IP Library Granted Patent US 8,952,118
Granted Patent B2
US 8,952,118 · App. 13/569,638 · Granted Feb 10, 2015

Dual functional linear siloxanes, step-growth polymers derived therefrom, and methods of preparation thereof

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Quick Facts
Patent No.
US 8,952,118
App. No.
13/569,638
Granted
Feb 10, 2015
Kind
B2
Abstract

Linear siloxane polymers having low viscosities, precise molecular weights and two distinct polymer termini are provided. Preferred viscosities are greater than 5 cSt and less than 20,000 cSt, and the preferred functionalities at the polymer termini are one hydrogen and one vinyl group, each attached to a silicon atom. Methods for producing such siloxane polymers are also described In the presence of catalysts, such as Pt 0 complexes, these siloxanes undergo step-growth polymerization to form elastomers at temperatures below 150° C.

Claims (27)

1. A linear siloxane polymer having one unsaturated group terminus and one hydride group terminus, wherein the siloxane polymer has a degree of polymerization of at least 20 and a polydispersity less than about 1.2, and wherein a ratio of unsaturated group termini to hydride group termini is substantially 1:1.

2. The siloxane polymer according to claim 1 , wherein the degree of polymerization is at least 20 to about 1000.

3. The siloxane polymer according to claim 2 , wherein the degree of polymerization is about 20 to about 200.

4. The siloxane polymer according to claim 1 , wherein the unsaturated group is selected from the group consisting of vinyl, styryl, allyl, methallyl, hexenyl, and octenyl.

5. The siloxane polymer according to claim 1 , wherein the siloxane backbone is selected from the group consisting of diphenylsiloxane, phenylmethylsiloxane, trifluoropropylmethylsiloxane, dimethylsilylethylsiloxane, and alkylmethylsiloxane.

6. The siloxane polymer according to claim 5 , wherein the siloxane backbone is dimethylsiloxane and the unsaturated group is vinyl.

7. The siloxane polymer according to claim 1 , wherein the polymer has a viscosity of about 20 to about 20,000 cSt.

8. The siloxane polymer according to claim 1 , wherein the polymer is isolated from a reaction mixture.

9. A method of forming a monovinyl-monohydride terminated siloxane polymer having a degree of polymerization greater than 6 comprising reacting an alkyl or aryl lithium compound with trivinyltrimethylcyclotrisiloxane to form a lithium vinylalkylmethylsilanolate or lithium vinylarylmethylsilanolate, followed by reaction with a strained cyclic siloxane and termination with a hydride-containing chlorosilane.

10. The method according to claim 9 , wherein the alkyl or aryl lithium compound is selected from the group consisting of methyl lithium, butyl lithium, and phenyl lithium.

11. The method according to claim 9 , wherein the strained cyclic siloxane is selected from the group consisting of hexamethylcyclotrisiloxane; (3,3,3-trifluoropropyl)methylcyclotrisiloxane; 2,2,5,5-tetramethyl-2,5-disila-1-oxacyclopentane; triphenyltrimethylcyclotrisiloxane; and hexaphenylcyclotrisiloxane.

12. The method according to claim 9 , wherein the monovinyl-monohydride terminated siloxane polymer has a polydispersity less than about 1.6.

13. The method according to claim 9 , wherein the hydride-containing chlorosilane is selected from the group consisting of dimethylchlorosilane, phenylmethylchlorosilane, diphenylchlorosilane, and diisopropylchlorosilane.

14. A method of forming a monounsaturated-monohydride terminated siloxane polymer having a degree of polymerization greater than 6 comprising reacting an alkyl or aryl lithium compound with tetramethylcyclotetrasiloxane to form a lithium alkylmethylhydrogensilanolate or lithium arylmethylhydrogensilanolate, followed by reaction with a strained cyclic siloxane and termination with an alkyl- or aryl-methylchlorosilane having an unsaturated functionality.

15. The method according to claim 14 , wherein the unsaturated functionality is vinyl or allyl.

16. The method according to claim 14 , wherein the alkyl or aryl lithium compound is selected from the group consisting of methyl lithium, butyl lithium, and phenyl lithium.

17. The method according to claim 14 , wherein the strained cyclic siloxane is selected from the group consisting of hexamethylcyclotrisiloxane; (3,3,3-trifluoropropyl)methylcyclotrisiloxane; 2,2,5,5-tetramethyl-2,5-disila-1-oxacyclopentane; triphenyltrimethylcyclotrisiloxane; and hexaphenylcyclotrisiloxane.

18. The method according to claim 14 , wherein the monounsaturated-monohydride terminated siloxane polymer has a polydispersity less than about 1.6.

19. A linear elastomeric product having no apparent crosslinking, wherein the product is formed from a linear siloxane polymer having one unsaturated group terminus and one hydride group terminus, wherein the siloxane polymer has a degree of polymerization of at least 20 and a ratio of unsaturated group termini to hydride group termini is substantially 1:1.

20. The elastomeric product according to claim 19 , wherein the linear siloxane polymer is a monovinyl-monohydride terminated polysiloxane.

21. The elastomeric product according to claim 19 , wherein the product is formed via hydrosilylation step-growth polymerization of the linear siloxane polymer.

22. The elastomeric product according to claim 19 , wherein the linear siloxane polymer is uncompounded or compounded with a reinforcing agent or filler.

23. A method of producing an elastomeric product according to claim 19 , comprising reacting the siloxane polymer with a Pt 0 catalyst.

24. The method according to claim 23 , further comprising compounding the siloxane polymer with a filler or reinforcing agent prior to reaction with the Pt 0 catalyst.

25. The method according to claim 24 , wherein the filler is fumed silica.

26. The method according to claim 23 , wherein the linear siloxane polymer is a monovinyl-monohydride terminated polydimethylsiloxane.

27. The method according to claim 23 , wherein the reaction with the catalyst is performed at a temperature of not greater than about 150° C.

Assignments (9)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 22, 2024
From: GELEST TECHNOLOGIES, INC.
To: GELEST, INC.
Reel/Frame 068467/0243 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 10, 2022
From: GELEST TECHNOLOGIES, INC.
To: GELEST, INC.
Reel/Frame 058668/0350 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 28, 2021
From: GELEST TECHNOLOGIES, INC.
To: GELEST, INC.
Reel/Frame 058595/0701 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 7, 2021
From: GELEST TECHNOLOGIES, INC.
To: GELEST, INC.
Reel/Frame 056272/0183 →
RELEASE OF SECURITY INTEREST Recorded Oct 1, 2020
From: ANTARES CAPITAL LP
To: GELEST BIOSYSTEMS, LLC; GELEST, INC.; GELEST TECHNOLOGIES, INC.
Reel/Frame 053946/0556 →
RELEASE OF SECURITY INTEREST Recorded Jun 24, 2019
From: WELLS FARGO BANK, NATIONAL ASSOCIATION
To: GELEST TECHNOLOGIES, INC.; GELEST, INC.; GELEST BIOSYSTEMS, LLC
Reel/Frame 049567/0194 →
PATENT SECURITY AGREEMENT Recorded Jun 21, 2019
From: GELEST, INC.; GELEST TECHNOLOGIES, INC.; GELEST BIOSYSTEMS, LLC
To: ANTARES CAPITAL LP
Reel/Frame 049557/0526 →
SECURITY INTEREST Recorded Aug 14, 2017
From: GELEST, INC.; GELEST TECHNOLOGIES, INC.; GELEST BIOSYSTEMS, LLC
To: WELLS FARGO BANK, NATIONAL ASSOCIATION
Reel/Frame 043540/0963 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 8, 2012
From: ARKLES, BARRY C.; GOFF, JONATHAN D.
To: GELEST TECHNOLOGIES, INC.
Reel/Frame 028750/0564 →