KR930009992A - Method for producing ε-caprolactam - Google Patents

Method for producing ε-caprolactam Download PDF

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Publication number
KR930009992A
KR930009992A KR1019920021889A KR920021889A KR930009992A KR 930009992 A KR930009992 A KR 930009992A KR 1019920021889 A KR1019920021889 A KR 1019920021889A KR 920021889 A KR920021889 A KR 920021889A KR 930009992 A KR930009992 A KR 930009992A
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South Korea
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producing
caprolactam
caprolactam according
zeolite
alcohol
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KR1019920021889A
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Korean (ko)
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KR100287085B1 (en
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히로시 이치하시
마사루 키타무라
히로시 카지쿠리
에이지 타사카
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모리 히테오
수미토모카가쿠 코오교오 카부시키가이샤
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D201/00Preparation, separation, purification or stabilisation of unsubstituted lactams
    • C07D201/02Preparation of lactams
    • C07D201/04Preparation of lactams from or via oximes by Beckmann rearrangement

Abstract

본 발명은, 암모니아, 메틸아민류 및 ε-카프로락탐에서 선택되는 적어도 1종이상의 함질소화합물의 공존하에기상으로 시클로헥사논옥심을 고체촉매와 접촉시켜서 ε-카프로락탐을 제조하는 방법을 개시한다.The present invention discloses a method for producing epsilon caprolactam by contacting a cyclohexanone oxime with a solid catalyst in the presence of ammonia, methylamines and at least one nitrogen-containing compound selected from epsilon caprolactam.

Description

ε-카프로락탐의 제조방법.Method for producing ε-caprolactam.

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

Claims (18)

암모니아, 메틸아민류 및 ε-카프로락탐에서 선택되는 적어도 1종이상의 함질소화합물의 공존하에 기상(氣相)으로 시클로헥사논옥심을 고체촉매와 접촉시키는 것을 특징으로 하는 ε-카프로락탐의 제조방법.A method for producing epsilon -caprolactam, comprising contacting a cyclohexanone oxime with a solid catalyst in the gas phase in the presence of at least one nitrogen-containing compound selected from ammonia, methylamines, and epsilon -caprolactam. 제1항에 있어서, 고체촉매가 제올라이트인 것을 특징으로 하는 ε-카프로락탐의 제조방법.The process for producing ε-caprolactam according to claim 1, wherein the solid catalyst is zeolite. 제1항에 있어서, 제올라이트가 결정성 금속규산염인 것을 특징으로 하는 ε-카프로락탐의 제조방법.The method for producing ε-caprolactam according to claim 1, wherein the zeolite is a crystalline metal silicate. 제3항에 있어서, 결정성 금속규산염의 Si/금속원자비가 5이상인 것을 특징으로 하는 ε-카프로락탐의 제조방법.The method for producing ε-caprolactam according to claim 3, wherein the Si / metal atomic ratio of the crystalline metal silicate is 5 or more. 제4항에 있어서, 전기한 금속은, Al, Ga, Fe, B, Zn, Cr, Be, Co, La, Ge, Ti, Zr, Hf, V, Ni, Sb, Bi, Cu 및 Nb에서 선택되는 적어도 1종이상인 것을 특징으로 하는 ε-카프로락탐의 제조방법.5. The metal of claim 4, wherein the metal described above is selected from Al, Ga, Fe, B, Zn, Cr, Be, Co, La, Ge, Ti, Zr, Hf, V, Ni, Sb, Bi, Cu, and Nb. Method for producing ε-caprolactam characterized in that at least one or more. 제2항에 있어서, 제올라이트가 결정성 실리카인 것을 특징으로 하는 ε-카프로락탐의 제조방법.The method for producing ε-caprolactam according to claim 2, wherein the zeolite is crystalline silica. 제2항에 있어서, 제올라이트가 펜타실형구조인 것을 특징으로 하는 ε-카프로락탐의 제조방법.The method for producing ε-caprolactam according to claim 2, wherein the zeolite has a pentasil structure. 제1항에 있어서, 함질소 화합물의 사용량이 시클로헥사논옥심의 공급량에 대하여 몰비로 10배이상인 것을 특징으로 하는 ε-카프로락탐의 제조방법.The method for producing ε-caprolactam according to claim 1, wherein the amount of the nitrogen-containing compound is 10 times or more in molar ratio with respect to the supply amount of cyclohexanone oxime. 제1항에 있어서, 반응계에 하기의 일반식(1)The general formula (1) according to claim 1, wherein the reaction system is R1-O-R2 R 1 -OR 2 (식중, R1은 불소원자가 치환되어 있어도 좋은 저급알킬기를 나타내고, R2는 수소원자, 불소원자가 치환되어 있어도 좋은 저급알킬기 또는 페닐기를 나타낸다.)로 표시되는 화합물을 공존시키는 것을특징으로 하는 ε-카프로락탐의 제조방법.Ε-, it characterized in that the coexistence of the compound represented by (wherein, R 1 is optionally substituted with a fluorine atom represents a good lower alkyl group, R 2 is optionally substituted hydrogen atom, a fluorine atom shows a good lower alkyl group or a phenyl group.) Process for preparing caprolactam. 제9항에 있어서, 일반식(1)로 표시되는 화합물이 탄소수 6이하인 알코올인 것을 는 적어도 특징으로 하는 ε-카프로락탐의 제조방법.The method for producing ε-caprolactam according to claim 9, wherein the compound represented by the general formula (1) is an alcohol having 6 or less carbon atoms. 제10항에 있어서, 탄소수 6이하인 알코올이 메탄올 및 에탄올에서 선택되는 적어도 1종이상인 것을 특징으로 하는 ε-카프로락탐의 제조방법.The method for producing ε-caprolactam according to claim 10, wherein the alcohol having 6 or less carbon atoms is at least one selected from methanol and ethanol. 제1항에 있어서, 반응온도가 250-500℃인 것을 특징으로 하는 ε-카프로락탐의 제조방법.The process for producing ε-caprolactam according to claim 1, wherein the reaction temperature is 250-500 ° C. 제1항에 있어서, 반응압력이 0.05-10㎏/㎠인 것을 특징으로 하는 ε-카프로락탐의 제조방법.The process for producing ε-caprolactam according to claim 1, wherein the reaction pressure is 0.05-10 kg / cm 2. 제1항에 있어서, 시클로헥사논옥심의 공간속도가 0.1-40hr-1인 것을 특징으로 하는 ε-카프로락탐의 제조방법.The method for producing ε-caprolactam according to claim 1, wherein the space velocity of cyclohexanone oxime is 0.1-40 hr −1 . 제1항에 있어서, 제올라이트촉매가, 활성이 저하된 제올라이트촉매를 분자상산소함유가스중에서 소성한것임을 특징으로 하는 ε-카프로락탐의 제조방법.The method for producing ε-caprolactam according to claim 1, wherein the zeolite catalyst is a calcined zeolite catalyst having reduced activity in a molecular oxygen-containing gas. 제15항에 있어서, 분자상산소함유가스가 공기인 것을 특징으로 하는 ε-카프로락탐의 제조방법.The process for producing ε-caprolactam according to claim 15, wherein the molecular oxygen-containing gas is air. 제15항에 있어서, 분자상산소함유가스가 알코올을 함유하고 있는 것을 특징으로 하는 ε-카프로락탐의 제조방법.The method for producing ε-caprolactam according to claim 15, wherein the molecular oxygen-containing gas contains an alcohol. 제17항에 있어서, 알코올이 메탄올인 것을 특징으로 하는 ε-카프로락탐의 제조방법.18. The process for producing epsilon caprolactam according to claim 17, wherein the alcohol is methanol. ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.※ Note: The disclosure is based on the initial application.
KR1019920021889A 1991-11-27 1992-11-20 Method for preparing E-caprolactam KR100287085B1 (en)

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JP31249291 1991-11-27
JP91-312492 1991-11-27

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20010006615A (en) * 1999-02-09 2001-01-26 고사이 아끼오 PROCESS FOR PRODUCING ε-CAPROLACTAM
KR100411284B1 (en) * 1998-10-16 2004-02-14 주식회사 포스코 Resin solution having good adhesion and corrosion resistance for thin film and the method of manufacturing coated steel by using it
KR100671976B1 (en) * 2005-02-21 2007-01-24 한국과학기술연구원 Silica solid catalysts, method for preparing the same and method for preparing ?-caprolactam using the same

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5071802A (en) * 1989-03-08 1991-12-10 Sumitomo Chemical Co., Ltd. Regeneration of catalysts by burning in the presence of alcohols

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100411284B1 (en) * 1998-10-16 2004-02-14 주식회사 포스코 Resin solution having good adhesion and corrosion resistance for thin film and the method of manufacturing coated steel by using it
KR20010006615A (en) * 1999-02-09 2001-01-26 고사이 아끼오 PROCESS FOR PRODUCING ε-CAPROLACTAM
KR100671976B1 (en) * 2005-02-21 2007-01-24 한국과학기술연구원 Silica solid catalysts, method for preparing the same and method for preparing ?-caprolactam using the same

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