以上。

Description

D-D混剂精馏分离工艺 技术领域
本发明涉及化工精馏分离工艺技术领域,具体而言,涉及一种D-D混剂精馏分离工艺。
背景技术
在氯丙烯生产工艺中,一般利用丙烯和氯气反应生产氯丙烯,在氯丙烯生产过程中主要产品是氯丙烯,还会产生副产品D-D混剂及盐酸,D-D混剂作为副产品直接出售,产品价值不高,利用率较低,因此如何将D-D混剂进行精馏分离得到价值和纯度较高的可利用产品成为亟待解决的技术问题。
发明内容
本发明旨在至少解决现有技术或相关技术中存在的技术问题之一。
为此,本发明的目的在于提供一种D-D混剂精馏分离工艺,能够将自氯丙烯精制工艺塔底得到的副产品D-D混剂分离,从而能够混合回收1,2-二氯丙烷及轻组分,顺式1,3二氯丙烯,反式1,3二氯丙烯,顺式1,3二氯丙烯和反式1,3二氯丙烯的产品纯度均可达到95%以上,而且在反式1,3二氯丙烯产品中的顺式1,3二氯丙烯含量不大于0.5%。
为了实现上述目的,本发明的技术方案提供了一种D-D混剂精馏分离工艺,包括以下步骤:
在减压操作条件下,将自氯丙烯精制工艺塔底得到的工艺母液D-D混剂送入脱重塔,经塔底再沸器蒸汽加热,工艺母液D-D混剂中的易碳化重组分与其轻组分在所述脱重塔内传质分离;
二氯丙烯及轻组分蒸发气相经塔顶分凝器控制回流,不凝气相直接送入脱轻塔,所述脱重塔的塔底重组分送入后工段处理;
在减压操作条件下,所述脱重塔的塔顶不凝气相送入所述脱轻塔,经所述脱轻塔的塔底再沸器蒸汽加热,二氯丙烷及轻组分与二氯丙烯在脱轻塔内传质分离;
二氯丙烷及轻组分蒸发气相到达所述脱轻塔的塔顶被冷凝器冷却,冷凝液进入回流罐,部分送塔回流,部分降温后送库收存,所述脱轻塔的塔底物料送入成品塔;
在真空操作条件下,将所述脱轻塔的的塔底物料送入成品塔,所述成品塔的塔底再沸器蒸汽加热后,顺、反式1,3二氯丙烯在成品塔内传质分离,顺式1,3二氯丙烯蒸发气相到达所述成品塔的塔顶被冷凝器冷却,冷凝液进入顺式罐,部分送塔回流,部分从塔顶连续馏出,经降温后送入顺式成品罐收存;
从所述成品塔下部侧线采出反式1,3二氯丙烯,经降温后送入反式罐,再送入反式成品罐收存,所述成品塔的塔底重组分残液间歇排至残液罐。
优选地,所述脱重塔的塔底温度为108℃,塔顶温度为70.5℃,塔底压力为45KPa,塔顶压力为35KPa。
优选地,所述脱轻塔的塔底温度为81℃,塔顶温度为59.1℃,塔底压力为44KPa,塔顶压力为32KPa。
优选地,所述成品塔的塔底温度为80℃,塔顶温度为64℃,塔底压力为37KPa,塔顶压力为25KPa。
优选地,所述工艺母液D-D混剂经预热器利用系统余热加热后送入所述脱重塔。
优选地,所述脱重塔、所述脱轻塔和所述成品塔的塔底再沸器为蒸汽PID自动控温加热,加热介质为压力0.7MPa的饱和蒸汽。
优选地,所述脱轻塔和所述成品塔的塔顶设有两个冷凝器,冷却介质为30℃软化水,供水压力0.4~0.6MPa。
本发明的技术方案具有以下有益技术效果:
(1)通过脱重塔首先脱除工艺母液D-D混剂中的重组分,之后通过脱轻塔,从顶部分离出二氯丙烷及轻组分杂质,可以进行回收利用,脱轻塔塔底的物料再进入成品塔进行传质分离,得到顺式1,3二氯丙烯,反式1,3二氯丙烯,其产品纯度均可达到95%以上,而且在反式1,3二氯丙 烯产品中的顺式1,3二氯丙烯含量不大于0.5%。
(2)采用气相分凝技术,将脱重塔的塔顶气相直接送入脱轻塔,可以节能20%以上。
(3)D-D混剂精馏分离工艺采用三塔连续、变压操作以及侧线采出,不但产品纯度高,而且更加节能,工艺母液D-D混剂经预热器利用系统余热加热后送入脱重塔,充分利用现有生产系统的热能,不但进一步节能,而且提升了工艺母液D-D混剂在脱重塔中的分离效率。
本发明的附加方面和优点将在下面的描述部分中给出,部分将从下面的描述中变得明显,或通过本发明的实践了解到。
具体实施方式
本发明公开了一种D-D混剂精馏分离工艺,本领域技术人员可以借鉴本文内容,适当改进工艺参数实现。特别需要指出的是,所有类似的替换和改动对本领域技术人员来说是显而易见的,它们都被视为包括在本发明。本发明的方法及应用已经通过较佳实施例进行了描述,相关人员明显能在不脱离本发明内容、精神和范围内对本文所述的方法和应用进行改动或适当变更与组合,来实现和应用本发明技术。
下面结合实施例,进一步阐述本发明:
利用丙烯和氯气反应生产氯丙烯,反应方程式如下:
主反应:
Figure PCTCN2020108858-appb-000001
副反应:CH 3-CH=CH 2+Cl 2→CH 3-CHCl-CH 2Cl
CH 3-CH=CH 2+Cl 2→CH 2Cl-CH=CHCl+HCl
CH 3-CH=CH 2+Cl 2→CH 3-CH 2-CH 2Cl+HCl
主产品是氯丙烯,还会产生副产品D-D混剂及盐酸,工艺母液D-D混剂的的组分大体为:轻组分+二氯丙烷50.9%,顺1,3二氯丙烯19.5%,反1,3二氯丙烯19%,重组分10.6%。
D-D混剂精馏分离工艺,包括以下步骤:
S102,在减压操作条件下,将自氯丙烯精制工艺塔底得到的工艺母液D-D混剂送入脱重塔,经塔底再沸器蒸汽加热,工艺母液D-D混剂中的易碳化重组分与其轻组分在脱重塔内传质分离;
其中,工艺母液D-D混剂的流量为2100kg/h,组分大体为:轻组分+二氯丙烷50.9%,顺1,3二氯丙烯19.5%,反1,3二氯丙烯19%,重组分10.6%;脱重塔的塔顶压力为35KPa,塔底压力为45KPa,塔顶温度为70.5℃,塔底温度为108℃。
S104,二氯丙烯及轻组分蒸发气相经塔顶分凝器控制回流,不凝气相直接送入脱轻塔,脱重塔的塔底重组分送入后工段处理;
S106,在减压操作条件下,脱重塔的塔顶不凝气相送入脱轻塔,经脱轻塔的塔底再沸器蒸汽加热,二氯丙烷及轻组分与二氯丙烯在脱轻塔内传质分离;
其中,脱重塔的塔顶不凝气相直接送入脱轻塔,采用气相分凝技术,更加节能,可节能20%以上,脱轻塔的塔顶压力为32KPa,塔底压力为44KPa,塔顶温度为59.1℃,塔底温度为81℃。
S108,二氯丙烷及轻组分蒸发气相到达脱轻塔的塔顶被冷凝器冷却,冷凝液进入回流罐,部分送塔回流,部分降温后送库收存,脱轻塔的塔底物料送入成品塔;
其中,冷凝器为两个,进入回流罐中的部分冷凝液经冷却器降温后送库收存,脱轻塔的塔顶馏出二氯丙烷及轻组分的流量为1070kg/h,组成包括轻组分+二氯丙烷99.5%,顺1,3二氯丙烯0.5%。
S110,在真空操作条件下,将脱轻塔的的塔底物料送入成品塔,成品塔的塔底再沸器蒸汽加热后,顺、反式1,3二氯丙烯在成品塔内传质分离,顺式1,3二氯丙烯蒸发气相到达成品塔的塔顶被冷凝器冷却,冷凝液进入顺式罐,部分送塔回流,部分从塔顶连续馏出,经降温后送入顺式成品罐收存;
其中,冷凝器为两个,进入顺式罐中的部分冷凝液经冷却器降温后送入顺式成品罐收存,成品塔的塔顶压力为25KPa,塔底压力为37KPa,塔顶温度为64℃,塔底温度为80℃,成品塔的塔顶馏出顺式成品的流量为409kg/h,组成包括轻组分+二氯丙烷2.5%,顺1,3二氯丙烯95.5%,反1,3二氯丙烯2%。
S112,从成品塔下部侧线采出反式1,3二氯丙烯,经降温后送入反式罐,再送入反式成品罐收存,成品塔的塔底重组分残液间歇排至残液罐。
其中,采用冷却器降温,成品塔下部侧线馏出反式成品的流量为 385kg/h,组成包括顺1,3二氯丙烯0.5%,反1,3二氯丙烯98%,重组分1.5%,塔底重组分残液的流量为236kg/h,组成包括反1,3二氯丙烯5%,重组分95%。
通过脱重塔首先脱除工艺母液D-D混剂中的重组分,之后通过脱轻塔,从顶部分离出二氯丙烷及轻组分杂质,可以进行回收利用,脱轻塔塔底的物料再进入成品塔进行传质分离,得到顺式1,3二氯丙烯,反式1,3二氯丙烯,其产品纯度均可达到95%以上,而且在反式1,3二氯丙烯产品中的顺式1,3二氯丙烯含量不大于0.5%,提升了产品价值。D-D混剂精馏分离工艺采用三塔连续、变压操作以及侧线采出,不但产品纯度高,而且更加节能。
进一步地,工艺母液D-D混剂经预热器利用系统余热加热后送入脱重塔。
进一步地,脱重塔、脱轻塔和成品塔的塔底再沸器为蒸汽PID自动控温加热,加热介质为压力0.7MPa的饱和蒸汽。
进一步地,脱轻塔和成品塔的塔顶设有两个冷凝器,冷却介质为30℃软化水,供水压力0.4~0.6MPa。
通过将工艺母液D-D混剂经预热器利用系统余热加热后送入脱重塔,充分利用现有生产系统的热能,不但进一步节能,而且提升了工艺母液D-D混剂在脱重塔中的分离效率。通过蒸汽PID自动控温加热,温度控制更加精确,节能,设两个冷凝器进一步保障了冷凝效果,整体上,进一步提升了精馏分离效果,节约了能量。
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。

Claims (7)

  1. 一种D-D混剂精馏分离工艺,其特征在于,包括以下步骤:
    在减压操作条件下,将自氯丙烯精制工艺塔底得到的工艺母液D-D混剂送入脱重塔,经塔底再沸器蒸汽加热,工艺母液D-D混剂中的易碳化重组分与其轻组分在所述脱重塔内传质分离;
    二氯丙烯及轻组分蒸发气相经塔顶分凝器控制回流,不凝气相直接送入脱轻塔,所述脱重塔的塔底重组分送入后工段处理;
    在减压操作条件下,所述脱重塔的塔顶不凝气相送入所述脱轻塔,经所述脱轻塔的塔底再沸器蒸汽加热,二氯丙烷及轻组分与二氯丙烯在脱轻塔内传质分离;
    二氯丙烷及轻组分蒸发气相到达所述脱轻塔的塔顶被冷凝器冷却,冷凝液进入回流罐,部分送塔回流,部分降温后送库收存,所述脱轻塔的塔底物料送入成品塔;
    在真空操作条件下,将所述脱轻塔的的塔底物料送入成品塔,所述成品塔的塔底再沸器蒸汽加热后,顺、反式1,3二氯丙烯在成品塔内传质分离,顺式1,3二氯丙烯蒸发气相到达所述成品塔的塔顶被冷凝器冷却,冷凝液进入顺式罐,部分送塔回流,部分从塔顶连续馏出,经降温后送入顺式成品罐收存;
    从所述成品塔下部侧线采出反式1,3二氯丙烯,经降温后送入反式罐,再送入反式成品罐收存,所述成品塔的塔底重组分残液间歇排至残液罐。
  2. 根据权利要求1所述的D-D混剂精馏分离工艺,其特征在于,
    所述脱重塔的塔底温度为108℃,塔顶温度为70.5℃,塔底压力为45KPa,塔顶压力为35KPa。
  3. 根据权利要求1所述的D-D混剂精馏分离工艺,其特征在于,
    所述脱轻塔的塔底温度为81℃,塔顶温度为59.1℃,塔底压力为44KPa,塔顶压力为32KPa。
  4. 根据权利要求1所述的D-D混剂精馏分离工艺,其特征在于,
    所述成品塔的塔底温度为80℃,塔顶温度为64℃,塔底压力为37KPa,塔顶压力为25KPa。
  5. 根据权利要求1所述的D-D混剂精馏分离工艺,其特征在于,
    所述工艺母液D-D混剂经预热器利用系统余热加热后送入所述脱重塔。
  6. 根据权利要求1所述的D-D混剂精馏分离工艺,其特征在于,
    所述脱重塔、所述脱轻塔和所述成品塔的塔底再沸器为蒸汽PID自动控温加热,加热介质为压力0.7MPa的饱和蒸汽。
  7. 根据权利要求1所述的D-D混剂精馏分离工艺,其特征在于,
    所述脱轻塔和所述成品塔的塔顶设有两个冷凝器,冷却介质为30℃软化水,供水压力0.4~0.6MPa。
PCT/CN2020/108858 2020-07-23 2020-08-13 D-d混剂精馏分离工艺 WO2022016631A1 (zh)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN202010716145.7 2020-07-23
CN202010716145.7A CN111807925B (zh) 2020-07-23 2020-07-23 D-d混剂精馏分离工艺

Publications (1)

Publication Number Publication Date
WO2022016631A1 true WO2022016631A1 (zh) 2022-01-27

Family

ID=72862301

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2020/108858 WO2022016631A1 (zh) 2020-07-23 2020-08-13 D-d混剂精馏分离工艺

Country Status (2)

Country Link
CN (1) CN111807925B (zh)
WO (1) WO2022016631A1 (zh)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115385772A (zh) * 2022-07-04 2022-11-25 中船(邯郸)派瑞特种气体股份有限公司 一种电子级一氟甲烷的纯化方法
CN115490236A (zh) * 2022-09-20 2022-12-20 云南通威高纯晶硅有限公司 一种电子级多晶硅生产用三氯氢硅的制备方法及系统
CN116440951A (zh) * 2023-06-19 2023-07-18 山东河清化工科技有限公司 一种顺反异构催化剂及其制备方法与应用

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113144655B (zh) * 2021-04-28 2022-06-21 安徽金轩科技有限公司 一种佳乐麝香精馏单元及其精馏工艺

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5689020A (en) * 1996-03-11 1997-11-18 Laroche Industries Inc. High temperature chlorination process for the preparation of polychloroolefins
CN102432426A (zh) * 2011-12-14 2012-05-02 青岛科技大学 一种二氯丙烷和二氯丙烯的分离纯化方法
CN103664505A (zh) * 2013-12-24 2014-03-26 山东海益化工科技有限公司 一种氯丙烯生产工艺
CN107879891A (zh) * 2017-11-20 2018-04-06 天津辰力工程设计有限公司 一种利用dd混剂提纯二氯丙烷和二氯丙烯的方法
CN110078584A (zh) * 2019-06-12 2019-08-02 山东凯泰科技股份有限公司 一种从dd混剂中回收二氯丙烷和二氯丙烯工艺
CN110498728A (zh) * 2019-09-06 2019-11-26 湖南莱万特化工有限公司 反式1,3-二氯丙烯和顺式1,3-二氯丙烯化合物及其工艺流程
CN110845298A (zh) * 2019-12-03 2020-02-28 湖南莱万特化工有限公司 反式、顺式或顺反式1,3-二氯丙烯化合物及其精馏方法

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2690155B1 (fr) * 1992-04-21 1994-05-27 Atochem Elf Sa Procede de preparation du chlorure de vinyle par ultrapyrolyse du 1,2 dichloroethane.
WO1995017366A1 (fr) * 1993-12-22 1995-06-29 Daikin Industries, Ltd. Procede de purification de 1,1,1,3,3-pentafluoro-2,3-dichloropropane
CN1133610C (zh) * 1999-07-31 2004-01-07 崔英武 从d-d混剂中提纯二氯丙烯的方法
JP4650968B2 (ja) * 2000-09-27 2011-03-16 鹿島ケミカル株式会社 高純度で着色の少ないトランス−1,3−ジクロロプロペンの製造方法
CN100402476C (zh) * 2005-03-31 2008-07-16 沈阳化工学院 一种利用dd混剂分离1,2-二氯丙烷的方法
JP6449791B2 (ja) * 2013-03-09 2019-01-09 ブルー キューブ アイピー エルエルシー クロロアルカンの製造方法
CN106977367A (zh) * 2017-04-26 2017-07-25 山东海益化工科技有限公司 一种高效氯丙烯的生产工艺

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5689020A (en) * 1996-03-11 1997-11-18 Laroche Industries Inc. High temperature chlorination process for the preparation of polychloroolefins
CN102432426A (zh) * 2011-12-14 2012-05-02 青岛科技大学 一种二氯丙烷和二氯丙烯的分离纯化方法
CN103664505A (zh) * 2013-12-24 2014-03-26 山东海益化工科技有限公司 一种氯丙烯生产工艺
CN107879891A (zh) * 2017-11-20 2018-04-06 天津辰力工程设计有限公司 一种利用dd混剂提纯二氯丙烷和二氯丙烯的方法
CN110078584A (zh) * 2019-06-12 2019-08-02 山东凯泰科技股份有限公司 一种从dd混剂中回收二氯丙烷和二氯丙烯工艺
CN110498728A (zh) * 2019-09-06 2019-11-26 湖南莱万特化工有限公司 反式1,3-二氯丙烯和顺式1,3-二氯丙烯化合物及其工艺流程
CN110845298A (zh) * 2019-12-03 2020-02-28 湖南莱万特化工有限公司 反式、顺式或顺反式1,3-二氯丙烯化合物及其精馏方法

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115385772A (zh) * 2022-07-04 2022-11-25 中船(邯郸)派瑞特种气体股份有限公司 一种电子级一氟甲烷的纯化方法
CN115490236A (zh) * 2022-09-20 2022-12-20 云南通威高纯晶硅有限公司 一种电子级多晶硅生产用三氯氢硅的制备方法及系统
CN115490236B (zh) * 2022-09-20 2024-03-29 云南通威高纯晶硅有限公司 一种电子级多晶硅生产用三氯氢硅的制备方法
CN116440951A (zh) * 2023-06-19 2023-07-18 山东河清化工科技有限公司 一种顺反异构催化剂及其制备方法与应用
CN116440951B (zh) * 2023-06-19 2023-08-11 山东河清化工科技有限公司 一种顺反异构催化剂及其制备方法与应用

Also Published As

Publication number Publication date
CN111807925B (zh) 2021-11-02
CN111807925A (zh) 2020-10-23

Similar Documents

Publication Publication Date Title
WO2022016631A1 (zh) D-d混剂精馏分离工艺
JP4620694B2 (ja) 高純度トリクロロシランの製造方法
CN108329235B (zh) 一种生产高纯度百菌清的工艺方法
CN105481640B (zh) 一种低能耗低损失的氯乙烯精馏工艺
CN108728318A (zh) 一种超纯净特级食用酒精差压蒸馏生产装置及其生产工艺
CN111807981A (zh) 一种从三氯乙烷中回收dmf的方法
CN112142618B (zh) 一种低浓度二甲基甲酰胺废水回收系统及方法
CN110922302A (zh) 一种燃料乙醇双负压粗馏塔差压蒸馏脱水生产工艺
CN107311878A (zh) 一种回收甘氨酸废液的装置及回收甘氨酸废液的方法
CN111393257B (zh) 乙基麦芽酚及其同系物生产中从含氯乙烷废气中回收氯乙烷的方法
CN108083984A (zh) 用于草甘膦溶剂及副产物回收的方法
CN106431836A (zh) 一种萃取精馏与闪蒸耦合分离乙醇‑水物系的工艺
CN114656342B (zh) 一种危废中脱除2-苯基异丙醇杂质生产苯乙酮的方法
US2573244A (en) Recovery of phenol from dilute aqueous solutions
CN112125794A (zh) 三氟氯菊酸的改进的制备方法
CN111202999B (zh) 一种从三甲苯异构化反应生成油中提取高纯度均三甲苯产品的精馏装置及方法
CN103819042A (zh) 一种盐酸废液净化处理方法
CN111517913A (zh) 一种三氯蔗糖生产中三氯乙烷回收的方法
CN110921630A (zh) 一种盐酸解析制备氯化氢的方法
CN112745346A (zh) 一种磷酸酯制备设备及其制备方法
CN110540486A (zh) 一种四氯乙烯生产中副产高沸物的分离系统及分离方法
CN104693132B (zh) 一种1h‑1,2,4三氮唑循环母液回收利用的方法
CN111847481B (zh) 永固紫捏合废水中资源化回收氯化钠和二乙二醇的方法和装置
CN214088348U (zh) 一种多效精馏回收焦油中苯酚的装置
CN113943217B (zh) 环己烷氧化副产物x油中二聚酮的回收方法

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 20946425

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 20946425

Country of ref document: EP

Kind code of ref document: A1