EP0366252A1
Expired / Lapsed
EP
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Porous rigid resins and process of preparation
Assignee: Supelco Inc
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Filing: 1989-09-15
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Granted: —
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Expires: 2009-09-15
Abstract
Abstract Porous, rigid resin particles are prepared having a predetermined particle size distribution, surface area and porosity by polymerizing in the pores of porous inorganic template particles a reaction mixture comprising monoethylenically unsaturated monomer, polyethylenically unsaturated crosslinking monomer and polymerization initiator in a liquid medium in which the monomers and initiator are phase separable and extractable therefrom into the pores of the template particles. The extracted mixture is polymerized in the pores of the template particles, and the template particles are removed without destruction of the polymerizate. The isolated polymerizate mirrors the characteristics of the template particles. The surface of the polymerizate may be modified in various ways to contain desired functionality. The particles of the invention are useful in chromatography, adsorption, ion exchange, and in catalysis.
Inventors
- 👤 Binyamin Feibush
- 👤 Nai-Hong Li
Bibliographic Details
Application Number
—
Jurisdiction
EP
Data Source
google_patents
Last Synchronized
2026-10-24 13:21
CPC Classifications
B; B01; B01J; B01J41/00; B01J41/08; B01J41/12; B01J41/14; B01J20/00; B01J20/22; B01J20/26; B01J20/28; B01J20/28002; B01J20/28004; B01J20/28014; B01J20/28026; B01J20/2803; B01J20/28054; B01J20/28057; B01J20/28069; B01J20/28078; B01J20/28095; B01J20/28097; B01J20/30; B01J20/305; B01J20/3057; B01J31/00; B01J31/02; B01J31/06; B01J31/063; B01J31/067; B01J31/08; B01J39/00; B01J39/08; B01J39/16; B01J39/18; B01J39/20
Claims Analysis
Total Claims: 18
Claim 1
Independent Claim
92 words
A porous, rigid resin comprising particles of crosslinked copolymer derived from monoethylenically unsaturated monomer and polyethylenically unsaturated crosslinking monomer, said copolymer resulting from polymerization, in the pores of porous inorganic template particles, of a reaction mixture comprising said monomers and polymerization initiator in a liquid medium in which the monomers and initiator are phase separable and extractable therefrom into the pores of the template particles, followed by removal of the template particles without destruction of the copolymer, whereby the isolated copolymer mirrors the size, surface area and porosity of the template particles.
Claim 2
Dependent Claim
92 words
A porous, rigid resin comprising particles of crosslinked copolymer derived from monoethylenically unsaturated monomer and polyethylenically unsaturated crosslinking monomer, said copolymer resulting from polymerization, in the pores of porous inorganic template particles, of a reaction mixture comprising said monomers and polymerization initiator in a liquid medium in which the monomers and initiator are phase separable and extractable therefrom into the pores of the template particles, followed by removal of the template particles without destruction of the copolymer, whereby the isolated copolymer mirrors the size, surface area and porosity of the template particles.
Claim 3
Dependent Claim
25 words
A resin as claimed in claim 1 wherein the template particles comprise a porous silica gel, silica, alumina, zirconia, a mineral, or a refractory material.
Claim 4
Dependent Claim
27 words
A resin as claimed in claim 1 or claim 2 wherein the monomers, the initiator and the template particles are hydrophobic, and the liquid medium is aqueous.
Claim 5
Dependent Claim
57 words
A resin as claimed in claim 3 wherein the template particles comprise (a) silanized silica gel particles, for example silica gel particles silanized with trialkyl (C₁-C₁₈) halosilane, or (b) alkoxylated silica gel particles, for example silica gel particles alkoxylated using as an alkoxylation reagent alkanols or arylalcohols, the alkoxylation reagent having from 1 to 25 carbon atoms.
Claim 6
Dependent Claim
40 words
A resin as claimed in claim 4 wherein the silica gel has an average pore size from about 3 to about 2000 nm, a porosity of at least 30% and a surface area from about 5 to about 1000 m²/g.
Claim 7
Dependent Claim
27 words
A resin as claimed in claim 1 or claim 2 wherein the monomers, the initiator and the template particles are hydrophilic, and the liquid medium is hydrophobic.
Claim 8
Dependent Claim
27 words
A resin as claimed in any preceding claim wherein the copolymer carries polar functionality which is:- (i) cationic, e.g. cationic functionality comprising pyridinyl groups; or (ii) anionic.
Claim 9
Dependent Claim
26 words
A resin as claimed in any preceding claim wherein the monoethylenically unsaturated monomer comprises aromatic monomer, acrylic monomer, or a mixture of aromatic and acrylic monomers.
Claim 10
Dependent Claim
42 words
A resin as claimed in any preceding claim wherein the copolymer is: (i) a styrenic copolymer, for example a copolymer of styrene and divinylbenzene; or (ii) an acrylic copolymer, for example a copolymer of divinylbenzene and an alkyl (C₁-C₈) acrylate or methacrylate.
Claim 11
Dependent Claim
120 words
A process for preparing porous, rigid resin particles as claimed in any of Claims 1 to 9, which comprises (a) contacting porous inorganic template particles with a reaction mixture comprising monoethylenically unsaturated monomer, polyethylenically unsaturated monomer and polymerization initiator in a liquid medium, the volume of the reaction mixture being approximately equal to the pore volume of the inorganic particles, said monomers and initiator being phase separable from the reaction medium and extractable into the pores of the inorganic particles, (b) polymerizing the monomers in the pores of the template particles to form crosslinked copolymer, and (c) removing the inorganic particles from the copolymer, whereby the isolated copolymer particles mirror the size, surface area and porosity of the template particles.
Claim 12
Dependent Claim
21 words
A process as claimed in claim 10 wherein the template particles are contacted with the reaction mixture by vigorously agitated admixture.
Claim 13
Dependent Claim
50 words
A process as claimed in claim 10 or claim 11 wherein the surface of the copolymer is functionalized by adsorption onto the template particles of a compound carrying the desired functionality, e.g. cationic functionality, and bonding of said compound to the copolymer during polymerization and/or removal of the template particles.
Claim 14
Dependent Claim
38 words
A process as claimed in claim 12 wherein the template particles comprise silanized silica gel particles, the liquid medium is aqueous, the functional compound is vinylpyridine, and the silica gel particles are removed by treatment with hydrogen fluoride.
Claim 15
Dependent Claim
60 words
A process as claimed in claim 10 or claim 11 wherein the surface of the copolymer is functionalized by providing in the reaction mixture a compound carrying the desired functionality, said template particles being modified with functional groups capable of associating with the functionality of said compound, whereby said functional groups are populated on the surface of the copolymer particles.
Claim 16
Dependent Claim
42 words
A process as claimed in claim 14 wherein the functional compound is a perfluoroalkyl compound and the functional groups with which the template particles are modified are perfluoroalkyl groups, whereby the surface of the copolymer particles is modified with said perfluoroalkyl groups.
Claim 17
Dependent Claim
46 words
A process as claimed in claim 10 or claim 11 wherein the surface of the copolymer is functionalized by chemically bonding a compound carrying the desired functionality onto the template particles, said functionality being transferred to the copolymer during polymerization and/or removal of the template particles.
Claim 18
Dependent Claim
28 words
A process as claimed in claim 16 wherein the template particles comprise hydroxy silanized silica gel particles, and the compound carrying the desired functional groups is acryloyl halide.
References Cited (Backward Citations)
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