Supported micropore-mesopore composite molecular sieve membrane and preparation method thereof

A composite molecular sieve and molecular sieve membrane technology, applied in molecular sieve catalysts, chemical instruments and methods, organic carbonate preparation, etc., can solve the problems of poor hydrothermal stability and low equilibrium conversion rate of mesoporous materials, and achieve improved equilibrium conversion rate, The effect of enhancing hydrothermal stability

Inactive Publication Date: 2018-02-16
晋中市智诚科技服务中心
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  • Abstract
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Problems solved by technology

[0005] Luo Shuwen and others found that the Ti-HMS mesoporous molecular sieve prepared by introducing Ti into the pore wall of pure silicon mesoporous molecular sieve HMS made the reaction of diphenyl carbonate prepared by transesterification of dimethyl carbonate and phenol have high selectivity, but the balance The conversion rate is low, and the hydrothermal stability of the mesoporous material is poor

Method used

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  • Supported micropore-mesopore composite molecular sieve membrane and preparation method thereof
  • Supported micropore-mesopore composite molecular sieve membrane and preparation method thereof
  • Supported micropore-mesopore composite molecular sieve membrane and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Preparation of TS-1 microporous precursor solution: Add 14.013g tetrapropylammonium hydroxide (TPAOH) (10.676wt%) and 12.026g water into a three-neck flask, stir vigorously for 20min; slowly add 5.676g ethyl orthosilicate ( TEOS) was vigorously stirred for 3 hours until clarified to obtain a silicon-containing clear liquid; 0.3091 g of tetrabutyl titanate was dissolved in 1.326 g of isopropyl

[0020] Alcohol to obtain titanium-containing isopropanol solution, in ice-salt bath and N 2 Add the obtained titanium-containing isopropanol solution dropwise into the silicon-containing clear solution under protection and slow stirring. After about 1 hour, remove the isopropanol at a constant temperature in a water bath at 80°C for about 0.5 hours, and evaporate to remove the isopropanol. After adding deionized water to the original volume, the molar ratio obtained is SiO 2 : TiO 2 : TPAOH: H 2 O=1:0.033:0.27:50 clear microporous structure synthesis liquid; then transfer the ...

Embodiment 2

[0023] The preparation of TS-1 microporous precursor solution was the same as in Example 1. In the synthesis steps of Ti-HMS-1 molecular sieve membrane, except that the crystallization temperature was 100 °C and the crystallization time was 96 h, the rest were the same as in Example 1.

Embodiment 3

[0025] In the preparation steps of the TS-1 microporous precursor solution, except that the amount of tetrapropylammonium hydroxide (10.676%) was 10.4g, and the amount of ionized water was 15.3g, the rest were the same as in Example 1.

[0026] In the synthesis steps of Ti-HMS-1 molecular sieve membrane, except that the dosage of mesoporous template DDA is 1g, the dosage of TS-1 microporous precursor solution is 25ml, the crystallization temperature is 160℃, and the crystallization time is 36h, the rest are Same as Example 1.

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Abstract

The invention relates to a supported micropore-mesopore composite molecular sieve membrane and a preparation method thereof. The supported micropore-mesopore composite molecular sieve membrane is composed of a porous carrier and a layered compact Ti-HMS-1-micropore-mesopore composite molecular sieve membrane loaded on the porous carrier. The Ti-HMS-1-micropore-mesopore composite molecular sieve membrane is prepared by introducing a TS-1 micropore secondary structure unit into the pore walls of a pure silicon mesoporous molecular sieve HMS. The Ti-HMS-1-micropore-mesopore composite molecular sieve membrane can be applied to reactions with a low equilibrium conversion rate, such as exchange reactions between dimethyl carbonate and phenol ester to prepare diphenyl carbonate, as a catalytic separation membrane, so that catalytic reactions and separation are carried out at the same time during the reaction process. Through the separation effect of the catalytic membrane, products are removed out of the reaction system continuously, the thermodynamic equilibrium is broken down, and the yield is improved.

Description

technical field [0001] The invention relates to a loaded microporous-mesoporous composite molecular sieve membrane and a preparation method thereof, which belongs to the technical field of molecular sieve materials, and more specifically relates to a Ti-HMS-1 microporous-mesoporous composite molecular sieve loaded on a porous carrier and its preparation method. Background technique [0002] In 1992, Mobil Corporation reported for the first time the ordered siliceous mesoporous molecular sieve series material M 41S, which opened the prelude to the scientific research on mesoporous molecular sieves. Compared with microporous molecular sieves, mesoporous molecular sieves not only have a uniform and regular pore structure, a larger adjustable pore size, but also a larger specific surface area. Therefore, once the material came out, it has attracted extensive attention from researchers in related disciplines. However, the hydrothermal stability of mesoporous molecular sieves is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89C07C68/06C07C69/96
Inventor 胡晓军
Owner 晋中市智诚科技服务中心
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