Patent US3989649A successfully refreshed from Google Patents.
US3989649A
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Process for production of spherical porous fillers for liquid chromatography by suspension polymerization of monovinyl and polyvinyl aromatic monomers in the presence of paraffin wax
Assignee: Resonac Holdings Corp
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Filing: 1975-06-03
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Granted: 1976-11-02
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Expires: 1995-06-03
Abstract
Abstract Spherical porous fine particles of a cross-linked polymer can be obtained in the continuous phase by subjecting a mixture of a monovinyl aromatic compound and a polyvinyl aromatic compound to aqueous suspension polymerization in the presence of a paraffin wax with use of an initiator. This product is very suitable as a filler for gel permeation chromatography. Ion exchange groups can be introduced into the obtained polymer and a column filler suitable for ion exchange chromatography of amino acids, substances related to nucleic acids, proteins and the like is thus obtained.
Inventors
- 👤 Isao Kaiho
- 👤 Ryuji Takahashi
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-23 09:16
CPC Classifications
B; B01; B01J; B01J39/00; B01J39/04; B01J39/05; B01J20/00; B01J20/22; B01J20/26; B01J39/08; B01J39/16; B01J39/18; B01J39/20; B01J39/26; B01J2220/00; B01J2220/50; B01J2220/54
Claims Analysis
Total Claims: 16
Claim 1
Independent Claim
123 words
A process for the production of spherical porous polymer fillers for liquid chromatography which comprises dissolving a paraffin wax in a mixture of up to 95% by weight of at least one monovinyl aromatic monomer and at least 5% by weight of at least one polyvinyl aromatic monomer to obtain a homogeneous oil phase, dispersing said oil phase into an aqueous medium to form an aqueous suspension of fine oil phase particles, subjecting said monomers to an aqueous suspension polymerization in the presence of a free-radical generating polymerization initiator to form a cross-linked polymer containing paraffin wax deposited as fine particles therein and thereafter removing the paraffin wax from said cross-linked polymer. and, fillers if desired, introducing ion exchange groups into the polymer
Claim 2
Dependent Claim
123 words
A process for the production of spherical porous polymer fillers for liquid chromatography which comprises dissolving a paraffin wax in a mixture of up to 95% by weight of at least one monovinyl aromatic monomer and at least 5% by weight of at least one polyvinyl aromatic monomer to obtain a homogeneous oil phase, dispersing said oil phase into an aqueous medium to form an aqueous suspension of fine oil phase particles, subjecting said monomers to an aqueous suspension polymerization in the presence of a free-radical generating polymerization initiator to form a cross-linked polymer containing paraffin wax deposited as fine particles therein and thereafter removing the paraffin wax from said cross-linked polymer. and, fillers if desired, introducing ion exchange groups into the polymer
Claim 3
Dependent Claim
36 words
The process according to claim 1, wherein said monomer mixture comprises 45 to 95% by weight of at least one monovinyl aromatic monomer and 5 to 55% by weight of at least one polyvinyl aromatic monomer.
Claim 4
Dependent Claim
19 words
The process according to claim 7, wherein said polyvinyl aromatic monomer is divinyl benzene, trivinyl benzene or mixtures thereof.
Claim 5
Dependent Claim
36 words
The process according to claim 1, wherein the amount of the paraffin wax is 5 to 100% by weight based on the weight of the mixture of the monovinyl aromatic monomer and the polyvinyl aromatic monomer.
Claim 6
Dependent Claim
26 words
The process according to claim 1, wherein the paraffin wax has a melting point of 40° to 80` C. and contains 20 to 100 carbon atoms.
Claim 7
Dependent Claim
108 words
The process according to claim 1, wherein the process includes dissolving the paraffin wax and the initiator in said monomer mixture at a temperature of about 30° to 40° C to obtain said oil phase, pouring said oil phase into water maintained at about 40° to about 50° C as said aqueous medium to thereby disperse said oil phase in the water in the form of fine oil phase particles, and increasing the temperature of said dispersion to a polymerization temperature to advance the polymerization, whereby the paraffin wax is deposited in the form of fine particles and the resulting cross-linked polymer is obtained in the continuous phase.
Claim 8
Dependent Claim
27 words
The process according to claim 1, wherein said polyvinyl aromatic monomer is divinyl benzene, divinyl toluene, divinyl xylene, divinyl naphthalene, divinyl ethylbenzene, trivinyl benzene or mixtures thereof.
Claim 9
Dependent Claim
19 words
The process according to claim 1, wherein said monovinyl aromatic monomer is styrene, a nucleus-substituted styrene or mixtures thereof.
Claim 10
Dependent Claim
29 words
The process according to claim 8, wherein said monovinyl aromatic monomer is styrene, methyl styrene, dimethyl styrene, ethylvinyl benzene, chlorostyrene, vinyl naphthalene, methylvinyl naphthalene, sec-butyl styrene or mixtures thereof.
Claim 11
Dependent Claim
20 words
The process according to claim 1, wherein said free radical generating polymerization initiator is a peroxide or an azo compound.
Claim 12
Dependent Claim
32 words
The process according to claim 10, wherein the amount of said initiator is 0.5 to 5% by weight based on the weight of the monovinyl aromatic monomer and the polyvinyl aromatic monomer.
Claim 13
Dependent Claim
18 words
The process according to claim 1, wherein said aqueous medium contains a suspension stabilizer and a dispersing agent.
Claim 14
Dependent Claim
27 words
The process according to claim 1, wherein ratio of the volume of said oil phase to the volume of said aqueous medium ranges from 1:1 to 1:5.
Claim 15
Dependent Claim
26 words
The process according to claim 1, wherein subsequent to the removal of the paraffin wax, said process further includes introducing ion exchange groups into said polymer.
Claim 16
Dependent Claim
20 words
The process of claim 14, wherein the introducing of ion exchange groups into said polymer is by sulfonating said polymer.
References Cited (Backward Citations)
US3379664A
Cited
US3630981A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1979-11-02 | 1980-05-03 | 1980-11-02 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1983-11-02 | 1984-05-03 | 1984-11-02 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1987-11-02 | 1988-05-03 | 1988-11-02 | $7700.00 | Window Closed / Lapsed |