KR930007924A - Method for preparing ε-caprolactone - Google Patents

Method for preparing ε-caprolactone Download PDF

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Publication number
KR930007924A
KR930007924A KR1019910017471A KR910017471A KR930007924A KR 930007924 A KR930007924 A KR 930007924A KR 1019910017471 A KR1019910017471 A KR 1019910017471A KR 910017471 A KR910017471 A KR 910017471A KR 930007924 A KR930007924 A KR 930007924A
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South Korea
Prior art keywords
acid
cyclohexanone
process according
mol
percarboxylic
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KR1019910017471A
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Korean (ko)
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KR0175309B1 (en
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이나바 유키오
우에노 요수케
히라카와 타카푸미
타키구찌 수주오
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나까아즈마 스나오
우베 고상 가부시끼가이샤
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Priority to KR1019910017471A priority Critical patent/KR0175309B1/en
Publication of KR930007924A publication Critical patent/KR930007924A/en
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Publication of KR0175309B1 publication Critical patent/KR0175309B1/en

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D303/00—Compounds containing three-membered rings having one oxygen atom as the only ring hetero atom

Abstract

본 발명은 과산화수소와 붕산 촉매 존재하의 유기 용매중에서 유기 카르복시산을 산화시키므로서 얻어진 퍼카르복시산 용액과 시클로헥사논을 사용하여 ε-카프로락톤을 제조하는 과정으로서, 반응계 내에서 시클로헥사논의 몰당 1-1.5몰의 퍼카르복시산, 0.012몰이하의 과산화수소 및 0.04몰 이하의 붕산 촉매를 공급하여, 상기의 시클로헥사논과 상기의 퍼카르복시산을 반응시켜서, ε-카프로락톤을 형성시키는 제조방법에 관한 것이다.The present invention is a process for preparing ε-caprolactone using a percarboxylic acid solution and cyclohexanone obtained by oxidizing an organic carboxylic acid in an organic solvent in the presence of hydrogen peroxide and a boric acid catalyst. Percarboxylic acid, 0.012 mol or less hydrogen peroxide, and 0.04 mol or less boric acid catalyst are supplied, and the said cyclohexanone and said percarboxylic acid are made to react, and it is related with the manufacturing method which forms (epsilon) -caprolactone.

Description

ε-카프로락톤의 제조방법Method for producing ε-caprolactone

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

제 1 도는 본 발명을 실행하기 위해 이용되는 퍼카르복시산 용액을 제조하는 단계, ε-카프로락톤을 형성하는 단계(초기 ε-카프로락톤 용액을 제조한 단계) 및 초기 ε-카프로락톤 용액을 정제하는 단계를 나타내는 제조 플루우 챠트의 한 예이다.1 shows the steps of preparing a percarboxylic acid solution used to practice the present invention, forming ε-caprolactone (preparing the initial ε-caprolactone solution) and purifying the initial ε-caprolactone solution It is an example of the production flue chart which shows the following.

Claims (19)

과산화수소와 붕산 촉매 존재하의 유기 용매중에서 유기 카르복시산을 산호시키므로서 얻어진 퍼카르복시산 용액과 시클로헥사논을 사용하여 ε-카프로락톤을 제조하는 과정으로서, 반응계 내에서 시클로헥사논의 몰당 1-1.5몰의 퍼카르복시산, 0.012몰 이하의 과산화수소 및 0.04몰 이하의 붕산 촉매를 공급하여, 상기의 시클로헥사논과 상기의 퍼카르복시산을 반응시켜서, ε-카프로락톤을 형성시키는 제조방법.1-1.5 mole percarboxylic acid per mole of cyclohexanone in the reaction system by preparing ε-caprolactone using a percarboxylic acid solution and cyclohexanone obtained by corals of organic carboxylic acid in an organic solvent in the presence of hydrogen peroxide and a boric acid catalyst. And 0.012 mol or less of hydrogen peroxide and 0.04 mol or less of boric acid catalyst to react the cyclohexanone with the percarboxylic acid to form ε-caprolactone. 제 1 항에 있어서, 상기의 퍼카르복시산의 사용량이 상기의 시클로헥사논의 몰당 약1.05-1.4몰인 제조방법.The method according to claim 1, wherein the amount of percarboxylic acid used is about 1.05-1.4 moles per mole of cyclohexanone. 제 2 항에 있어서, 상기의 퍼카르복시산의 사용량이 상기의 시클로헥사논의 몰당 약1.1-1.3몰인 제조방법.3. A process according to claim 2 wherein the amount of percarboxylic acid used is about 1.1-1.3 moles per mole of said cyclohexanone. 제 2 항에 있어서, 상기의 퍼카르복시산의 사용량이 상기의 시클로헥사논의 몰당 약0.001-0.01몰인 제조방법.3. A process according to claim 2 wherein the amount of percarboxylic acid used is about 0.001-0.01 moles per mole of cyclohexanone. 제 1 항에 있어서, 상기의 붕산 촉매의 사용량이 상기의 시클로헥사논의 몰당0.001-0.03몰인 제조방법.The method according to claim 1, wherein the amount of said boric acid catalyst used is 0.001-0.03 mol per mol of said cyclohexanone. 제 5 항에 있어서, 상기의 붕산 촉매의 사용량이 상기의 시클로헥사논의 몰당 0.005-0.018몰인 제조방법.The production method according to claim 5, wherein the amount of said boric acid catalyst used is 0.005-0.018 mol per mol of said cyclohexanone. 제 1 항에 있어서, 반응 온도가 30-80℃범위인 제조방법.The process of claim 1 wherein the reaction temperature is in the range of 30-80 ° C. 3. 제 7 항에 있어서, 반응 온도가 40-70℃범위인 제조방법.8. A process according to claim 7, wherein the reaction temperature is in the range of 40-70 ° C. 제 1 항에 있어서, 반응 시간이 1-8시간 범위인 제조방법.The process according to claim 1, wherein the reaction time is in the range of 1-8 hours. 제 9 항에 있어서, 반응시간이 1-5시간 범위인 제조방법.10. The process according to claim 9, wherein the reaction time is in the range of 1-5 hours. 제 1 항에 있어서, 반응압력이 1-100mmHg범위인 제조방법.The method of claim 1 wherein the reaction pressure is in the range of 1-100 mmHg. 제 1 항에 있어서, 상기의 퍼카르복시산이 퍼클로피온산인 제조방법.The method according to claim 1, wherein the percarboxylic acid is perclopionic acid. 제 1 항에 있어서, 상기의 퍼카르복시산이 유기 용매를 더 함유하는 제조방법.The production method according to claim 1, wherein the percarboxylic acid further contains an organic solvent. 제 13 항에 있어서, 상기의 유기 용매가 방향족 카르복시산의 저급알킬 에스테르인 제조방법.The process according to claim 13, wherein said organic solvent is a lower alkyl ester of aromatic carboxylic acid. 제 14 항에 있어서, 상기의 유기 용매가 프로피온산의 저급 알킬 에스테르인 제조방법.15. The process of claim 14 wherein said organic solvent is a lower alkyl ester of propionic acid. 제 15 항에 있어서, 상기의 유기 용매가 에틸 프로피오네이트인 제조방법.The process according to claim 15, wherein said organic solvent is ethyl propionate. 제 1 항에 있어서, 반응이 안정제를 더 함유하는 제조방법.The process according to claim 1, wherein the reaction further contains a stabilizer. 제 17 항에 있어서, 상기의 안정제가 포스페이트, 포스페이트 에스테르, 피콜린산, 디피콜린산, 피콜린 및 루티딘 그룹에서 최소한 한가지 화합물이 선택되는 제조방법.18. The process according to claim 17, wherein said stabilizer is at least one compound selected from the group of phosphates, phosphate esters, picolinic acid, dipicolinic acid, picoline and lutidine. ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.※ Note: The disclosure is based on the initial application.
KR1019910017471A 1991-10-05 1991-10-05 Process for preparing epsilon-caprolactone KR0175309B1 (en)

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KR0175309B1 KR0175309B1 (en) 1999-02-18

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20190115897A (en) 2018-04-04 2019-10-14 삼양화학산업 주식회사 Composition of post treatment agent for metal surface treatment

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20190115897A (en) 2018-04-04 2019-10-14 삼양화학산업 주식회사 Composition of post treatment agent for metal surface treatment

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