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A strip-shaped grain titanium-silicon molecular sieve and its synthesis method and application

A titanium-silicon molecular sieve and a synthesis method technology are applied in molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolite, etc., and can solve the problems of complex synthesis process and high production cost

Active Publication Date: 2020-02-18
CHINA CATALYST HLDG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The synthesis process of this method is complex and the production cost is high

Method used

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  • A strip-shaped grain titanium-silicon molecular sieve and its synthesis method and application
  • A strip-shaped grain titanium-silicon molecular sieve and its synthesis method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] At 30°C, add 26.0g of tetrapropylammonium hydroxide aqueous solution (0.76mol / L) dropwise to 19.6g of tetrapropylammonium hydroxide solution for 4 hours; at 30°C, mix 6.0g of isopropanol with 0.8g of titanium Mix tetrabutyl ammonium hydroxide evenly, add 20.0g tetrapropylammonium hydroxide aqueous solution (0.38mol / L) dropwise therein, and hydrolyze for 2 hours; mix the two hydrolyzates evenly, remove alcohol at 85°C and add 30.0g deionized water , under strong stirring, add 1.14g of ammonium citrate; put it into a high-pressure reactor with a polytetrafluoroethylene liner, crystallize at 180°C for 72h; after leaving the kettle, filter, wash, dry at 100°C, 550 It was calcined at ℃ to obtain sample TS-1-2.

Embodiment 2

[0032] At 30°C, add 26.0g of tetrapropylammonium hydroxide aqueous solution (0.76mol / L) dropwise to 19.6g of tetrapropylammonium hydroxide solution for 4 hours; at 30°C, mix 6.0g of isopropanol with 0.8g of titanium Mix tetrabutyl ammonium hydroxide evenly, add 20.0g tetrapropylammonium hydroxide aqueous solution (0.38mol / L) dropwise therein, and hydrolyze for 2 hours; mix the two hydrolyzates evenly, remove alcohol at 85°C and add 30.0g deionized water , under strong stirring, add 2.28g of ammonium citrate; put it into a high-pressure reactor with a polytetrafluoroethylene liner, and crystallize at 180°C for 72h; after leaving the kettle, filter, wash, dry at 100°C, 550 It was calcined at ℃ to obtain sample TS-1-3. The XRD pattern and SEM pattern of sample TS-1-3 are shown in the accompanying drawings.

Embodiment 3

[0034] At 30°C, add 26.0g of tetrapropylammonium hydroxide aqueous solution (0.76mol / L) dropwise to 19.6g of tetrapropylammonium hydroxide solution for 4 hours; at 30°C, mix 6.0g of isopropanol with 0.8g of titanium Mix tetrabutyl ammonium hydroxide evenly, add 20.0g tetrapropylammonium hydroxide aqueous solution (0.38mol / L) dropwise therein, and hydrolyze for 2 hours; mix the two hydrolyzates evenly, remove alcohol at 85°C and add 30.0g deionized water , under strong stirring, add 4.56g of ammonium citrate; put it into a high-pressure reaction kettle with a polytetrafluoroethylene liner, and crystallize at 180°C for 72h; after leaving the kettle, filter, wash, dry at 100°C, and Calcined at ℃ to obtain sample TS-1-4.

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Abstract

The invention discloses synthesis and application of a strip-shaped crystal grain titanium silicate molecular sieve. The titanium silicate molecular sieve is synthesized by adopting a hydrothermal method; titanium silicate molecular sieve powder is obtained by taking orthosilicate as a silicon source, titanate as a titanium source, tetrapropyl ammonium hydroxide as a template agent, water and fatty alcohol as a solvent, and ammonium citrate as an additive, crystallizing at 160 DEG C to 180 DEG C for 48h to 120h after uniformly mixing through steps of hydrolysis, removal alcohol and the like, and then filtering, washing, drying and roasting. The titanium silicate molecular sieve synthesized by the invention has an MFI topological structure, a crystal grain is strip-shaped and the length of the crystal grain is 1mu m to 2mu m; the crystal grain is relatively large, so that the crystal grain is easy to separate and recycle after being used; a catalyst has good catalysis performance in phenol hydroxylation reaction.

Description

technical field [0001] The invention belongs to the field of molecular sieve material preparation, and relates to a synthesis method of strip-shaped grain titanium-silicon molecular sieve and its application in phenol hydroxylation reaction. Background technique [0002] Titanium-silicon molecular sieve TS-1 belongs to the orthorhombic crystal system and has the same MFI topology as ZSM-5 molecular sieve. Due to the introduction of transition metal titanium, TS-1 has a unique catalytic oxidation performance. TS-1 is widely used in olefin epoxidation, hydroxylation of phenol and benzene, partial oxidation of alkanes, oxidation of alcohols, oximation of ketones and other catalytic oxidation reactions. [0003] Titanium-silicon molecular sieves are usually synthesized by hydrothermal method, and the grain size is between 100-500nm. Due to the small grain size, it is not easy to separate and recover after use, which increases the cost of use in industrial applications. Under t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/89C01B39/08C01B39/04C07C37/60C07C39/08
CPCB01J29/89C01B39/04C01B39/08C01P2002/72C01P2004/03C07C37/60C07C39/08
Inventor 李进孙红影王建青王炳春孙小惠
Owner CHINA CATALYST HLDG CO LTD
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