Synthesis of molecular sieving metallosilicates using silica-transition metal oxide sols

Claim 3

The method of claim 1 wherein the solids content of said dispersion ranges up to about 70% by weight solids.

Claim 4

The method of claim 1 wherein the solids content of said dispersion ranges from about 5% to about 40% by weight solids.

Claim 5

The method of claim 1 wherein the mole ratio of Si to transition metal in said dispersion is in the range of about 5 to about 100.

Claim 6

The method of claim 1 wherein the mole ratio of Si to transition metal in said dispersion is in the range of about 10 to about 50.

Claim 7

The method of claim 1 wherein said dispersion includes an effective amount of a stabilizing agent to stabilize said dispersion.

Claim 8

The method of claim 6 wherein said stabilizing agent is a cation or an anion.

Claim 9

The method of claim 1 wherein said transition metal is Cr, Zr, Ti or Fe.

Claim 10

The method of claim 1 wherein said dispersion comprises an aqueous dispersion of submicron silica particles coated with Cr 2 O 3 .

Claim 11

The method of claim 1 wherein said dispersion comprises an aqueous dispersion of submicron silica particles coated with TiO 2 .

Claim 12

The method of claim 1 wherein said dispersion comprises an aqueous dispersion of submicron silica particles coated with Fe 2 O 3 .

Claim 13

The method of claim 1 wherein said dispersion comprises an aqueous dispersion of submicron silica particles coated with ZrO 2 .

Claim 14

The method of claim 1 with the step of separating said metallosilicate from its mother liquor.

Claim 15

The method of claim 1 with the step of washing said metallosilicate.

Claim 16

The method of claim 1 with the step of heat treating said metallosilicate in an inert, oxidizing or reducing atmosphere.

Claim 17

The method of claim 15 with step of cation exchanging said heat treated metallosilicate with an ammonium salt or the salt of a catalytically active metal to provide a cation exchanged metallosilicate.

Claim 18

The method of claim 16 with the step of heat treating said cation exchanged metallosilicate in an inert, oxidizing or reducing atmosphere.

Claim 19

The method of claim 1 wherein the mole ratio of Si to said mineralizing and/or synthesis directing agent is in the range of about 0.1 to about 30.

Claim 20

The method of claim 1 wherein said mineralizing agent and/or synthesis directing agent is the cation of an amine or alkanol amine compound, ammonium or alkyl ammonium compound, alkali or alkaline earth metal compound, or alkyl phosphonium or alkyl arsonium compound.

Claim 21

The method of claim 19 wherein said alkyl ammonium compound is a mono-, di-, tri- or tetra-alkyl ammonium compound, each alkyl group having up to about six carbon atoms.

Claim 22

The method of claim 20 wherein said alkyl ammonium compound is a salt or hydroxide of tetrapropyl ammonium ion.

Claim 23

The method of claim 1 wherein said mineralizing agent and/or synthesis directing agent is a salt or hydroxide of sodium.

Claim 24

The method of claim 1 wherein said mineralizing agent and/or synthesis directing agent comprises a salt or hydroxide of sodium and a salt or hydroxide of tetrapropylammonium.

Claim 25

The method of claim 1 wherein said mixture is maintained in an enclosed container under at least the vapor pressure of water during step (C).

Claim 26

The method of claim 1 wherein the temperature during step (C) is in the range of about 125° C. to about 200° C.

Claim 27

The method of claim 1 wherein the time period for step (C) is from about 4 hours to about 30 days.

Claim 28

The method of claim 1 wherein the time period for step (C) is from about one to about ten days.

Claim 29

The method of claim 1 wherein said metallosilicate can be represented by the formula aA.sub.2 O:bDO.sub.n/2 :cEO.sub.m/2 :MO.sub.2 :dSiO.sub.2 :eH.sub.2 O wherein A is a hydrogen, ammonium, alkyl ammonium, alkyl phosphonium or alkyl arsonium ion, or a mixture thereof; D is an alkali or alkaline earth metal ion, or a mixture thereof; E is selected from the group consisting of Al, Ga or a mixture thereof; M is selected from the group consisting of Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Zn, Zr, Y or a mixture thereof; a is a number ranging from zero to about 25; b is a number ranging from zero to about 3; c is a number ranging from zero to about 0.4; d is a number ranging from about 3 to about 300; e is a number ranging from zero to about 120; n is the valence of D; and m is the valence of E.

Claim 30

The method of claim 1 wherein the x-ray diffraction pattern for said metallosilicate shows the following significant lines: ______________________________________ Interplanar Relative Spacing d(A) Intensity ______________________________________ 11.1 ± 0.2 s. 10.0 ± 0.2 m.-s. 7.45 ± 0.15 w. 6.40 ± 0.03 w. 4.61 ± 0.08 w. 4.39 ± 0.02 w. 3.84 ± 0.08 s. 3.77 ± 0.02 m.-s. 3.73 ± 0.01 s. 3.65 ± 0.05 m.-s. 3.05 ± 0.03 w. 2.99 ± 0.02 w. 2.00 ± 0.02 w. ______________________________________

Claim 31

The method of claim 15 wherein the X-ray diffraction pattern for said heat-treated metallosilcates shows the following significant lines: ______________________________________ Interplanar Relative Spacing d(A) Intensity ______________________________________ 11.2 ± 0.2 s. 10.2 ± 0.2 s. 9.8 ± 0.2 m. 6.74 ± 0.1 w. 6.38 ± 0.1 w. 6.01 ± 0.08 w. 5.75 ± 0.08 w. 5.61 ± 0.08 w. 4.38 ± 0.06 w. 3.86 ± 0.05 s. 3.84 ± 0.05 s. 3.73 ± 0.05 s. 3.66 ± 0.04 w.-m. 3.00 ± 0.02 w. 2.015 ± 0.01 w. 1.995 ± 0.01 w. ______________________________________