Amino-containing silica particle, composition for forming polyimide aerogel, polyimide aerogel and method of fabricating the same, polyimide aerogel-containing composite material

Patent metadata

Field	Value
Publication number	US-2017183470-A1
Application number	US-201615051685-A
Country	US
Kind code	A1
Filing date	Feb 24, 2016
Priority date	Dec 25, 2015
Publication date	Jun 29, 2017
Grant date	—

Abstract

An amino-containing silica particle is provided. The amino-containing silica particle is obtained by hydrolysis-condensation reaction of an alkoxy silane represented by formula (I), an alkoxy silane represented by formula (II) and a catalyst:
Si(OR 1 ) 4   formula (I)

(NH 2 —Y) m —Si(OR 2 ) 4-m   formula (II)

wherein in formula (I), R 1 is a C 1 -C 10 alkyl group, and in formula (II), Y is a C 1 -C 10 alkyl group or a C 2 -C 10 alkenyl group, R 2 is a C 1 -C 10 alkyl group, and m is an integer of 1 to 3.

First claim

What is claimed is:

1 . An amino-containing silica particle is obtained by hydrolysis-condensation reaction of an alkoxy silane represented by formula (I), an alkoxy silane represented by formula (II) and a catalyst:
Si(OR 1 ) 4   formula (I)
(NH 2 —Y) m —Si(OR 2 ) 4-m   formula (II)
wherein in formula (I), R1 is a C1-C10 alkyl group; and in formula (II), Y is a C 1 -C 10 alkyl group or a C 2 -C 10 alkenyl group, R 2 is a C 1 -C 10 alkyl group, and m is an integer of 1 to 3.

2 . The amino-containing silica particle according to claim 1 , wherein an equivalent number of amino group of the amino-containing silica particle is 5 mmole/g to 10 mmole/g.

3 . The amino-containing silica particle according to claim 1 , wherein the alkoxy silane represented by formula (I) comprises tetraethoxysilane, and the alkoxy silane represented by formula (II) comprises 3-aminopropyltriethoxysilane.

4 . A composition for forming a polyimide aerogel, comprising:
a diamine monomer; a tetracarboxylic dianhydride monomer, and a molar ratio of the diamine monomer to the tetracarboxylic dianhydride monomer is 1:1 to 1:1.5; the amino-containing silica particle according to claim 1 , and a weight percent of the amino-containing silica particle is 10 wt % to 40 wt %, based on a total weight of the composition for forming the polyimide aerogel; and a solvent.

5 . The composition for forming the polyimide aerogel according to claim 4 , wherein a solid content of the composition for forming the polyimide aerogel is 5 wt % to 20 wt %.

6 . The composition for forming the polyimide aerogel according to claim 4 , wherein the diamine monomer is 4,4′-oxydianiline (ODA), 3,3′-dimethylbenzidine (DMB), p-phenylenediamine (p-PDA), m-phenylenediamine (m-PDA), 2,2′-bis[4-(4-aminophenoxyphenyl)] propane (BAPP), or 2,2-bis(trifluoromethyl) benzidine (TFMB), and the tetracarboxylic dianhydride monomer is 3,3′,4,4′-biphenyltetracarboxylic dianhydride (BPDA), pyromellitic dianhydride (PMDA), 3,3′,4,4′-benzophenone tetracarboxylic dianhydride (BTDA), 4,4′-oxydiphthalic anhydride (ODPA), or 4,4′-(hexafluoroisopropylidene)diphthalic anhydride (6FDA).

7 . The composition for forming the polyimide aerogel according to claim 4 , wherein the solvent is selected from at least one of N-methylpyrrolidone, dimethylacetamide, dimethylformamide, tetrahydrofuran, and phenol.

8 . A method of fabricating a polyimide aerogel, comprising:
mixing a diamine monomer, a tetracarboxylic dianhydride monomer, and an amino-containing silica particle in a solvent uniformly to obtain the composition for forming the polyimide aerogel according to claim 4 ; performing a polycondensation and cyclization reaction of the composition for forming the polyimide aerogel to form a wet gel; performing a solvent exchange treatment on the wet gel with a mixture solution of acetone and water; and performing a drying treatment on the wet gel which has been subjected to the solvent exchange treatment.

9 . The method of fabricating the polyimide aerogel according to claim 8 , wherein a volume ratio of acetone to water in the mixture solution of acetone and water is 10:90 to 90:10.

10 . The method of fabricating the polyimide aerogel according to claim 8 , further comprising adding a crosslinking agent into the wet gel before performing the solvent exchange treatment.

11 . The method of fabricating the polyimide aerogel according to claim 10 , wherein an additive amount of the crosslinking agent is 1 wt % to 10 wt %, based on a total weight of the wet gel.

12 . The method of fabricating the polyimide aerogel according to claim 10 , wherein the crosslinking agent is a diisocyanate-based crosslinking agent, a diamine crosslinking agent, a triamine crosslinking agent, or a glycol-based crosslinking agent.

13 . The method of fabricating the polyimide aerogel according to claim 8 , further comprising adding a surfactant into the mixture solution of acetone and water.

14 . The method of fabricating the polyimide aerogel according to claim 13 , wherein an additive amount of the surfactant is 0.01 wt % to 1 wt %, based on a total weight of the mixture solution of acetone and water.

15 . The method of fabricating the polyimide aerogel according to claim 13 , wherein the surfactant is a fluorine-based surfactant.

16 . A polyimide aerogel is fabricated by the method of fabricating the polyimide aerogel according to claim 8 .

17 . The polyimide aerogel according to claim 16 , wherein a porosity of the polyimide aerogel is 85% to 95%.

18 . The polyimide aerogel according to claim 16 , wherein a thickness of the polyimide aerogel is 0.1 mm to 1 mm.

19 . A polyimide aerogel-containing composite material, comprising:
a fabric; and the polyimide aerogel according to claim 16 , wherein the fabric and the polyimide aerogel are composited with each other.

Assignees

• Taiwan Textile Res Inst

Inventors

• Chou Shang-Chih
• Hsiao Meng-Tzu

Classifications

• C08J9/16

  Making expandable particles · CPC title

• C01B33/12

  Silica; Hydrates thereof, e.g. lepidoic silicic acid · CPC title

• C08J9/286

  the liquid phase being a solvent for the monomers but not for the resulting macromolecular composition, i.e. macroporous or macroreticular polymers · CPC title

• C08J2379/08

  Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors · CPC title

• C08J2201/05

  Elimination by evaporation or heat degradation of a liquid phase · CPC title