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US4078133A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for producing water-soluble vinyl high-polymers by reversed-phase emulsion polymerization

Assignee: Individual
•
Filing: 1976-11-26
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Granted: 1978-03-07
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Expires: 1996-11-26
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Abstract

Abstract An improved process for producing powdery water-soluble vinyl high-polymers by reversed-phase emulsion polymerization. The vinyl monomer is polymerized in the form of W/O type emulsion dispersed as an aqueous solution in a non-polar organic solvent immiscible with water and having a boiling point in the polymerization temperature range of the vinyl monomer, under stationary evaporation and reflux of part of the solvent, whereby the oxygen in the polymerization system is completely removed and thus the polymerization is enhanced to achieve an extremely high polymerization degree. Further, the aqueous solution of the monomer is added and dispersed in the polymerizing system stepwise or continuously at such a rate that the concentration of the polymer produced in the particles of the emulsion is maintained to a value of 20% or more to the completion of the reaction, whereby the dispersed particles are substantially completely prevented from agglomeration by virtue of the non-tackiness of the particles having a high concentration of the polymer.

Inventors

  • 👤 Kazutaka Ozima

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-31 05:03
CPC Classifications
C; C08; C08F; C08F2/00; C08F2/32

Claims Analysis

Total Claims: 10
Claim 1
Independent Claim 335 words
A process for producing powdery, water-soluble, vinyl polymers having a high degree of polymerization, by W/O emulsion polymerization, which comprises the steps of: in a reaction vessel having a reflux condenser at its top, forming a reaction mixture consisting essentially of (1) an oil phase consisting essentially of a mixture of at least two non-polar organic solvents which are soluble with each other, and substantially immiscible with water and which have different boiling points, said solvent mixture having a boiling temperature in the range of from 30° to 60° C, said boiling temperature being in the temperature range for effecting polymerization of water-soluble vinyl monomers, (2) a W/O emulsifier and (3) a water phase consisting essentially of an aqueous solution of a water-soluble vinyl monomer or mixture of said monomers, said emulsifier being effective to emulsify said water phase in said oil phase, the amount of said water phase being less than twice the amount of said emulsifier whereby said water phase is solubilized by said emulsifier and is dispersed in said oil phase to form a W/O emulsion; heating said W/O emulsion reaction mixture to the boiling temperature of said solvent mixture, and simultaneously agitating said reaction mixture, and maintaining said reaction mixture at said boiling temperature under stable reflux conditions to start polymerization of said monomer to form vinyl polymer in the dispersed water phase of said reaction mixture; and then intermittently or continuously adding to said reaction mixture, while it is maintained under said reflux and agitation and in said W/O emulsion state, additional quantities of said aqueous solution of water-soluble vinyl monomer whereby to effect polymerization of said monomer, said additional quantities being added at such a rate that the concentration of the vinyl polymer present in the dispersed water phase of said W/O emulsion reaction mixture is continuously maintained at not less than 20 percent by weight, based on the weight of the water phase of said reaction mixture, during said adding step and until completion of the polymerization period.
Claim 2
Dependent Claim 335 words
A process for producing powdery, water-soluble, vinyl polymers having a high degree of polymerization, by W/O emulsion polymerization, which comprises the steps of: in a reaction vessel having a reflux condenser at its top, forming a reaction mixture consisting essentially of (1) an oil phase consisting essentially of a mixture of at least two non-polar organic solvents which are soluble with each other, and substantially immiscible with water and which have different boiling points, said solvent mixture having a boiling temperature in the range of from 30° to 60° C, said boiling temperature being in the temperature range for effecting polymerization of water-soluble vinyl monomers, (2) a W/O emulsifier and (3) a water phase consisting essentially of an aqueous solution of a water-soluble vinyl monomer or mixture of said monomers, said emulsifier being effective to emulsify said water phase in said oil phase, the amount of said water phase being less than twice the amount of said emulsifier whereby said water phase is solubilized by said emulsifier and is dispersed in said oil phase to form a W/O emulsion; heating said W/O emulsion reaction mixture to the boiling temperature of said solvent mixture, and simultaneously agitating said reaction mixture, and maintaining said reaction mixture at said boiling temperature under stable reflux conditions to start polymerization of said monomer to form vinyl polymer in the dispersed water phase of said reaction mixture; and then intermittently or continuously adding to said reaction mixture, while it is maintained under said reflux and agitation and in said W/O emulsion state, additional quantities of said aqueous solution of water-soluble vinyl monomer whereby to effect polymerization of said monomer, said additional quantities being added at such a rate that the concentration of the vinyl polymer present in the dispersed water phase of said W/O emulsion reaction mixture is continuously maintained at not less than 20 percent by weight, based on the weight of the water phase of said reaction mixture, during said adding step and until completion of the polymerization period.
Claim 3
Dependent Claim 50 words
A process according to claim 1 in which said additional quantities of said aqueous solution of water-soluble vinyl monomer are added to said reaction mixture in the form of a dispersion of said aqueous solution in a similar solvent mixture and a similar emulsifier prepared outside of said reaction vessel.
Claim 4
Dependent Claim 22 words
A process according to claim 1, wherein said mixture of nonpolar organic solvents is a petroleum fraction having a boiling point range.
Claim 5
Dependent Claim 26 words
A process according to claim 1, wherein an oil-soluble polymerization initiator is dissolved in said solvent mixture provided in said vessel before the reaction is started.
Claim 6
Dependent Claim 32 words
A process according to claim 1, wherein a water-soluble polymerization initiator is dissolved in the water phase that is dispersed in the oil phase in said vessel before the polymerization is started.
Claim 7
Dependent Claim 34 words
A process according to claim 1, wherein the amount of said emulsifier is in the range from 1 to 20% by weight, based on the total amount of said vinyl monomer to be polymerized.
Claim 8
Dependent Claim 51 words
A process according to claim 2 in which the total amount of emulsifier added before polymerization begins and with said additional quantities is in the range of from 1 to 20% by weight, based on the total amount of said vinyl monomer added before polymerization begins and with said additional quantities.
Claim 9
Dependent Claim 52 words
A process according to claim 1, wherein said water-soluble vinyl monomer is selected from the group consisting of acrylamide, methacrylamide, acrylic acid and salts thereof, 2-(dimethylamino)-ethyl methacrylate and salts thereof, 2-(dimethylamino)ethylacrylate and salts thereof, a mixture of the foregoing compounds, and a mixture of the foregoing compounds with other water-soluble vinyl monomers.
Claim 10
Dependent Claim 52 words
A process according to claim 2, wherein said water-soluble vinyl monomer is selected from the group consisting of acrylamide, methacrylamide, acrylic acid and salts thereof, 2-(dimethylamino)-ethyl methacrylate and salts thereof, 2-(dimethylamino)ethylacrylate and salts thereof, a mixture of the foregoing compounds, and a mixture of the foregoing compounds with other water-soluble vinyl monomers.

References Cited (Backward Citations)

US2982749A Cited
US2983717A Cited
US3284393A Cited
US3211708A Cited
US3278506A Cited
US3975341A Cited
US4037040A Cited
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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) 1981-03-06 1981-09-05 1982-03-07 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1985-03-06 1985-09-05 1986-03-07 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1989-03-06 1989-09-05 1990-03-07 $7700.00 Window Closed / Lapsed

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