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Method for processing cyclohexane oxidation liquid

A technology of cyclohexane oxidation solution and cyclohexyl hydrogen peroxide, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc. Weak, low effective utilization of active centers, etc., to achieve the effect of improving effective utilization, high alcohol-ketone ratio, and improving utilization

Active Publication Date: 2020-03-27
江西科因润滑材料有限公司
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  • 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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  • Method for processing cyclohexane oxidation liquid
  • Method for processing cyclohexane oxidation liquid
  • Method for processing cyclohexane oxidation liquid

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preparation example Construction

[0018] The invention provides a method for processing cyclohexane oxidation liquid, the method comprising: contacting cyclohexane oxidation liquid with a catalyst, the cyclohexane oxidation liquid contains cyclohexyl hydroperoxide, and the catalyst contains silicon-containing molecular sieve , the preparation method of the silicon-containing molecular sieve comprises: (1) hydrolyzing a silicon source, a Group VIII metal source, and a structure-directing agent to obtain a hydrolyzed material; (2) crystallizing the hydrolyzed material; wherein, the first 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), the hydrolyzed material is mixed with an organophosphorus compound and then The crystallization is carried out.

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

[0020...

Embodiment approach

[0022] According to a preferred embodiment of the present invention, the cyclohexane oxidation solution contains 3.0-3.6% by weight of cyclohexyl hydroperoxide, 0.6-1.0% by weight of cyclohexanol, 0.4-0.7% by weight of cyclohexanone, 0.15 - 0.3% by weight of organic acids, 0.2-0.4% by weight of organic esters, 94.00-95.65% by weight of cyclohexane.

[0023] According to the aforementioned technical scheme, the purpose of the present invention can be achieved. For the present invention, the molar ratio of the organic phosphorus compound to the silicon source is preferably P: SiO 2 =(0.001-0.5):1, more preferably P:SiO 2 =(0.1-0.3):1. Thus, the performance of the silicon-containing molecular sieve can be improved, for example, its catalytic decomposition performance used as a catalyst for processing cyclohexane oxidation liquid can be improved, the ratio of alcohol to ketone can be greatly improved, and the selectivity of alcohol to ketone can be high.

[0024] According to a ...

Embodiment 1

[0075] (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;

[0076] (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;

[0077] 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;

[0078] The molar ratio of each material feeding is SiO2: structure directing agent: Group VIII metal: H2O = 1: 0.05...

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Abstract

The invention relates to the field of the fine chemical industry, in particular to a method for processing a cyclohexane oxidation solution. The method comprises the step that the cyclohexane oxidation solution makes contact with a catalyst, wherein the catalyst contains a silicon-containing molecular sieve, and the cyclohexane oxidation solution contains cyclohexyl hydroperoxide. A preparation method of the silicon-containing molecular sieve comprises the steps that 1, a silicon source, a group VIII metal source and a structure guide agent are hydrolyzed to obtain a hydrolyzed material; 2, the hydrolyzed material is crystallized, wherein the group VIII metal source is an iron source or a mixture of the iron source and a cobalt source, and step 1 is conducted in the presence of an organophosphorus compound and / or before step 2, crystallization is conducted after the hydrolyzed material and the organophosphorus compound are mixed. The silicon-containing molecular sieve is used for processing the cyclohexane oxidation solution, extra alkaline reagents do not need to be added, the effects of a high alcohol-ketone ratio and high alcohol-ketone selectivity can be obtained at low temperature, and the method is high in industrial application value.

Description

technical field [0001] The invention relates to a method for processing cyclohexane oxidation liquid. 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 the conver...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/88C07C29/00C07C35/08C07C45/53C07C49/403C01B39/08C01B37/00
CPCB01J29/88B01J2229/16B01J2229/32C01B37/005C01B39/08C01B39/087C07C29/00C07C45/53C07C35/08C07C49/403
Inventor 廖维林王宝荣舒兴田陈飞彪
Owner 江西科因润滑材料有限公司
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