US4269813A — Crystalline borosilicate and process of preparati…

Claim 1

Independent Claim 107 words

A crystalline borosilicate which comprises a molecular sieve material having the following composition in terms of mole ratios of oxides: 0.9±0.2M.sub.2/n O:B.sub.2 O.sub.3 :YSiO.sub.2 :ZH.sub.2 O wherein M is at least one cation having a valence of n, Y is between 4 and about 600, and Z is between 0 and about 160, and providing an X-ray diffraction pattern comprising the following X-ray diffraction lines and assigned strengths: ______________________________________ d (A) Assigned Strength ______________________________________ 11.2 ± 0.2 W-VS 10.0 ± 0.2 W-MS 5.97 ± 0.07 W-M 3.82 ± 0.05 VS 3.70 ± 0.05 MS 3.62 ± 0.05 M-MS 2.97 ± 0.02 W-M 1.99 ± 0.02 VW-M ______________________________________

Claim 2

Dependent Claim 107 words

A crystalline borosilicate which comprises a molecular sieve material having the following composition in terms of mole ratios of oxides: 0.9±0.2M.sub.2/n O:B.sub.2 O.sub.3 :YSiO.sub.2 :ZH.sub.2 O wherein M is at least one cation having a valence of n, Y is between 4 and about 600, and Z is between 0 and about 160, and providing an X-ray diffraction pattern comprising the following X-ray diffraction lines and assigned strengths: ______________________________________ d (A) Assigned Strength ______________________________________ 11.2 ± 0.2 W-VS 10.0 ± 0.2 W-MS 5.97 ± 0.07 W-M 3.82 ± 0.05 VS 3.70 ± 0.05 MS 3.62 ± 0.05 M-MS 2.97 ± 0.02 W-M 1.99 ± 0.02 VW-M ______________________________________

Claim 3

Dependent Claim 88 words

The borosilicate of claim 1, wherein, after said borosilicate has been calcined at a temperature of about 1000° F. to about 1100° F., said calcined borosilicate provides an X-ray diffraction pattern comprising the following X-ray diffraction lines and assigned strengths: ______________________________________ d(A) Assigned Strength ______________________________________ 11.2 ± 0.2 M - VS 10.0 ± 0.2 M - MS 5.97 ± 0.07 W - M 3.82 ± 0.05 VS 3.70 ± 0.05 MS 3.62 ± 0.05 M 2.97 ± 0.02 W - M 1.99 ± 0.02 VW - M ______________________________________

Claim 4

Dependent Claim 13 words

The borosilicate of claim 1, wherein Z is between 0 and about 40.

Claim 5

Dependent Claim 13 words

The borosilicate of claim 1, wherein Y is between 4 and about 500.

Claim 6

Dependent Claim 28 words

The borosilicate of claim 1, wherein M comprises a member selected from the group consisting of alkylammonium cation, ammonium cation, hydrogen cation, a metal cation, and mixtures thereof.

Claim 7

Dependent Claim 11 words

The borosilicate of claim 1, wherein M is a nickel cation.

Claim 8

Dependent Claim 13 words

The borosilicate of claim 2, wherein Y is between 4 and about 500.

Claim 9

Dependent Claim 14 words

The borosilicate of claim 4, wherein Y is between about 4 and about 300.

Claim 10

Dependent Claim 14 words

The borosilicate of claim 7, wherein Y is between about 4 and about 300.

Claim 11

Dependent Claim 14 words

The borosilicate of claim 8, wherein Y is between about 40 and about 160.

Claim 12

Dependent Claim 14 words

The borosilicate of claim 9, wherein Y is between about 40 and about 160.

Claim 13

Dependent Claim 13 words

The borosilicate of claim 10, wherein Z is between 0 and about 40.

Claim 14

Dependent Claim 13 words

The borosilicate of claim 11, wherein Z is between 0 and about 40.

Claim 15

Independent Claim 218 words

A method for preparing a crystalline borosilicate which comprises a molecular sieve material providing an X-ray diffraction pattern comprising the following X-ray diffraction lines and assigned strengths: ______________________________________ d(A) Assigned Strength ______________________________________ 11.2 ± 0.2 W - VS 10.0 ± 0.2 W - MS 5.97 ± 0.07 W - M 3.82 ± 0.05 VS 3.70 ± 0.05 MS 3.62 ± 0.05 M - MS 2.97 ± 0.02 W - M 1.99 ± 0.02 VW - M ______________________________________ and having the following composition in terms of mole ratios of oxides: 0.9±0.2M.sub.2/n O:B.sub.2 O.sub.3 :YSiO.sub.2 :ZH.sub.2 O wherein M is at least one cation having a valence of n, Y is between 4 and about 600, and Z is between 0 and about 160, which method comprises: (1) preparing a mixture containing an oxide of silicon, an oxide of boron, a hydroxide of an alkali metal or an alkaline earth metal, an alkylammonium cation or a precursor of an alkylammonium cation, and water; and (2) maintaining said mixture at suitable reaction conditions to effect formation of said borosilicate, said reaction conditions comprising a reaction temperature within the range of about 25° C. to about 300° C., a pressure of at least the vapor pressure of water at the reaction temperature, and a reaction time that is sufficient to effect crystallization.

Claim 16

Independent Claim 218 words

A method for preparing a crystalline borosilicate which comprises a molecular sieve material providing an X-ray diffraction pattern comprising the following X-ray diffraction lines and assigned strengths: ______________________________________ d(A) Assigned Strength ______________________________________ 11.2 ± 0.2 W - VS 10.0 ± 0.2 W - MS 5.97 ± 0.07 W - M 3.82 ± 0.05 VS 3.70 ± 0.05 MS 3.62 ± 0.05 M - MS 2.97 ± 0.02 W - M 1.99 ± 0.02 VW - M ______________________________________ and having the following composition in terms of mole ratios of oxides: 0.9±0.2M.sub.2/n O:B.sub.2 O.sub.3 :YSiO.sub.2 :ZH.sub.2 O wherein M is at least one cation having a valence of n, Y is between 4 and about 600, and Z is between 0 and about 160, which method comprises: (1) preparing a mixture containing an oxide of silicon, an oxide of boron, a hydroxide of an alkali metal or an alkaline earth metal, an alkylammonium cation or a precursor of an alkylammonium cation, and water; and (2) maintaining said mixture at suitable reaction conditions to effect formation of said borosilicate, said reaction conditions comprising a reaction temperature within the range of about 25° C. to about 300° C., a pressure of at least the vapor pressure of water at the reaction temperature, and a reaction time that is sufficient to effect crystallization.

Claim 17

Dependent Claim 17 words

The method of claim 14, wherein said reaction time is about 1 hour to about 4 weeks.

Claim 18

Dependent Claim 17 words

The method of claim 14, wherein said reaction temperature is about 90° C. to about 250° C.

Claim 19

Dependent Claim 76 words

The method of claim 14, wherein said mixture prepared during said method of preparation has the ratios of the initial reactant concentrations in the following ranges: OH - /SiO 2 : 0.01-11 R 2 O/(R 2 O+M 2/n O): 0.2-0.97 H 2 O/OH - : 10-4000 SiO 2 /B 2 O 3 : 5-400 wherein R is an alkylammonium cation, M is an alkali metal or alkaline earth metal, and n is the valence of M.

Claim 20

Dependent Claim 17 words

The method of claim 17, wherein said reaction time is about 1 hour to about 4 weeks.

Claim 21

Dependent Claim 17 words

The method of claim 18, wherein said reaction temperature is about 90° C. to about 250° C.

Claim 22

Dependent Claim 17 words

The method of claim 18, wherein said reaction time is about 6 hours to about 1 week.

Claim 23

Dependent Claim 61 words

A crystalline borosilicate having a composition in terms of mole ratios of oxides as follows: 0.9±0.2M.sub.2/n O:B.sub.2 O.sub.3 :YSiO.sub.2 :ZH.sub.2 O wherein M is at least one cation having a valence of n, Y is between 4 and about 500, and Z is between 0 and about 160, said borosilicate showing the X-ray diffraction lines of Table V of the specification.

Claim 24

Dependent Claim 61 words

A crystalline borosilicate having a composition in terms of mole ratios of oxides as follows: 0.9±0.2M.sub.2/n O:B.sub.2 O.sub.3 :YSiO.sub.2 :ZH.sub.2 O wherein M is at least one cation having a valence of n, Y is between 4 and about 500, and Z is between 0 and about 160, said borosilicate showing the X-ray diffraction lines of Table V of the specification.

Claim 25

Dependent Claim 67 words

A crystalline borosilicate having a composition in terms of mole ratios of oxides as follows: 0.9±0.2M.sub.2/n O:B.sub.2 O.sub.3 :YSiO.sub.2 :ZH.sub.2 O wherein M is at least one cation having a valence of n, Y is between 4 and about 500, and Z is between 0 and about 160, said borosilicate showing the X-ray diffraction lines and assigned strengths substantially as described in Table V of the specification.

Claim 26

Dependent Claim 67 words

A crystalline borosilicate having a composition in terms of mole ratios of oxides as follows: 0.9±0.2M.sub.2/n O:B.sub.2 O.sub.3 :YSiO.sub.2 :ZH.sub.2 O wherein M is at least one cation having a valence of n, Y is between 4 and about 500, and Z is between 0 and about 160, said borosilicate showing the X-ray diffraction lines and assigned strengths substantially as described in Table V of the specification.

Claim 27

Dependent Claim 23 words

The composition of claim 22 further characterized in that Y is a value in the range of from about 4 to about 200.

Claim 28

Dependent Claim 27 words

The composition of claim 22 further characterized in that M is a member selected from the group consisting of alkylammonium, ammonium, hydrogen, metal cations, and mixtures thereof.

Claim 29

Dependent Claim 17 words

The composition of claim 22 further characterized in that M comprises hydrogen, nickel, and an alkali metal.

Claim 30

Dependent Claim 20 words

The composition of claim 22 further characterized in that Z is in the range of from 0 to about 40.

Claim 31

Dependent Claim 21 words

The composition of claim 22 further characterized in that Y is in the range of from about 50 to about 160.

Claim 32

Dependent Claim 76 words

A crystalline borosilicate having a composition in terms of oxides as follows: 0.9±0.2[WR.sub.2 O+(1-W)]M.sub.2/n O:B.sub.2 O.sub.3 :YSiO.sub.2 :ZH.sub.2 O wherein R is tetrapropylammonium cation, M is an alkali metal cation, W is greater than 0 and less than or equal to 1, Y is between about 4 and about 500, Z is between 0 and about 160, said borosilicate showing the X-ray diffraction lines and assigned strengths substantially as described in Table VI of the specification.

Claim 33

Dependent Claim 76 words

A crystalline borosilicate having a composition in terms of oxides as follows: 0.9±0.2[WR.sub.2 O+(1-W)]M.sub.2/n O:B.sub.2 O.sub.3 :YSiO.sub.2 :ZH.sub.2 O wherein R is tetrapropylammonium cation, M is an alkali metal cation, W is greater than 0 and less than or equal to 1, Y is between about 4 and about 500, Z is between 0 and about 160, said borosilicate showing the X-ray diffraction lines and assigned strengths substantially as described in Table VI of the specification.

Claim 34

Dependent Claim 27 words

The crystalline borosilicate formed by calcining the crystalline borosilicate of claim 28 at a temperature in the range of from about 500° F. to about 1500° F.

Claim 35

Dependent Claim 67 words

A crystalline borosilicate having a composition in terms of mole ratios of oxides as follows: 0.9±0.2M.sub.2/n O:B.sub.2 O.sub.3 :YSiO.sub.2 :ZH.sub.2 O wherein M is at least one cation having a valence of n, Y is between 4 and about 300, and Z is between 0 and about 160, said borosilicate having the X-ray diffraction lines and assigned strengths substantially as described in Table II of the specification.

Claim 36

Dependent Claim 67 words

A crystalline borosilicate having a composition in terms of mole ratios of oxides as follows: 0.9±0.2M.sub.2/n O:B.sub.2 O.sub.3 :YSiO.sub.2 :ZH.sub.2 O wherein M is at least one cation having a valence of n, Y is between 4 and about 300, and Z is between 0 and about 160, said borosilicate having the X-ray diffraction lines and assigned strengths substantially as described in Table II of the specification.

Claim 37

Dependent Claim 25 words

The composition of claim 30 further characterized in that M is selected from the group consisting of alkylammonium, ammonium, hydrogen, metal cations, or mixtures thereof.

Claim 38

Dependent Claim 12 words

The composition of claim 31 further characterized in that M comprises nickel.

Claim 39

Dependent Claim 17 words

The composition of claim 30 further characterized in that M comprises hydrogen, nickel, and an alkali metal.

Claim 40

Dependent Claim 20 words

The composition of claim 30 further characterized in that Z is in the range of from 0 to about 40.

Claim 41

Dependent Claim 21 words

The composition of claim 34 further characterized in that Y is in the range of from about 50 to about 160.

Claim 42

Dependent Claim 27 words

The composition of claim 30 further characterized in that said borosilicate has X-ray diffraction lines and assigned strengths substantially as described in Table I of the specification.

Claim 43

Dependent Claim 25 words

The composition of claim 36 further characterized in that Y is between about 4 and about 200 and Z is between 0 and about 40.

Claim 44

Dependent Claim 77 words

A crystalline borosilicate having a composition in terms of oxides as follows: 0.9±0.2[WR.sub.2 O+(1-W)M.sub.2/n O]:B.sub.2 O.sub.3 :YSiO.sub.2 :ZH.sub.2 O wherein R is a tetrapropylammonium cation, M is an alkali metal cation, W is greater than 0 and less than or equal to 1, Y is between about 4 and about 300, Z is between 0 and about 160, said borosilicate having the X-ray diffraction lines and assigned strengths substantially as described in Table IV of the specification.

Claim 45

Dependent Claim 77 words

A crystalline borosilicate having a composition in terms of oxides as follows: 0.9±0.2[WR.sub.2 O+(1-W)M.sub.2/n O]:B.sub.2 O.sub.3 :YSiO.sub.2 :ZH.sub.2 O wherein R is a tetrapropylammonium cation, M is an alkali metal cation, W is greater than 0 and less than or equal to 1, Y is between about 4 and about 300, Z is between 0 and about 160, said borosilicate having the X-ray diffraction lines and assigned strengths substantially as described in Table IV of the specification.

Claim 46

Dependent Claim 26 words

The crystalline borosilicate formed by calcining the crystalline borosilicate of claim 38 at a temperature in the range of about 500° F. to about 1600° F.

Claim 47

Independent Claim 77 words

A method for preparing a crystalline borosilicate possessing X-ray diffraction lines and assigned strengths substantially as shown in Table III, which method comprises preparing a mixture containing an oxide of silicon, an oxide of boron, a base of an alkali or alkaline earth metal, a tetraethylammonium cation, and water; maintaining said mixture at reaction conditions including a temperature in the range of from about 100° C. to about 250° C. to effect formation of said crystalline borosilicate.

Claim 48

Independent Claim 77 words

A method for preparing a crystalline borosilicate possessing X-ray diffraction lines and assigned strengths substantially as shown in Table III, which method comprises preparing a mixture containing an oxide of silicon, an oxide of boron, a base of an alkali or alkaline earth metal, a tetraethylammonium cation, and water; maintaining said mixture at reaction conditions including a temperature in the range of from about 100° C. to about 250° C. to effect formation of said crystalline borosilicate.

Claim 49

Dependent Claim 68 words

The method of claim 40 further characterized in that said mixture is further characterized in terms of mole ratios of oxides in the following ranges: OH - /SiO 2 : 0.06-11 SiO 2 /B 2 O 3 : 5-300 R 2 O/R 2 O+M 2/n O): 0.2-0.97 wherein M is the alkali or alkaline earth metal, n is the valence of M, and R is a tetraethylammonium cation.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1984-05-25	1984-11-24	1985-05-26	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1988-05-25	1988-11-24	1989-05-26	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	1992-05-25	1992-11-24	1993-05-26	$7700.00	Window Closed / Lapsed

Crystalline borosilicate and process of preparation

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