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A kind of method of catalytic decomposition of cyclohexyl hydroperoxide

A cyclohexyl hydroperoxide, catalytic decomposition technology, applied in chemical instruments and methods, physical/chemical process catalysts, molecular sieve catalysts, etc., can solve the problem of difficulty in ensuring uniform distribution of active components, weak interaction between metal oxides and carriers, Low effective utilization of active centers and other issues, to achieve the effect of improving effective utilization, high alcohol-ketone ratio, and improving utilization

Inactive Publication Date: 2020-03-27
江西科因润滑材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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  • A kind of method of catalytic decomposition of cyclohexyl hydroperoxide
  • A kind of method of catalytic decomposition of cyclohexyl hydroperoxide
  • A kind of method of catalytic decomposition of cyclohexyl hydroperoxide

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preparation example Construction

[0018] The invention provides a method for catalytic decomposition of cyclohexyl hydroperoxide, the method comprising: contacting cyclohexyl hydroperoxide with a catalyst, the catalyst containing a silicon-containing molecular sieve, the preparation method of the silicon-containing molecular sieve comprising: (1 ) hydrolyzing the silicon source, the Group VIII metal source and the structure-directing agent to obtain a hydrolyzed material; (2) crystallizing the hydrolyzed material; wherein, step (1) is carried out in the presence of an organophosphorus compound and / or in the step (2) Before proceeding, the crystallization is carried out after mixing the hydrolyzed material and the organophosphorus compound.

[0019] In the present invention, the organophosphorus compound refers to an organic compound containing phosphorus.

[0020] The catalyst of the present invention is used for the catalytic decomposition of cyclohexyl hydroperoxide without adding additional alkaline reagent...

Embodiment approach

[0022] According to a preferred embodiment of the present invention, the preparation method comprises:

[0023] (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;

[0024] (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.

[0025] 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 orga...

Embodiment 1

[0073] (1) tetraethyl orthosilicate, cobalt trifluoride, tripropyl phosphate, tetrapropyl ammonium hydroxide aqueous solution (concentration is 25% by weight) are hydrolyzed to obtain hydrolyzed material; The temperature of hydrolysis is 30 ℃, and the time is 10h;

[0074] (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;

[0075] 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;

[0076] The molar ratio of each material feeding is SiO 2 : Structure directing agent: Group VIII metal: ...

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Abstract

The invention relates to the field of fine chemical engineering, and particularly provides a catalytic decomposition method of cyclohexyl hydroperoxide. The catalytic decomposition method comprises the following step of enabling the cyclohexyl hydroperoxide to be in contact with catalyst, wherein the catalyst contains a silicon-containing molecular sieve. The preparation method of the silicon-containing molecular sieve comprises the following steps: (1) carrying out hydrolysis on a silicon source, the eighth group of metal source and structure-directing agent to obtain hydrolysis materials; (2) carrying out crystallization on the hydrolysis material. The step (1) is carried out in the presence of organic phosphorus compound, and / or before the step (2) is carried out, the hydrolysis material and the organic phosphorus compound are mixed to be subjected to crystallization. The silicon-containing molecular sieve disclosed by the invention is used for the catalytic decomposition of the cyclohexyl hydroperoxide, no additional alkaline reagents need to be added, a high alcohol-ketone ratio and a high alcohol-ketone selectivity reaction effect can be obtained at a lower temperature, and the silicon-containing molecular sieve has very high industrial application value.

Description

technical field [0001] The invention relates to a method for catalytically decomposing cyclohexyl hydroperoxide. 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 process, and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C27/00C07C45/53C07C45/00C07C49/403C07C29/00C07C35/08B01J29/03B01J29/00
CPCB01J29/00B01J29/03C07C29/00C07C45/002C07C45/53C07C49/403C07C35/08
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