Noble metal modified mesoporous titanium silicalite molecular sieve, compounding method and application thereof and method for oxidizing cyclic ketone

A technology of titanium-silicon molecular sieves and precious metals, applied in the field of oxidized cyclic ketones, to achieve the effects of improving synthesis efficiency, reducing dosage, and high crystallinity

Active Publication Date: 2017-06-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the yield, mesoporous order (relative crystallinity) and catalytic performance of Ti-MCM-41 prepared by existing methods still need to be further improved.

Method used

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  • Noble metal modified mesoporous titanium silicalite molecular sieve, compounding method and application thereof and method for oxidizing cyclic ketone
  • Noble metal modified mesoporous titanium silicalite molecular sieve, compounding method and application thereof and method for oxidizing cyclic ketone
  • Noble metal modified mesoporous titanium silicalite molecular sieve, compounding method and application thereof and method for oxidizing cyclic ketone

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Embodiment approach

[0021] According to a preferred embodiment of the present invention, the method of the present invention comprises:

[0022] (1) Hydrolyze the organosilicon source, titanium source, precious metal source, alkali source and surfactant to obtain a mixture A, perform the first crystallization on the obtained mixture A, and dry or not dry the solid product after the first crystallization After roasting;

[0023] (2) In the presence of water, the calcined product is mixed with an inorganic silicon source to obtain a mixture B, and the obtained mixture B is subjected to a second crystallization.

[0024] According to the method of the present invention, preferably in step (2), the molar ratio of the inorganic silicon source in terms of silicon oxide to water is 1:(5-250). Wherein, the water in step (2) can be derived from raw materials such as inorganic silicon sources, or can be additionally added, as long as the requirements of the present invention are met.

[0025] According t...

Embodiment 1

[0100] First, 50 grams of tetraethyl orthosilicate and cetyltrimethylammonium bromide were added to the tetrapropylammonium hydroxide aqueous solution in which tetrabutyl titanate and palladium chloride were pre-dispersed and stirred, and the orthosilicate The molar ratio of tetraethyl titanate, tetrabutyl titanate, palladium chloride, tetrapropylammonium hydroxide, cetyltrimethylammonium bromide and water is 1:0.02:0.01:0.45:0.15:85, Among them, organosilicates are represented by SiO 2 Meter, titanium source as TiO 2 Alkali source is measured in N. After the silicon ester is hydrolyzed (the hydrolysis rate of the organic silicon source is 100%), the mixture is transferred to a sealed reactor for hydrothermal crystallization at 110°C for 12 hours. After cooling, the reactor is opened to the crystallization system Add silica gel A and mix well, wherein the molar ratio of silica gel to organic silicon source is 1:0.2 in terms of silica, and then continue to crystallize the mixt...

Embodiment 2

[0102] First, 50 grams of tetramethyl orthosilicate and surfactant tetradecyltrimethylammonium bromide are added to the tetrapropylammonium hydroxide aqueous solution in which tetraethyl titanate and palladium acetate have been dispersed in advance and stirred and mixed, wherein The molar ratio of tetramethyl orthosilicate, tetraethyl titanate, palladium acetate, tetrapropylammonium hydroxide, surfactant and water is 1:0.008:0.02:0.15:0.05:25, in which organic silicate is SiO 2 Meter, titanium source as TiO 2 Alkali source is calculated in N. After the silicon ester is hydrolyzed (the hydrolysis rate of the organic silicon source is 50%), the mixture is transferred to a sealed reactor for hydrothermal crystallization at 120°C for 5 hours. After cooling, the reactor is opened to the crystallization system Add silica gel B and mix well, wherein the molar ratio of silica gel to organic silicon source is 1:0.1 in terms of silica, and then continue to crystallize the mixture in a ...

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Abstract

The invention relates to the field of catalytic material synthesis and specifically provides a noble metal modified mesoporous titanium silicalite molecular sieve and a compounding method thereof. The method comprises the following steps: (1) hydrolyzing an organic silicon source, a titanium source, a noble metal source, an alkali source and a surface active agent, so as to obtain a mixture A, and then performing first crystallization on the obtained mixture A; and (2) mixing the material after the first crystallization with the inorganic silicon source, so as to obtain a mixture B, and then performing second crystallization on the obtained mixture B. The invention provides the noble metal modified mesoporous titanium silicalite molecular sieve compounded according to the method provided by the invention. The invention provides an application of the noble metal modified mesoporous titanium silicalite molecular sieve provided by the invention in oxidizing reaction. The invention provides a method for oxidizing cyclic ketone. According to the compounding method for the noble metal modified mesoporous titanium silicalite molecular sieve, provided by the invention, the relative low-cost inorganic silicon source, such as, silica gel or silica sol, can be used as a part and even main silicon source, so that the dosage of organic silicone can be reduced and the compounding benefit can be greatly increased.

Description

technical field [0001] The invention relates to a synthesis method of a noble metal modified mesoporous titanium silicon molecular sieve, a noble metal modified mesoporous titanium silicon molecular sieve synthesized by the method and its application in an oxidation reaction, and a method for oxidizing cyclic ketones. Background technique [0002] Titanium-silicon molecular sieve is a new molecular sieve containing heteroatom titanium, which was developed in the early 1980s. Among them, TS-1 molecular sieve is a new type of titanium-silicon molecular sieve with excellent directional oxidation catalytic performance formed by introducing transition metal element titanium into the molecular sieve framework with ZSM-5 structure. However, TS-1 only has a microporous (about 0.55 nanometer) structure, and it is difficult for large organic molecules to diffuse and be catalyzed and oxidized in it, making it difficult to exert its excellent catalytic oxidation performance in a wider f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08B01J29/89C07C407/00C07C409/22
CPCB01J29/89C01B39/085C01P2002/70C01P2002/84C01P2006/12C01P2006/17C07C407/00C07C409/22
Inventor 林民史春风朱斌
Owner CHINA PETROLEUM & CHEM CORP
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