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Tin-titanium-silicon molecular sieve, preparation method and application thereof, and a method for hydroxylation of phenol

A technology of tin-titanium-silicon molecular sieve and silicon molecular sieve, which is applied in molecular sieve catalysts, chemical instruments and methods, and the preparation of organic compounds, etc.

Active Publication Date: 2018-01-05
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] CN1301599A, CN1338427A and CN1338428A etc. disclose titanium-silicon molecular sieves and all-silicon molecular sieves with a hollow structure, but so far, there is no report of a tin-titanium-silicon molecular sieve with a cavity structure inside the grain

Method used

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  • Tin-titanium-silicon molecular sieve, preparation method and application thereof, and a method for hydroxylation of phenol
  • Tin-titanium-silicon molecular sieve, preparation method and application thereof, and a method for hydroxylation of phenol
  • Tin-titanium-silicon molecular sieve, preparation method and application thereof, and a method for hydroxylation of phenol

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preparation example Construction

[0038] The aforementioned tin-titanium-silicon molecular sieve of the present invention has the advantages of high catalytic activity, good selectivity, and is conducive to the diffusion of reactants and products. Tin-titanium-silicon molecular sieves are sufficient. According to a preferred embodiment of the present invention, the present invention provides a method for preparing tin-titanium-silicon molecular sieves, wherein the method includes:

[0039] (1) contacting the tin source, the titanium source and the templating agent in the presence of an aqueous solvent to obtain the first mixture;

[0040] (2) mixing the first mixture with silicon molecular sieves to obtain a second mixture;

[0041] (3) Under hydrothermal crystallization conditions, the second mixture is crystallized.

[0042] According to the present invention, the temperature of the contact can be selected in a wide range. For the preferred step (1) of the present invention, the conditions of the contact in...

Embodiment 1

[0086] (1) At 25°C, stirring and contacting tetrapropylammonium hydroxide aqueous solution (concentration: 15% by weight) with tetrabutyl titanate and tin tetrachloride pentahydrate for 30 minutes to obtain a mixture;

[0087] (2) At 60°C, add silicon molecular sieve S-1 to the above mixture and stir for 0.5h to obtain the mixture (during this contact process, add water or not add water as required, if the feeding in step (1) can meet the requirement of water Feeding requirements, there is no need to add water, if it is not met, you can add water when the mixture containing tetrapropylammonium hydroxide, tetrabutyl titanate and tin chloride is stirred and contacted with silicon molecular sieve, or distill off water, and the rest Embodiment is similar, no longer repeat description); Wherein, the molar ratio that guarantees each material is: silicon source (silicon molecular sieve): alkali source templating agent (tetrapropyl ammonium hydroxide): titanium source (tetrabutyl titan...

Embodiment 2

[0099] (1) At 25°C, stirring and contacting tetrapropylammonium hydroxide aqueous solution (concentration: 20% by weight) with tetrabutyl titanate and tin tetrachloride pentahydrate for 30 minutes to obtain a mixture;

[0100] (2) At 25°C, add silicon molecular sieve S-1 to the above mixture and stir for 0.5h to obtain the mixture; wherein, ensure that the molar ratio of each substance is: silicon source (silicon molecular sieve): alkali source template (four Propyl ammonium hydroxide): titanium source (tetrabutyl titanate): tin source (tin tetrachloride): water=100:15:2:0.1:200, wherein the silicon source is SiO 2 In terms of titanium source as TiO 2 Tin source is calculated as tin element;

[0101] (3) Transfer the above mixture into a sealed stainless steel reaction kettle, crystallize at 160°C for 120 hours under autogenous pressure, filter the resulting crystallized product, wash with water, and dry at 110°C for 120 minutes, then heat at 550°C Roasting at high temperatu...

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Abstract

The invention provides a tin-titanium-silicon molecular sieve and its preparation method and application. The tin-titanium-silicon molecular sieve contains silicon, titanium, tin and oxygen, wherein at least part of the tin-titanium-silicon molecular sieve has hole structure. The invention provides a method for hydroxylation of phenol, which comprises: under the condition of hydroxylation of phenol, contacting phenol and hydrogen peroxide with a catalyst, wherein the catalyst contains the tin-titanium-silicon molecular sieve of the invention. The tin-titanium-silicon molecular sieve of the present invention has a good catalytic oxidation effect, such as for phenol hydroxylation reaction, compared with the titanium-silicon molecular sieve not containing tin or the titanium-silicon molecular sieve loaded with tin, the tin-titanium-silicon molecular sieve of the present invention has high Catalytic oxidation activity, especially the high selectivity of para-product hydroquinone.

Description

technical field [0001] The present invention relates to a tin-titanium-silicon molecular sieve, a method for preparing a tin-titanium-silicon molecular sieve, a tin-titanium-silicon molecular sieve prepared by the preparation method of a tin-titanium-silicon molecular sieve, and an oxidation reaction of the tin-titanium-silicon molecular sieve of the present invention. Application and a method of hydroxylation of phenol. Background technique [0002] Silica molecular sieve, also known as all-silica zeolite, is a molecular sieve whose skeleton is entirely composed of silicon and oxygen elements. For example, Silicalite-1 (S-1) molecular sieve is an all-silicon molecular sieve with a molecular sieve framework of ZSM-5 (MFI) structure. Silicon molecular sieves can be directly used as membrane separation materials, or heteroatom molecular sieve materials can be formed by using other heteroatoms to replace part of the silicon in the framework, and have broad application prospect...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C37/60C07C39/08C01B39/02C01B39/04B01J29/06
Inventor 林民史春风朱斌
Owner CHINA PETROLEUM & CHEM CORP
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