KR950005796A - 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
KR950005796A
KR950005796A KR1019930016122A KR930016122A KR950005796A KR 950005796 A KR950005796 A KR 950005796A KR 1019930016122 A KR1019930016122 A KR 1019930016122A KR 930016122 A KR930016122 A KR 930016122A KR 950005796 A KR950005796 A KR 950005796A
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South Korea
Prior art keywords
reactor
carboxylic acid
unsaturated carboxylic
water
column
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KR1019930016122A
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Korean (ko)
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우부곤
박광호
주화명
이한선
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최근선
주식회사 럭키
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Priority to KR1019930016122A priority Critical patent/KR950005796A/en
Publication of KR950005796A publication Critical patent/KR950005796A/en

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)

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 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 contacting the azeotropic composition of water and alcohol vaporized by the heat exchanger with the reflux in the column column, the high boiling point component is returned to the reactor and the light component is brought to the top of the column. Moved and liquefied in the condenser and separated into organic and water in decanters The base layer is the reflux is to create a method and apparatus characterized in that it produced through the reaction process is 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.

도면은 본 발명 방법을 실시하기 위한 주요부인 반응기의 일예를 나타낸 개략도이다.The figure is a schematic diagram showing an example of a reactor which is the main part for carrying out the method of the present invention.

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 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 alcohol refluxed in the column column so that the high boiling point component is returned to the reactor and the lighter component is moved to the top of the column to condense. Liquefied in and separated into organic and water in decanters Current is generated number is characterized in that the manufacturing process through the reaction is removed. 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 a phenolic form of about 100 to 500 (ppm). 제 1항에 있어서, 반응수의 단수는 3단으로 구성됨을 특징으로 하는 방법.The method of claim 1, wherein the number of stages of the reaction water consists of three stages. 탄소수 1 내지 8인(지방족) 알코올과 불포화 카르복실산과의 에스테르화 반응에서 양이온 교환수지 촉매를 이용하여 대응하는 불포화 카르복실산 에스테르류를 연속적으로 제조함에 있어서, 반응기(22)는 1~10단으로 분리된 고정층 형태이며 바람직하게는 3단으로 구성되고, 각 단은 촉매층⑵, 필터⑶, 공기 주입구로서 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 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 the continuous preparation of the corresponding unsaturated carboxylic acid esters using a cation exchange resin catalyst in the esterification reaction of an aliphatic alcohol having 1 to 8 carbon atoms with an unsaturated carboxylic acid, the reactor 22 has 1 to 10 stages. It is composed of a fixed bed separated into two, preferably consisting of three stages, each stage is a catalyst bed ⑵, filter 구, air inlet, the outer wall is adiabatic through the reactor in contact with the catalyst layer continuously from top to bottom circulating and extracting the product water The heat of vaporization is supplied through the heat exchanger outside the reactor, and the circulating pump circulates the reactant 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. The point component is returned to the reactor and the light component is moved to the top of the column to liquefy in the condenser and Reaction process particularly suitable for the present invention, wherein the organic layer is refluxed and the generated water is removed after separation into organic layer and water in 8), and a new manufacturing apparatus specially designed accordingly. ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.※ Note: The disclosure is based on the initial application.
KR1019930016122A 1993-08-19 1993-08-19 Improved manufacturing method of unsaturated carboxylic acid esters and its new manufacturing apparatus (process) KR950005796A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20030037475A (en) * 2001-11-05 2003-05-14 삼성정밀화학 주식회사 A method for manufacturing halohydroxypropyltrialkyl ammonium halide by using an external cyclic reactor

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20030037475A (en) * 2001-11-05 2003-05-14 삼성정밀화학 주식회사 A method for manufacturing halohydroxypropyltrialkyl ammonium halide by using an external cyclic reactor

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