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US4156689A Expired / Lapsed US ⏱️ 0.0 years remaining

Purification of hydrosilanes and siloxanes

Assignee: General Electric Co
•
Filing: 1978-02-13
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Granted: 1979-05-29
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Expires: 1998-02-13
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Abstract

Abstract A process for the purification of hydrogen-containing silanes and siloxanes containing no phenyl substituent groups comprising contacting the silanes and siloxanes with an adsorbent bed formed from material selected from charcoal and molecular sieves and removing the purified silanes and siloxanes from the adsorbent bed. Through this procedure all the impurities which would poison the platinum catalyst are removed and as such the hydrosilanes and siloxanes will undergo SiH-olefin platinum-catalyzed reactions instantly and without difficulty.

Inventors

  • 👤 Bruce A. Ashby
  • 👤 Harry R. McEntee

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-05 14:23
CPC Classifications
C; C07; C07F; C07F7/00; C07F7/02; C07F7/08; C07F7/20; C01; C01B; C01B33/00; C01B33/08; C01B33/107; C01B33/10778; C01B33/10784; C07F7/12; C07F7/121

Claims Analysis

Total Claims: 27
Claim 1
Independent Claim 65 words
A process for the purification of hydrogen-containing silanes and siloxanes comprising (1) contacting hydrogen-containing silanes and siloxanes having no aromatic substituent groups with an adsorbent bed comprising an adsorbent material selected from the class consisting of charcoal, and molecular sieves so as to remove therefrom all impurities which would poison a platinum catalyst, and (2) removing the purified silanes and siloxanes from the adsorbent bed.
Claim 2
Dependent Claim 65 words
A process for the purification of hydrogen-containing silanes and siloxanes comprising (1) contacting hydrogen-containing silanes and siloxanes having no aromatic substituent groups with an adsorbent bed comprising an adsorbent material selected from the class consisting of charcoal, and molecular sieves so as to remove therefrom all impurities which would poison a platinum catalyst, and (2) removing the purified silanes and siloxanes from the adsorbent bed.
Claim 3
Dependent Claim 40 words
The process of claim 1 wherein said hydrogen-containing silanes having no aromatic substituent groups are selected from the class consisting of CH 3 (H)SiCl 2 , HSiCl 3 , (CH 3 ) 2 HSiCl and H 2 SiCl 2 .
Claim 4
Dependent Claim 63 words
The process of claim 1 further comprising contacting the said adsorbent bed with a first volume of the hydrogen-containing silane and siloxane until the adsorbent bed is thoroughly wetted; waiting until the adsorbent bed has reached room temperature; segregating said first volume; passing additional volumes of the hydrogen-containing silane and siloxane through the adsorbent bed and collecting the purified hydrogen silanes and siloxanes.
Claim 5
Dependent Claim 21 words
The process of claim 3 wherein the segregated first volume of hydrogen-containing silanes and siloxanes is recycled through said adsorbent bed.
Claim 6
Dependent Claim 29 words
The process of claim 1 wherein the adsorbent bed is formed from molecular sieves having a size in the range varying from 1/8 of an inch to 125 microns.
Claim 7
Dependent Claim 18 words
The process of claim 1 wherein the adsorbent bed comprises a form of charcoal which is activated carbon.
Claim 8
Dependent Claim 22 words
The process of claim 6 wherein the activated carbon has a size varying from one quarter of an inch to 3-4 microns.
Claim 9
Dependent Claim 23 words
The process of claim 1 wherein the adsorption process is carried out at a temperature in the range of 0° to 35° C.
Claim 10
Dependent Claim 15 words
The process of claim 8 wherein the adsorption process is carried out at room temperature.
Claim 11
Dependent Claim 32 words
The process of claim 1 wherein the hydrogen-containing silanes and siloxanes are doubly distilled so as to be purified before said silanes and siloxanes are passed into contact with said adsorbent bed.
Claim 12
Dependent Claim 25 words
The process of claim 1 wherein the hydrogen-containing silanes and siloxanes have a residence time in said adsorbent bed ranging from 0.5 to 10 hours.
Claim 13
Dependent Claim 25 words
The process of claim 11 wherein the hydrogen-containing silanes and siloxanes have a residence time in said adsorbent bed varying from 1 to 4 hours.
Claim 14
Dependent Claim 47 words
The process of claim 1 wherein in said process sufficient hydrogen-containing silanes and siloxanes are passed through said adsorbent bed such that there is at least 75 pounds of said hydrogen-containing silanes and siloxanes purified per pound of adsorbent material before said bed has to be replaced.
Claim 15
Dependent Claim 47 words
The process of claim 13 wherein in said process sufficient hydrogen-containing silanes and siloxanes are passed through said adsorbent bed such that from 75 to 500 pounds of said hydrogen-containing silanes and siloxanes are purified per pound of adsorbent material before said bed has to be replaced.
Claim 16
Dependent Claim 20 words
The process of claim 14 wherein said adsorbent bed is discarded after it has absorbed the maximum amount of impurities.
Claim 17
Dependent Claim 14 words
The process of claim 1 wherein said adsorbent bed is placed in a column.
Claim 18
Dependent Claim 36 words
The process of claim 1 wherein said hydrogen-containing silanes and siloxanes are passed through said adsorbent bed at a rate varying from 5 to 800 pounds per hour, per square foot of adsorbent bed cross-sectional area.
Claim 19
Dependent Claim 45 words
The process of claim 4 wherein the segregation of said first volume of hydrogen-containing silanes, the passing of additional volumes of hydrogen-containing silanes and siloxanes through said adsorbent bed and the recycling of said segregated silanes and siloxanes are carried out in a continuous manner.
Claim 20
Dependent Claim 49 words
The process of claim 18 wherein after the adsorbent bed is saturated with impurities the stream of hydrogen-containing silanes and siloxanes is passed to a second bed which has been wetted with silanes and siloxanes previously such that the purification of the hydrogen-containing silanes and siloxanes is continuously maintained.
Claim 21
Dependent Claim 28 words
The process of claim 1 such that after said silane is purified, which is methyldichlorosilane, it will react immediately with 3,3,3-trifluoropropene in the presence of a platinum catalyst.
Claim 22
Dependent Claim 29 words
The process of claim 1 such that after said silane is purified, which silane is dimethylchlorosilane, it will react immediately with vinylacetonitrile in the presence of a platinum catalyst.
Claim 23
Dependent Claim 42 words
The process of claim 1 such that after said siloxane, which is a polymethylhydrogensiloxane, is purified it will react immediately with an olefinic compound selected from the class consisting of a methyl styrene and hexene in the presence of a platinum catalyst.
Claim 24
Dependent Claim 66 words
A process for the purification of olefinic silanes or siloxanes comprising (1) contacting said olefinic silanes and siloxanes having no aromatic substituent groups with an adsorbent bed comprising an adsorbent material selected from the class consisting of charcoal, and molecular sieves so as to remove therefrom all impurities which would poison a platinum catalyst and (2) removing the purified silanes and siloxanes from the adsorbent bed.
Claim 25
Dependent Claim 66 words
A process for the purification of olefinic silanes or siloxanes comprising (1) contacting said olefinic silanes and siloxanes having no aromatic substituent groups with an adsorbent bed comprising an adsorbent material selected from the class consisting of charcoal, and molecular sieves so as to remove therefrom all impurities which would poison a platinum catalyst and (2) removing the purified silanes and siloxanes from the adsorbent bed.
Claim 26
Dependent Claim 279 words
A process for the continuous purification of hydrogen-containing silanes comprising (1) contacting said adsorbent bed with a first volume of the hydrogen-containing silane which is selected from the class consisting of CH 3 (H)SiCl 2 , HSiCl 3 , (CH 3 ) 2 HSiCl 3 , and H 2 SiCl 2 until the bed is thoroughly wetted; wherein the adsorbent bed is formed from molecular sieves having a size varying from 1/8 of an inch to 125 microns, (2) waiting until the adsorbent bed has reached room temperature, (3) segregating said first volume of silanes, (4) continuously passing additional volumes of the hydrogen-containing silanes through said adsorbent bed so as to remove all impurities therefrom which would poison a platinum catalyst, (5) removing the purified hydrogen-containing silanes, (6) recycling said segregated first volume of hydrogen-containing silanes through said adsorbent bed so as to purify them, (7) discarding said adsorbent bed when it is saturated with impurities, and (8) continuously passing said hydrogen-containing silanes through a new adsorbent bed which has already been wetted with silanes so as to continuously remove purified hydrogen-containing silanes wherein the adsorption process is carried out at a temperature in the range of 0° to 35° C., wherein said hydrogen-containing silanes and siloxanes have a residence time in said adsorbent bed varying from 0.5 to 10 hours, wherein from 75 to 500 pounds of such hydrogen-containing silanes are purified per pound of adsorbent material in said adsorbent bed before said adsorbent material has to be replaced and wherein said hydrogen-containing silanes are passed through said bed at a rate varying from 5 to 800 pounds per hour, per square foot of adsorbent bed cross-sectional area.
Claim 27
Dependent Claim 279 words
A process for the continuous purification of hydrogen-containing silanes comprising (1) contacting said adsorbent bed with a first volume of the hydrogen-containing silane which is selected from the class consisting of CH 3 (H)SiCl 2 , HSiCl 3 , (CH 3 ) 2 HSiCl 3 , and H 2 SiCl 2 until the bed is thoroughly wetted; wherein the adsorbent bed is formed from molecular sieves having a size varying from 1/8 of an inch to 125 microns, (2) waiting until the adsorbent bed has reached room temperature, (3) segregating said first volume of silanes, (4) continuously passing additional volumes of the hydrogen-containing silanes through said adsorbent bed so as to remove all impurities therefrom which would poison a platinum catalyst, (5) removing the purified hydrogen-containing silanes, (6) recycling said segregated first volume of hydrogen-containing silanes through said adsorbent bed so as to purify them, (7) discarding said adsorbent bed when it is saturated with impurities, and (8) continuously passing said hydrogen-containing silanes through a new adsorbent bed which has already been wetted with silanes so as to continuously remove purified hydrogen-containing silanes wherein the adsorption process is carried out at a temperature in the range of 0° to 35° C., wherein said hydrogen-containing silanes and siloxanes have a residence time in said adsorbent bed varying from 0.5 to 10 hours, wherein from 75 to 500 pounds of such hydrogen-containing silanes are purified per pound of adsorbent material in said adsorbent bed before said adsorbent material has to be replaced and wherein said hydrogen-containing silanes are passed through said bed at a rate varying from 5 to 800 pounds per hour, per square foot of adsorbent bed cross-sectional area.

References Cited (Backward Citations)

US3493595A Cited
US3428530A Cited
US3440264A Cited
US3872145A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1982-05-28 1982-11-27 1983-05-29 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1986-05-28 1986-11-27 1987-05-29 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1990-05-28 1990-11-27 1991-05-29 $7700.00 Window Closed / Lapsed

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