← Back to Patent Explorer
US3976629A Expired / Lapsed US ⏱️ 0.0 years remaining

Process of manufacturing spherical polymeric beads

Assignee: Commonwealth Scientific and Industrial Research Organisation
•
Filing: 1974-11-08
•
Granted: 1976-08-24
•
Expires: 1994-11-08
📄 Original PDF 🌐 Google Patents 🔄 Sync Now

Abstract

Abstract A process of manufacturing approximately spherical polymeric beads of average size less than 20 microns, which process comprises copolymerizing an unsaturated carboxylic acid and a crosslinking agent characterized in that the polymerization is initiated by means of a two part redox free radical system and is carried out in a reaction mixture comprising a fine suspension of droplets of an organic phase in an aqueous phase wherein the organic phase comprises an acid chosen from the group consisting of methacrylic acid and crotonic acid; a crosslinking agent; and an oil soluble and water insoluble first part of a redox free radical initiated system; and wherein the aqueous phase comprises water, at least 15% weight inert salt per volume of aqueous phase, and a suspending agent; and the second part of the redox free radical initiator is at least partially soluble in both the organic and the aqueous phase and is added to the reaction mixture during the course of polymerization while the reaction mixture is maintained at a temperature in the range from 0 DEG C to 50 DEG C.

Inventors

  • 👤 Malcolm Edwin Hayward
  • 👤 Volker Elmar Maier

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-23 17:49
CPC Classifications
C; C08; C08F; C08F220/00; C08F220/02; C08F220/04; C08F220/06; B; B01; B01J; B01J39/00; B01J39/08; B01J39/16; B01J39/18; B01J39/20; Y; Y10; Y10S; Y10S526/00; Y10S526/909; Y10T; Y10T428/00; Y10T428/29; Y10T428/2982; Y10T428/2991; Y10T428/2998

Claims Analysis

Total Claims: 12
Claim 1
Independent Claim 240 words
A process of manufacturing approximately spherical polymeric beads of average size less than 20 microns, which process comprises copolymerising an unsaturated carboxylic acid and a crosslinking agent characterised in that the polymerisation is initiated by means of a two part redox free radical system and is carried out in a reaction mixture comprising a fine suspension of droplets of an organic phase in an aqueous phase wherein the organic phase comprises an acid chosen from the group consisting of methacrylic acid and crotonic acid; a crosslinking agent chosen from the group consisting of divinyl benzene, divinyl toluene, divinyl xylene, divinyl chlorobenzene, divinyl naphthalene, divinyl ethylbenzene and trivinyl benzene, butadiene, isoprene, dimethallyl, diethallyl, diallyl, cyclopentadiene, piperylene, chloroprene, 2,3-dimethyl-3-butadiene, 2,3-pentadiene, 1,4-pentadiene, 1,5-hexadiene, 2,4-hexadiene, 2,5-dimethyl-2,4-hexadiene, octadiene, 3,7-dimethyl-2,4-octadiene, 2-methyl-6-methylene-2,7-octadiene, 1,3-decadiene, 1,3,5-hexatriene, hexachlorocyclopentadiene, dicyclopentadiene and divinyl-ether, and an oil soluble and water insoluble first organic oxidant part of a redox free radical initiator system; and wherein the aqueous phase comprises a solution of water, at least 15% weight inert salt per volume aqueous phase and a suspending agent which is soluble in water and not salted out of solution by said inert salt; and the second inorganic reductant part of the redox free radical initiator is at least partially soluble in both the organic and the aqueous phase and is added to the reaction mixture during the course of polymerisation while the mixture is maintained at a temperature in the range from 0°C to 50°C.
Claim 2
Dependent Claim 240 words
A process of manufacturing approximately spherical polymeric beads of average size less than 20 microns, which process comprises copolymerising an unsaturated carboxylic acid and a crosslinking agent characterised in that the polymerisation is initiated by means of a two part redox free radical system and is carried out in a reaction mixture comprising a fine suspension of droplets of an organic phase in an aqueous phase wherein the organic phase comprises an acid chosen from the group consisting of methacrylic acid and crotonic acid; a crosslinking agent chosen from the group consisting of divinyl benzene, divinyl toluene, divinyl xylene, divinyl chlorobenzene, divinyl naphthalene, divinyl ethylbenzene and trivinyl benzene, butadiene, isoprene, dimethallyl, diethallyl, diallyl, cyclopentadiene, piperylene, chloroprene, 2,3-dimethyl-3-butadiene, 2,3-pentadiene, 1,4-pentadiene, 1,5-hexadiene, 2,4-hexadiene, 2,5-dimethyl-2,4-hexadiene, octadiene, 3,7-dimethyl-2,4-octadiene, 2-methyl-6-methylene-2,7-octadiene, 1,3-decadiene, 1,3,5-hexatriene, hexachlorocyclopentadiene, dicyclopentadiene and divinyl-ether, and an oil soluble and water insoluble first organic oxidant part of a redox free radical initiator system; and wherein the aqueous phase comprises a solution of water, at least 15% weight inert salt per volume aqueous phase and a suspending agent which is soluble in water and not salted out of solution by said inert salt; and the second inorganic reductant part of the redox free radical initiator is at least partially soluble in both the organic and the aqueous phase and is added to the reaction mixture during the course of polymerisation while the mixture is maintained at a temperature in the range from 0°C to 50°C.
Claim 3
Dependent Claim 12 words
A process according to claim 1 wherein the acid is methacrylic acid.
Claim 4
Dependent Claim 67 words
A process according to claim 1 wherein the first part of the redox system is chosen from the group consisting of lauroyl peroxide, isobutyryl peroxide, di-cetyl peroxydicarbonate, cumene hydro peroxide, di-cumyl peroxide, benzyl peroxide and t-butyl peroxy pivalate, and the second part of the redox system is chosen from the group consisting of Fe + + , Ti + + + , and Co + + .
Claim 5
Dependent Claim 16 words
A process according to claim 1 wherein the inert salt is calcium chloride or magnesium chloride.
Claim 6
Dependent Claim 20 words
A process according to claim 4 wherein the concentration of inert salt in the aqueous phase is above 20% w/v.
Claim 7
Dependent Claim 24 words
A process according to claim 1 wherein the suspending agent is from 0.1% to 10% weight of polyvinyl alcohol per volume of aqueous phase.
Claim 8
Dependent Claim 22 words
A process according to claim 6 wherein the concentration of polyvinyl alcohol in the aqueous phase is from 0.5% to 2% w/v.
Claim 9
Dependent Claim 30 words
A process according to claim 1 wherein the concentration of inert salt is between 15 and 25% w/v and wherein the organic phase comprises a substantially water insoluble organic solvent.
Claim 10
Dependent Claim 30 words
A process according to claim 8 wherein the organic solvent is chosen from the group consisting of diethyl ether, benzene, toluene and aliphatic hydrocarbons having six or more carbon atoms.
Claim 11
Dependent Claim 22 words
A process according to claim 1 wherein the reaction is carried out at a temperature in the range from 5° to 40°C.
Claim 12
Dependent Claim 21 words
A process according to claim 1 wherein the particles have an average size in the range from 0.4 to 2 microns.

References Cited (Backward Citations)

US2706192A Cited
US2810716A Cited
US3211708A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1979-08-24 1980-02-23 1980-08-24 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1983-08-24 1984-02-23 1984-08-24 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1987-08-24 1988-02-23 1988-08-24 $7700.00 Window Closed / Lapsed

Assigned Categories & Tags

No categories assigned to this patent yet.

Assign Category Tag