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GB924098A - Improvements relating to the recovery of caprolactam and ammonium sulphate - Google Patents

Improvements relating to the recovery of caprolactam and ammonium sulphate

Info

Publication number
GB924098A
GB924098A GB3843260A GB3843260A GB924098A GB 924098 A GB924098 A GB 924098A GB 3843260 A GB3843260 A GB 3843260A GB 3843260 A GB3843260 A GB 3843260A GB 924098 A GB924098 A GB 924098A
Authority
GB
United Kingdom
Prior art keywords
caprolactam
ammonium sulphate
recovered
layers
reaction mixture
Prior art date
Legal status (The legal status 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 status listed.)
Expired
Application number
GB3843260A
Inventor
Denis George Harold Ballard
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Akzo Nobel UK PLC
Original Assignee
Courtaulds PLC
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
Application filed by Courtaulds PLC filed Critical Courtaulds PLC
Priority to GB3843260A priority Critical patent/GB924098A/en
Priority to ES0271859A priority patent/ES271859A1/en
Publication of GB924098A publication Critical patent/GB924098A/en
Expired legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00Ammonia; Compounds thereof
    • C01C1/24Sulfates of ammonium
    • C01C1/242Preparation from ammonia and sulfuric acid or sulfur trioxide

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Other In-Based Heterocyclic Compounds (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

Ammonium sulphate is recovered from a reaction mixture obtained by nitrosylating a compound containing a cyclohexyl group with a tertiary carbon atom in the ring, in the presence of sulphuric acid, by neutralizing with ammonia to a pH of 6 to 6,5, allowing the mixture to separate into two layers, separating and, after extracting caprolactam from the denser layer, recovering ammonium sulphate therefrom, e.g. by crystallisation. According to the Provisional Specification, the process is applicable to the mixture obtained by the Beckmann rearrangement process. Specifications 904,302, 904,413 and 912,034 are referred to.ALSO:Caprolactam is recovered from a reaction mixture obtained by nitrosylating a compound containing a cyclohexyl group with a tertiary carbon atom in the ring, in the presence of sulphuric acid, by neutralising with ammonia to a pH of 6 to 6.5, allowing the mixture to separate into two layers, separating, adding ammonia to both fractions to complete the neutralisation, extracting the caprolactam from both layers using a solvent, and ammonium sulphate is recovered from the denser layer. The starting material may be hexahydrobenzoic acid which may be removed from the reaction mixture by cyclohexane. The solvent for caprolactam may be methylene chloride. According to the Provisional Specification, the process may also be applied to the recovery of caprolactam prepared by the p Beckmann rearrangement process. Specifications 904,302, 904,413 and 912,034 are referred to.
GB3843260A 1960-11-09 1960-11-09 Improvements relating to the recovery of caprolactam and ammonium sulphate Expired GB924098A (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
GB3843260A GB924098A (en) 1960-11-09 1960-11-09 Improvements relating to the recovery of caprolactam and ammonium sulphate
ES0271859A ES271859A1 (en) 1960-11-09 1961-11-09 CAPROLACTAM AND AMMONIUM SULPHATE RECOVERY PROCEDURE

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB3843260A GB924098A (en) 1960-11-09 1960-11-09 Improvements relating to the recovery of caprolactam and ammonium sulphate

Publications (1)

Publication Number Publication Date
GB924098A true GB924098A (en) 1963-04-24

Family

ID=10403390

Family Applications (1)

Application Number Title Priority Date Filing Date
GB3843260A Expired GB924098A (en) 1960-11-09 1960-11-09 Improvements relating to the recovery of caprolactam and ammonium sulphate

Country Status (2)

Country Link
ES (1) ES271859A1 (en)
GB (1) GB924098A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2651195A1 (en) * 1976-11-10 1978-05-18 Basf Ag Recovering large crystals of pure ammonium sulphate - from caprolactam synthesis, by neutralising, removing lactam and evapn.

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2651195A1 (en) * 1976-11-10 1978-05-18 Basf Ag Recovering large crystals of pure ammonium sulphate - from caprolactam synthesis, by neutralising, removing lactam and evapn.

Also Published As

Publication number Publication date
ES271859A1 (en) 1962-03-01

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