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WO1997038041B1 - Siloxane star-graft polymers, ceramic powders coated therewith and method of preparing coated ceramic powders - Google Patents

Siloxane star-graft polymers, ceramic powders coated therewith and method of preparing coated ceramic powders

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Publication number
WO1997038041B1
WO1997038041B1 PCT/US1997/005179 US9705179W WO9738041B1 WO 1997038041 B1 WO1997038041 B1 WO 1997038041B1 US 9705179 W US9705179 W US 9705179W WO 9738041 B1 WO9738041 B1 WO 9738041B1
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WO
WIPO (PCT)
Prior art keywords
ceramic powder
coated
ceramic
siloxane
powder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/US1997/005179
Other languages
French (fr)
Other versions
WO1997038041A1 (en
Filing date
Publication date
Application filed filed Critical
Priority to AU24271/97A priority Critical patent/AU715859B2/en
Priority to EP97919963A priority patent/EP0891387B1/en
Priority to JP9536259A priority patent/JP2000508684A/en
Priority to CA002250962A priority patent/CA2250962C/en
Priority to DE69729290T priority patent/DE69729290T2/en
Publication of WO1997038041A1 publication Critical patent/WO1997038041A1/en
Publication of WO1997038041B1 publication Critical patent/WO1997038041B1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Abstract

A coated ceramic powder comprises a plurality of ceramic particles and a siloxane star-graft coating polymer encapsulating at least a portion of the particles. The coating polymer comprises Si(w,x,y,z), where w, x, y and z are the mole percent tetrafunctional, trifunctional, difunctional and monofunctional monomeric units, respectively, and wherein w is about 20-100 and x, y and z are about 0-30, 0-50 and 0-10, respectively, and at least one of x, y and z is greater than zero. A method of preparing a coated ceramic powder comprises the steps of a) polymerizing a tetrafunctional siloxane monomer and at least one of a trifunctional siloxane monomer, a difunctional siloxane monomer and a monofunctional siloxane monomer, b) adding a quantity of ceramic powder to a reaction vessel, c) shear mixing the ceramic powder for a time sufficient to wet substantially all of the powder surface, d) adding the siloxane polymer prepared in step (a) to the reaction vessel containing the shear mixed ceramic powder, e) shear mixing the shear mixed ceramic powder and the siloxane polymer for a time sufficient to form a siloxane polymer coated ceramic powder, and f) separating the coated ceramic powder from the components remaining in the reaction vessel.

Claims

- -AMENDED CLAIMS[received by the International Bureau on 1 October 1997 (01.10.97); original claims 1, 12 and 24 amended; remaining claims unchanged (6 pages)]
1. A coated ceramic powder comprising a plurality of ceramic particles and a siloxane star- graft coating polymer encapsulating at least a portion of said particles, said coating polymer comprising:
Si(w,x.y,z)
where w, x, y and z are the mole percent tetrafunctional, trifunctional, difunctional and monofunctional monomeric units, respectively, and wherein w, x, y and z are about 45-75, 5-25, 5-45 and 5-10, respectively.
2. The coated ceramic powder of claim 1 wherein said ceramic is Ti02.
3. The coated ceramic powder of claim 2 further comprising Al"5 centers to introduce surface defects into the Ti02 powder, thereby rendering said coated Ti02 powder non-photoactive.
4. The coated ceramic powder of claim 1 wherein said ceramic iε Al203.
5. The coated ceramic powder of claim 1 wherein said ceramic is ZnO.
6. The coated ceramic powder of claim 1 wherein said ceramic is an iron oxide.
7. The coated ceramic powder of claim 6 wherein said iron oxide is 7-Fe203. - -
8. The coated ceramic powder of claim 6 wherein said iron oxide is α-Fe-Oj.
9. The coated ceramic powder of claim 6 wherein said iron oxide is Fe30,.
10. The coated ceramic powder of claim 1 wherein said ceramic is Si02.
11. The coated ceramic powder of claim l wherein: w is tetraethylorthosilicate; x is selected from the group consisting of γ-glycidoxypropyltrimethoxysilane, n- hexyltrimethoxysilaπe, isobutyltrimethoxy-' silane, γ-methacryloxypropyltrimethoxysilane, n-octadecyltrimethoxyεilane, and n-propyltri- methoxysilane; y is selected from the group consisting of dicyclohexyldimethoxysilane, diethyldieth- oxysilane, dimethyldichlorosilane, dimethyl- diethoxysilane, dimethyldimethoxysilane, diphenyldiethoxysilane, diphenyldimethoxy- silane, di-n-hexyldichlorosilane, n-hexyl- methyldichlorosilane, methyldodecyldiethoxy- silane, neophylmethyldimethoxysilane, and n- octylmethyldimethoxysilane; and z is selected from the group consisting of n-octadecyldimethylmethoxysilane, triethyl- silanol, trimethylethoxysilane, and trimethyl- methoxysilane.
12. A method of preparing a coated ceramic powder comprising a plurality of ceramic particles and a siloxane star-graft coating polymer encapsulating at least a portion of said particles, the method comprising the steps of : (a) polymerizing tetrafunctional, trifunctional, difunctional and monofunctional siloxane monomers;
(b) adding a quantity of ceramic powder to a reaction vessel;
(c) shear mixing said ceramic powder for a time sufficient to wet substantially all of said powder surface; (d) adding the siloxane polymer prepared in step (a) to said reaction vessel containing said shear mixed ceramic powder;
(e) shear mixing said shear mixed ceramic powder and said siloxane polymer for a time sufficient to form a siloxane polymer coated ceramic powder;
(f) separating said coated ceramic powder from the components remaining in said reaction vessel.
13. The method of claim 12 wherein said ceramic is Tiθ2.
14. The method of claim 13 wherein a further quantity of aluminum tri-sec-butoxide is added to the reaction vessel in step (b) to introduce surface defects into said TiO- powder, thereby rendering said coated Ti02 powder non-photoactive.
15. The method of claim 12 wherein said ceramic is A1203.
16. The method of claim 12 wherein said ceramic is ZnO.
17. The method of claim 12 wherein said ceramic is an iron oxide.
18. The method of claim 17 wherein said iron oxide is γ-Fe203.
19. The method of claim 17 wherein said iron oxide is α-Fe203.
20. The method of claim 17 wherein said iron oxide is Fe30<.
21. The method of claim 12 wherein said ceramic is Si02.
22. The method of claim 12 wherein: said tetrafunctional siloxane monomer is tetraethylorthosilicate,- said trifunctional siloxane monomer is selected from the group consisting of γ- glycidoxypropyltrimethoxyeilane, n- hexyltrimethoxysilane, isobutyltrimethoxy- silane, γ-methacryloxypropyltrimethoxysilane, n-octadecyltrimethoxysilane, and n-propyltri- methoxysi1ane; said difunctional siloxane monomer is selected from the group conεisting of dicyclohexyldimethoxysilane, diethyldiethoxysilane, dimethyldichlorosilane, dimethyldiethoxyεilane, dimethyldimeth- oxyeilane, diphenyldiethoxysilane, diphenyldi- methoxysilane, di-n-hexyldichlorosilane, n- hexylmethyldichlorosilane, methyldodecyl- diethoxysilane, neophylmethyldimethoxysilane, and n-octylmethyldimethoxysilane; and said monofunctional siloxane monomer is selected from the group consisting of n- _24_ 1
octadecyldimethylmethoxysilane, triethyleilanol, trimethylethoxysilane, and trimethyl-methoxysilaπe.
23. The coated ceramic powder prepared according to the method of any one of claims 12-22.
24. A siloxane star-graft polymer for coating and encapsulating ceramic particles, said coating polymer comprising:
Figure imgf000007_0001
where w, x, y and z are the mole percent tetrafunctional, trifunctional, difunctiσnal and monofunctional monomeric units, respectively, and wherein w, x, y and z are about 45-75, 5-25, 5-45 and 5-10, respectively.
25. The star-graft polymer of claim 24 wherein: w is tetraethylorthosilicate,- x is selected from the group consisting of γ-glycidoxypropyltrimethoxysilane, n- hexyltrimethoxysilane, isobutyltrimethoxy- silane, γ-methacryloxypropyltrimethoxysilane, n-octadecyltrimethoxysilane, and n-propyltri- methoxysilane; y ie selected from the group consisting of dicyclohexyldimethoxyεilane, diethyldieth¬ oxysilane, dimethyldichlorosilane, dimethyl- diethoxyεilane, dimethyldimethoxysilane, diphenyldiethoxysilane, diphenyldimethoxy- silane, di-n-hexyldichlorosilane, n-hexyl- methyldichlorosilane, methyldodecyldiethoxy- εilane, neophylmethyldimethoxysilane, and n- octylmethyldimethoxysilane; and z is selected from the group consisting of n-octadecyldimethylmethoxysilane, triethyl- εilanol, trimethylethoxysilane, and trimethyl- methoxysilane.
PCT/US1997/005179 1996-04-04 1997-03-28 Siloxane star-graft polymers, ceramic powders coated therewith and method of preparing coated ceramic powders Ceased WO1997038041A1 (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
AU24271/97A AU715859B2 (en) 1996-04-04 1997-03-28 Siloxane star-graft polymers, ceramic powders coated therewith and method of preparing coated ceramic powders
EP97919963A EP0891387B1 (en) 1996-04-04 1997-03-28 Siloxane star-graft polymers, ceramic powders coated therewith and method of preparing coated ceramic powders
JP9536259A JP2000508684A (en) 1996-04-04 1997-03-28 Siloxane star graft polymer, ceramic powder coated thereby, and method for preparing coated ceramic powder
CA002250962A CA2250962C (en) 1996-04-04 1997-03-28 Siloxane star-graft polymers, ceramic powders coated therewith and method of preparing coated ceramic powders
DE69729290T DE69729290T2 (en) 1996-04-04 1997-03-28 STARTER-MOLDED SILOXANE POLYMERS, CERAMIC POWDER COATED THEREFOR, AND A METHOD FOR THE PRODUCTION THEREOF

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US1483896P 1996-04-04 1996-04-04
US60/014,838 1996-04-04

Publications (2)

Publication Number Publication Date
WO1997038041A1 WO1997038041A1 (en) 1997-10-16
WO1997038041B1 true WO1997038041B1 (en) 1997-11-06

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Country Status (7)

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US (1) US6033781A (en)
EP (1) EP0891387B1 (en)
JP (2) JP2000508684A (en)
AU (1) AU715859B2 (en)
CA (1) CA2250962C (en)
DE (1) DE69729290T2 (en)
WO (1) WO1997038041A1 (en)

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