US3627744A
Expired / Lapsed
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Method for polymerizing vinyl halide polymers
Assignee: Monsanto Co
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Filing: 1968-09-12
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Granted: 1971-12-14
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Expires: 1988-09-12
Abstract
Abstract In a substantially isothermal process for the polymerization of vinyl halide monomer formulations in aqueous dispersion, the desired polymerization temperature is maintained by heat-exchange contact with the liquid phase, by condensation and return of vapors and by injection of a relatively low temperature inert liquid. Stable dispersion for the suspension/reflux polymerization temperature may be enhanced by use of a mixture of a cellulose ether, a partially hydrolyzed polyvinyl acetate and a sorbitan fatty acid ester.
Inventors
- 👤 Byrd Hopkins
- 👤 Robert A Bonsall
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-08 21:30
CPC Classifications
B; B01; B01J; B01J19/00; B01J19/0006; B01J19/0013; C; C08; C08F; C08F14/00; C08F14/02; C08F14/04; C08F14/06; B01J2219/00; B01J2219/00049; B01J2219/00051; B01J2219/00074; B01J2219/00087; B01J2219/00094; B01J2219/00103; B01J2219/00105; B01J2219/00108; Y; Y10; Y10S; Y10S526/00; Y10S526/909; Y10S526/918
Claims Analysis
Total Claims: 10
Claim 1
Independent Claim
4 words
a dispersing agent formulation,
Claim 2
Dependent Claim
41 words
allowing a portion of the monomers to escape from the body of the polymerization mixture as a vapor phase and returning the condensate to said body to provide cooling concurrently with liquid-phase heat exchange during the bulk of the polymerization cycle;
Claim 3
Dependent Claim
40 words
The method of claim 1 wherein said heat-exchange coNtact is essentially the sole heat exchange step employed until about 10-20 percent of the polymerizable monomer in said monomer formulation is converted to polymer and wherein said inert liquid is water.
Claim 4
Dependent Claim
131 words
The method of claim 21 wherein said dispersing agent formulation is a mixture of dispersing agents comprising a water-soluble cellulose ether selected from the group consisting of methyl cellulose, ethyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl cellulose and mixtures thereof; a partially hydrolyzed polyvinyl acetate; and about 0.1- 0.25 percent of a sorbitan fatty acid ester surfactant, based upon the weight of polymerizable monomers in the monomer formulation, the fatty acid chain of the sorbitan ester containing 12 to 18 carbon atoms, the polyvinyl acetate and cellulose ether being included in a ratio of their respective weights ranging from about 0.3 to 3.0:1 and the combination thereof being present in said polymerization mixture in an amount of about 0.04 to 0.1 percent based upon the weight of polymerizable monomers in said formulation.
Claim 5
Dependent Claim
163 words
while concurrently extracting heat from said mixture by said liquid-phase heat exchange and vapor-phase condensation, introducing inert liquid into said polymerization mixture at about the point of conversion of the monomers at which the polymerization reaction accelerates rapidly, the temperature of said inert liquid being lower than the batch temperature existing in the body of said mixture, said point of acceleration of the polymerization reaction being at about 65 to 80 percent conversion of the polymerizable monomers in said monomer formulation to polymer with said low temperature inert liquid introduced serving to help control the temperature at and after the point of rapid acceleration of the polymerization reaction at which viscosity of the polymerization mixture is increased; D. allowing the polymerization reaction to continue after the rapid acceleration to the desired degree of completion of conversion of monomers to polymer; E. terminating the polymerization reaction; and F. withdrawing the polymerization mixture from the reaction vessel and recovering the polymer from said polymerization mixture.
Claim 6
Dependent Claim
27 words
0.005 to 1.0 percent, based upon monomer, of a highly active polymerization initiator having a half-life of less than 5 hours at 50* C. in 1,2-dichloroethane, and
Claim 7
Dependent Claim
87 words
water B. adjusting the temperature of said polymerization mixture within said reaction vessel to a desired polymerization temperature in the range from about 45* to 70* C. to effect polymerization of the polymerizable monomers therein; C. maintaining said polymerization mixture under substantially isothermal conditions during the polymerization of the monomer therein, the maximum temperature fluctuation from the desired polymerization temperature in said polymerization mixture being limited to 2.5* C. during the polymerization reaction and until said reaction is substantially complete by a combination of heat-exchange steps comprising:
Claim 8
Dependent Claim
94 words
The method of claim 3 wherein said surfactant is included in an amount ranging from about 0.15 to 0.18 percent based upon the weight of polymerized monomers, wherein said polyvinyl acetate has a residual acetate content of about 20 to 45 weight percent, and wherein said surfactant is a sorbitan monoester selected from the group consisting of the esters of lauric acid, oleic acid, palmitic acid, stearic acid and mixtures of said acids, and wherein the combination is present in an amount of about 0.07 to 0.09 percent by weight of the polymerizable monomers.
Claim 9
Dependent Claim
29 words
The method of claim 1 wherein the said polymerization initiator is selected from the group consisting of dialkylperoxydicarbonates, acyl persulfonates, symmetrical peroxides and symmetrical azo compounds and mixtures thereof.
Claim 10
Dependent Claim
28 words
The method of claim 1 wherein a portion of said monomer formulation is substantially continuously introduced into said water during at least a portion of the polymerization reaction.
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) | 1974-12-13 | 1975-06-14 | 1975-12-14 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1978-12-13 | 1979-06-14 | 1979-12-14 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1982-12-13 | 1983-06-14 | 1983-12-14 | $7700.00 | Window Closed / Lapsed |