US4782040A — Porous materials having a dual surface

Claim 1

Independent Claim 142 words

A method of preparing a dual surface, porous material which comprises (I) contacting a porous material with a reactive silane intermediate capable of forming covalent bonds with hydroxyl groups on the exterior surface of the porous material wherein said reactive silane intermediate is selected from a group consisting essentially of (i) silenes; (ii) silylenes and (iii) silanones; (II) allowing the mixture from (I) to react thereby treating the porous material exterior surface; (III) thereafter, contacting and mixing the treated porous material from (II) with a reactive silane, or its hydrolysis product, for a period of time to allow the reactive silane, or its hydrolysis product, to diffuse into the interior of the porous material and covalently bond with hydroxyl groups on the interior surface of the porous material, and (IV) subsequently isolating the dual surface porous material from the mixture of (III).

Claim 2

Independent Claim 142 words

A method of preparing a dual surface, porous material which comprises (I) contacting a porous material with a reactive silane intermediate capable of forming covalent bonds with hydroxyl groups on the exterior surface of the porous material wherein said reactive silane intermediate is selected from a group consisting essentially of (i) silenes; (ii) silylenes and (iii) silanones; (II) allowing the mixture from (I) to react thereby treating the porous material exterior surface; (III) thereafter, contacting and mixing the treated porous material from (II) with a reactive silane, or its hydrolysis product, for a period of time to allow the reactive silane, or its hydrolysis product, to diffuse into the interior of the porous material and covalently bond with hydroxyl groups on the interior surface of the porous material, and (IV) subsequently isolating the dual surface porous material from the mixture of (III).

Claim 3

Dependent Claim 25 words

A method as claimed in claim 1, wherein in step (I), the reactive silane intermediate is contacted with a liquid suspension of the porous material.

Claim 4

Dependent Claim 22 words

A method as claimed in claim 1, wherein a solution of reactive silane intermediate is brought into contact with non-particulate porous material.

Claim 5

Dependent Claim 26 words

A method as claimed in claim 1, wherein in step (I), the reactive silane intermediate in the vapor phase is intimately contacted with the porous material.

Claim 6

Dependent Claim 36 words

A method as claimed in claim 1, wherein in step (I), a solution of a precursor to the reactive silane intermediate is brought into contact with the porous material before the reactive silane intermediate is formed.

Claim 7

Dependent Claim 33 words

A method as claimed in claim 1, wherein in step (I), a solution of the reactive silane intermediate is brought into contact with the porous material after the reactive silane intermediate is formed.

Claim 8

Dependent Claim 22 words

A method as claimed in claim 5, wherein in step (I), adsorbed water is used to reduce entry of precursors into pores.

Claim 9

Dependent Claim 33 words

A method as claimed in claim 5, wherein in step (II), adsorbed water is used to destroy that portion of the reactive silane intermediate which would otherwise reach and treat the interior hydroxyls.

Claim 10

Dependent Claim 41 words

A method as claimed in claim 1, wherein the reactive silane intermediate is generated at a site different than the site of the porous material and the reactive silane intermediate is transported from the generation site to the porous material site.

Claim 11

Dependent Claim 19 words

A method as claimed in claim 9, wherein the reactive silane intermediate is transported by its own vapor pressure.

Claim 12

Dependent Claim 18 words

A method as claimed in claim 9, wherein the reactive silane intermediate is transported by a carrier liquid.

Claim 13

Dependent Claim 18 words

A method as claimed in claim 9, wherein the reactive silane intermediate is transported by a carrier gas.

Claim 14

Dependent Claim 24 words

A method as claimed in claim 1, wherein in step (III), the product from step (II) is contacted with the reactive silane in solution.

Claim 15

Dependent Claim 31 words

A method as claimed in claim 1 wherein in step (III), the product from step (II) is contacted with the reactive silane when the reactive silane is in the vapor phase.

Claim 16

Dependent Claim 27 words

A method as claimed in claim 1 wherein steps (I) and (II) are carried out at a temperature in the range of 0° C. to 400° C.

Claim 17

Dependent Claim 27 words

A method as claimed in claim 1 wherein steps (I) and (II) are carried out at a temperature in the range of 25° C. to 200° C.

Claim 18

Dependent Claim 25 words

A method as claimed in claim 1 wherein step (III) is carried out at a temperature in the range of 0° C. and 300° C.

Claim 19

Dependent Claim 25 words

A method as claimed in claim 1 wherein step (III) is carried out at a temperature in the range of 70° C. to 120° C.

Claim 20

Dependent Claim 17 words

A method as claimed in claim 1 wherein the reactive silane intermediates of step (I) are silenes.

Claim 21

Dependent Claim 18 words

A method as claimed in claim 19 wherein the silene is (CH 3 ) 2 Si═CH 2 .

Claim 22

Dependent Claim 12 words

A method as claimed in claim 19 wherein the silene is ##STR9##

Claim 23

Dependent Claim 22 words

A method as claimed in claim 19 wherein the silene is (CH 3 ) 2 Si═CHCH 2 CH 2 CH═CH 2 .

Claim 24

Dependent Claim 12 words

A method as claimed in claim 19 wherein the silene is ##STR10##

Claim 25

Dependent Claim 20 words

A method as claimed in claim 19 wherein the silene is (CH 3 ) 2 Si═CHCH═Si(CH 3 ) 2 .

Claim 26

Dependent Claim 12 words

A method as claimed in claim 19 wherein the silene is ##STR11##

Claim 27

Dependent Claim 12 words

A method as claimed in claim 19 wherein the silene is ##STR12##

Claim 28

Dependent Claim 12 words

A method as claimed in claim 19 wherein the silene is ##STR13##

Claim 29

Dependent Claim 12 words

A method as claimed in claim 19 wherein the silene is ##STR14##

Claim 30

Dependent Claim 12 words

A method as claimed in claim 19 wherein the silene is ##STR15##

Claim 31

Dependent Claim 12 words

A method as claimed in claim 19 wherein the silene is ##STR16##

Claim 32

Dependent Claim 17 words

A method as claimed in claim 1 wherein the reactive silane intermediates of step (I) are silylenes.

Claim 33

Dependent Claim 12 words

A method as claimed in claim 31 wherein the silylene is ##STR17##

Claim 34

Dependent Claim 16 words

A method as claimed in claim 31 wherein the silylene is (CH 3 ) 2 Si:.

Claim 35

Dependent Claim 12 words

A method as claimed in claim 31 wherein the silylene is ##STR18##

Claim 36

Dependent Claim 12 words

A method as claimed in claim 31 wherein the silylene is ##STR19##

Claim 37

Dependent Claim 17 words

A method as claimed in claim 1 wherein the reactive silane intermediates of step (I) are silanones.

Claim 38

Dependent Claim 16 words

A method as claimed in claim 36 wherein the silanone is (CH 3 ) 2 Si═O.

Claim 39

Dependent Claim 12 words

A method as claimed in claim 36 wherein the silanone is ##STR20##

Claim 40

Dependent Claim 108 words

A method as claimed in claim 19 wherein the reactive silane of step (III) has the general formula (R'O).sub.a (R").sub.b SiQ.sub.c wherein R' is an alkyl radical having 1 to 4 carbon atoms or hydrogen R" is an alkyl radical of 1 to 4 carbon atoms or phenyl; the value of a is 1, 2 or 3; the value of b is 0, 1 or 2; the value of c is 1 or 2 wherein a+b+c equals 4; Q is a radical selected from a group consisting of ##STR21## (l) alkyl group of less than tewnty carbon atoms, and (m) aryl group of less than twelve carbon atoms.

Claim 41

Dependent Claim 21 words

A method as claimed in claim 39 wherein Q is --(CH 2 ) 3 NH)CH 2 ) 2 NH 2 .

Claim 42

Dependent Claim 17 words

A method as claimed in claim 39 wherein Q is --(CH 2 ) 3 NH 2 .

Claim 43

Dependent Claim 11 words

A method as claimed in claim 39 wherein Q is ##STR22##

Claim 44

Dependent Claim 26 words

A method as claimed in claim 39 wherein Q is --(CH 2 ) 3 N.sup.⊕ (CH 3 ) 2 C 18 H 37 Cl - .

Claim 45

Dependent Claim 17 words

A method as claimed in claim 39 wherein Q is --(CH 2 ) 9 CH 3 .

Claim 46

Dependent Claim 17 words

A method as claimed in claim 39 wherein Q is --(CH 2 ) 17 CH 3 .

Claim 47

Dependent Claim 26 words

A method as claimed in claim 19 wherein the reactive silane in step (III) is selected from a group consisting of N,N-disubstituted amidosilanes and N,O-disubstituted amidosilanes.

Claim 48

Dependent Claim 13 words

A method as claimed in claim 46 wherein the N,N-disubstituted amide is N-trimethylsilyl-N-methylacetamide.

Claim 49

Dependent Claim 13 words

A method as claimed in claim 46 wherein the N,O-disubstituted amide is N,O-bis(trimethylsilyl)acetamide.

Claim 50

Dependent Claim 14 words

A method as claimed in claim 46 wherein the N,N-disubstituted amido silane is N-trimethylsilyl,N-methyltrifluoroacetamide.

Claim 51

Dependent Claim 14 words

A method as claimed in claim 46 wherein the N,O-disubstituted amido silane is N,O-bis(trimethylsilyl)trifluoroacetamide.

Claim 52

Dependent Claim 14 words

A method as claimed in claim 46 wherein the N,N-disubstituted amido silane is N-hydrodimethylsilyl-N-methylacetamide.

Claim 53

Dependent Claim 14 words

A method as claimed in claim 46 wherein the N,N-disubstituted amido silane is N-vinyldimethylsilyl-N-methylacetamide.

Claim 54

Dependent Claim 25 words

A method as claimed in claim 46 wherein the N,N-disubstituted amido silane is N-dimethylalkylsilyl,N-methylacetamide wherein the alkyl group has from 2 to 20 carbon atoms.

Claim 55

Dependent Claim 24 words

A method as claimed in claim 46 wherein the N,N-disubstituted amido silane is N-dimethylarylsilyl,N-methylacetamide wherein the aryl group has less than twelve carbon atoms.

Claim 56

Dependent Claim 213 words

A method as claimed in claim 19 wherein the reactive silane of step (III) is selected from a group consisting of (i) N,N,N-trisubstituted aminosilanes selected from a group consisting of (a) aminosilanes having the general formula R v 3 SiNR vi R vii wherein R v is independently selected from a group consisting of hydrogen, vinyl, and Q wherein Q is a radical selected from a group consisting of ##STR23## (k) alkyl group of less than twenty carbon atoms, and (l) aryl group of less than twelve carbon atoms; R vi and R vii are each independently selected from a group consisting of alkyl groups of 1 to 3 carbon atoms; and (b) aminosilanes which are heterocyclic aminosilanes containing a group selected from the group consisting of ##STR24## wherein R viii has the same meaning as R vi , and (ii) thiodhensilanes having the general formula R ix 3 SiSR x each R ix is independently selected from alkyl groups having 1 to 20 carbon atoms; aryl groups of less than twelve carbon atoms, hydrogen and vinyl; and R x is selected from alkyl groups of 1 to 6 carbon atoms and R xi 3 Si-- wherein each R xi is independently selected from alkyl groups having from 1 to 3 carbon atoms.

Claim 57

Dependent Claim 93 words

A method as claimed in claim 55 wherein the reactive silane of step (III) is an N,N,N-trisubstituted amine having the general formula R.sup.v SiNR.sup.vi R.sup.vii wherein R v is independently selected from a group consisting of hydrogen, vinyl, and Q wherein Q is a radical selected from a group consisting of ##STR25## (k) alkyl group of less than twenty carbon atoms, and (l) aryl group of less than twelve carbon atoms; R vi and R vii are each independently selected from a group consisting of alkyl groups of 1 to 3 carbon atoms.

Claim 58

Dependent Claim 23 words

A method as claimed in claim 56 wherein the N,N,N-trisubstituted aminosilane is (CH 3 ) 3 SiN(C 2 H 5 ) 2 .

Claim 59

Dependent Claim 21 words

A method as claimed in claim 56 wherein the N,N,N-trisubstituted aminosilane is (CH 3 ) 3 SiN(CH 3 ) 2 .

Claim 60

Dependent Claim 23 words

A method as claimed in claim 55 wherein the reactive silane of step (III) is a N,N,N-trisubstituted aminosilane which is a heterocyclic aminosilane.

Claim 61

Dependent Claim 13 words

A method as claimed in claim 59 wherein the heterocyclic aminosilanes is ##STR26##

Claim 62

Dependent Claim 13 words

A method as claimed in claim 59 wherein the heterocyclic aminosilane is ##STR27##

Claim 63

Dependent Claim 13 words

A method as claimed in claim 59 wherein the heterocyclic aminosilane is ##STR28##

Claim 64

Dependent Claim 13 words

A method as claimed in claim 59 wherein the heterocyclic aminosilane is ##STR29##

Claim 65

Dependent Claim 85 words

A method as claimed in claim 55 wherein the reactive silane of step (III) consists of thioethersilanes having the general formula R.sup.ix.sub.3 SiSR.sup.x wherein each R ix is independently selected from alkyl groups having 1 to 6 carbon atoms and R x is selected from alkyl groups of 1 to 20 carbon atoms; aryl groups of less than twelve carbon atoms, hydrogen and vinyl; and R xi 3 Si-- wherein each R xi is independently selected from alkyl groups having 1 to 3 carbon atoms.

Claim 66

Dependent Claim 18 words

A method as claimed in claim 64 wherein the thioether is {(CH 3 ) 3 Si} 2 S.

Claim 67

Dependent Claim 18 words

A method as claimed in claim 64 wherein the thioether is (CH 3 ) 3 SiSCH 3 .

Claim 68

Dependent Claim 22 words

A method as claimed in claim 64 wherein the thioether is (CH 3 ) 3 SiS(CH 2 ) 5 CH 3 .

Claim 69

Dependent Claim 15 words

A method as claimed in claim 19 wherein the porous material is a silica gel.

Claim 70

Dependent Claim 13 words

A method as claimed in claim 19 wherein the porous material is alumina.

Claim 71

Dependent Claim 13 words

A method as claimed in claim 19 wherein the porous material is stannia.

Claim 72

Dependent Claim 13 words

A method as claimed in claim 19 wherein the porous material is titania.

Claim 73

Dependent Claim 108 words

A method as claimed in claim 31 wherein the reactive silane of step (III) has the general formula (R'O).sub.a (R").sub.b SiQ.sub.c wherein R' is an alkyl radical having 1 to 4 carbon atoms or hydrogen; R" is an alkyl radical of 1 to 4 carbon atoms or phenyl; the value of a is 1, 2 or 3; the value of b is 0, 1 or 2; the value of c is 1 or 2 wherein a+b+c equals 4; Q is a radical selected from a group consisting of ##STR30## (l) alkyl group of less than twenty carbon atoms, and (m) aryl group of less than twelve carbon atoms.

Claim 74

Dependent Claim 19 words

A method as claimed in claim 72 wherein Q is --(CH 2 ) 3 NH(CH 2 ) 2 NH.

Claim 75

Dependent Claim 17 words

A method as claimed in claim 72 wherein Q is --(CH 2 ) 3 NH 2 .

Claim 76

Dependent Claim 11 words

A method as claimed in claim 72 wherein Q is ##STR31##

Claim 77

Dependent Claim 26 words

A method as claimed in claim 72 wherein Q is --(CH 2 ) 3 N.sup.⊕ (CH 3 ) 2 C 18 H 37 Cl - .

Claim 78

Dependent Claim 17 words

A method as claimed in claim 72 wherein Q is --(CH 2 ) 9 CH 3 .

Claim 79

Dependent Claim 17 words

A method as claimed in claim 72 wherein Q is --(CH 2 ) 17 CH 3 .

Claim 80

Dependent Claim 26 words

A method as claimed in claim 31 wherein the reactive silane of step (III) is selected from a group consiting of N,N-disubstituted amidosilanes and N,O-disubstituted amides.

Claim 81

Dependent Claim 13 words

A method as claimed, in claim 79 wherein the N,N-disubstituted amido-silane is N-trimethylsilyl-N-methylacetamide.

Claim 82

Dependent Claim 13 words

A method as laimed in claim 79 wherein the N,O-disubstituted amidosilane is N,O-bis(trimethylsilyl)acetamide.

Claim 83

Dependent Claim 13 words

A method as claimed in claim 79 wherein the N,N-disubstituted amidosilane is N-trimethylsilyl,N-methyltrifluoroacetamide.

Claim 84

Dependent Claim 13 words

A method as claimed in claim 79 wherein the N,O-disubstituted amidosilane is N,O-bis(trimethylsilyl)trifluoroacetamide.

Claim 85

Dependent Claim 13 words

A method as claimed in claim 79 wherein the N,N-disubstituted amidosilane is N-hydrodimethylsilyl-N-methylacetamide.

Claim 86

Dependent Claim 13 words

A method as claimed in claim 79 wherein the N,N-disubstituted amidosilane is N-vinyldimethylsilyl-N-methylacetamide.

Claim 87

Dependent Claim 24 words

A method as claimed in claim 79 wherein the N,N-disubstituted amidosilane is N-drmethylalkylsilyl,N-methylacetamide wherein the alkyl group has from two to twenty carbon atoms.

Claim 88

Dependent Claim 23 words

A method as claimed in claim 79 wherein the N,N-disubstituted amidosilane is N-dimethylarylsilyl,N-methylacetamide wherein the aryl group has less than twelve carbon atoms.

Claim 89

Dependent Claim 15 words

A method as claimed in claim 31 wherein the porous material is a silica gel.

Claim 90

Dependent Claim 13 words

A method as claimed in claim 31 wherein the porous material is alumina.

Claim 91

Dependent Claim 13 words

A method as claimed in claim 31 wherein the porous material is stannia.

Claim 92

Dependent Claim 13 words

A method as claimed in claim 31 wherein the porous material is titania.

Claim 93

Dependent Claim 108 words

A method as claimed in claim 36 wherein the reactive silane of step (III) has the general formula (R'O).sub.a (R").sub.b SiQ.sub.c wherein R' is an alkyl radical having 1 to 4 carbon atoms or hydrogen; R" is an alkyl radical of 1 to 4 carbon atoms or phenyl; the value of a is 1, 2 or 3; the value of b is 0, 1 or 2; the value of c is 1 or 2 wherein a+b+c equals 4; Q is a radical selected from a group consisting of ##STR32## (k) alkyl group of less than twenty carbon atoms, and (l) aryl group of less than twelve carbon atoms.

Claim 94

Dependent Claim 19 words

A method as claimed in claim 92 wherein Q is --(CH 2 ) 3 NH(CH 2 ) 2 NH.

Claim 95

Dependent Claim 17 words

A method as claimed in claim 92 wherein Q is --(CH 2 ) 3 NH 2 .

Claim 96

Dependent Claim 11 words

A method as claimed in claim 92 wherein Q is ##STR33##

Claim 97

Dependent Claim 26 words

A method as claimed in claim 92 wherein Q is --(CH 2 ) 3 N.sup.⊕ (CH 3 ) 2 C 18 H 37 Cl - .

Claim 98

Dependent Claim 108 words

A method as claimed in claim 36 wherein the reactive silane of step (III) has the general formula (R"O).sub.a (R").sub.b SiQ.sub.c wherein R is an alkyl radical having 1 to 4 carbon atoms or hydrogen; R' is an alkyl radical of 1 to 4 carbon atoms or phenyl; the value of a is 1, 2 or 3; the value of b is 0, 1 or 2; the value of c is 1 or 2 wherein a+b+c equals 4; Q is a radical selected from a group consisting of ##STR34## (i) alkyl group of less than twenty carbon atoms; and (j) aryl group of less than twelve carbon atoms.

Claim 99

Dependent Claim 21 words

A method as claimed in claim 97 wherein Q is --CH 2 CH 2 CH 2 OC(O)C(CH 3 )═CH 2 .

Claim 100

Dependent Claim 11 words

A method as claimed in claim 97 wherein Q is ##STR35##

Claim 101

Dependent Claim 11 words

A method as claimed in claim 97 wherein Q is ##STR36##

Claim 102

Dependent Claim 17 words

A method as claimed in claim 97 wherein Q is --CH 2 CH 2 CH 2 SH.

Claim 103

Dependent Claim 17 words

A method as claimed in claim 97 wherein Q is --CH 2 CH 2 CH 2 Cl.

Claim 104

Dependent Claim 28 words

A method as claimed in claim 97 wherein Q is --CH 2 CH 2 CH 2 N.sup.⊕ (CH 3 ) 2 C 18 H 37 Cl - .

Claim 105

Dependent Claim 26 words

A method as claimed in claim 97 wherein Q is -CH 2 CH 2 CH 2 N.sup.⊕ (C 12 H 25 ) 2 Cl - .

Claim 106

Dependent Claim 11 words

A method as claimed in claim 97 wherein Q is ##STR37##

Claim 107

Dependent Claim 15 words

A method as claimed in claim 36 wherein the porous material is a silica gel.

Claim 108

Dependent Claim 13 words

A method as claimed in claim 36 wherein the porous material is alumina.

Claim 109

Dependent Claim 13 words

A method as claimed in claim 36 wherein the porous material is stannia.

Claim 110

Dependent Claim 13 words

A method as claimed in claim 36 wherein the porous material is titania.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1991-11-01	1992-05-02	1992-11-01	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1995-11-01	1996-05-02	1996-11-01	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	1999-11-01	2000-05-02	2000-11-01	$7700.00	Window Closed / Lapsed

Porous materials having a dual surface

Abstract

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