Inorganic/organic hybrid totally porous metal oxide particles, methods for making them and separation devices using them
원문보기
IPC분류정보
국가/구분
United States(US) Patent
등록
국제특허분류(IPC7판)
C08G-077/00
B01J-020/00
C01B-033/12
C01G-023/047
C01G-027/02
C01F-007/02
출원번호
US-0201817
(2008-08-29)
등록번호
US-8357628
(2013-01-22)
발명자
/ 주소
Wei, Ta-Chen
Chen, Wu
Barber, William E.
출원인 / 주소
Agilent Technologies, Inc.
인용정보
피인용 횟수 :
1인용 특허 :
7
초록
The present invention is a process for making an inorganic/organic hybrid totally porous spherical silica particles by self assembly of surfactants that serve as organic templates via pseudomorphic transformation.
대표청구항▼
1. A method for making totally porous organically modified metal oxide hybrid particles, comprising: subjecting substantially totally porous metal oxide particles selected from silica, alumina, zirconia, or titania, in an aqueous solution to agitation for a time and a pH sufficient to pseudomorphica
1. A method for making totally porous organically modified metal oxide hybrid particles, comprising: subjecting substantially totally porous metal oxide particles selected from silica, alumina, zirconia, or titania, in an aqueous solution to agitation for a time and a pH sufficient to pseudomorphically transform said metal oxide particles, in the presence of one or more surfactants, wherein the pseudomorphic transformation of the metal oxide particles is carried out in the presence of an organic metal alkoxide to form the totally porous organically modified metal oxide hybrid particles. 2. The method of claim 1 wherein the starting totally porous particles are substantially pure metal oxide particles selected from silica, titania or zirconia and the pseudomorphic transformation of the particles is carried out in the presence of an organic metal alkoxide selected from one or more of the formulae I-IV (RO)3M-R2-M(OR)3 (I)(RO)2R1M-R2-MR1(OR)2 (II)(RO)3M-R1 (III)(RO)2M-R1R1 (IV)whereinR is selected independently in each instance from methyl and ethyl,R1 is independently selected in each instance from a substituted or unsubstituted C1 to C18 alkyl, alkenyl, alkynyl, or aryl group, wherein the substituents are selected from halogen, diol, amino-, alcohol, amide, cyano, ether, nitro, carbonyl, epoxide, sulfonyl, cation exchanger, anion exchanger, carbamate and urea, andR2 is selected from a substituted or unsubstituted C1 to C7 alkylene, alkenylene, alkynylene, or arylene group bridging two or more M atoms; and M is selected from Si, Ti and Zr. 3. The method of claim 2 wherein M is Si. 4. The method of claim 3 wherein the organic metal alkoxide is selected from one or more of methyltriethoxysilane, ethyltriethoxysilane, 1,2-bis(triethoxysilyl)methane, 1,2-bis(triethoxysilyl)ethane and 1,2-bis(triethoxysilyl)benzene. 5. The method of claim 2 wherein M is Ti. 6. The method of claim 2 wherein M is Zr. 7. The method of claim 1 wherein the starting totally porous particles are substantially pure alumina particles and the organic metal alkoxide is selected from one or more of the formulae V or VI: (RO)2Al—R3—Al(OR)2 (V)(RO)2Al—R1 (VI)whereinR is selected independently in each instance from methyl and ethyl,R1 is selected from a substituted or unsubstituted C1 to C18 alkyl, alkenyl, alkynyl, or aryl group, wherein the substituents are selected from halogen, diol, amino-, alcohol, amide, cyano, ether, nitro, carbonyl, epoxide, sulfonyl, cation exchanger, anion exchanger, carbamate and urea, andR3 is selected from a substituted or unsubstituted C1 to C7 alkylene, alkenylene, alkynylene, or arylene group bridging two or more Al atoms. 8. The method of claim 1 wherein the starting totally porous metal oxide particles have a median particle size from about 0.5 μm to about 100 μm. 9. The method of claim 1 wherein the starting totally porous metal oxide particles comprise an organic metal oxide selected from one or more of the formulae VII or VIII MO2/(R1pR1qMOt)n (VII)MO2/[R2(R1rMOt)m]n (VIII)whereinR1 is independently selected in each instance from a substituted or unsubstituted C1 to C15 alkyl, alkenyl, alkynyl, or aryl group, wherein the substituents are selected from halogen, diol, amino-, alcohol, amide, cyano, ether, nitro, carbonyl, epoxide, sulfonyl, cation exchanger, anion exchanger, carbamate and urea,R2 is a substituted or unsubstituted C1 to C7 alkylene, alkenylene, alkynylene, or arylene group moiety bridging two or more M atoms,p and q are 0, 1, or 2, provided that p+q=1 or 2, and that when p+q=1, t=1.5, and when p+q=2,r is 0 or 1, provided that when r=0, t=1.5, and when r=1, t=1;m is an integer greater than or equal to 2; and n is a number from 0.01 to 100; andM is selected from Si, Ti, or Zr. 10. The method of claim 1 wherein the starting totally porous metal oxide particles comprise an organic metal oxide selected from one or more of the formulae IX or X: Al2O3/(R1AlO)n (IX)Al2O3/[R2(AlO)m]n (X)whereinR1 is a substituted or unsubstituted C1 to C18 alkyl, alkenyl, alkynyl, or aryl group, wherein the substituents are selected from halogen, diol, amino-, alcohol, amide, cyano, ether, nitro, carbonyl, epoxide, sulfonyl, cation exchanger, anion exchanger, carbamate and urea,R2 is a substituted or unsubstituted C1 to C7 alkylene, alkenylene, alkynylene, or arylene, or polar embedded C1 to C7 alkylene, alkenylene, alkynylene, or arylene group moiety bridging two or more Al atoms;m is an integer greater than or equal to 2; andn is a number from 0.01 to 100. 11. The method of claim 1 wherein said surfactant is selected from one or more ionic surfactants or non-ionic surfactants. 12. The method of claim 11, wherein the surfactant is selected from one or more of the group of polyoxyethylene sorbitans, polyoxythylene ethers, tri-block copolymers, alkyltrimethylammonium, alkyl phosphates, alkyl sulfates, alkyl sulfonates, sulfosuccinates, carboxylic acid, surfactants comprising an octylphenol polymerized with ethylene oxide, and combinations thereof. 13. The method of claim 12 wherein the surfactant is selected from one or more of a compound of the formula CnH2n+1(CH3)3NX wherein X is chlorine or bromine and n is an integer from 10 to 20. 14. The method of claim 13 wherein the surfactant is selected from one or more of trimethyloctadecylammonium bromide and hexadecyltrimethylammonium bromide. 15. The method of claim 1 wherein the starting totally porous particles comprise silica and the pH of the solution is from about 10 to about 13.5. 16. The method of claim 15 wherein the pH of the solution is from about 12 to about 13.5. 17. The method of claim 1 wherein the particles comprise silica and the solution comprises a fluoride ion from a source selected from hydrofluoric acid or ammonium fluoride. 18. The method of claim 1 wherein the agitation is done under reflux for less than about 7 days. 19. The method of claim 1 wherein the solid particles and surfactant are subjected to reflux in the presence of a swelling agent, which swelling agent adjusts the size of micelles formed by the surfactant. 20. The method of claim 19 wherein the swelling agent is selected from an alkyl substituted benzene, a dialkylamine, a trialkylamine, a tertraalkyl ammonium salt or an alkane of the formula CnH2n+2 where n is an integer from 5 to 20, a cycloalkane of the formula (CnH2n) where n is an integer of 5-20, a substituted alkane of the formula (X—CnH2n+1) where n is an integer of 5-20 and X is chloro-, bromo-, or —OH, or a substituted cycloalkane of the formula (X—CnH2n−1) where n is an integer of 5-20 and X is chloro-, bromo-, or —OH. 21. The method of claim 20 wherein the swelling agent is selected from trimethylbenzene, triisopropylbenzene, N,N-dimethylhexadecylamine, N,N-dimethyldecylamine, trioctylamine, tridodecylamine, cyclohexane, cyclohexanol, dodecanol, chlorododecane and tetramethylammonium and tetraethylammonium sodium salts.
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이 특허에 인용된 특허 (7)
Beck Jeffrey S. (Princeton NJ), Method for synthesizing mesoporous crystalline material.
Jiang, Zhiping; Fisk, Raymond P.; O'Gara, John; Walter, Thomas H.; Wyndham, Kevin D., Porous inorganic/organic hybrid particles for chromatographic separations and process for their preparation.
Jiang,Zhiping; Fisk,Raymond P.; O'Gara,John; Walter,Thomas H.; Wyndham,Kevin D., Porous inorganic/organic hybrid particles for chromatographic separations and process for their preparation.
Kresge Charles T. (West Chester PA) Leonowicz Michael E. (Medford Lakes NJ) Roth Wieslaw J. (Sewell NJ) Vartuli James C. (West Chester PA), Synthetic mesoporous crystaline material.
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