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Preparation method of mesoporous-microporous titanium silicalite molecular sieves

A technology of silicon molecular sieve and microporous titanium, which is applied in the field of molecular sieve preparation, can solve the problems of poor catalytic oxidation activity and hydrothermal stability, etc., and achieve the effect of large specific surface area and good selectivity

Inactive Publication Date: 2013-02-06
SHAANXI QIYUAN TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalytic oxidation activity and hydrothermal stability of ordered mesoporous TiSi materials are greatly inferior to those of conventional microporous TiSi molecular sieves.

Method used

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  • Preparation method of mesoporous-microporous titanium silicalite molecular sieves

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Mix tetrapropylammonium hydroxide, n-tetrabutyl titanate, ethyl orthosilicate and deionized water at a mass ratio of 1:20:8:1500, react in a constant temperature water bath cup at 35°C for a certain period of time, and then put it into a Crystallize at 140° C. for 1 hour in a kettle lined with polymethyl fluoride to obtain a clear solution of the directing agent.

[0017] Mix hexadecyltrimethylammonium bromide, deionized water, 25% ammonia water, and nanoclusters in a certain proportion, react in a constant temperature water bath cup at 30°C for 5 hours, and then put them into a kettle with a polytetrafluoroethylene liner. Crystallize in an oven at 120°C for 72h, and the product obtained is suction filtered, washed, dried at room temperature, and calcined at 500°C for 4h.

Embodiment 2

[0019] Mix tetrapropylammonium hydroxide, tetrabutyl titanate, ethyl orthosilicate and deionized water evenly at a mass ratio of 1:90:8:1500, react in a constant temperature water bath cup at 35°C for a certain period of time, and then put it into a Crystallize at 140° C. for 1 hour in a kettle lined with polymethyl fluoride to obtain a clear solution of the directing agent.

[0020] Mix hexadecyltrimethylammonium bromide, deionized water, 25% ammonia water, and nanoclusters in a certain proportion, react in a constant temperature water bath cup at 30°C for 5 hours, and then put them into a kettle with a polytetrafluoroethylene liner. Crystallize in an oven at 120°C for 72h, and the product obtained is suction filtered, washed, dried at room temperature, and calcined at 500°C for 4h.

Embodiment 3

[0022] Mix tetrapropylammonium hydroxide, n-tetrabutyl titanate, orthosilicate ethyl ester and deionized water at a mass ratio of 1:30:8:1500, and put them in a constant temperature water bath cup at 35°C for a certain period of time before putting them into a Crystallize at 140° C. for 1 hour in a kettle lined with polymethyl fluoride to obtain a clear solution of the directing agent.

[0023] Mix hexadecyltrimethylammonium bromide, deionized water, 25% ammonia water, and nanoclusters in a certain proportion, react in a constant temperature water bath cup at 30°C for 5 hours, and then put them into a kettle with a polytetrafluoroethylene liner. Crystallize in an oven at 120°C for 72h, and the product obtained is suction filtered, washed, dried at room temperature, and calcined at 500°C for 4h.

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Abstract

The invention relates to a preparation method of molecular sieves, in particular to a preparation method of mesoporous-microporous titanium silicalite molecular sieves. The method includes: uniformly mixing tetrapropylammonium hydroxide, tetrabutyl titanate, tetraethyl orthosilicate and deionized water in the mass ratio of 1:20-90:8:1500, reacting at the constant temperature of 35 DEG C prior to mixing with polymethyl vinyl fluoride, and crystallizing for 1 hour at the temperature of 140 DEG C to obtain nano-clusters; and mixing hexadecyl trimethyl ammonium bromide, the deionized water, ammonia water 25% in concentration and the polymethyl vinyl fluoride, crystallizing for 72 hours at the temperature of 120 DEG C to obtain a product, and subjecting the product to suction filtration, washing, drying at the room temperature and roasting for 4 hours at the temperature of 500 DEG C so that the mesoporous-microporous titanium silicalite molecular sieves are obtained. Experimental results show that the mesoporous-microporous titanium silicalite molecular sieves prepared by the method are large in specific surface area, and micropores are reserved in pore walls of mesopores; primary and secondary building units of TS-1 molecular sieves are successfully introduced into the pore walls of the mesoporous molecular sieves; and the mesoporous-microporous titanium silicalite molecular sieves prepared by the method has good selectivity on generation of styrene oxide in epoxidation reaction of styrene.

Description

technical field [0001] The invention relates to a preparation method of molecular sieves. Background technique [0002] In the process of fine chemical industry, such as green catalytic oxidation reaction, the traditional catalyst is TS-1 molecular sieve, which was first synthesized by Taramasso et al. in 1983. Its unique catalytic oxidation performance has attracted widespread attention. The catalytic oxidation process using TS-1 molecular sieve as a catalyst has no pollution and mild reaction conditions, which overcomes the shortcomings of serious pollution and lengthy and complicated reaction process in the traditional process. As early as 1987, a plant with an annual output of 1 Mt of phenol hydroxylation to produce diphenols using TS-1 as a catalyst was built and put into operation in Italy. However, due to its pore size between 0.5 and 0.6 nm, its current applications are limited to catalyzing olefin epoxidation, phenol hydroxylation, cyclohexanone ammoxidation, etc. ...

Claims

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Application Information

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IPC IPC(8): C01B39/08
Inventor 张淑芬
Owner SHAANXI QIYUAN TECH DEV
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