Self-supporting nickel phosphide catalyst and preparation method and application thereof

A technology of nickel phosphide and catalyst, which is applied in the field of catalysis, can solve the problems of catalyst specific surface area reduction, limitation of industrial application, sintering and agglomeration of copper nanoparticles, and achieve high selectivity of methyl glycolate, significant industrial application value, inhibition The effect of surface agglomeration

Active Publication Date: 2018-02-16
EAST CHINA NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although noble metal catalysts have good catalytic activity and product selectivity, their high price greatly limits their further industrial applications.
Current copper-based catalysts usually use oxide powder supports, and Chinese patent CN201410048657.5 discloses a Cu-Zn/SiO 2 Catalyst, at a reaction temperature of 250°C, a reaction pressure of 2.0MPa, a hydrogen ester molar ratio of 30, and a feed liquid hourly space velocity of 1h -1 Under these conditions, the conversion rate of DMO was 85.8%, and the selectivity of methyl glycolate reached 83.6%. Although the catalyst has a good conversion rate, it still faces many problems in further industrial application: first, copper nanoparticles are prone to formation under high temperature and pressure. sintering and agglomeration; secondly, the carrier SiO 2 It is easy to react with methanol at high temperature to form tetramethoxysilane, which seriously affects the product quality of methyl glycolate, and

Method used

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  • Self-supporting nickel phosphide catalyst and preparation method and application thereof
  • Self-supporting nickel phosphide catalyst and preparation method and application thereof
  • Self-supporting nickel phosphide catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0058] Example 1

[0059] 1) take by weighing 1g nickel foam, ultrasonically treat 30 minutes in 20mL industrial alcohol, use the dilute nitric acid of 1M to process 2 minutes after the distilled water washing, be immersed in the hydrothermal reactor containing nickel nitrate and ammonium chloride aqueous solution after the distilled water washing, Wherein the nickel nitrate concentration is 0.01M, the ammonium chloride concentration is 0.04M, the hydrothermal temperature is 100 °C, and the hydrothermal time is 3 hours, the reaction is completed, washed with distilled water, and dried at 100 °C, that is, in situ on the skeleton matrix A self-supporting nickel phosphide catalyst precursor grown with a nickel hydroxide crystal layer;

[0060] 2) The prepared self-supporting nickel phosphide catalyst precursor was placed in a reaction tube, and after purging with 50 mL / min nitrogen for 30 minutes, it was introduced into the atmosphere of phosphine, and the temperature rise and ph...

Example Embodiment

[0072] Example 2

[0073] 1) with the step 1 of embodiment 1);

[0074] 2) Weigh 1 g of the prepared self-supporting nickel phosphide catalyst precursor, impregnate it in an equal volume with an aqueous ammonium phosphate solution (1.5 g of ammonium phosphate is dissolved in 0.7 g of water), ultrasonically treat it for 10 minutes after the impregnation, and place it at 100° C. Dry in an oven for 6 hours, then place it in a reaction tube for hydrogen reduction treatment at 20-800°C: in a mixed atmosphere of hydrogen and nitrogen (the volume fraction of hydrogen is 10%), the gas flow rate is 50mL / min, and at 20- In the temperature range of 250 °C, the heating rate is 10 °C / min, in the temperature range of 250 to 350 °C, the heating rate is 2 °C / min, and in the temperature range of 350 to 800 °C, the heating rate is 1 °C / min. Self-supporting nickel phosphide catalyst.

[0075] Figure 5 is the X-ray diffraction pattern of the self-supporting nickel phosphide catalyst prepared ...

Example Embodiment

[0079] Example 3

[0080] 1) with the step 1 of embodiment 1);

[0081] 2) Weigh 1 g of the prepared self-supporting nickel phosphide catalyst precursor, impregnate it with an equal volume of ammonium phosphate aqueous solution (1 g of ammonium phosphate is dissolved in 0.7 g of water), ultrasonically treat it for 10 minutes after dipping, and place it in a 100°C oven. , dried for 6 hours, and then placed in a reaction tube to carry out temperature-programmed reduction treatment at 20-650 °C: the reducing gas is hydrogen, the hydrogen flow rate is 10 mL / min, and the temperature rise rate is 10 °C / min in the temperature range of 20-250 °C , in the temperature range of 250-350 °C, the heating rate is 2 °C / min, and in the temperature range of 350-650 °C, the heating rate is 1 °C / min, that is, the self-supporting nickel phosphide catalyst is obtained.

[0082] Image 6 is the X-ray diffraction pattern of the self-supporting nickel phosphide catalyst prepared in this example, whi...

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Abstract

The invention discloses a self-supporting nickel phosphide catalyst and a preparation method and application thereof. The self-supporting nickel phosphide catalyst is a nickel phosphide catalyst obtained by in-situ growing of a nickel oxalate or nickel hydroxide crystal layer on a framework matrix through a hydrothermal method and performing phosphating while secondary forming is not needed, and the nickel phosphide catalyst is composed of the framework matrix and a nickel-phosphorus compound, wherein the nickel-phosphorus compound is at least one of Ni3P, Ni12P5, Ni2P and Ni5P4, total mass ratio of the nickel-phosphorus compound is 0.1-50%, and the balance is the framework matrix. Experiments show that the self-supporting nickel phosphide catalyst is high in stability and thermal conductivity, easy to form and fill, high in flux and low in pressure drop, especially has the advantages of high low-temperature activity, high dimethyl oxalate conversion rate and high methyl glycolate selectivity and can be used as a reaction catalyst for hydrogenating dimethyl oxalate to prepare methyl glycolate.

Description

technical field [0001] The present invention relates to a kind of catalyst and its preparation method and application, specifically, relate to a kind of self-supporting nickel phosphide catalyst and its preparation method and its application in the hydrogenation of dimethyl oxalate to methyl glycolate reaction, It belongs to the field of catalytic technology. Background technique [0002] Methyl glycolate (MG) has a unique molecular structure and has both the chemical properties of alcohol and ester. It is an important chemical product and synthetic intermediate, and is widely used in the fields of medicine, pesticides, dyes, and spices. At present, glycolic acid is mainly produced by chloroacetic acid method and formaldehyde and hydrocyanic acid addition method in China, and then esterified to obtain MG. These two production processes not only have long process flow, high energy consumption and serious pollution, but also have many impurities in the product, which affects ...

Claims

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Application Information

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IPC IPC(8): B01J27/185B01J27/188B01J27/228C07C67/31C07C69/675
CPCB01J27/1853B01J27/188B01J27/228B01J37/10B01J37/28C07C67/31C07C69/675
Inventor 路勇朱坚陈鹏静赵国锋刘晔
Owner EAST CHINA NORMAL UNIVERSITY
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