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Co (II) and Zn (II) bimetal doped carbon material as well as preparation method and application thereof

A carbon material and bimetallic technology, which is applied in the field of industrial catalysis and fine organic synthesis, can solve the problems of reducing the selectivity of cycloalkyl alcohols and cycloalkyl ketones, increasing the uncontrollability of the reaction system, and achieving cycloalkyl hydroperoxidation The effect of low substance content, inhibition of disordered diffusion, and less by-products

Pending Publication Date: 2021-11-16
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) At present, the industry is O 2 Oxidation of cycloalkane mainly undergoes disordered free radical diffusion process;
[0005] (2) Oxidation intermediate product, cycloalkyl hydroperoxide converts to target oxidation products cycloalkanol and cycloalkanone through free radical thermal decomposition path, which increases the uncontrollability of the reaction system and reduces the reaction rate of cycloalkyl alcohol and cycloalkyl ketone. selectivity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 58

[0036] Embodiment 58 is a scale-up experiment.

Embodiment 1

[0038] Get 2.2128g (12.50mmol) anhydrous cobalt acetate, 2.2935g (12.50mmol) anhydrous zinc acetate and dissolve in 250mL deionized water, stir on a magnetic stirrer for 15min, add 16.1180g chitosan (glucosamine The amount of the unit substance is 100mmol), and stirred on a magnetic stirrer for 6.0h. After standing for 30 minutes, filter under reduced pressure, wash 3 times with 3×100mL water until the filtrate is clear, dry in the shade at room temperature for 24.0 hours, and then vacuum-dry at 80°C. N 2Carbonization at 700°C for 2.0h under atmosphere. The obtained carbon material was dispersed in 50.0 mL of dilute hydrochloric acid (2.0 mol / L), stirred and washed for 6.0 h, then vacuum filtered, rinsed with 2×50 mL of deionized water until the pH value was 5.0 to 6.0, and vacuum-dried to obtain 12.1842 g Co(II), Zn(II) double metal doped carbon material C 4:0.50:0.50 -700-2.0 (glucosamine unit, Co, Zn material ratio is 8:1:1, 700 is the carbonization temperature, 2.0 is t...

Embodiment 2

[0040] Get 2.9509g (16.67mmol) anhydrous cobalt acetate, 1.5284g (8.33mmol) anhydrous zinc acetate are dissolved in 250mL deionized water, stir 15min on the magnetic stirrer, after the salt dissolves completely, add 16.1180g chitosan (glucosamine The amount of the unit substance is 100mmol), and stirred on a magnetic stirrer for 6.0h. After standing for 30 minutes, filter under reduced pressure, wash 3 times with 3×100mL water until the filtrate is clear, dry in the shade at room temperature for 24.0 hours, and then vacuum-dry at 80°C. N 2 Carbonization at 700°C for 2.0h under atmosphere. Disperse the obtained carbon material in 50.0 mL of dilute hydrochloric acid (2.0 mol / L), stir and wash for 6.0 h, filter under reduced pressure, rinse with 2×50 mL of deionized water until the pH value is 5.0 to 6.0, and dry in vacuum to obtain 13.2413 g Co(II), Zn(II) double metal doped carbon material C 4:0.67:0.33 -700-2.0 (glucosamine unit, Co, Zn material ratio is 4:0.67:0.33, 700 is...

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PUM

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Abstract

A Co (II) and Zn (II) bimetal doped carbon material is prepared according to the following method: dispersing chitosan in a mixed aqueous solution of a Co (II) element donor and a Zn (II) element donor, stirring and loading metal ions at 0-80 DEG C for 1-20 hours, then performing suction filtration, water washing and drying, carbonizing in N2 atmosphere at 100-800 DEG C for 1-10 hours, cooling to room temperature, stirring and washing with a 0.5-10 mol / L hydrochloric acid aqueous solution for 1-10 hours, performing suction filtration and water washing until the pH value is 3-8, and performing vacuum drying to obtain the Co (II) and Zn (II) bimetal doped carbon material, the preparation method is simple, low in cost and easy for industrial application; the method for synthesizing naphthenic alcohol and naphthenic ketone through synergistic catalytic oxidation of the obtained catalytic material has the advantages of being high in naphthenic alcohol and naphthenic ketone selectivity, low in reaction temperature, few in by-products, small in environmental influence and the like, the content of naphthenic hydroperoxide is low, and the safety coefficient is high.

Description

technical field [0001] The invention relates to a Co(II), Zn(II) bimetallic doped carbon material, a preparation method thereof and an application in catalytic oxidation of cycloalkane to synthesize cycloalkanol and cycloalkanone, belonging to the field of industrial catalysis and fine organic synthesis. Background technique [0002] Catalytic oxidation of naphthenes is a very important conversion process in the chemical industry. The oxidation products cycloalkanol and cycloalkanone are not only important organic solvents, but also important fine chemical intermediates, widely used in pesticides, medicines, dyes, surface Synthesis of fine chemical products such as active agents and resins, especially the production of polyamide fibers nylon-6 and nylon-66. [0003] At present, the industrial catalytic oxidation of naphthenes is mainly based on homogeneous Co 2+ or Mn 2+ As a catalyst, oxygen (O 2 ) is an oxidizing agent, which is carried out at 150-170°C. The main proble...

Claims

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Application Information

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IPC IPC(8): B01J23/80C07C29/50C07C45/33C07C35/06C07C35/20C07C35/205C07C35/08C07C49/403C07C49/395C07C49/413C07C27/12
CPCB01J23/80C07C29/50C07C45/33C07C35/06C07C35/20C07C35/205C07C35/08C07C49/395C07C49/413
Inventor 沈海民秦嘉伟佘远斌
Owner ZHEJIANG UNIV OF TECH
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