Organically modified hybrid aerogels

Patent metadata

Field	Value
Publication number	US-9284412-B2
Application number	US-201514726885-A
Country	US
Kind code	B2
Filing date	Jun 1, 2015
Priority date	Nov 18, 2010
Publication date	Mar 15, 2016
Grant date	Mar 15, 2016

Abstract

Disclosed and claimed herein are hybrid aerogels which are compositions of tetraalkoxysilanes and bis-(trialkoxysilyl) imides that exhibit low thermal conductivities and high compressive strengths. Methods for their preparation are also provided.

First claim

What is claimed is:

1. Hybrid aerogels comprising a polymeric network which comprises a silica component and diimide component, which are the reaction product of:
(a) at least one tetraalkoxysilane which may optionally be partially hydrolyzed,
(b) at least one bis-trialkoxysilane diimide, and
(c) a selected amount of water;
wherein a gelation catalyst is admixed to gel the reaction product; and wherein the gel is dried to obtain an aerogel.

2. The hybrid aerogel of claim 1 , wherein the at least one bis-trialkoxysilane diimide is a reaction product of: i) a primary amine terminated trialkoxysilane according to the following formula: H2N—R—Si—(OR′)3, wherein R comprises alkyl, alkenyl, alkynyl, cycloalkyl, or cycloalkenyl moities, or variations thereof which can contain at least one heteroatom comprising O, S, N, P, or Se, and R′ is a C1-C21 branched or unbranched alkyl group; and ii) a dicarboxylic anhydride.

3. The hybrid aerogel of claim 2 , wherein the diimide component of the polymeric network comprises a compound selected from Formula I, Formula II, or Formula III:

wherein R is selected from an alkyl, alkenyl, alkynyl, cycloalkyl, cycloalkenyl, aryl, aralkyl, or heterocyclic moiety, which can optionally contain one or more heteroatoms such as O, S, N, P, and Se;
A is selected from an alkyl, alkenyl, alkynyl, cycloalkyl, cycloalkenyl, aryl, aralkyl, or heterocyclic moiety, which can optionally contain a carbonyl moiety or one or more heteroatoms such as O, S, N, P, and Se;
X and Y are independently selected from a halogen, alkyl, alkenyl, alkynyl, cycloalkyl, cycloalkenyl, aryl, aralkyl, or heterocyclic moiety, which can optionally contain one or more heteroatoms such as O, S, N, P, and Se; and
B is an attachment to the silica component of the polymeric network.

4. The hybrid aerogel of claim 3 , wherein the diimide component of the polymeric network comprises a compound selected from Formula I; and wherein R is an alkyl moiety.

5. The hybrid aerogel of claim 4 , wherein the diimide content of the aerogel is 10 wt % or less; and wherein the compressive modulus of the aerogel is greater than about 175 pounds/square inch.

6. The hybrid aerogel of claim 3 , further comprising a fibrous material, comprising microfibers, mats, felts, woven fabrics, non-woven fabrics, fibrous battings, lofty battings or a combination thereof.

7. The hybrid aerogel of claim 3 , wherein the hybrid aerogel has a density of 0.40 g/cc or less.

8. A hybrid aerogel comprising a polymeric network which comprises a silica component and diimide component, wherein the diimide component is covalently bonded to one or more silica molecules within the silica component of the polymeric network, wherein the hybrid aerogel has a density of 0.70 g/cc or less.

9. The hybrid aerogel of claim 8 , wherein the hybrid aerogel has a density of 0.40 g/cc or less.

10. The hybrid aerogel of claim 9 , wherein the diimide component of the polymeric network comprises a compound selected from Formula I, Formula II, or Formula III:

wherein R is selected from an alkyl, alkenyl, alkynyl, cycloalkyl, cycloalkenyl, aryl, aralkyl, or heterocyclic moiety, which can optionally contain one or more heteroatoms such as O, S, N, P, and Se;
A is selected from an alkyl, alkenyl, alkynyl, cycloalkyl, cycloalkenyl, aryl, aralkyl, or heterocyclic moiety, which can optionally contain a carbonyl moiety or one or more heteroatoms such as O, S, N, P, and Se;
X and Y are independently selected from a halogen, alkyl, alkenyl, alkynyl, cycloalkyl, cycloalkenyl, aryl, aralkyl, or heterocyclic moiety, which can optionally contain one or more heteroatoms such as O, S, N, P, and Se; and
B is an attachment to the silica component of the polymeric network.

11. The hybrid aerogel of claim 10 , wherein R is selected from an alkyl, alkenyl, alkynyl, cycloalkyl, cycloalkenyl, aryl, aralkyl, or heterocyclic moiety.

12. The hybrid aerogel of claim 11 , wherein the diimide component of the polymeric network comprises a compound selected from Formula I; and wherein R is an alkyl moiety.

13. The hybrid aerogel of claim 10 , wherein the thermal conductivity of the aerogel is about 30 milliwatts/meter-degree Kelvin or less.

14. The hybrid aerogel of claim 10 , wherein the diimide content of the aerogel is 25 wt % or less.

15. The hybrid aerogel of claim 14 , wherein the compressive modulus of the aerogel is greater than about 175 pounds/square inch.

16. The hybrid aerogel of claim 10 , wherein the diimide content of the aerogel is 10 wt % or less.

17. The hybrid aerogel of claim 16 , wherein the compressive modulus of the aerogel is greater than about 175 pounds/square inch.

18. The hybrid aerogel of claim 10 , further comprising a fibrous material, comprising microfibers, mats, felts, woven fabrics, non-woven fabrics, fibrous battings, lofty battings or a combination thereof.

19. The hybrid aerogel of claim 10 , wherein the hybrid aerogel is a reaction product of: (a) at least one tetraalkoxysilane which may optionally be partially hydrolyzed; and (b) at least one bis-trialkoxysilane diimide.

20. The hybrid aerogel of claim 19 , wherein the at least one bis-trialkoxysilane diimide is a reaction product of: i) a primary amine terminated trialkoxysilane according to the following formula: H 2 N—R—Si—(OR′) 3 ; wherein R is selected from an alkyl, alkenyl, alkynyl, cycloalkyl, cycloalkenyl, aryl, aralkyl, or heterocyclic moiety, which can optionally contain one or more heteroatoms such as O, S, N, P, and Se; and R′ is a C1-C21 branched or unbranched alkyl group; and ii) a dicarboxylic anhydride.

Assignees

• Aspen Aerogels Inc
• Aspen Aerogel Inc

Inventors

• Dong Wenting
• Rhine Wendell E
• Coutinho Decio

Classifications

• B01J13/0091 Primary

  Preparation of aerogels, e.g. xerogels · CPC title

• C08K3/20

  Oxides; Hydroxides {(graphene oxides C08K3/042)} · CPC title

• C08G2220/00

  Compositions for preparing gels other than hydrogels, aerogels and xerogels · CPC title

• C08G77/54

  Nitrogen-containing linkages · CPC title

• E04B1/78

  Heat insulating elements {(E04B1/7662 takes precedence)} · CPC title