Silicon-containing molecular sieve and preparation method thereof

A silicon molecular sieve and silicon source technology, applied in the direction of molecular sieve compounds, molecular sieve characteristic aluminum phosphate, chemical instruments and methods, etc., can solve the problem of difficulty in ensuring uniform distribution of active components, weak interaction between metal oxides and carriers, and effective use of active centers Low efficiency and other problems, to achieve high selectivity of the target product, increase the effective utilization rate, good activity stability and hydrothermal stability

Inactive Publication Date: 2018-06-05
江西科因润滑材料有限公司
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0006] Although the above, the interaction between metal oxide and carrier is weak, the stability of the supported catalytic material needs to be improved; in the supported catalyst, the content of metal oxide is high (>1% mass fraction), which is difficult to ensure the active component can be evenly distributed; the pore size of the AFI and MFI structures is not greater than 0.55nm, while the molecular size of cyclohexyl hydroperoxide is about 0.74nm, the Cr active center in the two molecular sieves is difficult to interact with CHHP, and the active center of the heteroatom molecular sieve The effective utilization rate is low; although the mesoporous TUD has a large pore structure, its pore wall is an amorphous species, and its hydrothermal stability is not ideal

Method used

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  • Silicon-containing molecular sieve and preparation method thereof
  • Silicon-containing molecular sieve and preparation method thereof
  • Silicon-containing molecular sieve and preparation method thereof

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preparation example Construction

[0025] The invention provides a method for preparing a silicon-containing molecular sieve, the method comprising:

[0026] (1) hydrolyzing the silicon source, the Group VIII metal source and the structure directing agent to obtain the hydrolyzed material;

[0027] (2) crystallizing the hydrolyzed material;

[0028] Wherein, the Group VIII metal source is an iron source or a mixture of an iron source and a cobalt source, step (1) is carried out in the presence of an organophosphorus compound and / or before step (2) is carried out, the hydrolyzed material is mixed with an organic The crystallization is performed after the phosphorus compound is mixed.

[0029] In the present invention, the organophosphorus compound refers to an organic compound containing phosphorus.

[0030] The silicon-containing molecular sieve prepared by the method of the present invention has a large specific surface area, uniform distribution of active centers and good accessibility, strong surface hydro...

Embodiment approach

[0033] According to a preferred embodiment of the present invention, the method comprises:

[0034] (1) hydrolyzing the silicon source, the Group VIII metal source, the first part of the organophosphorus compound and the structure directing agent to obtain a hydrolyzed material;

[0035] (2) The crystallization is carried out after mixing the hydrolyzed material with the second part of organophosphorus compound. According to the aforementioned steps, the performance of the silicon-containing molecular sieve can be further improved, for example, its catalytic decomposition performance as a catalyst for the catalytic decomposition of cyclohexyl hydroperoxide can be improved, the ratio of alcohol to ketone can be greatly improved, and the selectivity of alcohol to ketone is high.

[0036] According to the method of the present invention, preferably based on the total amount of the organophosphorus compound being 100% by weight, the amount of the first part of the organophosphorus...

Embodiment 1

[0088] (1) hydrolyzing tetraethyl orthosilicate, ferric nitrate, tripropyl phosphate, tetrapropyl ammonium hydroxide aqueous solution (concentration: 25% by weight) to obtain hydrolyzed material; the temperature of hydrolysis is 30°C, and the time is 10h;

[0089] (2) The hydrolyzed material, tripropyl phosphate and methyltriethoxysilane are mixed and then transferred to a crystallization kettle for crystallization, wherein the mixing conditions include: the temperature is 70°C, the time is 4h, the crystallization The conditions for crystallization include: crystallization under autogenous pressure under airtight conditions, the temperature is 160°C, and the time is 24h;

[0090] Wherein, the consumption of the tripropyl phosphate in the step (1) and the step (2) is respectively 30% by weight and 70% by weight of the total consumption of the tripropylphosphate;

[0091] The molar ratio of each material feeding is SiO 2 : Structure directing agent: Group VIII metal: H 2 O=1:0...

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Abstract

The invention relates to the field of catalysis and in particular provides a silicon-containing molecular sieve and a preparation method thereof. The preparation method comprises the following steps:(1) hydrolyzing a silicon source, a VIII family metal source and a structure directing agent to obtain a hydrolyzed material; and (2) crystallizing the hydrolyzed material, wherein the step (1) is carried out in presence of an organic phosphorus compound and / or before the step (2), the hydrolyzed material is mixed with the organic phosphorus compound, then the crystallization is carried out, and the VIII family metal source is an iron source or a mixture of an iron source and a cobalt source. The silicon-containing molecular sieve prepared by adopting the preparation method can be applied to various fields such as dehydration reaction, selective dehydrogenation reaction, alkylation reaction, denitration reaction (reduction) and isomerization reaction. When the silicon-containing molecularsieve is applied to cyclohexyl hydroperoxide catalytic decomposition, an extra alkaline reagent does not need to be added, and reaction effects such as high alcohol ketone ratio and high alcohol ketone selectivity can be obtained at relatively low temperature.

Description

technical field [0001] The invention relates to a silicon-containing molecular sieve and a preparation method thereof. Background technique [0002] Cyclohexanone is an important basic chemical raw material, which has been used in the production of important chemical products such as caprolactam, adipic acid and ε-caprolactone. According to statistics, by the end of 2015, the production capacity of cyclohexanone in my country had reached 3.65 million tons. In my country, cyclohexanone is mainly produced through cyclohexane oxidation and cyclohexene hydration processes, and the production capacity of cyclohexane oxidation accounts for as high as 63%. [0003] The existing cyclohexane oxidation process mainly includes three processes: cyclohexane oxidation, cyclohexyl hydroperoxide decomposition and cyclohexanol dehydrogenation. Although the cyclohexanol dehydrogenation process is relatively mature and stable, there are many side reactions in the cyclohexane oxidation proces...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/06C01B39/08
CPCC01B37/065C01B39/08C01B39/087
Inventor 王宝荣廖维林舒兴田陈飞彪
Owner 江西科因润滑材料有限公司
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