IP Library Granted Patent US 9,428,629
Granted Patent B2
US 9,428,629 · App. 13/212,783 · Granted Aug 30, 2016

Use of Li

Inventors: Eric A. Eastwood (Raymore, MO); Daniel E. Bowen, III (Olathe, KS)
Assignee: Honeywell Federal Manufacturing & Technologies, LLC
C08K3/38
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Quick Facts
Patent No.
US 9,428,629
App. No.
13/212,783
Granted
Aug 30, 2016
Kind
B2
Abstract

Methods of adjusting the properties of a composition are provided. The compositions comprise a polymer-containing matrix and a filler comprising a hygroscopic salt. Preferred such salts comprise a cage compound selected from the group consisting of borane cage compounds, carborane cage compounds, metal complexes thereof, residues thereof, mixtures thereof, and/or agglomerations thereof, where the cage compound is not covalently bound to the matrix polymer.

Claims (63)

1. A method of adjusting the properties of a material, said method comprising:

providing a composition comprising:

a matrix comprising a polymer; and

a filler comprising a hygroscopic salt; and

exposing said composition to moisture under conditions for said composition to absorb said moisture,

wherein said filler comprises a cage compound selected from the group consisting of

(a) a closo-carborane salt having the general formula [CB n -H n+1 ]X, wherein n is in the range of from 6 to 11, and X is selected from the group consisting of Li + , Na + , K + , Cs + , and a quaternary ammonium;

(b) a closo-carborane salt having the general formula R[CB n H n ]X, wherein n is in the range of from 6 to 11, R is selected from the group consisting of a C 1 to C 20 n-alkyl, a hydroxy, a carboxy, an epoxy, an isocyanate, a primary amine, a silyl, and an alkoxy silyl, and X is selected from the group consisting of Li + , Na + , K + , Cs + , and a quatemary ammonium;

(c) a closo-borane salt having the general formula [B n H n ]X 2 , wherein n is in the range of from 7 to 12, and X is selected from the group consisting of Li + , Na + , K + , Cs + , and a quaternary ammonium;

(d) a closo-borane salt having the general formula [B n H m (OR) p ]X 2 , wherein n is in the range of from 7 to 12, wherein m+p=n, with p being in the range of from 1 to 12, each R is independently selected from the group consisting of a hydrogen atom and an aliphatic group, and X is selected from the group consisting of Li + , Na + , K + , Cs + , and a quaternary ammonium;

(e) a nido-carborane salt having the general formula R x [C 2 B n H n+2−x ]X 2 , wherein n is in the range of from 5 to 9, x is in the range of from 1 to 2, each R is independently selected from the group consisting of a C 1 to C 20 n-alkyl, a hydroxy, a carboxy, an epoxy, an isocyanate, a primary amine, a silyl, and an alkoxy silyl, and X is selected from the group consisting of Li + , Na + , K + , Cs + , and a quaternary ammonium;

(f) a nido-carborane salt having the general formula R x ([CB n H n+1−x ]X 3 wherein n is in the range of from 6 to 10, x is in the range of from 0 to 1, R is selected from the group consisting of a C 1 to C 20 n-alkyl, a hydroxy, a carboxy, an epoxy, an isocyanate, a primary amine, a silyl, and an alkoxy silyl, and X is selected from the group consisting of Li + , Na + , K + , Cs + , and a quaternary ammonium; and

(g) mixtures of two or more thereof.

2. The method of claim 1 , wherein said composition has a first glass transition temperature prior to said exposing, and a second glass transition after said exposing, said first glass transition temperature being at least about 1° C. greater than said second glass transition temperature within about 1 day after said exposing was begun.

3. The method of claim 1 , wherein said composition has a first glass transition temperature prior to said exposing, and a second glass transition after said exposing, said first glass transition temperature being at least about 10° C. greater than said second glass transition temperature within about 1 day after said exposing was begun.

4. The method of claim 1 , wherein said composition has a first glass transition temperature prior to said exposing, and a second glass transition after said exposing, said first glass transition temperature being from about 10° C. to about 100° C. greater than said second glass transition temperature within about 7 days after said exposing was begun.

5. The method of claim 1 , wherein said composition has a first glass transition temperature prior to said exposing, and a second glass transition after said exposing, said first glass transition temperature being from about 30° C. to about 100° C. greater than said second glass transition temperature within about 28 days after said exposing was begun.

6. The method of claim 1 , wherein said composition has a first storage modulus at room temperature prior to said exposing, and a second storage modulus at room temperature after said exposing, said second storage modulus being at least about 40% lower than said first storage modulus within about 1 day after said exposing was begun.

7. The method of claim 1 , wherein said composition has a first storage modulus at 0° C. prior to said exposing, and a second storage modulus at 0° C. after said exposing, said second storage modulus being at least about 30% lower than said first storage modulus within about 1 day after said exposing was begun.

8. The method of claim 1 , wherein said composition has a first storage modulus at −25° C. prior to said exposing, and a second storage modulus at −25° C. after said exposing, said second storage modulus being at least about 10% lower than said first storage modulus within about 1 day after said exposing was begun.

9. The method of claim 1 , said filler consisting essentially of said hygroscopic salt.

10. The method of claim 9 , said filler consisting of said hygroscopic salt.

11. The method of claim 1 , wherein said matrix comprises a plurality of polymers.

12. The method of claim 1 , wherein said polymer is selected from the group consisting of an epoxy polymer, a polyurethane, poly(ethylene-co-vinyl acetate), poly(ethylene-co-vinyl acetate-co-vinyl alcohol), poly(ethylene-co-ethyl acrylate), poly(ethylene-co-octene), a polycyanurate, and mixtures of two or more thereof.

13. The method of claim 1 , wherein said hygroscopic salt is Li 2 [B 12 H 12 ].

14. The method of claim 1 , wherein said composition is part of an article of manufacture.

15. The method of claim 1 , wherein said cage compound is (a).

16. The method of claim 1 , wherein said cage compound is (b).

17. The method of claim 1 , wherein said cage compound is (c).

18. The method of claim 1 , wherein said cage compound is (d).

19. The method of claim 1 , wherein said cage compound is (e).

20. The method of claim 1 , wherein said cage compound is (g).

21. A method of adjusting the properties of a material, said method comprising:

providing a composition comprising:

a matrix comprising a polymer, wherein said polymer comprises one or more residues of a cage compound monomer selected from the group consisting of a borane cage compound monomer, a carborane cage compound monomer, and mixtures thereof; and

a filler comprising a hygroscopic salt; and

exposing said composition to moisture under conditions for said composition to absorb said moisture,

wherein said filler comprises a cage compound selected from the group consisting of

(a) a closo-carborane salt having the general formula [CB n H n+1 ]X, wherein n is in the range of from 6 to 11, and X is selected from the group consisting of Li + , Na + , K + , Cs + , and a quaternary ammonium;

(b) a closo-carborane salt having the general formula R[CB n H n ]X, wherein n is in the range of from 6 to 11, R is selected from the group consisting of a C 1 to C 20 n-alkyl, a hydroxy, a carboxy, an epoxy, an isocyanate, a primary amine, a silyl, and an alkoxy silyl, and X is selected from the group consisting of Li + , Na + , K + , Cs + , and a quaternary ammonium;

(c) a closo-borane salt having the general formula [B n H n ]X 2 , wherein n is in the range of from 7 to 12, and X is selected from the group consisting of Li + , Na + , K + , Cs + , and a quaternary ammonium;

(d) a closo-borane salt having the general formula [B n H m (OR) p ]X 2 , wherein n is in the range of from 7 to 12, wherein m+p=n, with p being in the range of from 1 to 12, each R is independently selected from the group consisting of a hydrogen atom and an aliphatic group, and X is selected from the group consisting of Li + , Na + , K + , Cs + , and a quaternary ammonium;

(e) a nido-carborane salt having the general formula R x [C 2 B n H n+2−x ]X 2 , wherein n is in the range of from 5 to 9, x is in the range of from 1 to 2, each R is independently selected from the group consisting of a C 1 to C 20 n-alkyl, a hydroxy, a carboxy, an epoxy, an isocyanate, a primary amine, a silyl, and an alkoxy silyl, and X is selected from the group consisting of Li + , Na + , K + , Cs + , and a quaternary ammonium;

(f) a nido-carborane salt having the general formula R x [CB n H n+1−x ]X 3 wherein n is in the range of from 6 to 10, x is in the range of from 0 to 1, R is selected from the group consisting of a C 1 to C 20 n-alkyl, a hydroxy, a carboxy, an epoxy, an isocyanate, a primary amine, a silyl, and an alkoxy silyl, and X is selected from the group consisting of Li + , Na + , K + , Cs + , and a quaternary ammonium; and

(g) mixtures of two or more thereof.

22. The method of claim 21 , wherein said composition has a first glass transition temperature prior to said exposing, and a second glass transition after said exposing, said first glass transition temperature being at least about 1° C. greater than said second glass transition temperature within about 1 day after said exposing was begun.

23. The method of claim 21 , wherein said composition has a first glass transition temperature prior to said exposing, and a second glass transition after said exposing, said first glass transition temperature being at least about 10° C. greater than said second glass transition temperature within about 1 day after said exposing was begun.

24. The method of claim 21 , wherein said composition has a first glass transition temperature prior to said exposing, and a second glass transition after said exposing, said first glass transition temperature being from about 10° C. to about 100° C. greater than said second glass transition temperature within about 7 days after said exposing was begun.

25. The method of claim 21 , wherein said composition has a first glass transition temperature prior to said exposing, and a second glass transition after said exposing, said first glass transition temperature being from about 30° C. to about 100° C. greater than said second glass transition temperature within about 28 days after said exposing was begun.

26. The method of claim 21 , wherein said composition has a first storage modulus at room temperature prior to said exposing, and a second storage modulus at room temperature after said exposing, said second storage modulus being at least about 40% lower than said first storage modulus within about 1 day after said exposing was begun.

27. The method of claim 21 , wherein said composition has a first storage modulus at 0° C. prior to said exposing, and a second storage modulus at 0° C. after said exposing, said second storage modulus being at least about 30% lower than said first storage modulus within about 1 day after said exposing was begun.

28. The method of claim 21 , wherein said composition has a first storage modulus at −25° C. prior to said exposing, and a second storage modulus at −25° C. after said exposing, said second storage modulus being at least about 10% lower than said first storage modulus within about 1 day after said exposing was begun.

29. The method of claim 21 , said filler consisting essentially of said hygroscopic salt.

30. The method of claim 29 , said filler consisting of said hygroscopic salt.

31. The method of claim 21 , wherein said hygroscopic salt is Li 2 [B 12 H 12 ].

32. The method of claim 21 , wherein said matrix comprises an additional polymer, wherein said additional polymer is selected from the group consisting of an epoxy polymer, a polyurethane, a polysiloxane, poly(ethylene-co-vinyl acetate), poly(ethylene-co-vinyl acetate-co-vinyl alcohol), styrene-butadiene-styrene, poly(ethylene-co-ethyl acrylate), poly(ethylene-co-octene), a polycyanurate, and mixtures of two or more thereof, wherein said filler further comprises a material selected from the group consisting of carbon nanotubes, carbon fullerenes, polyhedral oligomeric silsesquioxane, boron nitride nanotubes, clay, and mixtures of two or more thereof.

33. The method of claim 21 , wherein said composition is part of an article of manufacture.

34. The method of claim 21 , wherein said cage compound is (a).

35. The method of claim 21 , wherein said cage compound is (b).

36. The method of claim 21 , wherein said cage compound is (c).

37. The method of claim 21 , wherein said cage compound is (d).

38. The method of claim 21 , wherein said cage compound is (e).

39. The method of claim 21 , wherein said cage compound is (g).

Assignments (2)
CONFIRMATORY LICENSE Recorded Nov 8, 2011
From: HONEYWELL FEDERAL MANUFACTURING & TECH., LLC (FM&T)
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 027190/0477 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 28, 2011
From: EASTWOOD, ERIC A.; BOWEN III, DANIEL E.
To: HONEYWELL FEDERAL MANUFACTURING & TECHNOLOGIES, LLC
Reel/Frame 027141/0057 →
Continuity (2)
Provisional Application 61374814 · Aug 18, 2010
Related Publication 20120043502A1 · Feb 23, 2012