Process for the preparation of pillared silicates

Patent metadata

Field	Value
Publication number	US-9260313-B2
Application number	US-201013254032-A
Country	US
Kind code	B2
Filing date	Mar 3, 2010
Priority date	Mar 3, 2009
Publication date	Feb 16, 2016
Grant date	Feb 16, 2016

Abstract

The present invention relates to a process for the preparation of a silicate compound, comprising (1) providing at least one layered silicate; and (2) mixing said layered silicate with water and at least one silicon containing compound according to formula R 4-m Si[—(SiR 2 ) n —R] m wherein at least one residue R is a leaving group and none of the residues R contains Si; m is 0, 1, 2, 3, or 4; and n is an integer greater than or equal to 0.

First claim

The invention claimed is:

1. A process for the preparation of a silicate compound, comprising
(1) providing at least one layered silicate;
(2) mixing said layered silicate with water and at least one silicon containing compound according to formula (I)
R 4-m Si[—(SiR 2 ) n —R] m   (I)

and
(3) subjecting the mixture obtained in (2) to hydrothermal conditions to provide a suspension comprising a silicate compound,
wherein the at least one layered silicate is selected from the group consisting of RUB-15, RUB-36, RUB-39, BLS-1, and BLS-3
wherein m is 1 , 2, 3, or 4; and
n is an integer greater than or equal to 0;
wherein when n is equal to 0, at least one residue R is a leaving group,
wherein none of the residues R contains Si, and
wherein the hydrothermal treatment of step (3) is carried out under autogenous pressure at a temperature above the boiling point of the solution according to step (2).

2. The process of claim 1 , wherein the leaving group is dissociated from the at least one silicon containing compound during the course of step (2) and/or (3).

3. The process of claim 1 , wherein R, independently from one another, are selected from the group consisting of C 1 to C 5 alkyl groups and leaving groups.

4. The process of claim 1 , wherein the at least one silicon containing compound according to formula (I) is selected from the group consisting of dichlorodimethylsilane, dimethoxydimethylsilane, diethoxydimethylsilane, dichlorodiethylsilane, dimethoxydiethylsilane, diethoxydiethylsilane, trimethylsilane, triethylsilane, chlorotrimethylsilane, chlorotriethylsilane, methoxytrimethylsilane, methoxytriethylsilane, ethoxytrimethylsilane, ethoxytriethylsilane, and hexamethyldisilane.

5. The process of claim 1 , wherein when n is equal to 0, only one residue R is a leaving group.

6. The process of claim 1 , wherein n is greater than or equal to 1.

7. The process of claim 6 , wherein m is equal to 1.

8. The process of claim 1 , wherein the at least one layered silicate is isomorphously substituted.

9. The process of claim 1 , wherein in the mixture obtained in (2), the weight ratio of the layered silicate and water (layered silicate : water) is in the range of 1: (20-80).

10. The process of claim 1 , wherein in the mixture obtained in (2), the molar ratio of silicon in the at least one silicon containing compound according to formula (I) and water (silicon:water) is in the range of 1: (500-3000).

11. The process of claim 1 , wherein the pH of the mixture subjected to hydrothermal treatment in (3) is adjusted to a value in the range of from 0.1 to 5.

12. The process of claim 1 , wherein the hydrothermal treatment in step (3) is carried out at a temperature in the range of from 120 to 200° C.

13. The process of claim 1 , wherein the temperature of the hydrothermal treatment in step (3) is maintained for a period of from 1 h to 48 h.

14. The process of claim 1 which further comprises
(4) separating the silicate compound from the suspension obtained according to (3);
(5) optionally washing the silicate compound obtained from (4) via filtration
(6) optionally drying the separated and/or optionally washed silicate compound.

15. The process of claim 14 which further comprises
(7) calcining the separated and/or optionally washed and/or dried product obtained in step (2) or (3) or (4) or (5) or (6).

Assignees

• Yilmaz Bilge
• Müller Ulrich
• Xiao Feng-Shou
• Gies Hermann
• Tatsumi Takashi
• De Vos Dirk
• Bao Xinhe
• Zhang Weiping
• Basf Se
• Tokyo Inst Tech

Inventors

• Yilmaz Bilge
• Müller Ulrich
• Xiao Feng-Shou
• Gies Hermann
• Tatsumi Takashi
• De Vos Dirk
• Bao Xinhe
• Zhang Weiping

Classifications

• C01B37/02

  Crystalline silica-polymorphs, e.g. silicalites {dealuminated aluminosilicate zeolites} · CPC title

• C01B37/005 Primary

  Silicates, i.e. so-called metallosilicalites or metallozeosilites · CPC title

• C04B2235/3201

  Alkali metal oxides or oxide-forming salts thereof · CPC title

• C01B31/02

  Chemistry & Metallurgy · mapped topic

• C01B39/48

  using at least one organic template directing agent · CPC title