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Method for preparing V-ZSM-5 molecular sieve and catalytic property of molecular sieve on preparation of cyclohexanol and cyclohexanone by oxidizing cyclohexane

A technology of V-ZSM-5 and ZSM-5, which is applied in the field of preparation of V-ZSM-5 molecular sieve and its catalytic performance for the oxidation of cyclohexane to prepare cyclohexanol and cyclohexanone, which can solve the problem of using ZSM-5 catalyst Restrictions, high cost of using precious metals, etc.

Inactive Publication Date: 2011-10-12
BEIJING UNIV OF CHEM TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Zhao Rui et al. (Molecular Catalysis, 2005, 19: 115-120) reported that the noble metal-supported ZSM-5 catalyst in a solvent-free system has higher activity and higher selectivity, and the conversion rate is 16%. The total selectivity of ketones is 92%; Ren Yongfeng et al. (Petroleum Refining and Chemical Industry, 2008, 39: 12-15) reported that the Au-Co / HZSM-5 catalyst prepared by impregnation method in a solvent-free system uses air as an oxidant The conversion rate of cyclohexane in the cyclohexane selective oxidation reaction process is 12.4%, and the total selectivity of cyclohexanol and cyclohexanone reaches 95.3%; patent [CN 1781889] adopts Pd or Pt noble metal supported ZSM-5 microporous molecular In the solvent-free oxidation reaction system, the highest conversion rate of cyclohexane is 14%, and the selectivity is lower than 95%. However, the use of noble metals in the above system is expensive, which leads to the use of ZSM-5 catalysts supported by noble metals. big limit

Method used

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  • Method for preparing V-ZSM-5 molecular sieve and catalytic property of molecular sieve on preparation of cyclohexanol and cyclohexanone by oxidizing cyclohexane
  • Method for preparing V-ZSM-5 molecular sieve and catalytic property of molecular sieve on preparation of cyclohexanol and cyclohexanone by oxidizing cyclohexane
  • Method for preparing V-ZSM-5 molecular sieve and catalytic property of molecular sieve on preparation of cyclohexanol and cyclohexanone by oxidizing cyclohexane

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Experimental program
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Effect test

Embodiment 1

[0013] After mixing the NaOH aqueous solution and white carbon black for 2h, the tetrabutylammonium bromide and NH 4 VO 3 The mixed solution is added to the above solution to form an emulsion, the pH is adjusted to 9 and stirred at room temperature for 16 hours, the molar composition of each component in the raw material is: SiO 2 : V 2 O 3 : Na 2 O: [(C 4 H 9 ) 4 N]Br:H 2 O=1:0.03:0.4:0.1:135. After stirring, the solution was transferred to an autoclave for crystallization at 180°C for 96 hours, and dried and roasted to synthesize V-ZSM-5. The catalytic oxidation reaction of cyclohexane is carried out in a 250ml autoclave equipped with a magnetic stirrer and a temperature controller. The reaction conditions are as follows: 40ml of cyclohexane and 0.15g of V-ZSM-5 catalyst are added to the reactor to react During the process, the oxygen pressure was maintained at 1.5MPa by continuous oxygenation, and the reaction temperature was 130°C. After 3 hours of reaction, the kettle was co...

Embodiment 2

[0015] After mixing the NaOH aqueous solution and white carbon black for 2h, the tetrabutylammonium bromide and NH 4 VO 3 The mixed solution is added to the above solution to form an emulsion. Adjust the pH to 10 and stir at room temperature for 16 hours. The molar composition of each component of the raw material is: SiO 2 : V 2 O 3 : Na 2 O: [(C 4 H 9 ) 4 N]Br:H 2 O=1:0.02:0.4:0.3:135, after the stirring, transfer to an autoclave for crystallization at 160C for 48h, dry and roast to synthesize V-ZSM-5. 40ml cyclohexane and 0.2g V-ZSM-5 catalyst It was added to the reaction kettle. During the reaction, the oxygen pressure was maintained at 2MPa by continuous oxygenation, the reaction temperature was 110°C, and the conversion rate of cyclohexane obtained after 4 hours of reaction was 12.19%, respectively. The selectivity of cyclohexanol and cyclohexanone was the highest. The sum is 86.2%.

Embodiment 3

[0017] After mixing the NaOH aqueous solution and white carbon black for 2h, the tetrabutylammonium bromide and NH 4 VO 3 The mixed solution is added to the above solution to form an emulsion. Adjust the pH to 11 and stir at room temperature for 16 hours. The molar composition of each component is: SiO 2 : V 2 O 3 : Na 2 O: [(C 4 H 9 ) 4 N]Br:H 2 O=1:0.01:0.4:0.2:135. After the stirring, the solution was transferred to an autoclave for crystallization at 150°C for 24 hours, and dried and roasted to synthesize V-ZSM-5. Add 40ml cyclohexane and 0.1g V-ZSM-5 catalyst to the reaction kettle, make the reaction pressure 1MPa, temperature 100℃, and react for 5 hours to obtain cyclohexane conversion rate 11.54%, cyclohexanol and cyclohexane The total selectivity of ketones is 91.8%.

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Abstract

The invention relates to a method for preparing cyclohexanol and cyclohexanone by oxidizing cyclohexane, in particular to a method for preparing a vanadium-doped ZSM-5 molecular sieve and a catalytic property of the molecular sieve on preparation of cyclohexanol and cyclohexanone by oxidizing cyclohexane. A molar ratio of vanadium to silicon in the microporous molecular sieve is 0.02-0.03, oxygen and the like are taken as an oxidant, reaction is performed at the temperature of between 80 and 150DEG C under the pressure of between 0.5 and 2.5MPa for 1 to 10 hours, the conversion rate of the cyclohexane is 14.68 percent, and the sum of the selectivity on the cyclohexanol and the cyclohexanone is 97.3 percent. The method has the characteristic that transition metal V atoms in the V-ZSM-5 molecular sieve prepared by a direct hydrothermal synthesis method can enter the skeleton of the molecular sieve so as to greatly improve the activity and selectivity of oxidation reaction.

Description

Technical field [0001] The invention relates to a direct hydrothermal synthesis method of V-ZSM-5 molecular sieve and its catalysis in the preparation of cyclohexanol from cyclohexane and the oxidation reaction of cyclohexanone. Background technique [0002] The selective oxidation of cyclohexane is of great significance in chemical production. The products cyclohexanol and cyclohexanone are intermediates of nylon-6 and nylon-66. Under the action of a catalyst, cyclohexane reacts with air to produce the main products cyclohexanol and cyclohexanone. Since cyclohexanol and cyclohexanone are more easily oxidized than cyclohexane, many by-products are formed. In order to reduce the formation of by-products and increase the selectivity and yield of products, the conversion rate of cyclohexane must be controlled. At present, the industry mainly uses cobalt salt as a catalyst or no catalyst, the conversion rate of cyclohexane is less than 5%, and the total selectivity of cyclohexanone ...

Claims

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Application Information

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IPC IPC(8): B01J29/48C07C27/12C07C27/16C07C35/08C07C29/48C07C29/50C07C49/403C07C45/33C07C45/28
Inventor 李保山叶燕慧
Owner BEIJING UNIV OF CHEM TECH
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