EP0331283A1
Expired / Lapsed
EP
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High stability porous zirconium oxide spherules
Assignee: University of Minnesota Twin Cities
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Filing: 1989-01-27
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Granted: —
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Expires: 2009-01-27
Abstract
Abstract The present invention provides a stable stationary phase for chromatography which comprises porous ZrO₂ spherules coated with a polymer coating wherein said coated spherules have a pore size from about 20-500 Å and a particle diameter range of about 0.5-500 microns, and are stable in basic media to pHs of up to about l4.
Inventors
- 👤 Peter W. Carr
- 👤 Martin O. Rigney
- 👤 Eric F. Funkenbusch
- 👤 Patrick L. Coleman
- 👤 Douglas A. Hanggi
Bibliographic Details
Application Number
—
Jurisdiction
EP
Data Source
google_patents
Last Synchronized
2026-10-27 04:44
CPC Classifications
B; B01; B01J; B01J20/00; B01J20/281; B01J20/282; B01J20/02; B01J20/06; B01J20/28; B01J20/28014; B01J20/28016; B01J20/28019; B01J20/286; B01J20/30; B01J20/32; B01J20/3202; B01J20/3204; B01J20/3231; B01J20/3242; B01J20/3268; B01J20/3272; B01J20/3274; B01J39/00; B01J39/08; B01J39/12; B82; B82Y; B82Y30/00; C; C01; C01G; C01G25/00; C01G25/02; C12; C12N; C12N11/00; C12N11/14; G; G01; G01N; G01N33/00; G01N33/48; G01N33/50; G01N33/53; G01N33/543; G01N33/551; G01N33/553; B01D; B01D15/00; B01D15/08; B01D15/26; B01D15/32; B01D15/325; C01P; C01P2004/00; C01P2004/30; C01P2004/32; C01P2004/60; C01P2004/61; C01P2004/62; C01P2004/64; C01P2004/80; C01P2006/00; C01P2006/12; C01P2006/14; C01P2006/16; C01P2006/17; G01N30/00; G01N30/02; G01N30/50; G01N30/52; G01N2030/524; G01N2030/525
Claims Analysis
Total Claims: 21
Claim 1
Independent Claim
48 words
A bed comprising porous ZrO₂ spherules of about 20-500 microns in diameter, about 1-200 m²/g surface area and of about 0.5-500 Å pore diameter; wherein said spherules form the packing of an HPLC column and are substantially stable in an aqueous solution of a pH of about 1-14.
Claim 2
Dependent Claim
48 words
A bed comprising porous ZrO₂ spherules of about 20-500 microns in diameter, about 1-200 m²/g surface area and of about 0.5-500 Å pore diameter; wherein said spherules form the packing of an HPLC column and are substantially stable in an aqueous solution of a pH of about 1-14.
Claim 3
Dependent Claim
31 words
The bed of claim 1 wherein the spherules are about 45-500 microns in diameter and have a surface area of about 40-150 m²/g and an average pore diameter of about 100-300Å.
Claim 4
Dependent Claim
106 words
The bed of claim 1 wherein the porous ZrO₂ spherules are characterized by having been prepared by a process consisting essentially of: (a) centrifuging an aqueous sol containing colloidal ZrO₂ particles to yield a residue of ZrO₂ particles and a supernatant; (b) recovering said residue; (c) redispersing said residue in an about equal volume of water to form an aqueous sol containing colloidal ZrO₂ particles; (d) dispersing the aqueous sol in a liquid medium which extracts the water from the sol to afford gelled ZrO₂ spherules; (e) recovering the gelled spherules from the medium; and (f) heating the gelled spherules to yield solid porous ZrO₂ spherules.
Claim 5
Dependent Claim
13 words
The bed of claim 3 wherein steps (a)-(c) are repeated about 2-5 times.
Claim 6
Dependent Claim
41 words
Porous ZrO₂ spherules coated with a hydrophobic crosslinked polymer coating wherein said coated spherules have a pore size from about 20-500 Å and a particle diameter range of about 0.5-500 microns, and are stable to about pH 14 in aqueous media.
Claim 7
Dependent Claim
41 words
Porous ZrO₂ spherules coated with a hydrophobic crosslinked polymer coating wherein said coated spherules have a pore size from about 20-500 Å and a particle diameter range of about 0.5-500 microns, and are stable to about pH 14 in aqueous media.
Claim 8
Dependent Claim
11 words
The spherules of claim 5 wherein the polymer coating comprises polybutadiene.
Claim 9
Dependent Claim
29 words
The spherules of claim 5 wherein the surface of the ZrO₂ spherules is modified by treatment with inorganic phosphate to impart both cation-exchange and hydrophobic characteristics to said spherules.
Claim 10
Dependent Claim
11 words
The spherules of claim 7 wherein the inorganic phosphate is H₃PO₄.
Claim 11
Dependent Claim
32 words
The spherules of claim 5 wherein the surface of the ZrO₂ spherules is deactivated by treatment with an effective amount of an organophosphorus compound prior to application of the hydrophobic polymer coating.
Claim 12
Dependent Claim
28 words
The ZrO₂ spherules of claim 9 wherein the surface of the coated spherules is deactivated by treatment with an effective amount of an unsaturated organophosphonate or organophosphonic acid.
Claim 13
Dependent Claim
11 words
The ZrO₂ spherules of claim 10 wherein the organophosphonate is allylphosphonate.
Claim 14
Dependent Claim
32 words
The ZrO₂ spherules of claim 5 wherein the surface of the coated spherules is deactivated by treatment with an effective amount of an organophosphorus compound following application of the hydrophobic polymer coating.
Claim 15
Dependent Claim
28 words
The ZrO₂ spherules of claim 5 wherein the surface of the coated spherules is deactivated by treatment with an effective amount of an unsaturated organophosphonate or organophosphonic acid.
Claim 16
Dependent Claim
12 words
The ZrO₂ spherules of claim 13 wherein the organophosphonate is allyl phosphonate.
Claim 17
Dependent Claim
30 words
A thin layer chromatography plate comprising a substrate coated with a mixture of a binder and a particulate support material comprising the spherules of claims 5, 7, 10 or 12.
Claim 18
Dependent Claim
24 words
The bed of claim 1 wherein the surface of the ZrO₂ spherules is modified by treatment with inorganic phosphate or with an organophosphorus compound.
Claim 19
Dependent Claim
45 words
A bed comprising porous ZrO₂ spherules of about 20-500 microns in diameter, about 1-200 m²/g surface area and of about 0.5-500 Å pore diameter; wherein said spherules are substantially stable in an aqueous solution of a pH of about 1-14, and comprise an immobilized protein.
Claim 20
Dependent Claim
45 words
A bed comprising porous ZrO₂ spherules of about 20-500 microns in diameter, about 1-200 m²/g surface area and of about 0.5-500 Å pore diameter; wherein said spherules are substantially stable in an aqueous solution of a pH of about 1-14, and comprise an immobilized protein.
Claim 21
Dependent Claim
13 words
The bed of claim 17 which comprises an enzyme immobilized on said spherules.
References Cited (Backward Citations)
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