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US5047438A
Expired / Lapsed
US
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Porous rigid resins and process of preparation
Assignee: Sigma-Aldrich Co LLC
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Filing: 1988-09-26
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Granted: 1991-09-10
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Expires: 2008-09-26
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 monovinyl monomers, polyvinyl crosslinking monomers and a 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
US
Data Source
google_patents
Last Synchronized
2026-11-01 15:31
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: 19
Claim 1
Independent Claim
112 words
A process for preparing porous, rigid resin particles which comprises (a) contacting porous inorganic template particles with a reaction mixture comprising monoethylenically unsaturated monomers, polyethylenically unsaturated monomers and a 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 copolymers, 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 2
Dependent Claim
112 words
A process for preparing porous, rigid resin particles which comprises (a) contacting porous inorganic template particles with a reaction mixture comprising monoethylenically unsaturated monomers, polyethylenically unsaturated monomers and a 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 copolymers, 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 3
Dependent Claim
24 words
The process of claim 1 wherein in template particles are selected from porous silica gel, silica, alumina, zirconia, a mineral and a refractory material.
Claim 4
Dependent Claim
22 words
The process of claim 1 wherein the monomers, the initiator and the template particles are hydrophobic and the liquid medium is aqueous.
Claim 5
Dependent Claim
22 words
The process of claim 1 wherein the monomers, the initiator and the template particles are hydrophilic and the liquid medium is hydrophobic.
Claim 6
Dependent Claim
13 words
The process of claim 4 wherein the template particles comprise silica gel particles.
Claim 7
Dependent Claim
14 words
The process of claim 3 wherein the template particles comprise silanized silica gel particles.
Claim 8
Dependent Claim
19 words
The process of claim 6 wherein the silanization is effected with a trialkyl (C 1 -C 18 ) halosilane.
Claim 9
Dependent Claim
13 words
The process of claim 3 wherein template particles comprise alkoxylated silica gel particles.
Claim 10
Dependent Claim
30 words
The process of claim 8 where the silica gel particles are alkoxylated using as an alkoxylation reagent alkanols or arylalkahols, the alkoxylation reagent having from 1 to 25 carbon atoms.
Claim 11
Dependent Claim
19 words
The process of claim 1 wherein the template particles are contacted with the reaction mixture by vigorously agitated admixture.
Claim 12
Dependent Claim
42 words
The process of claim 1 wherein the surface of the copolymer is functionalized by adsorption onto the template particles of a compound carrying the desired functionality and bonding of said compound to the copolymer during polymerization and/or removal of the template particles.
Claim 13
Dependent Claim
55 words
The process of claim 1 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 14
Dependent Claim
41 words
The process of claim 1 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 15
Dependent Claim
10 words
The process of claim 11 wherein said functionality is cationic.
Claim 16
Dependent Claim
36 words
The process of claim 11 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 17
Dependent Claim
40 words
The process of claim 12 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 18
Dependent Claim
26 words
The process of claim 13 wherein the template particles comprise hydroxy silanized silica gel particles, and the compound carrying the desired functional groups is acryloyl halide.
Claim 19
Dependent Claim
55 words
The process of claim 1 wherein the template particles comprise silanized silica gel particles and the reaction medium is aqueous; and 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 m 2 /g.
References Cited (Backward Citations)
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| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
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| 3.5 Years (Year 4) | 1994-09-09 | 1995-03-11 | 1995-09-10 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1998-09-09 | 1999-03-11 | 1999-09-10 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2002-09-09 | 2003-03-11 | 2003-09-10 | $7700.00 | Window Closed / Lapsed |