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Co/Co3O4 composite and preparation method and application of Co/Co3O4 composite

A composite material and reaction technology, applied in the preparation of organic compounds, catalyst activation/preparation, preparation of aminohydroxy compounds, etc., can solve the problems of low conversion rate and selectivity, difficult to generate, etc., and achieve a simple and repeatable synthesis method. The effect of using the ability

Active Publication Date: 2018-07-13
芜湖数字信息产业园有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, in the prior art, it is not only difficult to produce p-aminophenol by traditional methods, but also the conversion rate and selectivity are very low.

Method used

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  • Co/Co3O4 composite and preparation method and application of Co/Co3O4 composite
  • Co/Co3O4 composite and preparation method and application of Co/Co3O4 composite
  • Co/Co3O4 composite and preparation method and application of Co/Co3O4 composite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Example 1Co / Co 3 o 4 composite material

[0017] (1) Preparation method

[0018] 1)Co 6 (btb) 4 (4,4′-bipy) 3 Crystal preparation: 0.03g Co(NO 3 ) 2 and 0.01g H 3 Put btb in a 5ml glass bottle, add 2ml of N,N-dimethylformamide at the same time, ultrasonically treat for 20min, then put the 5ml glass bottle in an oven, and react for 72h at 85°C, after the reaction, remove the solution The liquid in the solution was washed with N,N-dimethylformamide, filtered, and the solid particles were placed in a vacuum drying oven at 80°C for vacuum drying.

[0019] 2)Co 6 (btb) 4 (4,4′-bipy) 3 Crystal activation: the Co 6 (btb) 4 (4,4′-bipy) 3 The crystals were placed in a vacuum drying oven at 120°C for 36 hours in vacuum to obtain the activated Co 6 (btb) 4 (4,4′-bipy) 3 Crystals, stored under nitrogen.

[0020] 3) will Co 6 (btb) 4 (4,4′-bipy) 3 Calcined in a tube furnace at 800 °C for 1 hour under nitrogen atmosphere to obtain Co / Co 3 o 4 composite material...

Embodiment 2

[0024] Example 2Co / Co 3 o 4 Composite Catalyzed Reduction of p-Nitrophenol

[0025] The method is as follows: 20ml of p-nitrophenol with a concentration of 50mg / L and 0.19g of sodium borohydride are dissolved in 30ml of water to obtain a mixed solution; 10mg of Co / Co prepared in Example 1 is added to the mixed solution 3 o 4 The composite material was placed in a 100mL Erlenmeyer flask, and the reaction device was fixed. React at room temperature, after reacting for 14min, get the reaction solution respectively and carry out the ultraviolet-visible light spectrophotometer to monitor, the result is as follows Figure 5 shown.

[0026] Figure 5 Co / Co synthesized for the present invention 3 o 4 The conversion rate diagram of the composite material after 0min and 14min of reaction. Depend on Figure 5 It can be seen that an absorption peak appears at a wavelength of 350nm at 0 min by ultraviolet analysis chromatography, and no product is generated at this time. When carr...

Embodiment 3

[0028] Example 3Co / Co 3 o 4 Composite material repeatability test

[0029]After the reaction of Example 2 is completed, the Co / Co 3 o 4 Composite material, repeat the experiment of embodiment 2 4 times. Image 6 It is the Co / Co synthesized in Example 1 3 o 4 The conversion rate diagram of the product after 0min and 14min in the fifth reduction reaction of p-nitrophenol catalyzed by the composite material. By repeating the experiment, the Co / Co of the fifth reaction 3 o 4 The conversion rate of the composite material is 95%, the selectivity of p-nitrophenol is 100%, and still has good catalytic activity and selectivity. Prove that the Co / Co synthesized by the present invention 3 o 4 Composite materials are highly recyclable.

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Abstract

The invention relates to a Co / Co3O4 composite and a preparation method and application of the Co / Co3O4 composite. The adopted technical scheme is as follows: ultrasonically dispersing cobalt nitrate and H3btb, putting the solution into a glass bottle, leaving to stand for 72 hours at the temperature of 85 DEG C, obtaining a Co6(btb)4(4,4'-bipy)3 composite, and calcining the material for 1 hour atthe temperature of 800 DEG C under the nitrogen environment to obtain the Co / Co3O4 composite. The synthesized Co / Co3O4 composite has an efficient catalytic activity for the reduction reaction of p-nitrophenol.

Description

technical field [0001] The invention belongs to the field of precious metal catalyzed organic compound synthesis, and the novel metal organic framework material Co 6 (btb) 4 (4,4′-bipy) 3 As a raw material, it is calcined to form a new Co / Co 3 o 4 Composite materials catalyze p-aminophenol which is difficult to generate by traditional methods and has low conversion rate and selectivity. Background technique [0002] p-aminophenol is an important organic synthesis intermediate and chemical raw material. p-aminophenol is an organic compound with multifunctional groups. The hydroxyl group in its molecule is weakly acidic, the amino group is weakly basic, and the benzene ring can be sulfonated and nitrated. , halogenation, alkylation and other reactions, thus generating a variety of derivatives, is the main raw material for the synthesis of a variety of organic products. [0003] In recent years, precious metal nanomaterials have been a hot spot in the field of catalysis. T...

Claims

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Application Information

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IPC IPC(8): B01J23/75B01J35/10B01J37/08C07C213/02C07C215/76
CPCC07C213/02B01J23/75B01J37/086B01J35/60C07C215/76
Inventor 韩正波张洪威刘琳
Owner 芜湖数字信息产业园有限公司
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