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Preparation method of bimetal organic framework material and application of bimetal organic framework material in decomposition reaction of cyclohexyl hydroperoxide

A technology of cyclohexyl hydroperoxide and skeleton materials, which is applied in the preparation of organic compounds, organic chemistry, organic compound/hydride/coordination complex catalysts, etc., and can solve the problems of long reaction residence time, difficulty in industrial application, and catalyst failure. In order to achieve stable and stable catalytic performance, increase the ratio of alcohol to ketone, and high catalytic performance

Active Publication Date: 2017-08-22
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Chinese inventions CN01118441.8 and CN01118438.8 disclose respectively a chromium-phosphorus-aluminum molecular sieve with an AFI structure and a chromium-silicon molecular sieve with an MFI structure. The chromium-containing molecular sieve has a higher yield for the decomposition of cyclohexyl hydroperoxide, but the The loss is fast so that the catalyst is deactivated quickly, the conversion rate is low, the reaction residence time is long, and industrial application is quite difficult

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Weigh 0.41 g of sodium acetate solid and dissolve it in 100 mL of deionized water, slowly add 3.32 g of terephthalic acid and 8 g of chromium nitrate nonahydrate to the above solution, and stir at room temperature for 30 min to completely dissolve the solid. The obtained solution was transferred to an autogenous autoclave lined with polytetrafluoroethylene, and the autoclave was placed in a blast drying oven heated to 200°C for 12 hours. After the reaction, the reaction kettle was left to stand until it was naturally cooled to room temperature, and the reaction product was obtained for centrifugation. The solid product was washed with N,N-dimethylformamide and ethanol at 70°C for 1 hour, and centrifuged after washing. The obtained solid was vacuum-dried at 150° C. for 12 h to obtain a metal-organic framework material MIL-101 (Cr). Take 1g of MIL-101 (Cr) solid and slowly add it to 25mL of anhydrous ethanol solution dissolved with 0.46g of cobalt acetate, stir and react ...

Embodiment 2

[0036]Take 0.1 g of the catalyst prepared in Example 1, 10 mL (about 8.32 g) of cyclohexane oxidation solution (composed of 8.16% cyclohexyl hydroperoxide, 1.71% cyclohexanone, 2.56% cyclohexanol, 0.76% acid, 1.98% ester %, cyclohexane 84.83%), was added into a 50mL three-necked flask, stirred and reacted at 80°C for 90min, after the reaction was completed, it was left to cool to room temperature, and the reaction solution was taken out for analysis. The analysis results show that the conversion rate of cyclohexyl hydroperoxide is 96.5%, the total selectivity of alcohol and ketone is 99%, and cyclohexanone:cyclohexanol=1:1.51 (molar ratio).

Embodiment 3

[0038] According to the operation process of embodiment 2, the difference from embodiment 2 is that the catalyst is the catalyzer after repeating embodiment 2 three times. The conversion rate of cyclohexyl hydroperoxide is 95.1%, the total selectivity of alcohol and ketone is 95.2%, cyclohexanone:cyclohexanol=1:1.53 (molar ratio).

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Abstract

The invention discloses a preparation method of a bimetal organic framework material and an application of the bimetal organic framework material in decomposition reaction of cyclohexyl hydroperoxide. The method comprises the steps of adopting a metal-organic framework material MIL-101 (Cr) as a carrier, introducing a second metal ion to obtain the bimetal organic framework material, and applying the material to a cyclohexyl hydroperoxide decomposition system as a catalyst under an alkali-free condition. The obtained catalyst is simple in preparation process, the catalyst is stable in property and not easy to go bad, the catalytic performance is high and stable, and the catalytic activity is essentially constant through multiple times of recycling. The catalyst is used for catalyzing the decomposition reaction of the cyclohexyl hydroperoxide; the conversion rate of the cyclohexyl hydroperoxide can reach over 96%, the overall selectivity of alcohol ketone can reach over 100%, and meanwhile, the ratio of cyclohexanol to cyclohexanone in the product is significantly increased.

Description

technical field [0001] The invention relates to the preparation of a bimetallic organic framework material and its application in catalytic decomposition of cyclohexyl hydroperoxide to generate cyclohexanol and cyclohexanone under alkali-free conditions. Background technique [0002] Cyclohexanone is an important organic chemical raw material, an important intermediate for the manufacture of nylon, oxalic acid, and caprolactam, and an important industrial solvent in the pharmaceutical, coating, and plastic recycling industries. It has a wide range of uses and its demand is constantly growing. [0003] At present, the commonly used method for industrial production of cyclohexanone is cyclohexane oxidation, and the most widely used method is the non-catalyzed oxidation method developed by DSM Company in the Netherlands. The process flow is mainly divided into two steps: the first step, cyclohexane is oxidized to generate the intermediate product cyclohexyl hydroperoxide (CHHP)...

Claims

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Application Information

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IPC IPC(8): C08G83/00B01J31/16C07C45/51C07C49/303C07C29/132C07C35/08
CPCB01J31/1691C07C29/132C07C45/517C08G83/008C07C35/08C07C49/303Y02P20/584
Inventor 吴剑夏莉萍袁霞郭露露
Owner XIANGTAN UNIV
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