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Nano needle-like nickel-coated graphite compound particle and preparation method and application thereof

A technology of nickel-coated graphite and composite particles is applied in the field of synthesizing nano-acicular nickel-coated graphite composite particles for p-aminophenol and its preparation, which can solve the problems of difficult recovery, small particle size and the like, achieves low cost, prevents agglomeration, and is convenient for The effect of promoting the application

Active Publication Date: 2014-08-13
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the particle size of this catalyst is small, and there are problems such as not easy to recycle.

Method used

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  • Nano needle-like nickel-coated graphite compound particle and preparation method and application thereof
  • Nano needle-like nickel-coated graphite compound particle and preparation method and application thereof
  • Nano needle-like nickel-coated graphite compound particle and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Using 200 mL of absolute ethanol as a solvent, 10 g of flake graphite particles were added to a 250 mL Soxhlet extractor and refluxed for 8 hours, filtered and dried in vacuum until use. Put the cleaned and dried graphite particles into the nickel sulfate solution to absorb for 12h, filter and dry for later use; then take the above graphite particles and put them in the ethanol solution of sodium borohydride and let stand, after the graphite particles and the ethanol solution are separated, filter and dry for later use . Separately prepare a solution, take 2.63g nickel sulfate hexahydrate, 25.4g potassium sodium tartrate tetrahydrate, 0.27g sodium hydroxide, 5.2mL 85% hydrazine hydrate solution to make 100mL solution; put 100mL solution into a three-necked flask and heat to 90 At ℃, add 0.5g of pre-treated graphite and react for 0.5h. Filter by suction, wash with deionized water twice, dry completely in a vacuum drying oven, and get image 3 The nano-shaped needle nicke...

Embodiment 2

[0039] Using 200 mL of absolute ethanol as a solvent, 10 g of flake graphite particles were added to a 250 mL Soxhlet extractor and refluxed for 8 hours, filtered and dried in vacuum until use. Put the cleaned and dried graphite particles into the nickel sulfate solution to absorb for 12h, filter and dry for later use; then take the above graphite particles and put them in the ethanol solution of sodium borohydride and let stand, after the graphite particles and the ethanol solution are separated, filter and dry for later use . Prepare another solution, take 5.25g nickel sulfate hexahydrate, 28.2g sodium potassium tartrate tetrahydrate, 0.4g sodium hydroxide, 22mL 85% hydrazine hydrate solution to make 200mL solution; put 200mL solution into a three-necked flask and heat to 80℃ , Add 0.5g of pre-treated graphite and react for 0.5h. Filter by suction, wash with deionized water twice, dry completely in a vacuum drying oven, and get image 3 The nano-shaped needle nickel-coated g...

Embodiment 3

[0042] Using 200 mL of absolute ethanol as a solvent, 10 g of flake graphite particles were added to a 250 mL Soxhlet extractor and refluxed for 8 hours, filtered and dried in vacuum until use. Put the cleaned and dried graphite particles into the nickel sulfate solution to absorb for 12h, filter and dry for later use; then take the above graphite particles and put them in the ethanol solution of sodium borohydride and let stand, after the graphite particles and the ethanol solution are separated, filter and dry for later use . Prepare a solution separately, take 7.88g nickel sulfate hexahydrate, 98.5g potassium sodium tartrate tetrahydrate, 1.8g sodium hydroxide, 21mL 85% hydrazine hydrate solution to make 300mL solution; put 300mL solution into a three-necked flask and heat to 70℃ , Add 0.5g of pre-treated graphite and react for 0.5h. Filter by suction, wash with deionized water twice, dry completely in a vacuum drying oven, and get Figure 4 The nano-shaped needle nickel-co...

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Abstract

The invention relates to a nano needle-like nickel-coated graphite compound particle and a preparation method and application thereof. The nano needle-like nickel-coated graphite compound particle is a nano needle-like nickel-coated flake graphite particle. The preparation method comprises the steps: processing the flake graphite particle, putting in a chemical nickel-plating solution, stirring while reacting, performing suction filtration, washing and drying to obtain the nano needle-like nickel-coated graphite compound particle. Compared with the prior art, the nano needle-like nickel-coated graphite compound particle has the main advantages that the activity of a catalyst prepared by adopting the preparation method is relatively high, for example, the reaction rate constant (k) for catalyzing reduction paranitrophenol by NaBH4 is 8.61*10<-2>min<-1>, and is greater than the k value (the rate constant is 14.82*10<-3>min<-1>) of a graphene oxide / nickel nano composite prepared by Ji and others and used for catalyzing the reaction. The nano needle-like nickel-coated graphite compound particle prepared by adopting the preparation method is magnetic, and is conveniently recycled. The preparation method disclosed by the invention is simple, low in cost and convenient to popularize and apply.

Description

Technical field [0001] The invention relates to the technical field of composite materials and catalysis, in particular to a nano-needle nickel-coated graphite composite particle for synthesizing p-aminophenol, and a preparation method and application thereof. Background technique [0002] Para-aminophenol (PAP) is an important pharmaceutical, dye and organic synthesis intermediate. It can also be used to manufacture various dyes, dyes, rubber antioxidants, photographic developers, pesticide antioxidants, and oil additives. At present, the synthesis methods of p-aminophenol mainly include p-nitrophenol iron powder reduction method, nitrobenzene method and p-nitrophenol catalytic hydrogenation method. Among them, the p-nitrophenol catalytic hydrogenation reduction method has the advantages of simple operation, high product yield and good quality, so it is widely used. In the process of the synthesis of p-aminophenol by the catalytic hydrogenation reduction of p-nitrophenol, the r...

Claims

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Application Information

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IPC IPC(8): B01J23/755B01J32/00B82Y30/00B82Y40/00C07C215/76C07C213/00
Inventor 官建国兰芳王一龙赵素玲刘丽君凌轩
Owner WUHAN UNIV OF TECH
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