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Mesoporous titanium silicate molecular sieve, its synthesis method and application, and a method for oxidation of 2,6-di-tert-butylphenol

A technology of di-tert-butylphenol and titanium-silicon molecular sieve is applied in the directions of molecular sieve catalyst, quinone oxide preparation, chemical instruments and methods, etc., to achieve the effect of improving synthesis efficiency, reducing dosage and high relative crystallinity

Active Publication Date: 2017-05-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the titanium-silicon molecular sieve Ti-SBA-15 prepared by the existing method needs to be further improved in terms of synthesis efficiency, catalytic performance and product yield.

Method used

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  • Mesoporous titanium silicate molecular sieve, its synthesis method and application, and a method for oxidation of 2,6-di-tert-butylphenol
  • Mesoporous titanium silicate molecular sieve, its synthesis method and application, and a method for oxidation of 2,6-di-tert-butylphenol

Examples

Experimental program
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Effect test

Embodiment 1

[0070] First mix 50 grams of tetraethyl orthosilicate and EO 20 PO 70 EO 20 (Pluronic P123) is added to the aqueous solution of hydrochloric acid pre-dispersed tetrabutyl titanate and stirred and mixed, wherein the molar ratio of tetraethyl orthosilicate, tetrabutyl titanate, hydrochloric acid, P123 and water is 1:0.02:0.45 : 0.15: 85, where the organosilicate is SiO 2 Meter, titanium source as TiO 2 meter, acid source as H + 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 add silica gel A to the crystallization system and mix well. , in which the molar ratio of the added silica gel to the organosilicon source is 1:0.2 in terms of silicon dioxide, and then the mixture is continuously crystallized in a sealed reaction vessel at a temperature of 150°C and autogenous pressure for 18 ho...

Embodiment 2

[0073] First, 50 grams of tetramethyl orthosilicate and surfactant P123 were added to the aqueous solution of hydrochloric acid in which tetraethyl titanate was dispersed in advance and stirred and mixed, wherein tetramethyl orthosilicate, tetraethyl titanate, hydrochloric acid, P123 The molar ratio of water and water is 1:0.008:0.15:0.05:25, wherein the organosilicate is SiO 2 Meter, titanium source as TiO 2 meter, acid source as H + 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, and after cooling, the reactor is opened to add silica gel B to the crystallization system and mix well , wherein the silica gel added and the organosilicon source molar ratio is 1:0.1 in terms of silicon dioxide, and then the mixture is continued to crystallize in a sealed reactor at a temperature of 140°C and autogenous pressure for 17h, and the o...

Embodiment 3

[0075] First, 50 grams of tetraethyl orthosilicate and P123 are added to the aqueous solution of sulfuric acid in which tetrabutyl titanate has been dispersed before stirring and mixing, wherein tetraethyl orthosilicate, tetrabutyl titanate, sulfuric acid, surfactant and water The molar ratio is 1:0.4:0.35:0.25:150, where the organosilicate is SiO 2 Meter, titanium source as TiO 2 meter, acid source as H + After the silicon ester is hydrolyzed (the hydrolysis rate of the organic silicon source is 60%), the mixture is transferred to a sealed reactor for hydrothermal crystallization at 100°C for 12 hours, and after cooling, the reactor is opened to add silica gel A to the crystallization system and mix well , in which the silica gel added and the organosilicon source molar ratio is 1:0.5 in terms of silicon dioxide, and then the mixture is continued to crystallize in a sealed reaction vessel at a temperature of 130°C and autogenous pressure for 20h, and the obtained crystallize...

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Abstract

The invention provides a method for synthesizing a mesoporous titanium silicate molecular sieve. The method comprises: (1) hydrolyzing an organic silicon source, a titanium source, an acid source and a surfactant to obtain a mixture A, and carrying out primary crystallization on the mixture A; and (2) mixing the materials subjected to primary crystallization with an inorganic silicon source to obtain a mixture B, and carrying out secondary crystallization on the obtained mixture B. The invention provides the mesoporous titanium silicate molecular sieve and an application thereof. The invention provides a method for oxidizing 2,6-di-tert-butylphenol. According to the method disclosed by the invention, the inorganic silicon source which is relatively cheap can be used as a partial or even main silicon source, so that dosage of the organic silicon is reduced while hydrolysis time is shortened and synthesis benefits are greatly improved; and the mesoporous titanium silicate molecular sieve synthesized by the method disclosed by the invention is high in relative crystallinity, high in catalytic oxidation activity and high in selectivity. In a probe reaction of phenol, for example an oxidation reaction of the 2,6-di-tert-butylphenol, the mesoporous titanium silicate molecular sieve has the characteristic of high catalytic oxidation activity.

Description

technical field [0001] The invention relates to a method for synthesizing mesoporous titanium-silicon molecular sieve, the mesoporous titanium-silicon molecular sieve synthesized by the method and its application in phenol oxidation, and a method for oxidizing 2,6-di-tert-butylphenol. 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 field, especially in the field of b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C50/02C01B39/08B01J29/89C07C46/06
Inventor 林民史春风朱斌
Owner CHINA PETROLEUM & CHEM CORP
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