KR950005797A - Improved manufacturing method of unsaturated carboxylic acid esters and its new manufacturing apparatus (process) - Google Patents

Improved manufacturing method of unsaturated carboxylic acid esters and its new manufacturing apparatus (process) Download PDF

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Publication number
KR950005797A
KR950005797A KR1019940012614A KR19940012614A KR950005797A KR 950005797 A KR950005797 A KR 950005797A KR 1019940012614 A KR1019940012614 A KR 1019940012614A KR 19940012614 A KR19940012614 A KR 19940012614A KR 950005797 A KR950005797 A KR 950005797A
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South Korea
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column
alcohol
reactor
carboxylic acid
unsaturated carboxylic
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KR1019940012614A
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Korean (ko)
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KR0122429B1 (en
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우부곤
박광호
주화명
이한선
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성재갑
주식회사 럭키
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/08Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/48Separation; Purification; Stabilisation; Use of additives
    • C07C67/52Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
    • C07C67/54Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation

Abstract

본 발명은 탄소수 1 내지 8인(지방족) 알코올과 불포화 카르복실산과의 에스테르화 반응에서 양이온 교환수지를 촉매로 사용하여 대응하는 불포화 카르복실산 에스테르류를 연속적으로 제조하는 방법에 있어서, 1~10단으로 분리된 고정층 형태이고 각단은 촉매층, 필터, 공기 주입구로 구성되고 외벽은 단열인 반응기를 통해 반응물이 위에서 아래로 연속적으로 촉매층과 접촉하여 순환하고 생성수 추출을 위한 기화열을 반응기 외부의 열교환기를 통해 공급하고 순환펌프로 반응물을 반응기와 열교환기 사이를 순환시키고 열교환기에 의하여 기화된 수분과 알코올의 공비조성을 컬럼탑에서 환류되는 알코올 또는 컬럼탑 탑정의 알코올 공급구로부터 공급되는 원료 알코올과 접촉하여 고비점 성분은 반응기로 환류되고 가벼운 성분은 컬럼 상부로 이동되어 응축기에서 액화되고 디캔터에서 유기층과 물로 분리된 후 유기층은 환류되고 생성수는 제거되는 반응공정을 통하여 제조함을 특징으로 하는 방법 및 장치에 관한 것이다.The present invention relates to a method of continuously producing corresponding unsaturated carboxylic acid esters by using a cation exchange resin as a catalyst in an esterification reaction of an aliphatic alcohol having 1 to 8 carbon atoms with an unsaturated carboxylic acid. In the form of a fixed bed separated into stages, each stage is composed of a catalyst layer, a filter, and an air inlet, and an outer wall of the reactor is adiabatic, and the reactants circulate in contact with the catalyst layer continuously from the top to the bottom. Through the circulating pump and circulating the reactant between the reactor and the heat exchanger, and azeotropic composition of water and alcohol vaporized by the heat exchanger in contact with the reflux of the column column or the raw alcohol supplied from the column top column The point component is fed back into the reactor and the lighter component moves to the top of the column Is liquefied in the condenser air after the organic layer was washed with water and the organic layer separated in the decanter is refluxed be generated, to a method which is characterized by producing through the reaction process and apparatus are removed.

Description

불포화 카르복실산 에스테르류의 개량된 제조방법 및 이의 새로운 제조장치(공정)Improved manufacturing method of unsaturated carboxylic acid esters and its new manufacturing apparatus (process)

본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음Since this is an open matter, no full text was included.

Claims (8)

탄소수 1 내지 8인(지방족) 알코올과 불포화 카르복실산과의 에스테르화 반응에서 양이온 교환수지를 촉매로 사용하여 대응하는 불포화 카르복실산 에스테르류를 연속적으로 제조하는 방법에 있어서, 1~10단으로 분리된 고정층 형태이고 각단은 촉매층, 필터, 공기 주입구로 구성되고 외벽은 단열인 반응기를 통해 반응물이 위에서 아래로 연속적으로 촉매층과 접촉하여 순환하고 생성수 추출을 위한 기화열을 반응기 외부의 열교환기를 통해 공급하고 순환펌프로 반응물을 반응기와 열교환기 사이를 순환시키고 열교환기에 의하여 기화된 수분과 알코올의 공비조성을 컬럼탑에서 환류되는 알코올 또는 컬럼탑 탑정의 알코올 공급구로부터 공급되는 원료 알코올과 접촉하여 고비점 성분은 반응기로 환류되고 가벼운 성분은 컬럼 상부로 이동되어 응축기에서 액화되고 디캔터에서 유기층과 물로 분리된 후 유기층은 환류되고 생성수는 제거되는 반응공정을 통하여 제조함을 특징으로 하는 방법.In the method of continuously producing the corresponding unsaturated carboxylic acid esters by using a cation exchange resin as a catalyst in the esterification reaction of an aliphatic alcohol having 1 to 8 carbon atoms with an unsaturated carboxylic acid, it is separated into 1 to 10 steps. It consists of a fixed bed, each stage is composed of a catalyst bed, a filter, an air inlet, and the outer wall is circulated through the reactor insulated from the top to the bottom continuously in contact with the catalyst bed and the heat of vaporization for the extraction of product water is supplied through a heat exchanger outside the reactor. The circulating pump circulates the reactants between the reactor and the heat exchanger, and the azeotropic composition of water and alcohol vaporized by the heat exchanger is brought into contact with the reflux of the column column or with the raw alcohol supplied from the column top column alcohol supply port. Reflux to the reactor and light components are transferred to the top of the column to condense Liquid and the organic layer after the organic layer with water and remove it from the decanter was refluxed to create and method characterized in that it produced through the reaction process are removed from the. 제 1항에 있어서, 불포화 카르복실산은 아크릴산, 메타아크릴산임을 특징으로 하는 방법.The method of claim 1 wherein the unsaturated carboxylic acid is acrylic acid, methacrylic acid. 제 1항에 있어서, 불포화 카르복실산과 알코올의 몰비는 약 1:08~1:1.3임을 특징으로 하는 방법.The method of claim 1 wherein the molar ratio of unsaturated carboxylic acid to alcohol is about 1:08 to 1: 1.3. 제 1항에 있어서, 반응온도는 약 70~100℃ 주위온도임을 특징으로 하는 방법.The method of claim 1 wherein the reaction temperature is about 70-100 ° C. ambient temperature. 제 1항에 있어서, 반응압력은 약 50~400 torr 정도임을 특징으로 하는 방법.The method of claim 1 wherein the reaction pressure is about 50-400 torr. 제 1항에 있어서, 중합금지제는 페놀릭 형태로 약 100~500 ppm 정도 사용함을 특징으로 하는 방법.The method of claim 1, wherein the polymerization inhibitor is used in the phenolic form of about 100 to 500 ppm. 제 1항에 있어서, 환류용으로 제공되는 알코올이 에스테르화 반응에 공급되는 알코올량의 적어도 10중량%임을 특징으로 하는 방법.The method of claim 1 wherein the alcohol provided for reflux is at least 10% by weight of the amount of alcohol supplied to the esterification reaction. 탄소수 1 내지 8인(지방족) 알코올과 불포화 카르복실산과의 에스테르화 반응에서 양이온 교환수지를 촉매로 이용하여 대응하는 불포화 카르복실산 에스테르류를 연속적으로 제조함에 있어서, 반응기(22)는 1~10단으로 분리된 고정층 형태이고 각단은 촉매층⑵, 필터⑶, 공기 주입구⑷로서 외벽은 단열인 반응기를 통해 반응물이 위에서 아래로 연속적으로 촉매층과 접촉하여 순환하고 생성수 추출을 위한 기화열을 반응기 외부의 열교환기⑽를 통해 공급하고 순환펌프⑻로 반응물을 반응기와 열교환기 사이를 순환시키고 열교환기에 의하여 기화된 수분과 알코올의 공비조성을 컬럼탑⒂에서 환류되는 알코올 또는 컬럼⒂의 탐정의 알코올 공급부(23)로부터 공급되는 원료 알코올과 접촉하여 고비점 성분은 반응기로 환류되고 가벼운 성분은 컬럼 상부로 이동되어 응축기에서 액화되고 디캔터(18)에서 유기층과 물로 분리된 후 유기층은 환류되고 생성수는 제거되도록 구성한 본 발명에 특히 적합한 반응공정과 이에 따라 특별히 설계된 새로운 제조장치.In continuously producing the corresponding unsaturated carboxylic acid esters by using a cation exchange resin as a catalyst in the esterification reaction of an aliphatic alcohol having 1 to 8 carbon atoms with an unsaturated carboxylic acid, the reactor 22 is 1 to 10 In the form of a fixed bed separated into stages, each stage is a catalyst bed, a filter, and an air inlet port, and the outer wall is circulated through the reactor which is adiabatic by contacting the catalyst layer continuously from the top to the bottom, and heat of vaporization for extraction of generated water is exchanged outside the reactor. From the alcohol supply 23 of the alcohol or column detective of the column or reflux in the column column and the azeotrope of the water and alcohol vaporized by the heat exchanger and the reaction product is circulated between the reactor and the heat exchanger with a circulation pump In contact with the feed alcohol, the high boiling point component is fed back into the reactor and the lighter component A reaction process particularly suitable for the present invention, wherein the organic layer is refluxed and product water is removed after being moved to liquefy in a condenser and separated into organic and water in decanters 18, and a new manufacturing apparatus specially designed accordingly. ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.※ Note: The disclosure is based on the initial application.
KR1019940012614A 1993-08-19 1994-06-04 Method and its new apparatus for producing unsaturated carboxylic acid esters KR0122429B1 (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113710640A (en) * 2019-07-04 2021-11-26 株式会社Lg化学 Diester-based material production unit and diester-based material production system comprising same
EP3995483A4 (en) * 2019-07-04 2022-09-07 Lg Chem, Ltd. Diester-based material manufacturing unit, and diester-based material manufacturing system including same

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100380017B1 (en) * 1998-12-30 2003-09-26 주식회사 엘지화학 Manufacturing method of unsaturated carboxylic ester by continuous process
KR102489173B1 (en) * 2019-07-04 2023-01-18 주식회사 엘지화학 System for Heat Exchange and System for Manufacturing Di-ester based Composition Comprising the Same
KR102489174B1 (en) * 2019-07-04 2023-01-18 주식회사 엘지화학 System and Method for Manufacturing Diester-based Composition

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113710640A (en) * 2019-07-04 2021-11-26 株式会社Lg化学 Diester-based material production unit and diester-based material production system comprising same
EP3995483A4 (en) * 2019-07-04 2022-09-07 Lg Chem, Ltd. Diester-based material manufacturing unit, and diester-based material manufacturing system including same
EP3995482A4 (en) * 2019-07-04 2022-09-07 Lg Chem, Ltd. Unit for preparing diester-based material, and system for preparing diester-based material, comprising same
CN113710640B (en) * 2019-07-04 2023-07-18 株式会社Lg化学 Diester-based material production unit and diester-based material production system including the same

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KR0122429B1 (en) 1997-11-11

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