A hydrophobic modified core-shell catalyst zif-67@sio 2 Method for preparing ka oil by catalytic cyclohexane oxidation

A ZIF-67, core-shell catalyst technology, applied in the direction of oxidation reaction preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve cyclohexane oxidation reaction is difficult to occur, preparation process is complicated, side reactions are difficult to control, etc. problem, to achieve the effect of increased selectivity, expanded application, and improved stability

Active Publication Date: 2022-03-18
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In summary, cyclohexane oxidation reaction is relatively difficult to occur, and usually needs to be carried out under high temperature and high pressure conditions, and the conversion rate of cyclohexane and the selectivity of KA oil are not high
At the same time, the side reactions of the cyclohexane oxidation reaction system are difficult to control, so in order to ensure the high selectivity of cyclohexanol and cyclohexanone in industry, it is usually necessary to control the lower conversion rate of cyclohexane
However, the catalysts currently used in the cyclohexane oxidation reaction have problems such as difficulty in recycling, low resource utilization, complex preparation process, and high cost.

Method used

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  • A hydrophobic modified core-shell catalyst zif-67@sio <sub>2</sub> Method for preparing ka oil by catalytic cyclohexane oxidation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] ZIF-67@SiO 2 Used to catalyze the oxidation reaction of cyclohexane

[0036] (1) Accurately weigh (0.005 mol) Co(NO 3 ) 2· 6H 2 O and (0.04mol) of 2-methylimidazole were dissolved in 80 ml of methanol solution;

[0037] (2) Stir with a glass rod to make it dissolve completely, transfer the two solutions to a round bottom flask (250 ml) after mixing, put in a magnet, and stir at room temperature for 24 h;

[0038] (3) Transfer the solution to a centrifuge tube, centrifuge at 8000 r / min for 3 min, and wash the crystals with methanol until the supernatant is colorless;

[0039] (4) Finally, ZIF-67 was obtained after vacuum drying at 80°C for 24 h;

[0040] (5) Ultrasonic disperse 20 mg of crystals obtained in step (4) in 50 ml of ethanol solution to prepare ZIF-67 ethanol dispersion;

[0041] (6) and use 0.1 mol / L NaOH alkali solution to adjust (5) the pH value of the prepared dispersion to 8~9;

[0042] (7) Add 500mg of cetyltrimethylammonium bromide (CTAB) as a po...

Embodiment 2

[0058] ZIF-67@SiO 2 Used to catalyze cyclohexane oxidation reaction cycle experiment test

[0059] (1) Accurately weigh (0.005 mol) Co(NO 3 ) 2· 6H 2 O and (0.04mol) of 2-methylimidazole were dissolved in 80 ml of methanol solution;

[0060] (2) Stir with a glass rod to make it dissolve completely, transfer the two solutions to a round bottom flask (250 ml) after mixing, put in a magnet, and stir at room temperature for 24 h;

[0061] (3) Transfer the solution to a centrifuge tube, centrifuge at 8000 r / min for 3 min, and wash the crystals with methanol until the supernatant is colorless;

[0062] (4) Finally, ZIF-67 was obtained after vacuum drying at 80°C for 24 h;

[0063] (5) Ultrasonic disperse 20 mg of crystals obtained in step (4) in 50 ml of ethanol solution to prepare ZIF-67 ethanol dispersion;

[0064] (6) and use 0.1 mol / L NaOH alkali solution to adjust (5) the pH value of the prepared dispersion to 8~9;

[0065] (7) Use cetyltrimethylammonium bromide (CTAB) a...

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Abstract

Hydrophobic modified core-shell catalyst ZIF‑67@SiO of the present invention 2 A method for preparing KA oil by catalytic cyclohexane oxidation. The present invention adopts the method of dehydration condensation to coat a layer of SiO on the surface of ZIF-67 material. 2 shell, to obtain a hydrophobically modified core-shell catalyst ZIF‑67@SiO 2 , by grafting hydrophobic groups on the surface to control the hydrophilic-hydrophobic properties of the catalyst surface, thereby regulating the adsorption and desorption behavior of cyclohexane, cyclohexanol and cyclohexanone, and avoiding the deep oxidation of alcohols and ketones. The modified catalyst surface has Good hydrophobic effect, the catalytic reaction shows that the conversion rate of cyclohexane and the selectivity of the target product are simultaneously improved, and the stability of the catalyst is also significantly improved.

Description

technical field [0001] The invention relates to the field of material preparation, in particular to a hydrophobically modified core-shell catalyst ZIF-67@SiO 2 A method for preparing KA oil by catalytic cyclohexane oxidation. Background technique [0002] The oxidation of hydrocarbons mainly includes the oxidation of open-chain hydrocarbons, alicyclic hydrocarbons, and aromatic hydrocarbons. Among them, the oxidation of alicyclic hydrocarbons and cyclohexane in the petrochemical industry is a typical representative of this type of important reaction process. The target products of cyclohexane oxidation are cyclohexanol and Cyclohexanone (commonly known as KA oil) is an intermediate in the synthesis of caprolactam and adipic acid, and is mainly used in the synthesis of nylon 6, nylon 66 and other resins. At present, the industrial oxidation of cyclohexane to KA oil usually adopts cobalt salt catalyst, the conversion rate of cyclohexane is controlled at 7-8%, and the selectiv...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22B01J31/18C07C27/12C07C35/08C07C29/50C07C49/403C07C45/33
CPCC07C27/12C07C29/50C07C45/33B01J31/1691B01J31/1815B01J2531/845C07C35/08C07C49/403
Inventor 刘平乐聂云飞郝芳熊伟吴生焘罗和安
Owner XIANGTAN UNIV
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