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A kind of vanadium silicon molecular sieve and preparation method thereof

The technology of silicon molecular sieve and vanadium source is applied in the field of vanadium silicon molecular sieve and its preparation, which can solve the problems of vanadium silicon molecular sieve and the like, and achieve the effect of good catalytic oxidation effect, high selectivity and improving effective utilization rate.

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

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 vanadium-silicon molecular sieve with a cavity structure inside the grain

Method used

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  • A kind of vanadium silicon molecular sieve and preparation method thereof
  • A kind of vanadium silicon molecular sieve and preparation method thereof
  • A kind of vanadium silicon molecular sieve and preparation method thereof

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preparation example Construction

[0024] According to the preparation method of the present invention, the type of vanadium source can be selected in a wide range, and any material containing vanadium (such as a compound containing vanadium element and / or vanadium element) can achieve the purpose of the present invention. In the invention, the vanadium source is preferably a compound containing vanadium element, which may be one or more of inorganic vanadium compounds and organic vanadium compounds. Inorganic vanadium compounds such as various inorganic salts of vanadium and their hydrates (such as vanadium trichloride, vanadium tetrachloride, vanadium pentachloride, vanadium nitrate, vanadium oxychloride, vanadium sulfate, vanadium phosphate, etc.), vanadium partial Acids and their salts (such as ammonium metavanadate, sodium metavanadate, etc.), vanadic acid and its salts (such as ammonium vanadate, sodium vanadate, etc.), vanadium oxides (such as vanadium trioxide, vanadium pentoxide etc.); organic vanadium...

Embodiment 1

[0047] (1) At 25°C, an aqueous solution of tetrapropylammonium hydroxide (concentration: 15% by weight) was stirred and contacted with vanadium trichloride for 30 minutes to obtain a mixture containing tetrapropylammonium hydroxide and vanadium chloride;

[0048] (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 according to the need, if the feeding in step (1) can meet the requirement of water Feeding requirements, then no need to add water, if not satisfied, you can additionally add water when the mixture containing tetrapropylammonium hydroxide and vanadium chloride is stirred and contacted with silicon molecular sieves, the rest of the examples are similar and will not be repeated); , to ensure that the molar ratio of each material is: silicon source (silicon molecular sieve): alkali source templating agent (tetrapropylammonium hydroxide): vanadium source (vanadium chlorid...

Embodiment 2

[0060] (1) At 25°C, an aqueous solution of tetrapropylammonium hydroxide (concentration: 20% by weight) was stirred and contacted with vanadium pentachloride for 30 minutes to obtain a mixture containing tetrapropylammonium hydroxide and vanadium chloride;

[0061] (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): vanadium source (vanadium chloride): water=100:15:0.1:800, wherein, the silicon source is calculated as SiO2, and the vanadium source is calculated as vanadium element;

[0062] (3) Transfer the above mixture into a stainless steel sealed reaction kettle, crystallize at 160°C and autogenous pressure for 120h, filter the resulting crystallized product, wash with water, and dry at 110°C for 120 minutes, then at 550°C Roasted at high temperature for 3 hours t...

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Abstract

The invention provides a vanadium-silicon molecular sieve, which is characterized in that it contains silicon element, vanadium element and oxygen element, all or part of the crystal grains have holes or cavity structures, and the total specific surface area is ≥300m2 / g, and the external specific surface area The proportion of total specific surface area is ≥5%. The vanadium silicon molecular sieve of the present invention has good catalytic oxidation effect, has high selectivity for para product hydroquinone when used in phenol hydroxylation reaction, and can improve the effective utilization rate of the oxidant.

Description

technical field [0001] The invention relates to a vanadium-silicon molecular sieve and a preparation method thereof. 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 prospects. [0003] Vanadium metal is introduced into molecular sieves, such as introduced into β-type all-silicon molecular sieves to form V-β molecular sieves, and introduced into molecular sieves with MFI structure to form VS-1 molecular sieves. Used in the process of catalytic oxidation reaction, it has good c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B37/06B01J29/03C07C37/60C07C39/08
CPCC01B39/08C07C37/60B01J29/03C01P2002/72C01P2006/12B01J2229/183B01J35/615C07C39/08
Inventor 史春风朱斌林民
Owner CHINA PETROLEUM & CHEM CORP