Process for preparing an extrudable composition comprising a titanium-containing zeolitic material, having framework type MWW

Patent metadata

Field	Value
Publication number	US-11291980-B2
Application number	US-201716461134-A
Country	US
Kind code	B2
Filing date	Dec 20, 2017
Priority date	Dec 20, 2016
Publication date	Apr 5, 2022
Grant date	Apr 5, 2022

Abstract

A process for preparing an extrudable composition comprising a titanium-containing zeolitic material having framework type MWW, the process comprising providing a titanium-containing zeolitic material having framework type MWW, having a water absorption capacity of at least 11 weight-%, subjecting the titanium-containing zeolitic material having framework type MWW an acid treatment, optionally incorporating zinc in the acid-treated titanium-containing zeolitic material having framework type MWW; preparing a composition comprising the titanium-containing zeolitic material having framework type MWW obtained from (ii) or (iii), a precursor of a silica binder, water, and a kneading agent, wherein the composition does not comprise a polyethylene oxide.

First claim

The invention claimed is:

1. A process for preparing a composition comprising a titanium-containing zeolitic material having framework type MWW, the process comprising
(i) providing a titanium-containing zeolitic material having framework type MWW, having a water absorption capacity in the range of from 12 to 18 weight % as determined according to Reference Example 1 herein
wherein the titanium-containing zeolitic material having framework type MWW provided in (i) is a calcined titanium-containing zeolitic material having framework type MWW;
(ii) subjecting the titanium-containing zeolitic material having framework type MWW provided in (i) to an acid treatment, comprising
(ii.1) preparing an aqueous suspension comprising an aqueous liquid phase and the titanium-containing zeolitic material having framework type MWW provided in (i), wherein the aqueous liquid phase comprises water and an acid;
(ii.2) heating the aqueous suspension according to (ii.1);
(ii.3) separating the acid-treated titanium-containing zeolitic material having framework type MWW from the liquid phase of the aqueous suspension according to (ii.2);

(iii) incorporating zinc in the acid-treated titanium-containing zeolitic material having framework type MWW according to (ii); and
(iv) preparing a composition comprising the titanium-containing zeolitic material having framework type MWW obtained from (ii) or (iii), a precursor of a silica binder, water, and a kneading agent, wherein the composition does not comprise a polyethylene oxide.

2. The process of claim 1 , wherein the titanium-containing zeolitic material having framework type MWW provided in (i) has a water absorption capacity in the range of from 12 to 16 weight %.

3. The process of claim 1 , wherein the titanium-containing zeolitic material having framework type MWW provided in (i) comprises titanium, calculated as elemental titanium, in an amount of from 0.1 to 5 weight-%, based on a total weight of the titanium-containing zeolitic material having framework type MWW.

4. The process of claim 1 , wherein the titanium-containing zeolitic material having framework type MWW provided in (i) comprises particles exhibiting a particle size distribution characterized by a Dv10 value in the range of from 1 to 5 micrometer, a Dv50 value in the range of from 7 to 15 micrometer, and a Dv90 value in the range of from 20 to 40 micrometer.

5. The process of claim 1 , wherein the acid comprised in the aqueous liquid phase comprises one or more inorganic acids.

6. The process of claim 1 , wherein in (ii.2), the aqueous suspension according to (ii.1) is heated to a temperature of the suspension in the range of from 50 to 175° C., dried in a gas atmosphere at a temperature of the gas atmosphere in the range of from 100 to 250° C., and calcined in a gas atmosphere at a temperature of the gas atmosphere in the range of from 400 to 800° C.

7. The process of claim 1 , comprising
(iii) incorporating zinc in the acid-treated titanium-containing zeolitic material having framework type MWW according to (ii); and
(iv) preparing a composition comprising the titanium-containing zeolitic material having framework type MWW obtained from (iii), a precursor of a silica binder, water, and a kneading agent, wherein the composition does not comprise a polyethylene oxide.

8. The process of claim 1 , wherein the kneading agent comprised in the composition according to (iv) comprises one or more hydrophilic polymer.

9. The process of claim 1 , wherein the precursor of the silica binder comprised in the composition according to (iv) comprises one or more of a silica gel, a precipitated silica, a fumed silica, and a colloidal silica.

10. The process of claim 1 , wherein the composition according to (iv) does not comprise a polyalkylene oxide.

11. The process of claim 1 , wherein at least 99 weight-% of the composition according to (iv) consist of the titanium-containing zeolitic material having framework type MWW, the precursor of the silica binder, the water, and the kneading agent.

12. The process of claim 1 , wherein the composition according to (iv) has a plasticity of at most 1,500 N.

13. The process of claim 1 , being a process for preparing a molding comprising a titanium-containing zeolitic material having framework type MWW and a silica binder, the process further comprising
(v) extruding the composition according to (iv), obtaining a molding;
(vi) drying the molding in a gas atmosphere; and
(vii) calcining the dried molding in a gas atmosphere.

14. A molding, obtained by the process according to claim 13 .

15. An extrudable composition, obtained by the process according to claim 1 .

16. An extrudable composition, comprising
a titanium-containing zeolitic material having framework type MWW,
a precursor of a silica binder,
water, and
a kneading agent,
wherein
said composition does not comprise polyethylene oxide,
at least 99 weight-% of the composition consist of the titanium-containing zeolitic material having framework type MWW, the precursor of a silica binder, the water, and the kneading agent, and
said composition has a plasticity of at most 1,500 N.

17. A catalyst precursor or a catalyst, comprising the extrudable composition of claim 16 .

18. A molding, comprising
a titanium-containing zeolitic material having framework type MWW and
a silica binder,
wherein
at least 99 weight-% of the molding consist of the titanium-containing zeolitic material having framework type MWW and the silica binder,
a weight ratio of the titanium-containing zeolitic material having framework type MWW relative to the silica binder, calculated as SiO 2 , is in the range of from 7:3 to 9:1, and said molding has a tortuosity parameter relative to water of at most 2.4.

19. A catalyst precursor or a catalyst, comprising the molding of claim 18 .

Assignees

• Basf Se

Inventors

• Parvulescu Andrei-Nicolae
• Mueller Ulrich
• Luetzel Hans-Juergen
• Uhl Georg
• Teles Joaquim Henrique
• Riedel Dominic
• Urbanczyk Daniel
• Wegerle Ulrike
• Weber Markus
• Woerz Nicolai Tonio
• Mueller Christian

Classifications

• B01J37/0018

  Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat) · CPC title

• B01J2229/37

  Acid treatment · CPC title

• B01J29/7038 Primary

  MWW-type, e.g. MCM-22, ERB-1, ITQ-1, PSH-3 or SSZ-25 · CPC title

• B01J2229/186

  not in framework positions · CPC title

• C01B37/005

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