Preparation method for graphene-based cobalt carbonate catalyst for oxidizing cyclohexene

A graphene-based, cobalt carbonate technology, which is applied in the preparation of organic compounds, catalysts for physical/chemical processes, carbon-based compounds, etc., can solve the problems that limit the wide application in the field of catalysis, high preparation costs, harsh reaction conditions, etc., and achieve High allylic oxidation conversion rate and selectivity, good catalytic activity, environmental protection and efficient catalytic reaction effect

Inactive Publication Date: 2017-08-18
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Graphene-based catalysts have shown excellent catalytic efficiency and catalytic stability in organic catalytic oxidation reactions, but the metal nanoparticles used in the catalyst synthesis methods reported are mainly noble metals, the preparation cost is relatively high, and the reaction conditions are harsh. , the yield is low and there are many by-products, which limit its wide application in the field of catalysis

Method used

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  • Preparation method for graphene-based cobalt carbonate catalyst for oxidizing cyclohexene
  • Preparation method for graphene-based cobalt carbonate catalyst for oxidizing cyclohexene
  • Preparation method for graphene-based cobalt carbonate catalyst for oxidizing cyclohexene

Examples

Experimental program
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Effect test

Embodiment 1

[0025] (1) Measure 46mL concentrated H 2 SO 4 , 2g graphite powder and 1g NaNO 3 In a 500mL three-necked flask, sonicate for 30min, then transfer the mixture to a constant temperature water bath at 5°C and stir for 1h, then continue to add 6.5g KMnO to the three-necked flask 4 powder, continue to stir and react at 5°C for 4h, then raise the temperature to 38°C, stir for 30min, then raise the temperature to 95°C and stir for 30min, then add dilute H 2 SO 4 The solution terminates the reaction, removes the water bath, and obtains the primary product of graphite oxide (GO).

[0026] (2) Add dropwise 30mL H to the mixture in step (1) 2 o 2 To remove excess oxidant in the mixture, then the mixture was vacuum filtered, washed twice with 40mL dilute HCl, and then washed with 30mL HCl 2 o 2 Wash once, filter with suction, then disperse the solid in H 2 o 2 with H 2 In the mixed solution with O volume ratio of 1:5, ultrasonic stripping was performed for 2 h; a uniform and sta...

Embodiment 2

[0030] (1) Measure 46mL concentrated H 2 SO 4 , 2g graphite powder and 1g NaNO 3 In a 500mL three-necked flask, sonicate for 30min, then transfer the mixture to a constant temperature water bath at 5°C and stir for 1h, then continue to add 6.5g KMnO to the three-necked flask 4 powder, continue to stir and react at 5°C for 4h, then raise the temperature to 38°C, stir for 30min, then raise the temperature to 95°C and stir for 30min, then add dilute H 2 SO 4 The solution terminates the reaction, removes the water bath, and obtains the primary product of graphite oxide (GO).

[0031] (2) Add dropwise 30mL H to the mixture in step (1) 2 o 2 To remove excess oxidant in the mixture, then the mixture was vacuum filtered, washed twice with 40mL dilute HCl, and then washed with 30mL HCl 2 o 2 Wash once, filter with suction, then disperse the solid in H 2 o 2 with H 2 In the mixed solution with O volume ratio of 1:5, ultrasonic stripping was performed for 2 h; a uniform and sta...

Embodiment 3

[0035] (1) Measure 46mL concentrated H 2 SO 4 , 2g graphite powder and 1g NaNO 3 In a 500mL three-necked flask, sonicate for 30min, then transfer the mixture to a constant temperature water bath at 5°C and stir for 1h, then continue to add 6.5g KMnO to the three-necked flask 4 powder, continue to stir and react at 5°C for 4h, then raise the temperature to 38°C, stir for 30min, then raise the temperature to 95°C and stir for 30min, then add dilute H 2 SO 4 The solution terminates the reaction, removes the water bath, and obtains the primary product of graphite oxide (GO).

[0036] (2) Add dropwise 30mL H to the mixture in step (1) 2 o 2 To remove excess oxidant in the mixture, then the mixture was vacuum filtered, washed twice with 40mL dilute HCl, and then washed with 30mL HCl 2 o 2 Wash once, filter with suction, then disperse the solid in H 2 o 2 with H 2 In the mixed solution with O volume ratio of 1:5, ultrasonic stripping was performed for 2 h; a uniform and sta...

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Abstract

The invention discloses a preparation method for a graphene-based cobalt carbonate catalyst for oxidizing cyclohexene. The method comprises the following steps: preparing graphite oxide (GO) with functional groups, such as, carboxyl, hydroxy and carbonyl on single-layer or multilayer surfaces by taking graphite powder as a raw material and taking concentrated sulfuric acid (H2SO4), sodium nitrate (NaNO3) and potassium permanganate (KMnO4) as co-oxidants, and then adopting a hydrothermal method and high-temperature calcination for preparing the graphene-based cobalt carbonate (CoCO3@RGO) catalyst by taking cobalt acetate (Co(AC)2.4H2O) under an alkaline condition. According to the method, a simple solvent thermal process is adopted for preparing CoCO3@RGO catalyst, H2O2 is used as an oxidizing agent for catalytically oxidizing cyclohexene into cyclohexenone under a room temperature condition, the conversion rate reaches up to 89.96% and the selectivity reaches up to 90.66%. The CoCO3@RGO catalyst prepared according to the method is low in cost, green and environment-friendly, has excellent catalytic performances and has an important application prospect in organic synthesis and catalytic reaction.

Description

technical field [0001] The invention relates to the field of nano catalyst preparation, in particular to a preparation method of a graphene-based cobalt carbonate catalyst used for cyclohexene oxidation. Background technique [0002] Cyclohexenone is an important intermediate in organic synthesis. It is often used to synthesize some complex polycyclic and heterocyclic compounds, such as cyclohexenone herbicides, substituted phenols and other intermediates. In the past few decades, the selective oxidation of cyclohexene to cyclohexenone has been extensively studied, and many methods and reagents have been developed for the selective oxidation of cyclohexene, but most of the methods require the use of noble metal nanoparticles. Particles, such as White, etc., use palladium to catalyze the allylic reaction of alkenes to non-enantioselectively synthesized aminated products (Fraunhoffer K.J., White M.C.syn-1,2-AminoAlcohols via Diastereoselective Allylic C-H Amination[J].Journal...

Claims

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Application Information

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IPC IPC(8): B01J27/232C07C45/34C07C49/603
CPCB01J27/232C07C45/34C07C49/603
Inventor 唐瑞仁刘友桃
Owner CENT SOUTH UNIV
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