Claims
- 1. 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-VS10.0 .+-. 0.2 W-MS5.97 .+-. 0.07 W-M3.82 .+-. 0.05 VS3.70 .+-. 0.05 MS3.62 .+-. 0.05 M-MS2.97 .+-. 0.02 W-M1.99 .+-. 0.02 VW-M______________________________________
- 2. The borosilicate of claim 1, wherein, after said borosilicate has been calcined at a temperature of about 1000.degree. F. to about 1100.degree. 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 - VS10.0 .+-. 0.2 M - MS5.97 .+-. 0.07 W - M3.82 .+-. 0.05 VS3.70 .+-. 0.05 MS3.62 .+-. 0.05 M2.97 .+-. 0.02 W - M1.99 .+-. 0.02 VW - M______________________________________
- 3. The borosilicate of claim 1, wherein Z is between 0 and about 40.
- 4. The borosilicate of claim 1, wherein Y is between 4 and about 500.
- 5. 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.
- 6. The borosilicate of claim 1, wherein M is a nickel cation.
- 7. The borosilicate of claim 2, wherein Y is between 4 and about 500.
- 8. The borosilicate of claim 4, wherein Y is between about 4 and about 300.
- 9. The borosilicate of claim 7, wherein Y is between about 4 and about 300.
- 10. The borosilicate of claim 8, wherein Y is between about 40 and about 160.
- 11. The borosilicate of claim 9, wherein Y is between about 40 and about 160.
- 12. The borosilicate of claim 10, wherein Z is between 0 and about 40.
- 13. The borosilicate of claim 11, wherein Z is between 0 and about 40.
- 14. 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 - VS10.0 .+-. 0.2 W - MS5.97 .+-. 0.07 W - M3.82 .+-. 0.05 VS3.70 .+-. 0.05 MS3.62 .+-. 0.05 M - MS2.97 .+-. 0.02 W - M1.99 .+-. 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.degree. C. to about 300.degree. 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.
- 15. The method of claim 14, wherein said reaction time is about 1 hour to about 4 weeks.
- 16. The method of claim 14, wherein said reaction temperature is about 90.degree. C. to about 250.degree. C.
- 17. 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.sup.- /SiO.sub.2 : 0.01-11
- R.sub.2 O/(R.sub.2 O+M.sub.2/n O): 0.2-0.97
- H.sub.2 O/OH.sup.- : 10-4000
- SiO.sub.2 /B.sub.2 O.sub.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.
- 18. The method of claim 17, wherein said reaction time is about 1 hour to about 4 weeks.
- 19. The method of claim 18, wherein said reaction temperature is about 90.degree. C. to about 250.degree. C.
- 20. The method of claim 18, wherein said reaction time is about 6 hours to about 1 week.
- 21. 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.
- 22. 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.
- 23. The composition of claim 22 further characterized in that Y is a value in the range of from about 4 to about 200.
- 24. 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.
- 25. The composition of claim 22 further characterized in that M comprises hydrogen, nickel, and an alkali metal.
- 26. The composition of claim 22 further characterized in that Z is in the range of from 0 to about 40.
- 27. The composition of claim 22 further characterized in that Y is in the range of from about 50 to about 160.
- 28. 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.
- 29. The crystalline borosilicate formed by calcining the crystalline borosilicate of claim 28 at a temperature in the range of from about 500.degree. F. to about 1500.degree. F.
- 30. 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.
- 31. 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.
- 32. The composition of claim 31 further characterized in that M comprises nickel.
- 33. The composition of claim 30 further characterized in that M comprises hydrogen, nickel, and an alkali metal.
- 34. The composition of claim 30 further characterized in that Z is in the range of from 0 to about 40.
- 35. The composition of claim 34 further characterized in that Y is in the range of from about 50 to about 160.
- 36. 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.
- 37. 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.
- 38. 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.
- 39. The crystalline borosilicate formed by calcining the crystalline borosilicate of claim 38 at a temperature in the range of about 500.degree. F. to about 1600.degree. F.
- 40. 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.degree. C. to about 250.degree. C. to effect formation of said crystalline borosilicate.
- 41. 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.sup.- /SiO.sub.2 : 0.06-11
- SiO.sub.2 /B.sub.2 O.sub.3 : 5-300
- R.sub.2 O/R.sub.2 O+M.sub.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.
CROSS REFERENCE TO RELATED APPLICATIONS
This application is a continuation-in-part application of applications, U.S. Ser. No. 733,267, filed on Oct. 18, 1976; U.S. Ser. No. 819,974, filed on July 28, 1977; and U.S. Ser. No. 836,403, filed on Sept. 26, 1977, each now abandoned. Each of these three co-pending applications is incorporated by reference herein and is made a part hereof, including but not limited to those portions of each which specifically appear hereinafter.
US Referenced Citations (15)
Foreign Referenced Citations (1)
Number |
Date |
Country |
984502 |
Feb 1965 |
GBX |
Related Publications (2)
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Number |
Date |
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819974 |
Jul 1977 |
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733267 |
Oct 1976 |
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Continuation in Parts (1)
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Number |
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Parent |
836403 |
Sep 1977 |
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