Titanium silicon molecular sieve, and preparation method and application thereof

A titanium-silicon molecular sieve and titanium source technology, applied in molecular sieve compounds, molecular sieve catalysts, molecular sieve characteristic silicates, etc., can solve the problems of restricting mesoporous materials, unable to achieve satisfactory results, and poor hydrothermal stability.

Active Publication Date: 2018-03-27
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although Ti-MCM-41, a titanium-containing mesoporous material, has been synthesized and achieved good results in many oxidation reactions; however, due to the amorphous pore wall of the mesoporous material, there is a hydrothermal The disadvantages of poor stability and low mechanical strength restrict the practical application of this mesoporous material
[0005] In addition, the prior art has attempted to introduce additional channels into molecular sieve crystals to improve the diffusion properties of molecular sieves, such as the development of Ti-β containing twelve-membered ring three-dimensional pore structures, molecular sieves containing twelve-membered ring supercage structures, and Ti- MWW, Ti-SBA-15, Ti-HMS and other titanium-silicon materials with large pores, but these catalytic materials still cannot achieve satisfactory results in catalytic reactions involving macromolecules

Method used

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  • Titanium silicon molecular sieve, and preparation method and application thereof
  • Titanium silicon molecular sieve, and preparation method and application thereof
  • Titanium silicon molecular sieve, and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0074] (1) Mix 31.0 g tetraethyl silicate, 1.8 g tetrabutyl titanate and 15 g tetrapropyl ammonium hydroxide solution (mass concentration 24.4%), add 25 g deionized water under stirring, and Hydrolyze and remove the alcohol for 4 hours while supplementing the evaporated water to obtain a slightly yellow transparent aqueous solution;

[0075] (2) Put the product obtained in step (1) into a closed stainless steel reaction kettle, and let it stand at 80° C. for 24 hours to obtain a precrystallized product;

[0076] (3) Add 2.0 g of the compound represented by formula (III) to the above pre-crystallized product, stir at room temperature for 2 hours to form a transparent viscous liquid, transfer the above liquid to a stainless steel airtight reaction kettle, and keep the temperature at 90°C After 12 hours, slowly raise the temperature to 165°C at a rate of 1°C / min, keep the temperature for 2 days, then filter, wash, dry at 120°C for 12 hours, and roast at 550°C for 6 hours to obtai...

Embodiment 2

[0082] (1) Mix 31.0 g tetraethyl silicate, 1.8 g tetrabutyl titanate and 15 g tetrapropyl ammonium hydroxide solution (mass concentration 24.4%), add 25 g deionized water under stirring, and Hydrolyze and remove the alcohol for 4 hours while supplementing the evaporated water to obtain a slightly yellow transparent aqueous solution;

[0083] (2) Put the product obtained in step (1) into a closed stainless steel reaction kettle, and let it stand at 100° C. for 6 hours to obtain a precrystallized product;

[0084] (3) Add 0.80 g of the compound represented by formula (IV) to the above pre-crystallized product, stir at room temperature for 2 hours to form a transparent viscous liquid, transfer the above liquid to a stainless steel airtight reaction kettle, and keep the temperature at 90°C After 48 hours, slowly raise the temperature to 165°C at a rate of 1°C / min, keep the temperature constant for 0.5 days, then filter, wash, dry at 120°C for 12 hours, and roast at 550°C for 6 hou...

Embodiment 3

[0090] (1) Mix 26.0g tetraethyl silicate, 1.27g tetrabutyl titanate and 10.4g tetrapropylammonium hydroxide solution (mass concentration 24.4%), add 26g deionized water under stirring, and Hydrolyze and remove the alcohol for 7 hours, and replenish the evaporated water at the same time to obtain a light yellow transparent aqueous solution;

[0091] (2) Put the product obtained in step (1) into a closed stainless steel reaction kettle, and let it stand at 80° C. for 24 hours to obtain a precrystallized product;

[0092] (3) Add 0.20 g of the compound represented by formula (III) to the above pre-crystallized product, stir at room temperature for 2 hours to form a transparent viscous liquid, transfer the above liquid to a stainless steel closed reaction kettle, and keep the temperature at 100°C After 24 hours, the temperature was slowly raised to 155°C at a rate of 1°C / min, and the temperature was kept constant for 3 days. Then the obtained material was filtered, washed, dried a...

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Abstract

The invention relates to a titanium silicon molecular sieve, and a preparation method and application thereof. The preparation method comprises the following steps: (1) mixing a titanium source, a template tetraalkoxysilane and water, carrying out hydrolysis and remove alcohol; and (2) adding a compound with a structure as shown in a formula (I) and carrying out crystallization. The method can prepare the titanium silicon molecular sieve containing more mesopores; and the prepared titanium silicon molecular sieve is applicable to catalysis of the reactions of macromolecules.

Description

technical field [0001] The invention relates to a titanium-silicon molecular sieve and its preparation method and application, in particular to a micro-mesoporous titanium-silicon molecular sieve and its preparation method and application. Background technique [0002] The pore size of porous materials is generally divided into three levels: pores with a pore size less than 2 nm are called micropores; pores with a pore size between 2 and 50 nm are called mesopores (also known as mesoporous materials); pores with a pore size greater than 50 nm to 1000 nm are called micropores. for large holes. Microporous molecular sieves have high specific surface area, developed microporous structure, strong acidity and high hydrothermal stability, but their small pore size limits their application in macromolecular catalytic reactions. Although the mesoporous molecular sieve has a larger pore size, its stability and acidity are weak. It is hoped in the field to prepare molecular sieves w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/00B01J29/89C07D303/42C07D301/19
CPCB01J29/89C01B37/005C01P2002/72C01P2006/12C01P2006/14C01P2006/17C07D301/19C07D303/42
Inventor 张耀林民朱斌王宝荣段庆华刘依农夏长久彭欣欣舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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