US4891420A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Continuous process for the hydrolytic production of polycaprolactam by tempering unextracted granular polymer material with moist inert gas
Assignee: BASF SE
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Filing: 1988-06-30
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Granted: 1990-01-02
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Expires: 2008-06-30
Abstract
Abstract A process for tempering unextracted polycaprolactam is disclosed which results in polycaprolactam having suitable physical and chemical properties for melt extrusion and spinning, without the need for conventional solvent/water extraction and drying of crude granules.
Inventors
- 👤 Wolfgang K. Martin
- 👤 James R. Ryffel
- 👤 Hans H. Schuster
- 👤 Chih-Peng Wen
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-05 04:00
CPC Classifications
C; C08; C08J; C08J3/00; C08J3/12; C08G; C08G69/00; C08G69/02; C08G69/08; C08G69/14; C08G69/16; C08G69/46; C08J2377/00; C08J2377/02
Claims Analysis
Total Claims: 12
Claim 1
Independent Claim
148 words
In a process for the hydrolytic polymerization of caprolactam into polycaprolactam in the presence of a chain regulator, the improvement comprising: (a) employing, during said polymerization, a chain regulator selected from the group consisting of (i) alkylammonium carboxylates and (ii) hexamethylenediamine/monocarboxylic acid mixtures wherein the mole ratio of hexamethylenediamine to monocarboxylic acid is from about 0.5:1 to about 1.1:1, to form crude polycaprolactam; (b) preparing granules from the crude, unextracted polycaprolactam thus produced; and (c) tempering said granules at a temperature of from about 130° C. to about 200° C. for a period of from 8 to about 100 hours in a stream of inert gas containing from 2 to about 15 weight percent water; whereby the granules thus tempered exhibit a higher polymer relative viscosity and lower extractables content than the crude unextracted granules while maintaining stable relative viscosity, amino end groups, and dyeability under extrusion conditions.
Claim 2
Dependent Claim
148 words
In a process for the hydrolytic polymerization of caprolactam into polycaprolactam in the presence of a chain regulator, the improvement comprising: (a) employing, during said polymerization, a chain regulator selected from the group consisting of (i) alkylammonium carboxylates and (ii) hexamethylenediamine/monocarboxylic acid mixtures wherein the mole ratio of hexamethylenediamine to monocarboxylic acid is from about 0.5:1 to about 1.1:1, to form crude polycaprolactam; (b) preparing granules from the crude, unextracted polycaprolactam thus produced; and (c) tempering said granules at a temperature of from about 130° C. to about 200° C. for a period of from 8 to about 100 hours in a stream of inert gas containing from 2 to about 15 weight percent water; whereby the granules thus tempered exhibit a higher polymer relative viscosity and lower extractables content than the crude unextracted granules while maintaining stable relative viscosity, amino end groups, and dyeability under extrusion conditions.
Claim 3
Dependent Claim
22 words
The process of claim 1 wherein said alkylammonium carboxylate is butylammonium acetate and said hexamethylenediamine/monocarboxylic acid mixture is a hexamethylenediamine/propionic acid mixture.
Claim 4
Dependent Claim
32 words
The process of claim 2 wherein said tempering is conducted at a temperature of from about 140° C. to about 180° C. for a period of from 16 to about 64 hours.
Claim 5
Dependent Claim
11 words
The process of claim 3 wherein said inert gas is nitrogen.
Claim 6
Dependent Claim
52 words
The process of claim 2 wherein said butylammonium acetate is present in an amount of from 0.3 to about 0.6 weight percent relative to the total monomer charge. wherein said mixture is present in an amount of from about 0.04 to about 0.5 weight percent hexamethylenediamine based upon the total monomer charge.
Claim 7
Dependent Claim
18 words
The process of claim 1 wherein said inert gas contains from 4 to about 10 weight percent water.
Claim 8
Dependent Claim
18 words
The process of claim 2 wherein said inert gas contains from 4 to about 10 weight percent water.
Claim 9
Dependent Claim
18 words
The process of claim 1 wherein said inert gas contains from 6 to about 10 weight percent water.
Claim 10
Dependent Claim
18 words
The process of claim 2 wherein said inert gas contains from 6 to about 10 weight percent water.
Claim 11
Dependent Claim
18 words
The process of claim 4 wherein said inert gas contains from 6 to about 10 weight percent water.
Claim 12
Dependent Claim
18 words
The process of claim 5 wherein said inert gas contains from 6 to about 10 weight percent water.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1993-01-01 | 1993-07-03 | 1994-01-02 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1997-01-01 | 1997-07-03 | 1998-01-02 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2001-01-01 | 2001-07-03 | 2002-01-02 | $7700.00 | Window Closed / Lapsed |