# US 5,328,936 A · Polymerization process for making porous polymeric particles > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 5,328,936 A - Document ID: US5328936A - Status: Granted - Kind: A - Application number: 08/012,082 - Filed: 1993-02-01 - Granted: 1994-07-12 - Earliest claimed: 1993-02-01 - Assignees: Rohm and Haas Company - Inventors: Paul J. Leifholtz; Thomas E. Meteyer - Web page: https://patentgrep.com/patent/US5328936A ## CPC - C08J 9/16: Making expandable particles - C08J 2325/00: Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers - Y10S 526/91: Suspending agents - Y10S 526/911: Emulsifying agents - C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29) - Y10S: TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS ## Abstract A process for making porous polymeric particles having high surface area includes suspending a discontinuous organic phase in an continuous aqueous phase, wherein the organic phase includes an ethylenically unsaturated monomer, a water soluble phase extender and a surfactant in an amount effective to solubilize the water soluble phase extender in the monomer and wherein the aqueous phase includes a diffusion barrier agent for limiting mass transfer of the phase extender from the organic phase to the aqueous phase, and then polymerizing the ethylenically unsaturated monomer to form the porous polymeric particles. ## Claims ### Claim 1 A process for making porous polymeric particles, comprising: suspending a discontinuous organic phase in a continuous aqueous phase; said organic phase comprising: an ethylenically unsaturated monomer; a water soluble phase extender selected from the group consisting of water, methanol, ethanol, n-propanol, 2-propanol, tert-butanol and acetone; and a surfactant in an amount effective to solubilize the water soluble phase extender in the monomer; and said aqueous phase comprising diffusion barrier means dispersed in the aqueous phase, for limiting mass transfer of the phase extender from the organic phase to the aqueous phase; and polymerizing the ethylenically unsaturated monomer to form the porous polymer particles. ### Claim 2 (depends on 1) The process of claim 1, wherein the aqueous phase further comprises anti-emulsion means, dissolved in said aqueous phase, for limiting interaction between the surfactant and the continuous aqueous phase. ### Claim 3 (depends on 1) The process of claim 1, wherein the ethylenically unsaturated monomer is selected from the group consisting of monoethylenically unsaturated monomers, polyethylenically unsaturated monomers and mixtures thereof. ### Claim 4 (depends on 3) The process of claim 3, wherein the ethylenically unsaturated monomer comprises a mixture of about 5 parts by weight to about 50 parts by weight of a monoethylenically unsaturated monomer and about 100 parts by weight of a polyethylenically unsaturated monomer. ### Claim 5 (depends on 4) The process of claim 4, wherein the monoethylenically unsaturated monomer is selected from the group consisting of styrene, ethyl vinyl benzene and mixtures thereof and the polyethylenically unsaturated monomer comprises divinyl benzene. ### Claim 6 (depends on 1) The process of claim 1, wherein the organic phase further comprises an effective amount of a polymerization initiator. ### Claim 7 (depends on 6) The process of claim 6, wherein the polymerization initiator is benzoyl peroxide ### Claim 8 A process for making porous polymeric particles, comprising: suspending a discontinuous organic phase in a continuous aqueous phase; said organic phase comprising: an ethylenically unsaturated monomer; a water soluble phase extender; and a surfactant in an amount effective to solubilize the water soluble phase extender in the monomer; and said aqueous phase comprising diffusion barrier means dispersed in the aqueous phase, for limiting mass transfer of the phase extender from the organic phase to the aqueous phase; and polymerizing the ethylenically unsaturated monomer to form the porous polymer particles. wherein the water soluble phase extender is water. ### Claim 9 (depends on 1) The process of claim 1, wherein the organic phase includes from about 5 parts by weight to about 50 parts by weight water soluble phase extender per 100 parts by weight ethylenically unsaturated monomer. ### Claim 10 (depends on 1) The process of claim 1, wherein the surfactant is selected from the group consisting of sodium dialkylsuccinates and polymeric phosphate esters. ### Claim 11 (depends on 10) The process of claim 10, wherein the sodium dialkylsuccinate comprises sodium dioctylsuccinate. ### Claim 12 (depends on 10) The process of claim 10, wherein the polymeric phosphate ester comprises an octylphenoxypolyethoxyethylphosphate. ### Claim 13 (depends on 1) The process of claim 1, wherein the organic phase includes from about 10 parts by weight to about 40 parts by weight surfactant per 100 parts by weight ethylenically unsaturated monomer. ### Claim 14 (depends on 1) The process of claim 1, wherein the combined organic and aqueous phases comprise from about 0.25 parts by volume to about 1.3 parts by volume organic phase to 1 part by volume aqueous phase. ### Claim 15 (depends on 1) The process of claim 1, wherein the ethylenically unsaturated monomer is polymerized by heating the aqueous phase and suspended organic phase. ### Claim 16 (depends on 1) The process of claim 1, wherein the organic phase is maintained in suspension by agitating the aqueous phase and suspended organic phase. ### Claim 17 (depends on 1) The process of claim 1, further comprising: separating the polymeric particles from the aqueous phase; and removing the water and surfactant from the polymeric particles to provide dry porous polymeric particles. ### Claim 18 (depends on 1) The process of claim 1, further comprising functionalizing the porous polymeric particles to make a particulate ion exchange resin. ### Claim 19 (depends on 1) The process of claim 1, wherein the diffusion barrier means comprise a finely divided hydrophobic material. ### Claim 20 (depends on 19) The process of claim 19, wherein the diffusion barrier agent comprises particles of magnesium silicate clay. ### Claim 21 (depends on 19) The process of claim 19, wherein the diffusion barrier means comprises particles of a copolymer of styrene and divinylbenzene. ### Claim 22 (depends on 1) The process of claim 1, wherein the organic phase includes from about 0.4 weight percent to about 3 weight percent diffusion barrier agent. ### Claim 23 (depends on 2) The process of claim 2, wherein the an anti-emulsion means comprises a metal salt. ### Claim 24 (depends on 23) The process of claim 23, wherein the metal salt comprises sodium chloride. ### Claim 25 (depends on 2) The process of claim 2, wherein the aqueous phase includes up to about 40 parts by weight of the anti-emulsion agent per 100 parts by weight water. ### Claim 26 (depends on 1) The process of claim 1, wherein the porous polymeric particles exhibit a BET surface area of greater than about 50 square meters per gram. ### Claim 27 (depends on 1) The process of claim 1, wherein the porous polymeric particles exhibit a BET surface area of greater than about 200 square meters per gram.