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US4096160A Expired / Lapsed US ⏱️ 0.0 years remaining

Continuous devolatilization of silanol-terminated silicone polymer

Assignee: General Electric Co
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Filing: 1976-04-21
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Granted: 1978-06-20
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Expires: 1996-04-21
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Abstract

Abstract An improved process is provided for preparing a linear diorganopolysiloxane fluid having terminal hydroxy groups, which is substantially free of cyclic polysiloxanes. In the process, a linear diorganopolysiloxane fluid containing lower boiling cyclic polysiloxanes is continuously fed with steam into an evacuated, tortuous, confined passageway to form a turbulent mixture of the silicone fluid and steam in the passageway, the mixture is passed through the passageway at elevated temperatures and moderate vacuum to form a vaporized mixture comprising steam and cyclic polysiloxanes which have been freed from the linear diorganopolysiloxane fluid, the vaporized mixture of steam and cyclics and the linear diorganopolysiloxane substantially free of cyclics are removed from the passageway, and the vaporized mixture of steam and cyclics is separated from the cyclic-free diorganopolysiloxane fluid.

Inventors

  • 👤 Bruce Allan Ashby

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-07 13:52
CPC Classifications
C; C08; C08G; C08G77/00; C08G77/04; C08G77/14; C08G77/16; C08G77/32; C08G77/36

Claims Analysis

Total Claims: 12
Claim 1
Independent Claim 162 words
A process for continuously producing a substantially cyclic polysiloxane-free linear diorganopolysiloxane fluid which is chain-stopped primarily with hydroxy groups, said process comprising the steps of: (i) feeding steam and a linear diorganopolysiloxane fluid chain-stopped primarily with hydroxy groups, said fluid also containing low-boiling cyclic polysiloxanes, into an evacuated, tortuous, confined passageway to form a turbulent mixture of said linear diorganopolysiloxane fluid and steam in the passageway; (ii) passing said mixture of linear diorganopolysiloxane fluid and steam through the tortuous passageway under partial vacuum and at a temperature below that at which said cyclic polysiloxanes would normally vaporize at atmospheric pressure, to form a vaporized mixture comprising steam and cyclic polysiloxanes freed from said linear diorganopolysiloxane fluid; (iii) removing said vaporized mixture comprising steam and cyclic polysiloxanes and said linear diorganopolysiloxane fluid which is substantially free of said cyclic polysiloxanes from the tortuous passageway; and (iv) separating said vaporized mixture of steam and cyclic polysiloxanes from said substantially cyclic polysiloxane-free linear diorganopolysiloxane fluid.
Claim 2
Dependent Claim 162 words
A process for continuously producing a substantially cyclic polysiloxane-free linear diorganopolysiloxane fluid which is chain-stopped primarily with hydroxy groups, said process comprising the steps of: (i) feeding steam and a linear diorganopolysiloxane fluid chain-stopped primarily with hydroxy groups, said fluid also containing low-boiling cyclic polysiloxanes, into an evacuated, tortuous, confined passageway to form a turbulent mixture of said linear diorganopolysiloxane fluid and steam in the passageway; (ii) passing said mixture of linear diorganopolysiloxane fluid and steam through the tortuous passageway under partial vacuum and at a temperature below that at which said cyclic polysiloxanes would normally vaporize at atmospheric pressure, to form a vaporized mixture comprising steam and cyclic polysiloxanes freed from said linear diorganopolysiloxane fluid; (iii) removing said vaporized mixture comprising steam and cyclic polysiloxanes and said linear diorganopolysiloxane fluid which is substantially free of said cyclic polysiloxanes from the tortuous passageway; and (iv) separating said vaporized mixture of steam and cyclic polysiloxanes from said substantially cyclic polysiloxane-free linear diorganopolysiloxane fluid.
Claim 3
Dependent Claim 44 words
A process as defined in claim 1 wherein said cyclic diorganosiloxanes comprise from about 9 to about 18% by weight of the feed stock, on a steam-free basis, in step (i), and less than 2% by weight of the final product, in step (iv).
Claim 4
Dependent Claim 28 words
A process as defined in claim 1 wherein said linear diorganopolysiloxane fluid is a dimethylpolysiloxane fluid chain-stopped primarily with hydroxy groups, and said cyclic polysiloxanes comprise cyclic methylpolysiloxanes.
Claim 5
Dependent Claim 28 words
A process as defined in claim 1 wherein said diorganopolysiloxane fluid has a viscosity in the range of from about 1,000 to about 1,000,000 cps. at 25° C.
Claim 6
Dependent Claim 21 words
A process as defined in claim 1 wherein the pressure is in the range from about 30 to about 70 mm.
Claim 7
Dependent Claim 21 words
A process as defined in claim 1 wherein the temperature is in the range from about 50° to about 175° C.
Claim 8
Dependent Claim 47 words
A process as defined in claim 1 wherein step (iv) is carried out in a separator, from which said vaporized mixture of steam and cyclic polysiloxanes is continuously removed as a first stream and said substantially cyclic polysiloxane-free linear diorganopolysiloxane fluid is removed as a second stream.
Claim 9
Dependent Claim 165 words
A process for continuously producing a substantially cyclic methylpolysiloxane-free linear dimethylpolysiloxane fluid which is chain-stopped primarily with hydroxy groups, said process comprising the steps of: (i) feeding steam and a linear dimethylpolysiloxane fluid chain-stopped primarily with hydroxy groups, said fluid also containing low-boiling cyclic methylpolysiloxanes, into an evacuated, tortuous, confined passageway to form a turbulent mixture of said linear dimethylpolysiloxane fluid and steam in the passageway; (ii) passing said mixture of linear dimethylpolysiloxane fluid and steam through the tortuous passageway at a pressure of from about 30 to about 70 mm Hg and a temperature of from about 50° to about 175° C., to form a vaporized mixture comprising steam and cyclic methylpolysiloxanes freed from said linear dimethylpolysiloxane fluid; (iii) removing said vaporized mixture comprising steam and cyclic dimethylsiloxanes and said linear dimethylpolysiloxane fluid which is substantially free of said cyclic dimethylsiloxanes from the tortuous passageway; and (iv) separating said vaporized mixture of steam and cyclic dimethylsiloxanes from said substantially cyclic methylpolysiloxane-free linear dimethylpolysiloxane fluid.
Claim 10
Dependent Claim 165 words
A process for continuously producing a substantially cyclic methylpolysiloxane-free linear dimethylpolysiloxane fluid which is chain-stopped primarily with hydroxy groups, said process comprising the steps of: (i) feeding steam and a linear dimethylpolysiloxane fluid chain-stopped primarily with hydroxy groups, said fluid also containing low-boiling cyclic methylpolysiloxanes, into an evacuated, tortuous, confined passageway to form a turbulent mixture of said linear dimethylpolysiloxane fluid and steam in the passageway; (ii) passing said mixture of linear dimethylpolysiloxane fluid and steam through the tortuous passageway at a pressure of from about 30 to about 70 mm Hg and a temperature of from about 50° to about 175° C., to form a vaporized mixture comprising steam and cyclic methylpolysiloxanes freed from said linear dimethylpolysiloxane fluid; (iii) removing said vaporized mixture comprising steam and cyclic dimethylsiloxanes and said linear dimethylpolysiloxane fluid which is substantially free of said cyclic dimethylsiloxanes from the tortuous passageway; and (iv) separating said vaporized mixture of steam and cyclic dimethylsiloxanes from said substantially cyclic methylpolysiloxane-free linear dimethylpolysiloxane fluid.
Claim 11
Dependent Claim 44 words
A process as defined in claim 8 wherein said cyclic methylpolysiloxanes comprise from about 9 to about 18% by weight of the feed stock, on a steam-free basis, in step (i), and less than 2% by weight of the final product, in step (iv).
Claim 12
Dependent Claim 53 words
A process as defined in claim 1 wherein said linear diorganopolysiloxane has the formula: ##STR2## wherein R and R 1 can be the same or different, and are each organic radicals selected from alkyl, aryl, haloalkyl, haloaryl, alkenyl, alkaryl, aralkyl, haloalkenyl, cyanoalkyl, cycloalkyl, cycloalkenyl, and n has a value of at least 10.

References Cited (Backward Citations)

US2834754A Cited
US3073380A Cited
US3469617A Cited
US3696090A Cited
US3803195A Cited
US3903047A Cited
US3853934A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1981-06-19 1981-12-19 1982-06-20 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1985-06-19 1985-12-19 1986-06-20 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1989-06-19 1989-12-19 1990-06-20 $7700.00 Window Closed / Lapsed

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