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Patent · US3852272A · A · US

Process for removing lactams

(11) Publication number
US3852272A
(21) Application number
US-24964272-A
(22) Filing date
1972-05-02
(30) Priority date
1971-05-07
(43) Publication date
1974-12-03
(45) Date of grant
1974-12-03
(52) CPC
  • C07D Heterocyclic compounds: 201/16
(73) Assignee
STAMICARBON
(54) Title
Process for removing lactams
(57) Abstract

A process for recovering lactam from a mixture of lactam and sulphuric acid is disclosed, wherein the mixture of lactam and sulphuric acid, such as that produced in a Beckmann rearrangement is partially neutralized and diluted by the addition of ammonia water. The amount of ammonia added is such that the molar ratio

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Claims (5)

  1. IN A PROCESS FOR RECOVERING LACTAM FROM A MIXTURE OF LACTAM AND SULPHURIC ACID, SAID PROCESS COMPRISING COUNTERCURRENTLY EXTRACTING LACTAM FROM SAID MIXTURE WITH A WATERIMMISCIBLE ORGANIC LACTAM SOLVENT, THE IMPROVEMENT COMPRISING PARTLY NEUTRALIZING AND DILUTING SAID MIXTURE OF LACTAM AND SULPHURIC ACID BY THE ADDITION OF AMMONIA AND WATER, WHEREIN THE AMOUNT OF AMMONIA ADDED IS SUCH THAT THE MOLAR RATIO
  2. Process according to claim 1, wherein the neutralization is conducted in two stages, the first neutralization stage involving the addition of all of the dilution water and one-half to two-thirds of the ammonia, thereafter the solution from the first neutralization stage is incompletely extracted in a first extraction by said solvent to form a solvent phase and a sulphuric acid/ammonium sulphate phase, thereafter the remainder of said ammonia is added in a second neutralization stage to the sulphuric acid/ammonium sulphate phase, and thereafter the lactam in said second neutralization stage solution is extracted in a second extraction with said solvent, the solution of lactam in said solvent produced by the second extraction being used to extract lactam in the first extraction.
  3. Process according to claim 1, wherein the partial neutralization of the mixture of lactam and sulphuric acid is conducted in the presence of said solvent, and the resulting mixture from said partial neutralization is subsequently separated into two phases, one phase comprising said solvent containing at least most of said lactam, and the other phase comprising an aqueous solution of ammonium sulphate and sulphuric acid.
  4. Process according to claim 3, wherein lactam is recovered from said aqueous phase by extraction therefrom with said solvent.
  5. Process according to claim 1, wherein said lactam is caprolactam.

Citations (13)

  • DE1199243B
  • DE1206404B
  • GB740891A
  • US2221369A
  • US2605261A
  • US2737511A
  • US2993889A
  • US3275407A
  • US3292996A
  • US3321275A
  • US3336298A
  • US3383170A
  • US3404947A
Record as JSON
{
  "publication_number": "US3852272A",
  "country": "US",
  "kind": "A",
  "title": "Process for removing lactams",
  "abstract": "A process for recovering lactam from a mixture of lactam and sulphuric acid is disclosed, wherein the mixture of lactam and sulphuric acid, such as that produced in a Beckmann rearrangement is partially neutralized and diluted by the addition of ammonia water. The amount of ammonia added is such that the molar ratio",
  "claims": [
    "1. IN A PROCESS FOR RECOVERING LACTAM FROM A MIXTURE OF LACTAM AND SULPHURIC ACID, SAID PROCESS COMPRISING COUNTERCURRENTLY EXTRACTING LACTAM FROM SAID MIXTURE WITH A WATERIMMISCIBLE ORGANIC LACTAM SOLVENT, THE IMPROVEMENT COMPRISING PARTLY NEUTRALIZING AND DILUTING SAID MIXTURE OF LACTAM AND SULPHURIC ACID BY THE ADDITION OF AMMONIA AND WATER, WHEREIN THE AMOUNT OF AMMONIA ADDED IS SUCH THAT THE MOLAR RATIO",
    "2. Process according to claim 1, wherein the neutralization is conducted in two stages, the first neutralization stage involving the addition of all of the dilution water and one-half to two-thirds of the ammonia, thereafter the solution from the first neutralization stage is incompletely extracted in a first extraction by said solvent to form a solvent phase and a sulphuric acid/ammonium sulphate phase, thereafter the remainder of said ammonia is added in a second neutralization stage to the sulphuric acid/ammonium sulphate phase, and thereafter the lactam in said second neutralization stage solution is extracted in a second extraction with said solvent, the solution of lactam in said solvent produced by the second extraction being used to extract lactam in the first extraction.",
    "3. Process according to claim 1, wherein the partial neutralization of the mixture of lactam and sulphuric acid is conducted in the presence of said solvent, and the resulting mixture from said partial neutralization is subsequently separated into two phases, one phase comprising said solvent containing at least most of said lactam, and the other phase comprising an aqueous solution of ammonium sulphate and sulphuric acid.",
    "4. Process according to claim 3, wherein lactam is recovered from said aqueous phase by extraction therefrom with said solvent.",
    "5. Process according to claim 1, wherein said lactam is caprolactam."
  ],
  "cpc": [
    "C07D 201/16"
  ],
  "assignees": [
    "STAMICARBON"
  ],
  "filing_date": "1972-05-02",
  "publication_date": "1974-12-03",
  "grant_date": "1974-12-03",
  "priority_date": "1971-05-07",
  "application_number": "US-24964272-A",
  "family_id": "19813111",
  "citations": [
    "DE1199243B",
    "DE1206404B",
    "GB740891A",
    "US2221369A",
    "US2605261A",
    "US2737511A",
    "US2993889A",
    "US3275407A",
    "US3292996A",
    "US3321275A",
    "US3336298A",
    "US3383170A",
    "US3404947A"
  ]
}

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