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A kind of preparation method of bifunctional titanium silicate molecular sieve

A titanium-silicon molecular sieve and dual-function technology, which is applied in the field of preparation of dual-function titanium-silicon molecular sieves, can solve the problems of complex preparation process, restricting industrial application and high preparation cost

Inactive Publication Date: 2011-12-14
CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The preparation cost of bifunctional titanium-silicon molecular sieve (M-TS-1) is mainly reflected in the usage amount of expensive tetrapropylammonium hydroxide (TPAOH). The usage amount of M-TS-1 is relatively large, which makes the preparation cost of M-TS-1 higher, and the preparation process is complicated, and the operation is stricter, which strictly restricts the industrial application of M-TS-1 molecular sieve.

Method used

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  • A kind of preparation method of bifunctional titanium silicate molecular sieve
  • A kind of preparation method of bifunctional titanium silicate molecular sieve
  • A kind of preparation method of bifunctional titanium silicate molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Weigh 6.4g of hydrogen peroxide (30wt%) in 92g of distilled water, add 4.61g of TBOT, add 28ml of n-butylamine (NBA) under vigorous stirring, and stir at room temperature for 30 minutes to obtain a light yellow solution of titanium.

[0026] Weigh 12.8g of TPABr into 80g of distilled water, dissolve under vigorous stirring, then add 92.7g of silica sol (30wt%), and continue stirring at room temperature for 30 minutes to obtain a silicon hydrolysis solution.

[0027] Weigh a certain mass of Al(NO 3 ) 3 9H 2 O was dissolved in 20 g of distilled water with stirring to obtain an aqueous solution of aluminum.

[0028] Add the aluminum aqueous solution dropwise into the titanium hydrolysis solution under vigorous stirring, and continue stirring for 30 minutes to obtain a mixed solution of titanium and aluminum.

[0029] Slowly pour the mixture of titanium and aluminum into the silicon source solution under vigorous stirring, continue stirring for 30 minutes, add 1.2g of TS...

Embodiment 2

[0032] Weigh 6.4g of hydrogen peroxide (30wt%) in 82g of distilled water, add 4.61g of TBOT, add 28ml of n-butylamine (NBA) under vigorous stirring, and stir at room temperature for 30 minutes to obtain a light yellow solution of titanium.

[0033] Weighed 12.8g of TPABr into 60g of distilled water, dissolved it under vigorous stirring, then added 92.7g of silica sol (30wt%), and continued to stir at room temperature for 30 minutes to obtain a silicon hydrolysis solution.

[0034] Weigh a certain mass of H according to the molar ratio of Si / Al=(100~400) 3 BO 3 In 50g of distilled water, stirred and dissolved to obtain an aqueous solution of boron.

[0035] Slowly add the titanium hydrolysis solution into the silicon hydrolysis solution under vigorous stirring, and stir at room temperature for 30 minutes to obtain a titanium-silicon mixture.

[0036] Under vigorous stirring, add boron aqueous solution dropwise to the mixed solution of titanium and silicon, continue stirring for...

Embodiment 3

[0039] Weigh 6.4g of hydrogen peroxide (30wt%) in 82g of distilled water, add 4.61g of TBOT, add 28ml of n-butylamine (NBA) under vigorous stirring, and stir at room temperature for 30 minutes to obtain a light yellow solution of titanium.

[0040] Weighed 12.8g of TPABr into 60g of distilled water, dissolved it under vigorous stirring, then added 92.7g of silica sol (30wt%), and continued to stir at room temperature for 30 minutes to obtain a silicon hydrolysis solution.

[0041] Weigh a certain mass of Fe(NO 3 ) 3 9H 2 O was dissolved in 50 g of distilled water with stirring to obtain an aqueous solution of iron.

[0042] Slowly add the titanium hydrolysis solution into the silicon hydrolysis solution under vigorous stirring, and stir at room temperature for 30 minutes to obtain a titanium-silicon mixture.

[0043] Under vigorous stirring, the aqueous solution of iron was added dropwise to the mixed solution of titanium and silicon, and the stirring was continued for 30 m...

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Abstract

The invention provides a preparation method of a bifunctional titanium-silicon molecular sieve, which is characterized in that it uses cheap silicon sources, titanium sources, template agents, alkali sources and trivalent metal salts as raw materials, and is synthesized by a hydrothermal synthesis method. The product prepared by the method of the invention not only has high selective oxidation activity, but also has strong acid catalytic activity.

Description

technical field [0001] The invention provides a preparation method of a bifunctional titanium-silicon molecular sieve, and more specifically relates to a preparation method of a titanium-silicon molecular sieve having redox catalytic activity and acid catalytic activity. Background technique [0002] Titanium silicate molecular sieve TS-1 is a new type of catalytic material with redox ability developed in the early 1980s. TS-1 molecular sieve for H 2 o 2 Participated in many organic oxidation reactions, such as propylene epoxidation to propylene oxide, phenol hydroxylation to quinone, cyclohexanone amine oxidation, cyclohexanone oxime, etc., have excellent catalytic activity and selective oxidation function. Prototype molecular sieve catalysts have good application prospects. Since then, efforts have been made to convert other metal ions (B 3+ 、Al 3+ , Ga 3+ and Fe 3+ ) and titanium are doped into the molecular sieve framework in order to modify the catalytic performa...

Claims

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Application Information

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IPC IPC(8): B01J29/89B01J37/00C07D301/12C07D303/08C07C43/04C07C41/09
Inventor 张小明李颢雷骞索继栓
Owner CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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