Titanium-silicon micro-mesoporous molecular sieve composite material and synthetic method thereof

A composite material, micro-mesoporous technology, applied in molecular sieves and alkali exchange compounds, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve the problem of low mesopore volume, achieve high oxidation activity, and save raw material costs , the effect of improving the utilization rate of raw materials

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

AI Technical Summary

Problems solved by technology

[0005] The titanium-silicon molecular sieves synthesized by the above existing methods are mainly micropores, and the mesopore volume is not high.

Method used

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  • Titanium-silicon micro-mesoporous molecular sieve composite material and synthetic method thereof
  • Titanium-silicon micro-mesoporous molecular sieve composite material and synthetic method thereof
  • Titanium-silicon micro-mesoporous molecular sieve composite material and synthetic method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] (1) 15g concentration is the tetrapropylammonium hydroxide aqueous solution of 25.05% by weight, 2.04g tetrabutyl titanate, 5.62g hexadecyltrimethylammonium hydroxide (code name MSDS), 8.5g tetraethyl silicate Ester, 2g concentration is that the ammoniacal liquor of 20% by weight and 38g water are successively added in the beaker of 500ml, put into the magnetic stirrer with heating and stirring function and mix evenly, and stir at 80 ℃ for 4 hours, supplement the evaporated Moisture, to obtain a colorless transparent hydrolyzate;

[0072] (2) Aging the obtained hydrolyzed solution at room temperature (26° C.) for 12 hours to obtain an aging product;

[0073] (3) Add 9.6g of white carbon black powder to the above aging product under stirring, and stir for 1 hour after adding, forming a "viscous body". After 2 days of melting, the crystallized sample was obtained, filtered, washed, dried at 120°C for 24 hours, and calcined at 550°C for 6 hours to obtain the titanium-sili...

Embodiment 2

[0076] (1) 7.4g concentration is 25.05% by weight of tetrapropylammonium hydroxide, 1.23g tetrabutyl titanate, 3.29g hexadecyltrimethylammonium bromide (code name CTMAB), 4.16g tetraethyl silicate Ester, 0.67g of 20% by weight ammonia and 14g of water were added to a 500ml beaker in turn, mixed evenly on a magnetic stirrer with heating and stirring functions, and stirred at 90°C for 1 hour, adding evaporation at any time water, to obtain a colorless transparent alkaline hydrolyzate.

[0077] (2) standing the hydrolyzed solution at room temperature for 3 hours to obtain an aging product;

[0078] (3) Slowly add 9.6g of white carbon black powder under stirring to the obtained aging product, stir for 1.5 hours after adding, transfer it to a closed stainless steel reaction kettle, crystallize at a constant temperature of 165°C for 2 days, filter and wash , dried at 120°C for 24 hours, and calcined at 550°C for 6 hours to obtain a titanium-silicon micro-mesoporous molecular sieve ...

Embodiment 3

[0081] (1) 43g concentration is 25.05% tetrapropyl ammonium bromide aqueous solution, 1.68g titanyl sulfate, 5.62g hexadecyltrimethylammonium hydroxide, 2.4g triethylamine, 33.3g tetraethyl silicate , 0.05g of ammonia water and 26g of water with a concentration of 20% by weight were added to a 500ml beaker in turn, put into a magnetic stirrer with heating and stirring functions, and mixed evenly, and heated at 65°C for 3 hours, replenishing the evaporated water at any time moisture to obtain an alkaline hydrolyzate.

[0082] (2) The obtained hydrolyzate was left to stand at room temperature for 9 hours to obtain an aged product.

[0083] (3) In the beaker containing the aging product, slowly add 9.6g of white carbon black powder under stirring, and stir for one hour to form a relatively uniform "viscous body". Crystallize at constant temperature for 2 days, filter, wash, dry at 120°C for 24 hours, and bake at 550°C for 6 hours to obtain the titanium-silicon micro-mesoporous m...

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Abstract

The invention relates to a titanium-silicon micro-mesoporous molecular sieve composite material and a synthetic method thereof. The titanium-silicon micro-mesoporous molecular sieve composite material is rich in silicon on the surfaces of crystal grains, wherein the surface silicon-titanium ratio is higher than that of a bulk phase. The synthetic method of the titanium-silicon micro-mesoporous molecular sieve composite material comprises the following steps: mixing a titanium source, a template, an organic silicon source, an inorganic ammonium source and water; hydrolyzing to propel alcohol, aging, and mixing with a solid silicon source; and then crystallizing in a closed reaction kettle and recovering the titanium-silicon micro-mesoporous molecular sieve composite material. The titanium-silicon micro-mesoporous molecular sieve composite material provided by the invention has high oxidative activity and the noneffective decomposition activity of hydrogen peroxide in side reaction is remarkably reduced.

Description

technical field [0001] The invention relates to a method for synthesizing 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. Using this titanium-silicon molecular sieve as a catalyst can catalyze various types of organic oxi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08
CPCC01B39/085C01P2002/72C01P2004/03C01P2004/04
Inventor 朱斌夏长久林民彭欣欣舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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