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Method for preparing loaded zeolite-like imidazole framework material and application of loaded zeolite-like imidazole framework material in cyclohexane oxidation reaction

A zeolite imidazole framework, supported technology, which is used in the preparation of oxidation reaction, the preparation of oxygen-containing compounds by hydrocarbon oxidation, and catalytic reaction, etc. The problem of high preparation cost, to achieve good industrial application prospects, high cyclohexane conversion rate and product selectivity, and the effect of improving the agglomeration phenomenon

Inactive Publication Date: 2017-04-26
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, the catalysts used in the cyclohexane oxidation reaction system generally have defects such as high preparation cost of metal catalysts, poor economy or low activity of non-metallic catalytic reactions, high energy consumption, etc., and the conversion rate of cyclohexane and the selectivity of the target product are both There are also often obvious contradictions that make further improvement very difficult. The present invention attempts to apply the zeolite-like imidazole framework material ZIFs to the oxidation reaction of cyclohexane in order to improve the conversion rate and selectivity

Method used

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  • Method for preparing loaded zeolite-like imidazole framework material and application of loaded zeolite-like imidazole framework material in cyclohexane oxidation reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Co-ZIF-67 / HZSM-5 is used to catalyze the oxidation of cyclohexane (loading capacity 15mg / g)

[0038] (1) The Co(NO 3 ) 2 ·6H 2 O and 2-methylimidazole were dissolved in an appropriate amount of N,N-dimethylformamide (DMF) at a molar ratio of 1:3, and crystallized at 140 °C for 24 hours in a crystallization kettle;

[0039] (2) Take out the product in the crystallization kettle, centrifuge it, wash it three times with an appropriate amount of methanol, and then continue to centrifuge;

[0040] (3) The precipitate obtained after several times of washing and centrifugation was dried at 80°C to obtain the catalyst Co-ZIF-67.

[0041] (4) Dissolve 2g molecular sieve HZSM-5 in an appropriate amount of anhydrous ethanol and stir rapidly for 1 hour;

[0042] (5) Disperse 30 mg of Co-ZIF-67 in an appropriate amount of anhydrous ethanol, add it to the solution in step (4), and mix the two in a water bath at 60°C for 6 hours;

[0043] (6) The mixture after the water bath in s...

Embodiment 2

[0053] Co-ZIF-67 / Kaolin was used to catalyze the oxidation of cyclohexane (loading capacity 15mg / g)

[0054] (1) The Co(NO 3 ) 2 ·6H 2 O and 2-methylimidazole were dissolved in an appropriate amount of N,N-dimethylformamide (DMF) at a molar ratio of 1:3, and crystallized at 140 °C for 24 hours in a crystallization kettle;

[0055] (2) Take out the product in the crystallization kettle, centrifuge it, wash it three times with an appropriate amount of methanol, and then continue to centrifuge;

[0056](3) The precipitate obtained after repeated washing and centrifugation was dried at 80°C to obtain the catalyst Co-ZIF-67.

[0057] (4) Dissolve 2g of kaolin clay in an appropriate amount of absolute ethanol, and stir rapidly for 1 hour;

[0058] (5) Disperse 30 mg of Co-ZIF-67 in an appropriate amount of absolute ethanol, add it to the solution in step (4), and mix the two in a water bath at 60°C for 6 hours;

[0059] (6) The mixture after the water bath in step (5) was coole...

Embodiment 3

[0068] Co-ZIF-67 / ZrO 2 Used to catalyze the oxidation reaction of cyclohexane (loading capacity 15mg / g)

[0069] (1) Co(NO 3 ) 2 ·6H 2 O and 2-methylimidazole were dissolved in an appropriate amount of N,N-dimethylformamide (DMF) at a molar ratio of 1:3, and crystallized in a crystallization kettle at 140°C for 24 hours;

[0070] (2) Take out the product in the crystallization kettle, centrifuge and wash with an appropriate amount of methanol for 3 times, and then continue to centrifuge;

[0071] (3) The precipitate obtained after repeated washing and centrifugation was dried at 80°C to obtain the catalyst Co-ZIF-67.

[0072] (4) 2gZrO 2 Dissolve in an appropriate amount of absolute ethanol, and stir rapidly for 1 hour;

[0073] (5) Disperse 30 mg of Co-ZIF-67 in an appropriate amount of absolute ethanol, add it to the solution in step (4), and mix the two in a water bath at 60°C for 6 hours;

[0074] (6) Cool and filter the mixture after the water bath in step (5), and...

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Abstract

The invention discloses a method for preparing a loaded zeolite-like imidazole framework material and application of the loaded zeolite-lie imidazole framework material in cyclohexane oxidation reaction. The method comprises the following steps: firstly, preparing a zeolite-like imidazole framework material by adopting a solvothermal method; then, loading the zeolite-like imidazole framework material; and applying the zeolite-like imidazole framework material to the cyclohexane oxidation reaction. By adopting the loaded zeolite-like imidazole framework material, the raw materials are low in prices, and the catalyst has a short preparation cycle and simple process, so that the cost is remarkably reduced; the loaded zeolite-like imidazole framework material is used in the cyclohexane oxidation reaction, a relatively cyclohexane conversion rate and product selectivity can be represented, and the catalyst has excellent reproducibility and can be easily recycled, so that the loaded zeolite-like imidazole framework material has excellent industrial application prospect.

Description

technical field [0001] The invention belongs to the field of material preparation, and particularly relates to a preparation method of a supported zeolite-like imidazole framework material and its application in cyclohexane oxidation reaction. Background technique [0002] At present, the industrial oxidation of cyclohexane is based on soluble cobalt salts as catalysts. Under suitable temperature and pressure, the conversion rate of cyclohexane is controlled at 4%, and the total selectivity of cyclohexanol and cyclohexanone is about 80%. Such industrial oxidation processes have problems such as high energy consumption, low efficiency, and metal ion pollution. [0003] In recent years, the research on new zeolite-like imidazole framework materials ZIFs has developed rapidly. It combines the characteristics of MOFs materials and zeolite-like materials, with excellent stability and adjustable structure and function. It is used in gas adsorption separation, ion exchange and func...

Claims

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Application Information

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IPC IPC(8): B01J31/26B01J31/38B01J31/22C07C29/50C07C35/08C07C45/33C07C49/403C07C27/12
CPCB01J31/1815B01J31/26B01J31/38B01J2231/70B01J2531/845C07C29/50C07C45/33C07C35/08C07C49/403
Inventor 郝芳李翔刘平乐熊伟吕崔华熊绍锋
Owner XIANGTAN UNIV
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