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US4711908A Expired / Lapsed US ⏱️ 0.0 years remaining

Skinless porous particle PVC resin and process for producing same

Assignee: Geon Co
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Filing: 1987-04-14
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Granted: 1987-12-08
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Expires: 2007-04-14
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Abstract

Abstract Porous particles of vinyl resin are disclosed where said particles are non-spherical in shape, highly porous, skinless and friable. Processes are also disclosed for producing these novel particles. The particles are preferably PVC and exhibit an ability to absorb large amounts of plasticizer in a short time.

Inventors

  • 👤 Roman B. Hawrylko

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-25 09:47
CPC Classifications
C; C08; C08F; C08F114/00; C08F114/02; C08F114/04; C08F114/06; C08J; C08J3/00; C08J3/12; C08F14/00; C08F14/02; C08F14/04; C08F14/06; C08F2/00; C08F2/12; C08F2/16; C08F2/18; C08J3/16; C08J2327/00; C08J2327/02; C08J2327/04; C08J2327/06

Claims Analysis

Total Claims: 26
Claim 1
Independent Claim 191 words
An agitated aqueous suspension process for producing porous, skinless, agglomerated polyvinyl chloride resin particles comprising polymerizing vinyl monomer in the presence of from about 0.01 part by weight to about 0.1 part by weight per 100 parts by weight of polymerizable monomer of at least one ionic sensitive primary dispersant capable of thickening water, and at least one secondary dispersant, wherein an a monovalent inorganic or organic ionic compound in amounts sufficient to desorb a substantial amount of said primary dispersant off the monomer droplets, is charged to the polymerization medium at from about 1% to about 5% conversion of monomer to polymer, thereby producing a skinless, agglomerated, porous PVC resin in particulate form, said resin particles having a mercury porosity of from about 0.1 cc/g to about 0.7 cc/g, and a particle size of from about 70 microns to about 1000 microns, and a friability of less than about 2, and a powder mix time of less than about 400 seconds, and a shape factor less than about 0.85 and wherein greater than about 20% of the area of the surface of said particle is PVC as measured by ESCA.
Claim 2
Dependent Claim 191 words
An agitated aqueous suspension process for producing porous, skinless, agglomerated polyvinyl chloride resin particles comprising polymerizing vinyl monomer in the presence of from about 0.01 part by weight to about 0.1 part by weight per 100 parts by weight of polymerizable monomer of at least one ionic sensitive primary dispersant capable of thickening water, and at least one secondary dispersant, wherein an a monovalent inorganic or organic ionic compound in amounts sufficient to desorb a substantial amount of said primary dispersant off the monomer droplets, is charged to the polymerization medium at from about 1% to about 5% conversion of monomer to polymer, thereby producing a skinless, agglomerated, porous PVC resin in particulate form, said resin particles having a mercury porosity of from about 0.1 cc/g to about 0.7 cc/g, and a particle size of from about 70 microns to about 1000 microns, and a friability of less than about 2, and a powder mix time of less than about 400 seconds, and a shape factor less than about 0.85 and wherein greater than about 20% of the area of the surface of said particle is PVC as measured by ESCA.
Claim 3
Dependent Claim 19 words
A process of claim 1 wherein said ionic sensitive primary dispersant is a lightly crosslinked interpolymer of acrylic acid.
Claim 4
Dependent Claim 19 words
A process of claim 2 wherein said secondary dispersant is a hydrolyzed polyvinyl acetate being less than 60% hydrolyzed.
Claim 5
Dependent Claim 12 words
A process of claim 1 wherein said ionic material is sodium hydroxide.
Claim 6
Dependent Claim 29 words
A process of claim 2 wherein the level of primary dispersant is from about 0.02 to about 0.06 part by weight per 100 parts by weight of vinyl monomer.
Claim 7
Dependent Claim 14 words
A process of claim 3 wherein said polyvinyl acetate is less than 55% hydrolyzed.
Claim 8
Dependent Claim 30 words
A process of claim 3 wherein the level of said secondary surfactant is from about 0.1 to about 0.4 part by weight per 100 parts by weight of vinyl monomer.
Claim 9
Dependent Claim 26 words
A process of claim 1 wherein said ionic material is added to the polymerization medium at from 1% to 2% conversion of vinyl monomer to polymer.
Claim 10
Dependent Claim 33 words
A process of claim 8 wherein the level of said ionic material is from about 0.001 part by weight to about 0.0100 part by weight per 100 parts by weight of vinyl monomer.
Claim 11
Dependent Claim 12 words
A process of claim 1 wherein said vinyl monomer is vinyl chloride.
Claim 12
Dependent Claim 325 words
A process for producing porous, skinless, agglomerated vinyl resin particles in an aqueous medium comprising: (a) charging water and at least one ion sensitive primary dispersant(s) capable of thickening water to a polymerization vessel equipped with agitation and cooling means; (b) agitating said water and said dispersant(s); (c) reducing or stopping said agitation such that non-turbulent flow is achieved; (d) charging at least one vinyl monomer to the polymerization vessel such that there is formed two liquid layers in the polymerization vessel, a bottom thickened aqueous layer and a top vinyl monomer layer; (e) charging to the top vinyl monomer layer a solution comprising at least one catalyst, at least one solvent, and at least one secondary dispersant, wherein said solvent has a density equal to or less than the vinyl monomer(s) being polymerized and said catalyst solution has a density less than 1.0 gg/cc; (f) allowing said catalyst to diffuse through the vinyl monomer top layer; (g) increasing the agitation such that the entire polymerization medium is emulsified to form monomer droplets suspended in an aqueous polymerization medium; (h) conducting the polymerization of the vinyl monomer to a conversion of from about 1% to about 5%; (i) charging an a monovalent inorganic or organic ionic compound to the polymerization medium in amounts sufficient to substantially desorb the primary dispersant off the monomer droplets; (j) continuing the polymerization of the vinyl monomer to form porous, agglomerated, skinless resin particles; (k) removing the polymerized resin from the reaction vessel, said resin particles having a mercury porosity of from about 0.1 cc/g to about 0.7 cc/g, and a particle size of from about 70 microns to about 1000 microns, and a friability of less than about 2, and a powder mix time of less than about 400 seconds, and a shape factor less than about 0.85 and wherein greater than about 20% of the area of the surface of said particle is PVC as measured by ESCA.
Claim 13
Dependent Claim 325 words
A process for producing porous, skinless, agglomerated vinyl resin particles in an aqueous medium comprising: (a) charging water and at least one ion sensitive primary dispersant(s) capable of thickening water to a polymerization vessel equipped with agitation and cooling means; (b) agitating said water and said dispersant(s); (c) reducing or stopping said agitation such that non-turbulent flow is achieved; (d) charging at least one vinyl monomer to the polymerization vessel such that there is formed two liquid layers in the polymerization vessel, a bottom thickened aqueous layer and a top vinyl monomer layer; (e) charging to the top vinyl monomer layer a solution comprising at least one catalyst, at least one solvent, and at least one secondary dispersant, wherein said solvent has a density equal to or less than the vinyl monomer(s) being polymerized and said catalyst solution has a density less than 1.0 gg/cc; (f) allowing said catalyst to diffuse through the vinyl monomer top layer; (g) increasing the agitation such that the entire polymerization medium is emulsified to form monomer droplets suspended in an aqueous polymerization medium; (h) conducting the polymerization of the vinyl monomer to a conversion of from about 1% to about 5%; (i) charging an a monovalent inorganic or organic ionic compound to the polymerization medium in amounts sufficient to substantially desorb the primary dispersant off the monomer droplets; (j) continuing the polymerization of the vinyl monomer to form porous, agglomerated, skinless resin particles; (k) removing the polymerized resin from the reaction vessel, said resin particles having a mercury porosity of from about 0.1 cc/g to about 0.7 cc/g, and a particle size of from about 70 microns to about 1000 microns, and a friability of less than about 2, and a powder mix time of less than about 400 seconds, and a shape factor less than about 0.85 and wherein greater than about 20% of the area of the surface of said particle is PVC as measured by ESCA.
Claim 14
Dependent Claim 12 words
A process of claim 11 wherein the vinyl monomer is vinyl chloride.
Claim 15
Dependent Claim 19 words
A process of claim 12 wherein the ionic sensitive primary dispersant is a lightly crosslinked interpolymer of acrylic acid.
Claim 16
Dependent Claim 34 words
A process of claim 13 wherein said secondary dispersant is at least one dispersant selected from the group consisting of sorbitan ester and hydrolyzed polyvinyl acetate having a hydrolysis level less than about 70%.
Claim 17
Dependent Claim 22 words
A process of claim 14 wherein said secondary dispersant is a hydrolyzed polyvinyl acetate having a hydrolysis level less than about 60%.
Claim 18
Dependent Claim 17 words
A process of claim 15 wherein said polyvinyl acetate has a hydrolysis level less than about 55%.
Claim 19
Dependent Claim 30 words
A process of claim 13 wherein the level of said primary dispersant is from about 0.02 to about 0.06 part by weight per 100 parts by weight of vinyl monomer.
Claim 20
Dependent Claim 26 words
A process of claim 17 wherein said ionic material is added to the polymerization medium at from 1% to 2% conversion of vinyl monomer to polymer.
Claim 21
Dependent Claim 32 words
A process of claim 18 wherein the level of said secondary dispersant is from about 0.1 part by weight to about 0.4 part by weight per 100 parts by weight vinyl monomer.
Claim 22
Dependent Claim 28 words
A process of claim 11 wherein said solvent in (e) is selected from the group consisting of an alcohol having at least 2 carbon atoms and a hydrocarbon.
Claim 23
Dependent Claim 11 words
A process of claim 20 wherein said solvent is isopropyl alcohol.
Claim 24
Dependent Claim 25 words
A process of claim 11 wherein at least one secondary dispersant is premixed with the vinyl monomer prior to being charged into the polymerization vessel.
Claim 25
Dependent Claim 26 words
A process of claim 11 wherein in (a) the water and dispersant(s) capable of thickening water are premixed prior to being added to the polymerization vessel.
Claim 26
Dependent Claim 35 words
A process of claim 11 wherein in (d) the catalyst solution containing catalyst, solvent and optionally at least one secondary dispersant is premixed with said vinyl monomer prior to being added to the polymerization vessel.

References Cited (Backward Citations)

US3706722A Cited
US4229547A Cited
US4435524A Cited
US4458057A Cited
US4603151A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1990-12-07 1991-06-08 1991-12-08 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1994-12-07 1995-06-08 1995-12-08 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1998-12-07 1999-06-08 1999-12-08 $7700.00 Window Closed / Lapsed

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