US5087683A
Expired / Lapsed
US
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Process for producing α, ω-hydroxyfluoroalkylpolysiloxanes
Assignee: Shin-Etsu Chemical Co Ltd
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Filing: 1990-02-06
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Granted: 1992-02-11
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Expires: 2010-02-06
Abstract
Abstract A process for producing an α, ω-hydroxyfluoroalkylpolysiloxane comprising polymerizing a cyclotrisiloxane in the presence of a polymerization catalyst of lithium hydroxide or a lithium salt of a diorganosiloxane, and a promoter of phtalic diorganoester and/or ortho-dialkoxybenzene, and stopping the polymerization by adding a neutralizer is disclosed. This process very easily obtains the α, ω-hydroxyfluoroalkylpolysiloxane of a desired viscosity. If a chloroethane of the general formula CHX, CCl X 2 (X is the hydrogen or chlorine atom) is used as the neutralizer, the α, ω-hydroxyfluoroalkylpolysiloxane does not exhibit any substantial change of viscosity over time.
Inventors
- 👤 Masatoshi Arai
- 👤 Shinichi Satoh
- 👤 Kesao Ide
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-08 12:37
CPC Classifications
C; C08; C08G; C08G77/00; C08G77/04; C08G77/06; C08G77/08; C08G77/22; C08G77/24
Claims Analysis
Total Claims: 15
Claim 1
Independent Claim
97 words
A process for producing an α, ω-hydroxyfluoroalkylpolysiloxane comprising polymerizing a cyclotrisiloxane of formula (I) in the presence of a polymerization catalyst of lithium hydroxide or a lithium salt of a diorganosiloxane obtained by blending and heating lithium hydroxide and a diorganosiloxane, and a promoter of a phthalic diorganoester and/or ortho-dialkoxybenzene, and adding an effective amount of a neutralizer to stop the polymerization reaction at the desired viscosity: ##STR2## wherein R 1 is a substituted or unsubstituted monovalent hydrocarbon group having 1 to 8 carbon atoms; R 2 is a fluoroalkyl group having 1 to 10 carbon atoms.
Claim 2
Dependent Claim
97 words
A process for producing an α, ω-hydroxyfluoroalkylpolysiloxane comprising polymerizing a cyclotrisiloxane of formula (I) in the presence of a polymerization catalyst of lithium hydroxide or a lithium salt of a diorganosiloxane obtained by blending and heating lithium hydroxide and a diorganosiloxane, and a promoter of a phthalic diorganoester and/or ortho-dialkoxybenzene, and adding an effective amount of a neutralizer to stop the polymerization reaction at the desired viscosity: ##STR2## wherein R 1 is a substituted or unsubstituted monovalent hydrocarbon group having 1 to 8 carbon atoms; R 2 is a fluoroalkyl group having 1 to 10 carbon atoms.
Claim 3
Dependent Claim
16 words
A process as in claim 1, wherein R 1 is methyl, vinyl, phenyl, or 3,3,3-trifluoropropyl group.
Claim 4
Dependent Claim
36 words
A process as in claim 1, wherein R 2 , is trifluoromethyl group, pentafluoroethyl group, 3,3,3-trifluoropropyl group, C 4 F 9 CH 2 ,CH 2 -, or C 8 F 17 CH 2 ,CH 2 ,-.
Claim 5
Dependent Claim
12 words
A process as in claim 1, wherein said cyclotrisiloxane is 1,3,5-trimethyl-1,3,5-tris (3,3,3-trifluoropropyl)cyclotrisiloxane.
Claim 6
Dependent Claim
19 words
A process as in claim 1, wherein said promoter is dimethyl phthalate, diethyl phthalate, diallyl phthalate, ortho-dimethoxybenzene, or orthodiethoxybenzene.
Claim 7
Dependent Claim
31 words
A process as in claim 1, 2, 3, 4, or 5, wherein said neutralizer is a chloroethane of the general formula: CHX.sub.2,CCl X.sub.2, wherein X is a hydrogen or chlorine atom.
Claim 8
Dependent Claim
11 words
A process as in claim 6, wherein said chloroethane is 1,1,2,2-tetrachloroethane.
Claim 9
Dependent Claim
35 words
A process as in claim 1, wherein the amount of lithium hydroxide in the form of salt of a diorganosiloxane is 0.005 to 0.50 parts by weight to 100 parts by weight of said cyclotrisiloxane.
Claim 10
Dependent Claim
29 words
A process as in claim 1, wherein the amount of dimethyl phthalate and/or ortho-dialkoxybenzene is 0.005 to 2.0 parts by weight to 100 parts by weight of said cyclotrisiloxane.
Claim 11
Dependent Claim
17 words
A process as in claim 1, wherein said polymerization catalyst and said promoter is used with tetrahydrofuran.
Claim 12
Dependent Claim
33 words
A process as in claim 1, wherein said diorganosiloxane used for preparing a lithium salt is a cyclotrisiloxane, cyclopentasiloxane, or cyclohexasiloxane containing said R 1 and R 2 groups in general formula (I).
Claim 13
Dependent Claim
18 words
A process as in claim 1, wherein the polymerization is conducted at 45 ° C. to 95° C.
Claim 14
Dependent Claim
22 words
A process as in claim 1, wherein H 2 O is further added to the reaction system before adding said polymerization catalyst.
Claim 15
Dependent Claim
22 words
A process as in claim 1, wherein R 1 is selected from alkyl, alkenyl, cycloalkyl, aryl, chloromethyl, 3,3,3-trifluoropropyl and 2-cyano ethyl groups.
References Cited (Backward Citations)
US3997496A
Cited
US4028338A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
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| 3.5 Years (Year 4) | 1995-02-10 | 1995-08-12 | 1996-02-11 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1999-02-10 | 1999-08-12 | 2000-02-11 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2003-02-10 | 2003-08-12 | 2004-02-11 | $7700.00 | Window Closed / Lapsed |