US5173558A
Expired / Lapsed
US
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Base catalyzed preparation of polyorganosiloxanes with controlled low levels of hydroxy substitution
Assignee: Dow Silicones Corp
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Filing: 1992-06-22
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Granted: 1992-12-22
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Expires: 2012-06-22
Abstract
Abstract The described process uses a Lewis base as a catalyst to effect the condensation of hydroxy end-substituted polyorganosiloxanes, in the presence of triorganosilyl endblocker to control polymer chain length. The inventors have discovered that within a base catalyst concentration range where the cation concentration is about 1×10 -3 to 2×10 -1 mole percent in relation to the silicon atoms present, the partial pressure of water can be controlled at a constant value to produce polyorganosiloxane polymers with a reproducible and predictable level of hydroxy substitution.
Inventors
- 👤 Sidney A. Hansen
- 👤 Charles E. Neal, Jr.
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-02 11:36
CPC Classifications
C; C08; C08G; C08G77/00; C08G77/04; C08G77/06; C08G77/14; C08G77/16
Claims Analysis
Total Claims: 18
Claim 1
Independent Claim
224 words
A process for preparing polyorganosiloxanes containing a controlled low-level of hydroxy substitution, the process comprising: (A) contacting a mixture comprising low molecular weight polyorganosiloxanes of formula ##STR3## and a source of triorganosilyl endblocker of formula R.sup.1.sub.3 Si--, with a Lewis base catalyst; where each X is independently selected from a group consisting of cations of the Lewis base catalyst and hydroxyl radicals; each R is independently selected from a group consisting of monovalent hydrocarbon radicals of one to six carbon atoms and 1,1,1-trifluoropropyl radical; each R 1 is independently selected from a group consisting of hydrocarbon radicals of one to six carbon atoms and 1,1,1-trifluoropropyl radical; and a is an average value of one to about 2,000; (B) controlling partial pressure of water in the process at a constant value within a range of about zero to 1,000 mmHg. (C) controlling temperature of the contacted mixtures and Lewis base catalyst at a value within a range of 40° C. to 300° C.; and (D) recovering product polyorganosiloxanes of formula ##STR4## where the product polyorganosiloxanes have a potential value for hydroxy substitution within a range of about zero to 1,000 ppm; where R is as previously described and R 2 is selected from a group consisting of R 1 and hydroxyl; and b is an average value within a range of a to about 2,000.
Claim 2
Dependent Claim
224 words
A process for preparing polyorganosiloxanes containing a controlled low-level of hydroxy substitution, the process comprising: (A) contacting a mixture comprising low molecular weight polyorganosiloxanes of formula ##STR3## and a source of triorganosilyl endblocker of formula R.sup.1.sub.3 Si--, with a Lewis base catalyst; where each X is independently selected from a group consisting of cations of the Lewis base catalyst and hydroxyl radicals; each R is independently selected from a group consisting of monovalent hydrocarbon radicals of one to six carbon atoms and 1,1,1-trifluoropropyl radical; each R 1 is independently selected from a group consisting of hydrocarbon radicals of one to six carbon atoms and 1,1,1-trifluoropropyl radical; and a is an average value of one to about 2,000; (B) controlling partial pressure of water in the process at a constant value within a range of about zero to 1,000 mmHg. (C) controlling temperature of the contacted mixtures and Lewis base catalyst at a value within a range of 40° C. to 300° C.; and (D) recovering product polyorganosiloxanes of formula ##STR4## where the product polyorganosiloxanes have a potential value for hydroxy substitution within a range of about zero to 1,000 ppm; where R is as previously described and R 2 is selected from a group consisting of R 1 and hydroxyl; and b is an average value within a range of a to about 2,000.
Claim 3
Dependent Claim
24 words
A process according to claim 1, where the source of triorganosilyl endblocker is selected from a group consisting of hexamethyldisiloxane and trimethylsilyl endblocked polydimethylsiloxanes.
Claim 4
Dependent Claim
14 words
A process according to claim 2, where the source of triorganosilyl endblocker is hexamethyldisiloxane.
Claim 5
Dependent Claim
26 words
A process according claim 1, where the available triorganosilyl endblocker groups are present at a concentration of about 0.1 to 5 weight percent of the mixture.
Claim 6
Dependent Claim
10 words
A process according to claim 1, where X is hydroxyl.
Claim 7
Dependent Claim
10 words
A process according to claim 1, where R is methyl.
Claim 8
Dependent Claim
104 words
A process according to claim 1, where the Lewis base catalyst s selected from a group consisting of hydroxides, alcoholates, silanolates, siloxanolates, and mercaptides of the Group IA alkali metals; quaternary ammonium and quaternary phosphonium bases and their siloxanolates; organosodium, organolithium, and organopotassium compounds; hydrocarbon compounds of general formula R 3 M, where R 3 is a hydrocarbon radical of one to 25 carbon atoms, and M is a Group IA alkali metal atom; organic nitrogen compounds of formula R 3 4 N + , and organic phosphorous compounds of formula R 3 4 P + , where R 3 is as previously described.
Claim 9
Dependent Claim
28 words
A process according to claim 1, where the Lewis base catalyst is selected from a group consisting Group IA alkali metal hydroxides and Group IA alkali metal silanolates.
Claim 10
Dependent Claim
14 words
A process according to claim 1, where the Lewis base catalyst is potassium silanolate.
Claim 11
Dependent Claim
19 words
A process according to claim 1, where a is an average value within a range of one to 50.
Claim 12
Dependent Claim
24 words
A process according to claim 1, where the partial pressure of water is a constant value within a range of 30 to 200 mmHg.
Claim 13
Dependent Claim
21 words
A process according to claim 1, where the temperature is a value within a range of 25° C. to 200° C.
Claim 14
Dependent Claim
18 words
A process according to claim 1, where the product polyorganosiloxanes chain length is controlled by the triorganosilyl endblocker.
Claim 15
Dependent Claim
21 words
A process according to claim 1, where hydroxy substitution of product polyorganosiloxanes is controlled by controlling the partial pressure of water.
Claim 16
Dependent Claim
43 words
A process according to claim 1, where the concentration of the Lewis base catalyst provides a cation concentration within a range of about 1×10 -3 to 2×10 -1 mole percent, in relation to the silicon atoms present in initial feed to the process.
Claim 17
Dependent Claim
29 words
A process according to claim 1, where the recovering of product polyorganosiloxanes is accomplished by neutralization of the Lewis base catalyst and separation of the aqueous and organic phases.
Claim 18
Dependent Claim
66 words
A process according to claim 1, where X is hydroxyl and R is methyl; the Lewis base catalyst is potassium silanolate; the partial pressure of water is controlled at a constant value within a range of 30 to 200 mmHg; the temperature is a value within a range of 25° C. to 200° C.; and the recovered polyorganosiloxanes are neutralized to remove the potassium silanolate catalyst.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1995-12-22 | 1996-06-22 | 1996-12-22 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1999-12-22 | 2000-06-22 | 2000-12-22 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2003-12-22 | 2004-06-22 | 2004-12-22 | $7700.00 | Window Closed / Lapsed |