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Method for the recovery of caprolactam

Assignee: Honeywell International Inc
•
Filing: 1971-08-27
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Granted: 1972-09-26
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Expires: 1991-08-27
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Abstract

Abstract A process comprising the steps of: A. CONTACTING AT A TEMPERATURE RANGING FROM ABOUT 40* C. to about 90* C. a rearrangement mass comprising Epsilon caprolactam and sulfuric acid with the following reactants: (I) SUBSTANTIALLY WATER-FREE AMMONIUM SULFATE IN AN AMOUNT RANGING FROM ABOUT 0.9 TO ABOUT 1.1 MOLES PER MOLE OF SULFURIC ACID PRESENT IN SAID REARRANGEMENT MASS, AND (II) AN AQUEOUS AMMONIUM BISULFATE SOLUTION SATURATED AT A TEMPERATURE WITHIN THE RANGE OF 20* TO 55* C., the amount of said aqueous solution being such as to dissolve at the contacting temperature the ammonium bisulfate formed by the reaction of the sulfuric acid component of the rearrangement mass with said ammonium sulfate, to thereby afford an Epsilon -caprolactam phase and an aqueous ammonium bisulfate phase; B. SEPARATING SAID Epsilon -CAPROLACTAM PHASE; C. COOLING SAID AQUEOUS AMMONIUM BISULFATE PHASE TO A TEMPERATURE WITHIN THE RANGE OF 20* TO 55* C. to thereby afford crystalline ammonium bisulfate and a saturated aqueous ammonium bisulfate solution; D. RECOVERING AND RECYCLING SAID SATURATED AQUEOUS SOLUTION TO STEP A).

Inventors

  • 👤 Leland J Beckham

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-31 22:55
CPC Classifications
C; C07; C07D; C07D201/00; C07D201/16

Claims Analysis

Total Claims: 4
Claim 1
Independent Claim 26 words
A process in accordance with claim 1 wherein said rearrangement mass is contacted with an additional reactant which is a water-immiscible organic solvent for epsilon -caprolactam.
Claim 2
Dependent Claim 12 words
A process in accordance with claim 2 wherein said solvent is chloroform.
Claim 3
Dependent Claim 38 words
A process in accordance with claim 2 wherein said aqueous ammonium bisulfate phase after separation of the epsilon -caprolactam phase and prior to said cooling is extracted at least once with a water-immiscible organic solvent for epsilon -caprolactam.
Claim 4
Dependent Claim 20 words
A process in accordance with claim 1 wherein said contacting temperature ranges from about 60* C. to about 80* C.

References Cited (Backward Citations)

US3264060A Cited
US3336298A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1975-09-26 1976-03-27 1976-09-26 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1979-09-26 1980-03-27 1980-09-26 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1983-09-26 1984-03-27 1984-09-26 $7700.00 Window Closed / Lapsed

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