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Method for synthesizing titanium-silicon micro-mesoporous composite material

A synthesis method and micro-mesoporous technology, applied in chemical instruments and methods, crystalline aluminosilicate zeolites, molecular sieves and alkali-exchange compounds, etc., can solve the problem of low activity of titanium-silicon molecular sieves

Active Publication Date: 2015-04-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In the preparation method of titanium silicon molecular sieve disclosed by Thangaraj et al. (Zeolites, 1992, Vol.12 pages 943-950), in order to balance the hydrolysis speed of organosilicon and titanium, isopropanol is introduced in the hydrolysis process of titanium, but this method The activity of the obtained titanium silicate molecular sieve is not high

Method used

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  • Method for synthesizing titanium-silicon micro-mesoporous composite material
  • Method for synthesizing titanium-silicon micro-mesoporous composite material
  • Method for synthesizing titanium-silicon micro-mesoporous composite material

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Embodiment approach

[0039] The method for synthesizing titanium-silicon micro-mesoporous molecular sieve provided by the present invention, a preferred embodiment, comprises the following steps:

[0040] (1) Mix template agent, titanium source, organosilicon source, water, polyhydric alcohol and optional inorganic ammonium source, hydrolyze the alcohol, and then add peroxide; Stir the resulting mixture for at least 10 minutes at ~100° C., such as 50 to 95° C., wherein the stirring time for stirring is 10 minutes to 50 hours; wherein the inorganic ammonium source (in the form of NH 4 + Calculated): Titanium source (as TiO 2 The molar ratio of meter) is 0~5:1;

[0041] (2) Aging the product obtained in step (1), the aging is to leave the product obtained in step (1) at room temperature to 50°C for 1 to 60 hours, such as 2 to 50 hours or 3 to 30 hours, further such as 3 to 30 hours 15 hours;

[0042] (3) Mix the aging product obtained in step (2) with the solid silicon source according to a weig...

Embodiment 1

[0094] Mix 8.5g tetraethyl silicate, 0.44g glycerol with 2.66g tetrapropylammonium hydroxide aqueous solution (25.05% by weight), 1.12g hexadecyltrimethylammonium hydroxide, 0.24g ethylenediamine, add 24.35 g of deionized water were uniformly mixed; then hydrolyzed at 60° C. for 1.0 h to obtain a hydrolyzed solution of tetraethyl silicate. Then, under the action of vigorous stirring, a solution consisting of 0.41 g of tetrabutyl titanate and 5.0 g of isopropanol was slowly dropped into the above solution, and the mixture was stirred at 75° C. for 3 h to obtain a clear and transparent colloid. Add 0.39 g of 30% by weight hydrogen peroxide. Then move the colloid into a closed stainless steel reaction kettle, and crystallize at a constant temperature at 170° C. for 3 days to obtain TS-1 molecular sieve. Mix 6g of TS-1 sample with 25.05% by weight TPAOH aqueous solution uniformly, the weight ratio of TS-1 and TPAOH aqueous solution is 1:5, crystallize in a closed reaction kettle ...

Embodiment 2

[0100] (1) 15g concentration is the tetrapropyl ammonium hydroxide aqueous solution of 25.05% by weight, 2.04g tetrabutyl titanate, 5.49g hexadecyltrimethylammonium hydroxide (represented by MSDS), 8.5g tetrasilicate Ethyl ester, 4.87g glycerin, 2.38g triethylamine, 1.96g concentration are that the ammoniacal liquor of 20% by weight and 46.87g water are added in the beaker of 500ml successively, put into and mix evenly on the magnetic stirrer with heating and stirring function, and heated at 80° C. for 4 hours, replenishing the evaporated water at any time to obtain a colorless transparent hydrolyzate, then adding 1.18 g of hydrogen peroxide with a concentration of 30% by weight, and stirring evenly;

[0101] (2) aging the product obtained in step (1) at room temperature for 12 hours to obtain an aging product;

[0102] (3) Add 9.36g of white carbon black powder to the above aging product under stirring, and stir for 1 hour after adding to form a "viscous body". After 2 days,...

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Abstract

The invention discloses a method for synthesizing a titanium-silicon micro-mesoporous composite material. The method comprises the following steps of: forming a crystallized mixture from a titanium source, a template agent, water, polyhydric alcohol, peroxide and a silicon source and optional inorganic ammonium source, crystallizing and recovering a titanium-silicon molecular sieve, wherein the template agent comprises an organic quaternary ammonium compound, a long-chained alkyl-ammonium compound and an optional organic ammonium compound. The method disclosed by the invention has the advantage that the activity of the synthesized titanium-silicon molecular sieve can be improved.

Description

technical field [0001] The invention relates to a method for synthesizing a titanium-silicon molecular sieve, and more particularly relates to a method for synthesizing a titanium-silicon micro-mesoporous molecular sieve composite material. Background technique [0002] Titanium-silicon molecular sieve is a new type of heteroatom molecular sieve developed in the early 1980s. At present, TS-1 with MFI structure, TS-2 with MEL structure, MCM-22 with MWW structure and TS-48 with larger pore structure have been synthesized. Among them, TS-1 was first developed and synthesized by Italian EniChem Company. It is a new type of titanium-silicon molecular sieve with excellent catalytic selective oxidation performance formed by introducing transition metal element titanium into the molecular sieve framework with ZSM-5 structure. TS-1 It not only has the catalytic oxidation effect of titanium, but also has the shape-selective effect and excellent stability of ZSM-5 molecular sieve. Us...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08
CPCC01B39/085C01P2002/72C01P2004/04C01P2006/90
Inventor 夏长久林民朱斌彭欣欣舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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