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Styrene suspension polymerization system for spheres

Assignee: Normac Inc
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Filing: 1975-04-28
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Granted: 1976-03-02
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Expires: 1995-04-28
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Abstract

Abstract An aqueous suspending agent solution or vehicle useful for suspension polymerization of a styrene-monomer such as styrene as well as derivatives of it and also mixtures with it to produce styrene-polymers. Also included is a suspension polymerization batch, as well as an improvement in the method, for the suspension polymerization of a styrene-monomer.

Inventors

  • 👤 Max Klein

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-02 05:20
CPC Classifications
C; C08; C08F; C08F12/00; C08F12/02; C08F12/04; Y; Y10; Y10S; Y10S526/00; Y10S526/909

Claims Analysis

Total Claims: 12
Claim 1
Independent Claim 276 words
A batch useful for the suspension polymerization of a styrene-monomer, which batch comprises (A) an aqueous phase which is the aqueous suspension vehicle which consists essentially of (a) water and dissolved therein (b) a water-soluble suspending agent inert to reaction with the styrene-monomer, which is at least one of (i) a hydroxyethylcellulose having a viscosity within the range of one whose 2% by weight, on dry basis, aqueous solution at 20° C. has a Hoopler viscosity of from 6175 to 7600 centipoises (ii) a hydroxyethylcellulose whose whole such 5% aqueous solution at 20° C. has a Hoopler viscosity of from 120 to 160 centipoises, (iii) carboxymethylcellulose, (iv) polyacrylic acid, (v) polymethacrylic acid, (vi) the sodium or ammonium salt of any of the carboxylic acid substances (iii), (iv), and (v), and (vii) polyvinyl alcohol; said suspending agent being present in said suspension vehicle in a concentration above that which will allow the produced styrene-polymer to agglomerate under the polymerization conditions and below about 0.4 weight percent, and (c) from about 0.01 to about 0.5 percent of a water-soluble organic solvent for said suspending agent, which solvent is selected from the group consisting of formic acid, dimethylformamide, dimethylacetamide, tetrahydrofuran, ethylenediamine, diethylenetriamine, 2-bromopyridine, and 3-cyanopyridine; and (B) an organic phase composed of a styrene-monomer having dissolved therein a styrene-monomer polymerization effective amount of a styrene-monomer polymerization free radical-providing catalyst; said suspending agent being present in the range of from about 0.2 to about 1 pound thereof for each about 50 pounds of the styrene-monomer, and said styrene-monomer is present in the range of from about 1 pound thereof for each from about 6 to about 7 pounds of water.
Claim 2
Dependent Claim 276 words
A batch useful for the suspension polymerization of a styrene-monomer, which batch comprises (A) an aqueous phase which is the aqueous suspension vehicle which consists essentially of (a) water and dissolved therein (b) a water-soluble suspending agent inert to reaction with the styrene-monomer, which is at least one of (i) a hydroxyethylcellulose having a viscosity within the range of one whose 2% by weight, on dry basis, aqueous solution at 20° C. has a Hoopler viscosity of from 6175 to 7600 centipoises (ii) a hydroxyethylcellulose whose whole such 5% aqueous solution at 20° C. has a Hoopler viscosity of from 120 to 160 centipoises, (iii) carboxymethylcellulose, (iv) polyacrylic acid, (v) polymethacrylic acid, (vi) the sodium or ammonium salt of any of the carboxylic acid substances (iii), (iv), and (v), and (vii) polyvinyl alcohol; said suspending agent being present in said suspension vehicle in a concentration above that which will allow the produced styrene-polymer to agglomerate under the polymerization conditions and below about 0.4 weight percent, and (c) from about 0.01 to about 0.5 percent of a water-soluble organic solvent for said suspending agent, which solvent is selected from the group consisting of formic acid, dimethylformamide, dimethylacetamide, tetrahydrofuran, ethylenediamine, diethylenetriamine, 2-bromopyridine, and 3-cyanopyridine; and (B) an organic phase composed of a styrene-monomer having dissolved therein a styrene-monomer polymerization effective amount of a styrene-monomer polymerization free radical-providing catalyst; said suspending agent being present in the range of from about 0.2 to about 1 pound thereof for each about 50 pounds of the styrene-monomer, and said styrene-monomer is present in the range of from about 1 pound thereof for each from about 6 to about 7 pounds of water.
Claim 3
Dependent Claim 14 words
A suspension polymerization batch as claimed in claim 1, wherein the styrene-monomer is styrene.
Claim 4
Dependent Claim 28 words
A batch as claimed in claim 2, wherein said catalyst is a mixture of (i) azobisisobutyronitrile as its major portion, and (ii) benzoyl peroxide as its minor portion.
Claim 5
Dependent Claim 27 words
A batch as claimed in claim 3, wherein both of said catalysts are present in about equal amounts and their total is under 0.5% of the styrene.
Claim 6
Dependent Claim 13 words
A batch as claimed in claim 3, wherein said organic solvent is dimethylformamide.
Claim 7
Dependent Claim 31 words
In the method of suspension polymerization of a styrene-monomer, the improvement wherein its suspension polymerization is carried out in a batch which is composed as is that claimed in claim 1.
Claim 8
Dependent Claim 18 words
The improvement in the method of suspension polymerization as claimed in claim 6, wherein the styrene-monomer is styrene.
Claim 9
Dependent Claim 22 words
The improvement in the method of suspension polymerization as claimed in claim 6, wherein the suspension batch is that of claim 4.
Claim 10
Dependent Claim 22 words
The improvement in the method of suspension polymerization as claimed in claim 6, wherein the suspension batch is that of claim 5.
Claim 11
Dependent Claim 62 words
The method as claimed in claim 6, wherein the batch is maintained at a temperature from about 155° to about 163° F. while it is fluid-tightly enclosed in a cylindrically confined reaction zone, and said batch is agitated by rotating it as so confined in said zone about an axis diametrically perpendicular to about the middle of the axis of said zone.
Claim 12
Dependent Claim 64 words
The method as claimed in claim 10, wherein there is included within the batch free fall agitation-enhancing pieces in a number below that which can crush the polymerizing styrene-monomer to the extent to prevent significant formation of the styrene-polymer spheres of a size from at least 2 millimeters in diameter and up to from 6 to 18 millimeters in diameter, during said polymerization operation.

References Cited (Backward Citations)

US3280089A Cited
US3328374A Cited
US3560468A Cited
US3706722A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1979-03-02 1979-09-01 1980-03-02 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1983-03-02 1983-09-01 1984-03-02 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1987-03-02 1987-09-01 1988-03-02 $7700.00 Window Closed / Lapsed

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