[미국특허]
Organically modified aerogels, processes for their preparation by surface modification of the aqueous gel, without prior solvent exchange, and subsequent drying, and their use
원문보기
IPC분류정보
국가/구분
United States(US) Patent
등록
국제특허분류(IPC7판)
C01B-033/18
C01B-033/00
C01B-033/193
B05D-007/00
B01J-013/00
출원번호
US-0817459
(2001-03-26)
등록번호
US-7470725
(2008-12-30)
우선권정보
DE-196 48 798(1996-11-26)
발명자
/ 주소
Schwertfeger,Fritz
Frank,Dierk
출원인 / 주소
Cabot Corporation
인용정보
피인용 횟수 :
8인용 특허 :
64
초록▼
The present invention relates to novel, organically modified aerogels, uses thereof, and a process for producing them in which a) a hydrogel is introduced as an initial charge, b) the hydrogel obtained in step a) is subjected to surface modification, and c) the surface-modified gel obtained in step
The present invention relates to novel, organically modified aerogels, uses thereof, and a process for producing them in which a) a hydrogel is introduced as an initial charge, b) the hydrogel obtained in step a) is subjected to surface modification, and c) the surface-modified gel obtained in step b) is dried. The present invention additionally relates to novel, organically modified wet gels, to a process for producing them, and to their use.
대표청구항▼
The invention claimed is: 1. A process for preparing an organically modified aerogel, which comprises: a) introducing an inorganic hydrogel formed at pH greater than 3 as initial charge, b) modifying the surface of the hydrogel obtained in step a) by mixing the hydrogel with a silylating agent to f
The invention claimed is: 1. A process for preparing an organically modified aerogel, which comprises: a) introducing an inorganic hydrogel formed at pH greater than 3 as initial charge, b) modifying the surface of the hydrogel obtained in step a) by mixing the hydrogel with a silylating agent to form a hydrophobic surface modified gel, and c) drying the surface-modified gel obtained in step b) to form the organically modified aerogel. 2. The process according to claim 1, wherein the hydrogel obtained in step a) is aged before being surface-modified in step b). 3. The process as claimed in claim 1, wherein the silylating agent is used in liquid form and/or as a gas or vapor. 4. The process as claimed in claim 1, wherein the silylating agent employed comprises at least one silane of the formula R4-n1SiCln or R4-n1Si(OR2)n where n=1 to 4 and where R1 and R2 independently of one another are identical or different and are each a hydrogen atom or a nonreactive, organic, linear, branched, cyclic, saturated or unsaturated, aromatic or heteroaromatic radical. 5. The process as claimed in claim 4, wherein trimethylchlorosilane is employed as silylating agent. 6. The process as claimed in claim 1, wherein the silylating agent employed comprises at least one disiloxane of the formula I and/or one disilazane of the formula II description="In-line Formulae" end="lead"R3Si--O--SiR3 (I)description="In-line Formulae" end="tail" description="In-line Formulae" end="lead"R3Si--N(H)--SiR3 (II)description="In-line Formulae" end="tail" where the radicals R, independently of one another, are identical or different and are each a hydrogen atom or a nonreactive, organic, linear, branched, cyclic, saturated or unsaturated, aromatic or heteroaromatic radical. 7. The process as claimed in claim 6, wherein the silylating agent employed in step b) is a symmetrical disiloxane. 8. The process as claimed in claim 6, wherein the silylating agent employed in step b) is disiloxane in which all radicals R are identical. 9. The process as claimed in claim 6, wherein the silylating agent employed is hexamethyldisiloxane. 10. The process as claimed in claim 1, wherein at least one acid and/or base is introduced as a catalyst in the hydrogel before surface modification. 11. The process as claimed in claim 10, wherein HCl is used as acid. 12. The process as claimed in claim 1, wherein the hydrogel is introduced as initial charge in the silylating agent, and then at least one acid and/or base is added. 13. The process as claimed in claim 12, wherein HMDSO is used as silylating agent. 14. The process as claimed in claim 12 wherein hydrochloric acid is used as acid. 15. The process as claimed in claim 1, wherein the silylating agent is generated shortly before and/or during the surface modification. 16. The process of claim 15, wherein the silylating agent is generated shortly before or during the surface modification by means of an acid. 17. The process as claimed in claim 1, wherein the surface modification is accelerated by means of a catalyst. 18. The process as claimed in claim 1, wherein at least one carrier gas or carrier gas stream is used in step b) in addition to the silylating agent. 19. The process as claimed in claim 1, wherein some of the water in pores of the hydrogel reacts with the silylating agent to form a water-insoluble compound. 20. The process as claimed in claim 19, wherein HMDSO is formed. 21. The process as claimed in claim 1, wherein an outer surface of the hydrogel obtained in step a) is dried prior to surface modification. 22. The process as claimed in claim 1, wherein the surface-modified gel is washed with a protic or aprotic solvent prior to step c). 23. The process as claimed in claim 1, wherein the surface-modified gel is washed with the a silylating agent prior to step c). 24. The process as claimed in claim 1, wherein the surface-modified gel is subjected to subcritical drying in step c). 25. The process as claimed in claim 1, wherein the gel obtained in step a) is reacted, prior to silylation, with a solution of a condensable orthosilicate of the formula R4-n1Si(OR2)n, where n=2 to 4 and R1 and R2 independently of one another are hydrogen atoms or linear or branched C1-C6-alkyl, cyclohexyl or phenyl radicals, or with an aqueous silicic acid solution. 26. The process of claim 25, wherein said condensible orthosilicate is an alkyl or aryl orthosilicate. 27. The process as claimed in claim 1, wherein surface modification is carried out in the presence of additives in the hydrogel. 28. The process as claimed in claim 27, wherein the additives comprise ionic compounds. 29. The process of claim 28, wherein the additives used comprise NaCl. 30. The process as claimed in claim 27, wherein the additives comprise opacifiers. 31. The process as claimed in claim 30, wherein the additives used as opacifiers comprise IR opacifiers. 32. The process according to claim 1, wherein step a) and b) are carried out as a semi-continuous process. 33. The process according to claim 1, wherein steps a) and b) are carried out as a continuous process. 34. The process according to claim 1, wherein step b) results in a hydrophobic gel in a liquid phase substantially immiscible with water, which liquid is separated from an aqueous phase formed by the water from the hydrogel. 35. The process as claimed in claim 1 in which the inorganic hydrogel is a silicatic hydrogel. 36. A process for preparing an organically modified aerogel, which comprises a) introducing a hydrogel formed at pH greater than 3 as initial charge, b) modifying the surface of the hydrogel obtained in step a) by mixing the hydrogel with a silylating agent to form a hydrophobic surface modified gel, and c) drying the surface-modified gel obtained in step b) to form the organically modified aerogel, wherein a silicatic hydrogel is introduced as initial charge in step a). 37. The process as claimed in claim 36, wherein the silicatic hydrogel introduced as initial charge in step a) is prepared by obtaining it from an aqueous waterglass solution with the aid of at least one organic and/or inorganic acid via the intermediate stage of a silica sol. 38. The process as claimed in claim 36, wherein additives are added before and/or during the preparation of the silicatic hydrogel. 39. The process as claimed in claim 38, wherein additives added are opacifiers and/or fibers. 40. The process according to claim 36 in which the silicatic hydrogel comprises zirconium, aluminum, titanium, vanadium and/or iron compounds. 41. A process for preparing an organically modified aerogel, which comprises: a) forming a silicatic hydrogel at pH≧3; b) subjecting the silicatic hydrogel formed in step a), optionally after intermediate treatment steps, to surface modification by mixing the hydrogel with a silylating agent to form a surface modified gel; and c) drying the surface modified gel obtained in step b), optionally after additional treatment steps, to form the organically modified aerogel wherein the silicatic hydrogel is prepared by bringing an aqueous waterglass solution to a pH≦3 with the aid of an acidic ion exchanger resin or a mineral acid, and polycondensing the resulting silicic acid by addition of a base to form an SiO2 gel. 42. The process of claim 41 further comprising washing the silicatic hydrogel with water to free it from any electrolyte. 43. A process for producing an organically modified aerogel, which comprises: a) forming a hydrogel at pH>3; b) surface modifying the hydrogel formed in step a), optionally after intermediate treatment steps, by mixing the hydrogel with a silylating agent to form a surface modified gel; and c) optionally after additional treatment steps, drying the surface modified gel obtained in step b) to form the organically modified aerogel; wherein steps a) and b) are carried out as a semi-continuous process, wherein a continuous or semi-continuous stream of acid is mixed with a continuous or semi-continuous stream of aqueous waterglass solution. 44. The process according to claim 43, wherein the acid stream is admixed with the aqueous waterglass solution through a mixing nozzle. 45. The process for producing an organically modified aerogels according to claim 43, wherein the hydrogel is formed in step a) at pH between pH 3 and pH 8. 46. A process for producing an organically modified aerogels, wherein: a) a hydrogel is formed at pH≧3; b) the hydrogel formed in step a), optionally after intermediate treatment steps, is subjected to surface modification by mixing the hydrogel with a silylating agent to form a surface modified gel; and c) the surface modified gel obtained in step b), optionally after additional treatment steps, is dried to form the organically modified aerogel; wherein step a) and b) are carried out as a continuous process and a continuous or semi-continuous stream of acid is mixed with a continuous or semi-continuous stream of aqueous waterglass solution.
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Mueller Hans-Joachim (Gruenstadt DEX) Follmer Godofredo (Maxdorf DEX) Konrad Rainer (Goennheim DEX) Saive Roland (Ludwigshafen DEX) Lux Martin (Dannstadt-Schauernheim DEX) Goertz Hans-Helmut (Freinsh, Preparation of a supported catalyst for the polymerization of a
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