RU97113722A - METHOD FOR CONTINUOUS CLEANING OF RAW CAPROLACTAM OBTAINED FROM 6-AMINOCAPRONITRIL - Google Patents

METHOD FOR CONTINUOUS CLEANING OF RAW CAPROLACTAM OBTAINED FROM 6-AMINOCAPRONITRIL

Info

Publication number
RU97113722A
RU97113722A RU97113722/04A RU97113722A RU97113722A RU 97113722 A RU97113722 A RU 97113722A RU 97113722/04 A RU97113722/04 A RU 97113722/04A RU 97113722 A RU97113722 A RU 97113722A RU 97113722 A RU97113722 A RU 97113722A
Authority
RU
Russia
Prior art keywords
mixture
solvent
crude caprolactam
caprolactam
aminocapronitril
Prior art date
Application number
RU97113722/04A
Other languages
Russian (ru)
Other versions
RU2159234C2 (en
Inventor
Ритц Йозеф
Фишер Рольф
Шнурр Вернер
Аххамер Гюнтер
Люйкен Херманн
Фукс Эберхард
Original Assignee
Басф Аг
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
Priority claimed from DE19500041A external-priority patent/DE19500041A1/en
Application filed by Басф Аг filed Critical Басф Аг
Publication of RU97113722A publication Critical patent/RU97113722A/en
Application granted granted Critical
Publication of RU2159234C2 publication Critical patent/RU2159234C2/en

Links

Claims (2)

1. Способ непрерывной очистки сырого капролактама гидрированием, последующей обработкой в кислой среде и затем перегонкой в щелочной среде, отличающийся тем, что 6-аминокапронитрил взаимодействием с водой превращают в сырой капролактам, отделяют из сырого капролактама из стадии а) низкокипящие и высококипящие компоненты, сырой капролактам со стадии б) обрабатывают водородом при температуре от 50 до 150oС и давлении от 1,5 до 250 бар в присутствии катализатора гидрирования и при необходимости растворителя с получением смеси А, пропускают смесь А в растворителе при температуре от 30 до 80oС и давлении от 1 до 5 бар через ионообменник, содержащий кислые группы, с получением смеси Б1, или смесь А перегоняют в присутствии серной кислоты, причем перед добавлением серной кислоты, при необходимости, удаляют имеющийся растворитель, с получением смеси Б2 и смесь Б1 или смесь Б2 перегоняют в присутствии основания с получением чистого капролактама.1. The method of continuous purification of crude caprolactam by hydrogenation, subsequent processing in an acidic medium and then distillation in an alkaline medium, characterized in that 6-aminocapronitrile is converted into crude caprolactam by reaction with water, separated from crude caprolactam from stage a) low-boiling and high-boiling components, crude caprolactam from step b) is treated with hydrogen at a temperature of from 50 to 150 o C and a pressure of from 1.5 to 250 bar in the presence of a hydrogenation catalyst and optionally a solvent to give a mixture a, passed mixtures And in a solvent at a temperature of from 30 to 80 o C and a pressure of from 1 to 5 bar over an ion exchanger containing acidic groups to give a mixture B1 or mixture A is distilled in the presence of sulfuric acid, which is removed before the addition of sulfuric acid, when necessary available solvent, to obtain a mixture of B2 and a mixture of B1 or a mixture of B2 is distilled in the presence of a base to obtain pure caprolactam. 2. Способ по п. 1, отличающийся тем, что в качестве растворителя используют воду. 2. The method according to p. 1, characterized in that water is used as a solvent.
RU97113722/04A 1995-01-03 1995-12-22 Method of continuous purification of raw caprolactam prepared by reacting 6-aminocapronitrile with water RU2159234C2 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19500041A DE19500041A1 (en) 1995-01-03 1995-01-03 Process for the continuous purification of crude caprolactam made from 6-aminocapronitrile
DE19500041.2 1995-01-03

Publications (2)

Publication Number Publication Date
RU97113722A true RU97113722A (en) 1999-06-27
RU2159234C2 RU2159234C2 (en) 2000-11-20

Family

ID=7750939

Family Applications (1)

Application Number Title Priority Date Filing Date
RU97113722/04A RU2159234C2 (en) 1995-01-03 1995-12-22 Method of continuous purification of raw caprolactam prepared by reacting 6-aminocapronitrile with water

Country Status (18)

Country Link
US (1) US5496941A (en)
EP (1) EP0801643B1 (en)
JP (1) JPH10511668A (en)
KR (1) KR100388869B1 (en)
CN (1) CN1068311C (en)
AU (1) AU4389396A (en)
BG (1) BG63387B1 (en)
BR (1) BR9510187A (en)
CA (1) CA2209336C (en)
CZ (1) CZ288217B6 (en)
DE (2) DE19500041A1 (en)
ES (1) ES2160729T3 (en)
MY (1) MY113742A (en)
PL (1) PL186443B1 (en)
RU (1) RU2159234C2 (en)
SK (1) SK84097A3 (en)
TW (1) TW283705B (en)
WO (1) WO1996020923A1 (en)

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DE19517823A1 (en) * 1995-05-18 1996-11-21 Basf Ag Process for the production of caprolactam
DE19628805A1 (en) * 1996-07-17 1998-01-22 Basf Ag Process for the production of caprolactam from 6-aminocapronitrile
FR2751962B1 (en) * 1996-08-02 1998-09-11 Rhone Poulenc Fibres LACTAM PURIFICATION PROCESS
US5877314A (en) * 1997-02-14 1999-03-02 Dsm N.V. Process to continuously prepare an aqueous mixture of episilon caprolactum and episilon caprolactum precursors
EP0943608A1 (en) * 1998-03-20 1999-09-22 Dsm N.V. Process for the continuous purification of crude epsilon--caprolactam
FR2781796B1 (en) † 1998-07-28 2000-09-22 Rhone Poulenc Fibres LACTAM DEHYDRATION PROCESS
FR2786180B1 (en) 1998-11-19 2001-11-23 Rhone Poulenc Fibres LACTAM TREATMENT METHOD AND LACTAM PURIFICATION METHOD
DE10080450T1 (en) * 1999-02-10 2001-05-17 Toshiba Kawasaki Kk Carbon monoxide conversion device for a fuel cell and fuel cell power generation system
DE19910504A1 (en) 1999-03-10 2000-09-14 Basf Ag Process for the purification of N-substituted lactams
FR2803296B1 (en) * 1999-12-30 2002-02-15 Rhodia Polyamide Intermediates LACTAM PURIFICATION PROCESS
DE10021199A1 (en) * 2000-05-03 2001-11-08 Basf Ag Process for the production of caprolactam
DE10021192A1 (en) 2000-05-03 2001-11-08 Basf Ag Process for the production of caprolactam
DE10021191A1 (en) 2000-05-03 2001-11-08 Basf Ag Process for producing a polymer using caprolactam
FR2809395B1 (en) 2000-05-26 2002-07-19 Rhodia Polyamide Intermediates LACTAM PURIFICATION PROCESS
JP4182273B2 (en) * 2000-06-27 2008-11-19 住友化学株式会社 Method for producing ε-caprolactam
DE10033518A1 (en) * 2000-07-11 2002-01-24 Basf Ag Process for the separation of ammonia from 2-phase reaction mixture obtained in amide preparation, involves separating phases and extracting organic phase with aqueous medium
DE60239205D1 (en) 2001-08-27 2011-03-31 Dsm Ip Assets Bv METHOD FOR RECOVERING CAPROLACTAM FROM AQUEOUS CAPROLACTAM PRODUCT USING A SITU-PRODUCED ALKALISAL OF AMINOCAPRONIC ACID
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DE10253094A1 (en) 2002-11-13 2004-05-27 Basf Ag Purification of crude caprolactam comprises a three stage distillation process with feeding of the crude caprolactam and an inorganic acid having a b. pt. above the b. pt. of the caprolactam to a first distillation column
DE10253095A1 (en) * 2002-11-13 2004-06-17 Basf Ag Process for the purification of caprolactam
US6858728B2 (en) * 2003-06-17 2005-02-22 Invista North America S.A.R.L. Method for making caprolactam from impure ACN in which THA is not removed until after caprolactam is produced
US7390897B2 (en) * 2005-03-18 2008-06-24 Invista North America S.A.R.L. Method for making caprolactam from impure 6-aminocapronitrile
WO2007099029A2 (en) * 2006-02-24 2007-09-07 Basf Aktiengesellschaft Method for the purification of caprolactam made from lysin
JP5708637B2 (en) 2010-03-15 2015-04-30 宇部興産株式会社 Method for producing amide compound
AU2011256697B2 (en) * 2010-05-21 2016-05-05 Exxonmobil Upstream Research Company Parallel dynamic compressor apparatus and methods related thereto
US20130150591A1 (en) * 2011-12-07 2013-06-13 Rolf Pinkos Method for purifying n-alkyl-substituted pyrrolidones by hydrogenation
TWI520944B (en) * 2015-02-13 2016-02-11 中國石油化學工業開發股份有限公司 Method for preparing caprolactam and system thereof
CN111153825A (en) * 2019-06-19 2020-05-15 浙江大学 Method for preparing amide compound by using supported metal oxide catalytic material
CN111122720B (en) * 2019-12-11 2022-09-02 湖北三宁碳磷基新材料产业技术研究院有限公司 Method for analyzing caprolactam, 6-aminocaproamide and 6-aminocapronitrile
CN111635330B (en) * 2020-06-24 2023-01-24 江苏扬农化工集团有限公司 Method for recycling reaction residues of key intermediate of hexamethylene diamine and co-producing carboxylic acid
CN114210361A (en) * 2021-12-27 2022-03-22 于向真 Catalyst for one-step synthesis of 6-aminocapronitrile from cyclohexanone oxime or caprolactam and preparation method thereof

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DE4441962A1 (en) * 1994-11-25 1996-05-30 Basf Ag Process for the production of caprolactam
DE19500041A1 (en) * 1995-01-03 1996-07-04 Basf Ag Process for the continuous purification of crude caprolactam made from 6-aminocapronitrile

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