Patent US4124754A successfully refreshed from Google Patents.
US4124754A
Expired / Lapsed
US
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Polymerization process with subsequent peptization
Assignee: EIDP Inc
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Filing: 1976-12-14
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Granted: 1978-11-07
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Expires: 1996-12-14
Abstract
Abstract A process for making sulfur-modified neoprenes, wherein chloroprene, which may be mixed with up to 20 weight percent of another unsatuated, organic monomer, is polymerized in an aqueous, alkaline emulsion in the presence of about 0.25-0.45 part of sulfur per 100 parts of total organic monomer to a conversion of at most 74%; peptization is initiated by adding to the resulting latex 0.3-1.5 parts of tetraethylthiuram disulfide or another tetraalkylthiuram disulfide, then adding sodium dibutyldithiocarbamate or another water-soluble dialkyldithiocarbamate in a ratio to tetraethylthiuram disulfide of at least 0.8:1; and peptization is contained until it is about 85-95% complete. The polymer then is isolated. Neoprenes made by this process have, when vulcanized, outstanding heat and flex resistance and superior tensile properties, tear strength, and compression set.
Inventors
- 👤 Kenneth L. Miller
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-04 20:47
CPC Classifications
C; C08; C08F; C08F36/00; C08F36/02; C08F36/04; C08F36/14; C08F36/16; C08F36/18
Claims Analysis
Total Claims: 11
Claim 1
Independent Claim
148 words
In a process for polymerizing chloroprene or copolymerizing chloroprene with up to 20 weight percent of another organic, unsaturated monomer, based on the weight of chloroprene, in the presence of elemental sulfur, the improvement of conducting the polymerization or copolymerization in the absence of chain transfer agents in an aqueous, alkaline emulsion in the presence of 0.25-0.45 part of sulfur per 100 parts of the total organic monomer or monomers present to a conversion of at most 74%; terminating the polymerization and initiating peptization by addition to the resulting polymer latex of a tetraalkylthiuram disulfide equivalent to 0.3-1.5 parts of tetraethylthiuram disulfide; all parts being by weight; adding a water-soluble dialkyldithiocarbamate in an amount equivalent to sodium dibutyldithiocarbamate in a weight ratio to the tetraalkylthiuram disulfide equivalent to tetraethylthiuram disulfide of at least 0.8:1, and continuing the peptization until it is about 85-95% complete; and isolating the polymer.
Claim 2
Dependent Claim
148 words
In a process for polymerizing chloroprene or copolymerizing chloroprene with up to 20 weight percent of another organic, unsaturated monomer, based on the weight of chloroprene, in the presence of elemental sulfur, the improvement of conducting the polymerization or copolymerization in the absence of chain transfer agents in an aqueous, alkaline emulsion in the presence of 0.25-0.45 part of sulfur per 100 parts of the total organic monomer or monomers present to a conversion of at most 74%; terminating the polymerization and initiating peptization by addition to the resulting polymer latex of a tetraalkylthiuram disulfide equivalent to 0.3-1.5 parts of tetraethylthiuram disulfide; all parts being by weight; adding a water-soluble dialkyldithiocarbamate in an amount equivalent to sodium dibutyldithiocarbamate in a weight ratio to the tetraalkylthiuram disulfide equivalent to tetraethylthiuram disulfide of at least 0.8:1, and continuing the peptization until it is about 85-95% complete; and isolating the polymer.
Claim 3
Dependent Claim
25 words
A process of claim 1 wherein the proportion of sulfur is 0.3-0.4 part per 100 parts by weight of the total organic monomer or monomers.
Claim 4
Dependent Claim
13 words
The process of claim 1 wherein the polymerization temperature is about 10°-60° C.
Claim 5
Dependent Claim
13 words
The process of claim 3 wherein the polymerization temperature is above 40° C.
Claim 6
Dependent Claim
21 words
The process of claim 1 wherein the initial concentration of total organic monomers in the polymerization emulsion is 30-55% by weight.
Claim 7
Dependent Claim
17 words
The process of claim 1 wherein the monomer conversion is at most 71% and at least 60%.
Claim 8
Dependent Claim
33 words
The process of claim 1 wherein the proportion of tetraalkylthiuram disulfide added to the polymer latex is equivalent to 0.8-1.2 tetraethylthiuram disulfide per 100 parts of total organic monomer in the initial emulsion.
Claim 9
Dependent Claim
15 words
The process of claim 1 wherein the peptization step is carried out at 23°-27° C.
Claim 10
Dependent Claim
19 words
The process of claim 1 wherein the peptization step is carried out at a pH of at least 10.
Claim 11
Dependent Claim
17 words
The process of claim 9 wherein the peptization step is carried out at a pH of 11-12.3.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1981-11-06 | 1982-05-08 | 1982-11-07 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1985-11-06 | 1986-05-08 | 1986-11-07 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1989-11-06 | 1990-05-08 | 1990-11-07 | $7700.00 | Window Closed / Lapsed |