IP Library Granted Patent US 10,287,411
Granted Patent B2
US 10,287,411 · App. 15/297,276 · Granted May 14, 2019

Highly branched non-crosslinked aerogel, methods of making, and uses thereof

Inventors: Garrett Poe (San Antonio, TX); Alan Sakaguchi (San Antonio, TX); Nicole Lambdin (San Antonio, TX)
Assignee: Blueshift Materials, Inc.
C08J9/286B01D71/64C08G73/10C08G73/1046C08J9/26C08J9/28C08J2201/048C08J2201/0482C08J2201/0502C08J2205/026C08J2205/05C08J2300/202C08J2379/08
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Quick Facts
Patent No.
US 10,287,411
App. No.
15/297,276
Granted
May 14, 2019
Kind
B2
Abstract

Aerogel compositions, methods for preparing the aerogel compositions, articles of manufacture that include or are made from the aerogel compositions are described and uses thereof. The aerogels include a branched polyimide matrix with little to no crosslinked polymers.

Claims (38)

1. An aerogel comprising:

(a) an open-cell structure; and

(b) a branched polyimide matrix comprising polyimide polymer chains, wherein matrix contains less than 5% by weight of crosslinked polymers, and

wherein the branched polyimide matrix has a degree of branching of at least 0.5 branches per polyimide polymer chain.

2. The aerogel of claim 1 , wherein the branched polyimide matrix contains less than 1% by weight of crosslinked polymers or is not crosslinked.

3. The aerogel of claim 1 , wherein the degree of branching is from 0.5 to 10.

4. The aerogel of claim 3 , wherein the degree of branching is 6.3.

5. The aerogel of claim 1 , wherein the branched polyimide matrix has a general structure of:

where:

R 1 is multifunctional amine residue;

Z is a dianhydride residue;

R 2 is a diamine residue;

R 3 and R 4 are each individually a capping group, and are independently selected from a hydrogen, an anhydride residue, an isocyanate residue, an acid residue, or an alkyl group;

m is a solution average number per chain ranging from 0.5 to 10; and

n is 1 to 25.

6. The aerogel of claim 5 , wherein the dianhydride residue is a 3,3′,4,4′-biphenyltetracarboxylic dianhydride residue, a pyromellitic dianhydride residue, or a 3,3′,4,4′-benzophenone-tetracarboxylic dianhydride residue.

7. The aerogel of claim 6 , wherein the dianhydride residue is a biphenyl-3,3′,4,4′-tetracarboxylic dianhydride residue.

8. The aerogel of claim 5 , wherein R 1 is a substituted or unsubstituted multifunctional amine residue comprising at least three primary amine functionalities and R 2 is at least one substituted or unsubstituted diamine residue.

9. The aerogel of claim 8 , wherein the multifunctional amine residue is a substituted or an unsubstituted aliphatic multifunctional amine residue or a substituted or an unsubstituted aromatic multifunctional amine residue.

10. The aerogel of claim 9 , wherein the aromatic multifunctional amine residue is a 1,3,5,-tris(4-aminophenoxy)benzene residue, a 4,4′,4″-methanetriyltrianiline residue, a N,N,N′,N′-tetrakis(4-aminophenyl)-1,4-phenylenediamine residue, or a polyoxypropylenetriamine residue.

11. The aerogel of claim 9 , wherein the diamine residue is a substituted or unsubstituted aromatic diamine residue, a substituted or an unsubstituted alkyldiamine residue, or combinations thereof.

12. The aerogel of claim 11 , wherein the diamine residue is a 4,4′-oxydianiline residue or a 2,2′-dimethylbenzidine residue, or both.

13. The aerogel of claim 5 , where:

R 1 is selected from:

or any combination thereof; and

R 2 is selected from:

or any combination thereof.

14. The aerogel of claim 5 , wherein the molar ratio of the anhydride residue to the total diamine residue is from 0.80:1 to 1.2:1.

15. The aerogel of claim 5 , wherein the molar ratio of the anhydride residue to the multifunctional amine residue is 8:1 to 125:1.

16. The aerogel of claim 1 , wherein the polyimide further comprises a mono-anhydride group.

17. A method of making the aerogel of claim 1 , the method comprising:

(a) providing at least one dianhydride compound to a solvent to form a solution or mixture;

(b) providing a multifunctional amine compound and at least one diamine compound to the solution or mixture of step (a) under conditions sufficient to form a branched polymer matrix solution, wherein the branched polymer matrix is solubilized in the solution; and

(c) subjecting the branched polymer matrix solution to conditions sufficient to form an aerogel having an open-cell structure.

18. A method of making the aerogel of claim 1 , the method comprising:

(a) providing a multifunctional amine compound and at least one diamine compound to a solvent to form a solution;

(b) providing at least one dianhydride compound to the solution of step (a) under conditions sufficient to form a branched polymer matrix solution, wherein the branched polymer matrix is solubilized in the solution; and

(c) subjecting the branched polymer matrix solution to conditions sufficient to form an aerogel having an open-cell structure.

Assignments (2)
CHANGE OF NAME Recorded Feb 21, 2019
From: BLUESHIFT INTERNATIONAL MATERIALS, INC.
To: BLUESHIFT MATERIALS, INC.
Reel/Frame 048408/0409 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 19, 2016
From: POE, GARRETT; SAKAGUCHI, ALAN; LAMBDIN, NICOLE; KOLDAN, KENNETH
To: BLUESHIFT INTERNATIONAL MATERIALS, INC.
Reel/Frame 040059/0485 →
Continuity (5)
Provisional Application 62248763 · Oct 30, 2015
Provisional Application 62262055 · Dec 2, 2015
Provisional Application 62337947 · May 18, 2016
Provisional Application 62408862 · Oct 17, 2016
Related Publication 20170121483A1 · May 4, 2017
Cited By (1)
US 12,404,382