US4602922A
Expired / Lapsed
US
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Method of making membranes for gas separation and the composite membranes
Assignee: Research Foundation of the State University of New York
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Filing: 1985-03-07
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Granted: 1986-07-29
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Expires: 2005-03-07
Abstract
Abstract Composite membranes suitable for separating gas mixtures are made by in situ crosslinking of aminoorganofunctional polysiloxane, 1 to 9 mol percent aminosiloxane units, with diisocyanate on the surface of a highly porous polymer substrate, such as polysulfone. Using the crosslinked polysiloxane as a gutter layer, a gas separating entity can be coated on the gutter layer to make a double layer composite membrane which has a higher separation factor than the crosslinked polysiloxane and can be used effectively for flat sheet membranes, as well as, hollow fiber membranes.
Inventors
- 👤 Israel Cabasso
- 👤 Kevin A. Lundy
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-01 19:15
CPC Classifications
B; B01; B01D; B01D69/00; B01D69/12; B01D69/125; B01D53/00; B01D53/22; B01D53/228; B01D67/00; B01D67/0002; B01D67/0006; B01D67/0081; B01D67/0088; B01D71/00; B01D71/06; B01D71/52; B01D71/522; B01D71/5223; B01D71/54; B01D2323/00; B01D2323/12; B01D2323/30; Y; Y10; Y10S; Y10S428/00; Y10S428/903; Y10T; Y10T428/00; Y10T428/249921; Y10T428/249953; Y10T428/25; Y10T428/254
Claims Analysis
Total Claims: 37
Claim 1
Independent Claim
151 words
A method for making a composite suitable for increasing the oxygen gas content of an oxygen-nitrogen gas mixture by passing the mixture through the composite, consisting essentially of coating an aminoorganofunctional polysiloxane on at least one surface of a 20 to 250 μm thick, highly porous, polymer substrate, where the polysiloxane is applied in a thickness sufficient to provide a cured membrane having a thickness of 0.1 μm to 20 μm, the polysiloxane consisting essentially of a random copolymer of from 1 to 9 mol percent aminosiloxane units having primary aminoorganofunctionality and 91 to 99 mol percent other repeating siloxane units contacting the polysiloxane coated on the substrate with a solution of a non-isocyanate-reactive organic solvent and diisocyanate for a sufficient time to cause a crosslinked membrane to form, where the weight ratio of the polysiloxane to the diisocyanate is in an inverse relationship to the permeability coefficient of the composite.
Claim 2
Independent Claim
151 words
A method for making a composite suitable for increasing the oxygen gas content of an oxygen-nitrogen gas mixture by passing the mixture through the composite, consisting essentially of coating an aminoorganofunctional polysiloxane on at least one surface of a 20 to 250 μm thick, highly porous, polymer substrate, where the polysiloxane is applied in a thickness sufficient to provide a cured membrane having a thickness of 0.1 μm to 20 μm, the polysiloxane consisting essentially of a random copolymer of from 1 to 9 mol percent aminosiloxane units having primary aminoorganofunctionality and 91 to 99 mol percent other repeating siloxane units contacting the polysiloxane coated on the substrate with a solution of a non-isocyanate-reactive organic solvent and diisocyanate for a sufficient time to cause a crosslinked membrane to form, where the weight ratio of the polysiloxane to the diisocyanate is in an inverse relationship to the permeability coefficient of the composite.
Claim 3
Dependent Claim
17 words
The method in accordance with claim 1 in which the polysiloxane has up to 15,000 siloxane units.
Claim 4
Dependent Claim
34 words
The method in accordance with claim 2 in which the aminosiloxane units of the polysiloxane are selected from units of the general formulae ##STR17## in which R is a divalent radical selected from ##STR18##
Claim 5
Dependent Claim
33 words
The method in accordance with claim 3 in which the polysiloxane is a random terpolymer of two trimethylsiloxy units, 2 to about 15,000 dimethylsiloxane units, and 2 to 160 of the aminosiloxane units.
Claim 6
Dependent Claim
30 words
The method in accordance with claim 4 in which the average total number of siloxane units in the polysiloxane is in the range of from 100 to 800 per molecule.
Claim 7
Dependent Claim
13 words
The method in accordance with claim 1 in which the diisocyanate is toluene-2,4-diisocyanate.
Claim 8
Dependent Claim
13 words
The method in accordance with claim 2 in which the diisocyanate is toluene-2,4-diisocyanate.
Claim 9
Dependent Claim
13 words
The method in accordance with claim 3 in which the diisocyanate is toluene-2,4-diisocyanate.
Claim 10
Dependent Claim
13 words
The method in accordance with claim 4 in which the diisocyanate is toluene-2,4-diisocyanate.
Claim 11
Dependent Claim
13 words
The method in accordance with claim 5 in which the diisocyanate is toluene-2,4-diisocyanate.
Claim 12
Dependent Claim
10 words
A composite membrane obtained from the method of claim 1.
Claim 13
Dependent Claim
10 words
A composite membrane obtained from the method of claim 5.
Claim 14
Dependent Claim
10 words
A composite membrane obtained from the method of claim 6.
Claim 15
Dependent Claim
10 words
A composite membrane obtained from the method of claim 10.
Claim 16
Dependent Claim
39 words
A method in accordance with claim 1 in which the product obtained is further processed by contacting the crosslinked membrane with poly(2,6-dimethyl-1,4-phenyleneoxide) in an amount sufficient to provide an ultrathin layer which is effective as a gas selective film.
Claim 17
Dependent Claim
21 words
The method in accordance with claim 15 in which the poly(2,6-dimethyl-1,4-phenyleneoxide) is in an organic solvent when contacting the crosslinked polysiloxane.
Claim 18
Dependent Claim
23 words
The method in accordance with claim 16 in which the concentration of the poly(2,6-dimethyl-1,4-phenyleneoxide) in organic solvent is 0.1 to 5 weight percent.
Claim 19
Dependent Claim
15 words
The method in accordance with claim 17 in which the organic solvent is carbon tetrachloride.
Claim 20
Dependent Claim
41 words
A method in accordance with claim 1 in which the product obtained is further processed by contacting the crosslinked membrane with a brominated poly(2,6-dimethyl-1,4-phenyleneoxide) in an amount sufficient to provide an ultrathin layer which is effective as a gas selective film.
Claim 21
Dependent Claim
23 words
The method in accordance with claim 19 in which the brominated poly(2,6-dimethyl-1,4-phenyleneoxide) consists essentially of a mixture of the following repeating units ##STR19##
Claim 22
Dependent Claim
22 words
The method in accordance with claim 20 in which the brominated poly(2,6-dimethyl-1,4-phenylenoxide) is in an organic solvent when contacting the crosslinked polysiloxane.
Claim 23
Dependent Claim
23 words
The method in accordance with claim 21 in which the concentration of the poly(2,6-dimethyl-1,4-phenyleneoxide) in organic solvent is 0.1 to 5 weight percent.
Claim 24
Dependent Claim
15 words
The method in accordance with claim 22 in which the organic solvent is carbon tetrachloride.
Claim 25
Dependent Claim
75 words
A double layer composite membrane suitable for separating gases consisting essentially of a 20 to 250 μm thick highly porous polymer substrate having tightly adhered thereto a gutter layer of a highly gas permeable rubber obtained by crosslinking an aminoorganofunctional polysiloxane having from 1 to 9 mol percent primary aminoorganofunctionality bearing siloxane units and 91 to 99 mol percent other siloxane units, and tightly adhered and overcoating the gutter layer is a gas separating entity.
Claim 26
Dependent Claim
75 words
A double layer composite membrane suitable for separating gases consisting essentially of a 20 to 250 μm thick highly porous polymer substrate having tightly adhered thereto a gutter layer of a highly gas permeable rubber obtained by crosslinking an aminoorganofunctional polysiloxane having from 1 to 9 mol percent primary aminoorganofunctionality bearing siloxane units and 91 to 99 mol percent other siloxane units, and tightly adhered and overcoating the gutter layer is a gas separating entity.
Claim 27
Dependent Claim
80 words
The composite membrane according to claim 24 in which the aminoorganofunctional polysiloxane crosslinked is derived from a random terpolymer polysiloxane having two trimethylsiloxy units, 2 to 15,000 dimethylsiloxane units, and 2 to 160 units selected from the general formulae ##STR20## in which R is a divalent radical selected from ##STR21## the polysiloxane is crosslinked with diisocyanate and the gutter layer is 0.1 to 20 μm thick, the gas separating entity is poly(2,6-dimethyl-1,4-phenyleneoxide) and is less than 2 82 m thick.
Claim 28
Dependent Claim
100 words
The composite membrane according to claim 24 in which the aminoorganofunctional polysiloxane crosslinked is derived from a random terpolymer polysiloxane having two trimethylsiloxy units, 2 to 15,000 dimethylsiloxane units, and 2 to 160 units selected from the general formulae ##STR22## in which R is a divalent radical selected from ##STR23## the polysiloxane is crosslinked with diisocyanate and the gutter layer is 0.1 to 20 μm thick, the gas separating entity is brominated-poly(2,6-dimethyl-1,4-phenyleneoxide) having an average molecular weight in the range of from 40,000 to 130,000 and a mixture of repeating units of ##STR24## and is less than 2 μm thick.
Claim 29
Dependent Claim
10 words
A composite membrane made by the method of claim 15.
Claim 30
Dependent Claim
10 words
A composite membrane made by the method of claim 16.
Claim 31
Dependent Claim
10 words
A composite membrane made by the method of claim 17.
Claim 32
Dependent Claim
10 words
A composite membrane made by the method of claim 18.
Claim 33
Dependent Claim
10 words
A composite membrane made by the method of claim 19.
Claim 34
Dependent Claim
10 words
A composite membrane made by the method of claim 20.
Claim 35
Dependent Claim
10 words
A composite membrane made by the method of claim 21.
Claim 36
Dependent Claim
10 words
A composite membrane made by the method of claim 22.
Claim 37
Dependent Claim
10 words
A composite membrane made by the method of claim 23.
References Cited (Backward Citations)
US3874986A
Cited
US3980456A
Cited
US4230463A
Cited
US4214020A
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JPS55105203A
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US4444662A
Cited
US4406673A
Cited
US4393113A
Cited
US4440643A
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US4493714A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1989-07-28 | 1990-01-27 | 1990-07-29 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1993-07-28 | 1994-01-27 | 1994-07-29 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1997-07-28 | 1998-01-27 | 1998-07-29 | $7700.00 | Window Closed / Lapsed |