Chemistry of inorganic compounds – Zeolite – Structure defined x-ray diffraction pattern
Patent
1999-04-14
1999-12-14
Bell, Mark L.
Chemistry of inorganic compounds
Zeolite
Structure defined x-ray diffraction pattern
423705, 423707, 423305, 423306, 423DIG30, 502208, 502214, 585640, C01B 3708, C01B 2536, C01B 2545, B01J 2983, B01J 2985
Patent
active
060013281
DESCRIPTION:
BRIEF SUMMARY
The present invention relates in general to a crystalline metallophosphates, and more particularly to crystalline aluminophosphates and silicoaluminophosphates of the molecular sieve type with a novel structure and the method for its preparation.
Microporous crystalline aluminophosphate compositions having open framework structures formed of AlO.sub.2 and PO.sub.2 tetrahedral units joined by the sharing of the comer oxygen atoms and characterised by having pore openings of uniform dimensions have heretofore been disclosed in a number of publications. U.S. Pat. No. 4,310,440 describes aluminophosphates which constitute a generic class of non-zeolite molecular sieve materials being capable of undergoing complete and reversible dehydration while retaining the same essential framework topology in both the anhydrous and hydrated state.
Microporous crystalline silicoaluminophosphate compositions having open framework structures formed of AlO.sub.2, PO.sub.2 and SiO.sub.2 tetrahedral units joined by sharing of corner oxygen atoms and characterised by having pore openings of uniform dimension is earlier disclosed for example in U.S. Pat. No. 4,440,871. These products have a chemical composition on a water-free basis as follows: present in the intracrystalline pore system; "m" is the number of moles of "R" present per mole of (Si.sub.x Al.sub.y P.sub.z)O.sub.2 and m has a value between 0 and 0.3, the maximum value in each case being dependent on the molecular dimensions of the template material and the available pore volume in the silico-alumino-phosphate structure in question; "x", "y" and "z" are molar fractions of silicon, aluminium and phosphorus respectively, present as tetrahedral oxides. The minimum value of "x", "y" and "z" is 0.01, and the maximum value of "x" is 0.98, of "y" 0.6 and of "z" 0.52. The minimum value of "m" in the formula above is 0.02.
Also the silicoaluminophosphates constitute a generic class of non-zeolite molecular sieve materials being capable of undergoing complete and reversible dehydration while retaining the same essential framework topology in both the anhydrous and hydrated state.
By the term "essential framework topology" or "essential framework structure" as used in the aforesaid patents, and also in the present specification and claims, is meant the spatial arrangement of the primary Al--O, Si--O and P--O bond linkages.
From U.S. Pat. No. 5,370,851 there is also known silico-alumino-phosphate molecular sieves of the same composition, but with different X-ray diffraction pattern. Chlorides are used in the synthesis.
WO93/13013 describes synthesis of silico-alumino-phosphates with improved stability to activation and with a controlled silicon content. Hydrochloric acid is used in the synthesis.
Other microporous aluminophosphates which undergo structure rearrangements, either reversibly or irreversibly, upon partial or complete dehydration are also known, for example the minerals variscite and metavaricite and certain of the synthetic metastable aluminophosphates reported by F. D'Yvoire [Bull.Soc.Chim. France, 1762 (1961)].
Synthesis of microporous crystalline silicoaluminophosphates where the reaction mixture is modified with fluoride ions, is earlier described for example in U.S. Pat. No. 4,786,487.
The present invention concerns a novel microporous crystalline metalloophosphate composition, and the method for its preparation.
The microporous crystalline metallophosphate composition has an essential framework structure whose chemical composition in the as synthesised form expressed in terms of mole ratios of oxides is: least one templating agent, x, y and z represent the mole fractions of silicon, aluminium and phosphorous present in the product, and where x may have a value from 0 to 0.5, y may have a value from 0.25 to 0.5 and z may have a value from 0.25 to 0.5, and where one reactive form of fluoride may be present in an effective amount to form the product, and having a characteristic X-ray powder diffraction pattern containing at least the d-spacings as set forth hereinaf
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Chemical Abstracts 114:34650z (1991), "Fluorine-19 MAS NMR studies of crystalline microporous solids synthesized in the fluoride medium", Delmotte et al., Zeolites 1990, 10(8), 778-83 (No Month).
Chemical Abstracts 121:259057f(1994), "Synthesis of new microporous AIPO.sub.4 and substituted derivatives with the LTA structure", Sierea et al., Microporous Mater. 1994, 3(1-2), 29-38 (No Month).
Akporiaye Duncan
Halvorsen Erling N.
Hustveit Jorun
Karlsson Arne
Lillerud Karl Petter
Bell Mark L.
Norsk Hydro ASA
Sample David
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