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Preparation method of mesoporous titanium silicalite molecular sieve nanoparticles

A titanium-silicon molecular sieve and nanoparticle technology, applied in molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve the problem that the catalytic performance cannot be well exerted, and the contact frequency between the reactant and the reactive center is low. , limit a wide range of applications, etc., to achieve the effects of excellent catalytic performance, inhibition of possible side reactions, and short preparation cycle

Inactive Publication Date: 2019-09-17
SHANGHAI NAT ENG RES CENT FORNANOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Studies have shown that the particle size of the existing mesoporous titanium-silicon materials is mostly in the micron range. Due to the large particle size, the contact frequency between the reactant and the active center in the catalytic reaction is low, so that its catalytic performance cannot be achieved. well played, which limits its wider application

Method used

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  • Preparation method of mesoporous titanium silicalite molecular sieve nanoparticles

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Experimental program
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Embodiment 1

[0026] A preparation method of mesoporous titanium silicon molecular sieve nanoparticles, according to the following steps:

[0027] 1. Weigh tetraethyl orthosilicate, polyvinyl alcohol, deionized water, ammonia water with a mass concentration of 25%, tetrabutyl titanate, hydrogen peroxide and polyquaternium-6, wherein, ethyl orthosilicate The molar ratio with polyvinyl alcohol is 1:0.1, the molar ratio of ethyl orthosilicate and deionized water is 1:50, the mass ratio of ethyl orthosilicate and ammonia water with a mass concentration of 25% is 1:1, The molar ratio of ethyl orthosilicate to tetrabutyl titanate is 1:0.03, the molar ratio of ethyl orthosilicate to hydrogen peroxide is 1:2, and the mass ratio of polyquaternium-6 to polyvinyl alcohol is 1:0.05;

[0028] 2. Add the polyvinyl alcohol, polyquaternium-6 and ammoniacal liquor with a mass concentration of 25% into deionized water successively in step 1. After mixing evenly, a mixed solution is obtained, and then under ...

Embodiment 2

[0033] A preparation method of mesoporous titanium silicon molecular sieve nanoparticles, according to the following steps:

[0034] 1. Weigh tetraethyl orthosilicate, polyvinyl alcohol, deionized water, ammonia water and tetrabutyl titanate, hydrogen peroxide and polyquaternium-6 with a mass concentration of 25%, wherein tetraethyl orthosilicate and The molar ratio of polyvinyl alcohol is 1:0.18, the molar ratio of ethyl orthosilicate to deionized water is 1:65, the mass ratio of ethyl orthosilicate to ammonia water with a mass concentration of 25% is 1:1, and The molar ratio of ethyl silicate to tetrabutyl titanate is 1:0.025, the molar ratio of tetraethyl orthosilicate to hydrogen peroxide is 1:2, and the mass ratio of polyquaternium-6 to polyvinyl alcohol is 1 : 4.5;

[0035] 2. Add the polyvinyl alcohol, polyquaternium-6 and ammoniacal liquor with a mass concentration of 25% into deionized water successively in step 1. After mixing evenly, a mixed solution is obtained, a...

Embodiment 3

[0040] A preparation method of mesoporous titanium silicon molecular sieve nanoparticles, according to the following steps:

[0041] 1. Weigh tetraethyl orthosilicate, polyvinyl alcohol, deionized water, ammonia water and tetrabutyl titanate, hydrogen peroxide and polyquaternium-6 with a mass concentration of 25%, wherein tetraethyl orthosilicate and The molar ratio of polyvinyl alcohol is 1:0.15, the molar ratio of ethyl orthosilicate to deionized water is 1:60, the mass ratio of ethyl orthosilicate to ammonia water with a mass concentration of 25% is 1:1.2, and The molar ratio of ethyl silicate to tetrabutyl titanate is 1:0.01, the molar ratio of tetraethyl orthosilicate to hydrogen peroxide is 1:4, and the mass ratio of polyquaternium-6 to polyvinyl alcohol is 1 : 2;

[0042] 2. Add the polyvinyl alcohol, polyquaternium-6 and ammoniacal liquor with a mass concentration of 25% into deionized water successively in step 1. After mixing evenly, a mixed solution is obtained, an...

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Abstract

The invention elates to a preparation method of mesoporous titanium silicalite molecular sieve nanoparticles. The preparation method comprises following steps polyvinyl alcohol, polyquaternium-6, and ammoniacal liquor are added into deionized water successively, uniform mixing is carried out so as to obtain a mixed solution, ethyl orthosilicate and tetrabutyl titanate are added into an obtained mixed solution drop by drop, and stirring is carried out continuously so as to obtain a precursor solution; the precursor solution is subjected to hydro-thermal treatment, a solid phase product is separated, washed, and dried, and is subjected to sintering in a muffle furnace so as to obtain the mesoporous titanium silicalite molecular sieve nanoparticles. Compared with the prior art, the advantages are that: the prepared mesoporous titanium silicalite molecular sieve nanoparticle possesses abundant mesoporous pores and channels which are communicated with each other, and excellent catalytic performance in ammoximation synthesis reaction of cyclohexanone-oxime from cyclohexanone.

Description

technical field [0001] The invention belongs to the technical field of molecular sieves, and relates to a method for preparing mesoporous titanium-silicon molecular sieve nanoparticles, and is particularly suitable for the field of preparation of cyclohexanone oxime catalysts by ammoxidation of cyclohexanone. Background technique [0002] Since Mobil first developed the M41S series of materials in 1992, mesoporous SiO2 has been widely used in the fields of ion exchange, adsorption and separation, host-guest chemistry and industrial catalysis because of its regular channels, large specific surface area and adjustable pore size. With broad application prospects, it has gradually become a research hotspot of mesoporous materials. A large number of studies have shown that introducing transition metal elements into the framework of mesoporous SiO2 can obtain highly active and highly selective mesoporous catalytic materials. Among them, mesoporous titanium-silicon materials conta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04B01J29/89
CPCC01B39/04B01J29/89
Inventor 胡丹赵昆峰童琴
Owner SHANGHAI NAT ENG RES CENT FORNANOTECH
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