Process for the preparation of a crystalline titanoborosilicate

Claim 1

A method for preparing a crystalline titanoborosilicate molecular sieve material having a composition in terms of mole ratios of oxides as follows: 0.9±0.2[xR.sub.2 O+(1-x)M.sub.2/n O]:TiO.sub.2 :B.sub.2 O.sub.3 :ySiO.sub.2.zH.sub.2 O wherein R is an alkylammonium cation, M is at least one cation of valence n selected from the group consisting of alkali metal of alkaline earth metal, y is a value of at least 8 up to 500, z is between 0 and 100 and x is a value greater than zero but less than 1, said material being further characterized by an X-ray diffraction pattern comprising the following diffraction lines and their relative intensities: ______________________________________ Interplanar spacing d (A) Relative intensity ______________________________________ 11.1 ± 0.2 .sup. W-S 10.05 ± 0.2 W-MS 5.18 ± 0.05 VW-M 4.11 ± 0.05 M-VS 3.83 ± 0.05 M-VS 3.71 ± 0.05 .sup. MS-VS 3.64 ± 0.05 MS-S 3.31 ± 0.05 .sup. W-S 2.98 ± 0.02 VW-M 2.50 ± 0.02 VW-M 1.99 ± 0.02 VW-M ______________________________________ which method comprises: (a) providing a reaction mixture comprising: (1) a titanium-oxide containing material and an alkali metal tetrahydroborate, (2) a compound of silicon selected from the group consisting of an oxide of silicon and sodium silicate, (3) a hydroxide of an alkali or alkaline earth metal, (4) an alkylammonium cation or a precursor thereof, and (5) water; and (b) maintaining said reaction mixture under alkaline pH, at a reaction temperature between 25° C. to about 300° C., and for a time sufficient to effect formation of said crystalline titanoborosilicate under autogeneous pressure at the reaction temperature, the composition of the reaction mixture in (a) being such as to provide mole ratios 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 : 8-4000 SiO 2 /TiO 2 : 8-400.

Claim 2

A method for preparing a crystalline titanoborosilicate molecular sieve material having a composition in terms of mole ratios of oxides as follows: 0.9±0.2[xR.sub.2 O+(1-x)M.sub.2/n O]:TiO.sub.2 :B.sub.2 O.sub.3 :ySiO.sub.2.zH.sub.2 O wherein R is an alkylammonium cation, M is at least one cation of valence n selected from the group consisting of alkali metal of alkaline earth metal, y is a value of at least 8 up to 500, z is between 0 and 100 and x is a value greater than zero but less than 1, said material being further characterized by an X-ray diffraction pattern comprising the following diffraction lines and their relative intensities: ______________________________________ Interplanar spacing d (A) Relative intensity ______________________________________ 11.1 ± 0.2 .sup. W-S 10.05 ± 0.2 W-MS 5.18 ± 0.05 VW-M 4.11 ± 0.05 M-VS 3.83 ± 0.05 M-VS 3.71 ± 0.05 .sup. MS-VS 3.64 ± 0.05 MS-S 3.31 ± 0.05 .sup. W-S 2.98 ± 0.02 VW-M 2.50 ± 0.02 VW-M 1.99 ± 0.02 VW-M ______________________________________ which method comprises: (a) providing a reaction mixture comprising: (1) a titanium-oxide containing material and an alkali metal tetrahydroborate, (2) a compound of silicon selected from the group consisting of an oxide of silicon and sodium silicate, (3) a hydroxide of an alkali or alkaline earth metal, (4) an alkylammonium cation or a precursor thereof, and (5) water; and (b) maintaining said reaction mixture under alkaline pH, at a reaction temperature between 25° C. to about 300° C., and for a time sufficient to effect formation of said crystalline titanoborosilicate under autogeneous pressure at the reaction temperature, the composition of the reaction mixture in (a) being such as to provide mole ratios 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 : 8-4000 SiO 2 /TiO 2 : 8-400.