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Hydrochloric acid-promoted efficient system for photocatalytic cyclohexane oxidation of pwv heteropolyacids to ka oil

A technology of cyclohexane and heteropolyacid, which is applied in the field of effective visible light catalytic conversion system, can solve the problems of poor selectivity, weak absorption, and low photocatalytic oxidation efficiency, and achieve the effects of improving absorption efficiency, saving costs, and reducing energy consumption

Inactive Publication Date: 2017-09-19
HUNAN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

As far as we know, there has been no literature report on the use of phosphotungstovanadium heteropolyacids in the photocatalytic selective oxidation reaction excited by visible light. The main reason is that they have weak absorption in the visible light region, low photocatalytic oxidation efficiency and poor selectivity.

Method used

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  • Hydrochloric acid-promoted efficient system for photocatalytic cyclohexane oxidation of pwv heteropolyacids to ka oil
  • Hydrochloric acid-promoted efficient system for photocatalytic cyclohexane oxidation of pwv heteropolyacids to ka oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-16

[0022] Examples 1-16: References [Tsigdinos G A and Hallada C, J. Inorg. Chem. 19687 437] Preparation H 4 PW 11 V 1 o 40 (HPW 11 V 1 ), H 5 PW 10 V 2 o 40 (HPW 10 V 2 ) and H 6 PW 9 V 3 o 40 (HPW 9 V 3 ) as a catalyst. Measure 5.0 mL of analytically pure acetocyanide, 1 mmol of analytically pure cyclohexane, 0.010 mmol of homemade PWV heteropolyacid catalyst, and concentrated hydrochloric acid (the concentration in acetonitrile is 0.04-0.3 Mol.L -1 ), put the solution formed by mixing these raw materials into the light source built-in reactor (see figure 1 ), insert a 35-60W halogen tungsten lamp set in the glass tube into the reaction solution, open the oxygen valve to maintain a pure oxygen atmosphere of 1 atmosphere above the reaction solution, and inject 0-5 o C ethanol cooling medium, turn on the magnetic stirring and light and time it. After 4-25 hours of light, the reaction solution was analyzed by Agilent 6890N gas chromatography, the analysis con...

Embodiment 17-28

[0024] Example 17-28: Introduce dry HCl gas into 5mL of analytically pure acetonitrile (HCl concentration is 0.18 Mol.L -1 ) Measure 0-0.12mL distilled water, 1-3mmol analytically pure cyclohexane and self-made HPW 9 V 3 Catalyst 0.001-0.015mmol. Then carry out the chromatographic analysis of photocatalytic oxidation reaction and reaction product according to the step described in [0022]. The specific results are shown in Table 2.

[0025] Table 2 Effects of other parameters on the oxidation of cyclohexane by molecular oxygen catalyzed by decatungstate under visible light.

[0026]

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Abstract

The invention relates to an effective visible light catalytic conversion system for preparing cyclohexanone (K) and cyclohexanol (A) by molecular selective oxidation of cyclohexane, and relates to a hydrochloric acid solution accelerator. With cyclohexane as reactant, molecular oxygen as oxidant, heteropolyacids H4PW11V1O40 (HPW11V1), H5PW10V2O40 (HPW10V2), and H6PW9V3O40 (HPW9V3) as catalysts, acetonitrile as reaction medium, hydrochloric acid solution as accelerator, 35-60W halogen A tungsten lamp is used as the light source, and a photoreactor with a built-in light source is used (see Figure 1). The reaction temperature is room temperature, and the reaction time is 6-36 hours. Cyclohexane can be effectively converted into the corresponding oxygen-containing product KA oil. The photocatalytic system has the advantages of mild reaction conditions, simple operation, easy catalyst preparation, high photocatalytic conversion efficiency and excellent cyclohexanone selectivity.

Description

technical field [0001] The invention relates to an effective visible light catalytic conversion system for synthesizing corresponding oxygen-containing product KA oil by molecular selective oxidation of cyclohexane, in particular to a hydrochloric acid solution promoter. Background technique [0002] Cyclohexanone and cyclohexanol (KA oil) synthesized by selective oxidation of cyclohexane are important raw materials for the preparation of chemical fibers and fine chemicals. In industry, cyclohexane oxidation uses cobalt or manganese salt as catalyst, at high temperature (170-230 o C) Operate in a high-pressure (10-20atm) pressure-resistant reactor. In order to obtain higher KA oil selectivity (75-80%), the conversion rate of raw materials is usually controlled below 10%. Although some effective catalytic conversion systems for the selective oxidation of cyclohexane under mild conditions have been developed, these systems usually use active oxidants such as hydrogen peroxid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/403C07C35/08C07C45/33C07C29/50B01J31/18
Inventor 伏再辉吴文锋汤森培尹笃林刘亚纯张超邹帅
Owner HUNAN NORMAL UNIVERSITY
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