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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
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  • 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 also causes the specific surface area of ​​the catalyst to decrease, resulting in a decrease in catalyst activity.
However, this patent uses 10-20% hydrogen peroxide solution to oxidize and etch the nickel metal substrate to grow nickel hydroxide on the nickel metal substrate. The hydrogen peroxide solution is used as a synthetic reagent, which is expensive, easy to decompose, and difficult to store, making the growth cost Higher; especially in the presence of metals and metal ions, 10-20% hydrogen peroxide solution will quickly decompose and release O under heating conditions above 100°C 2 , in a closed system, there is a very high risk of explosion, which makes the preparation process a high safety risk, and it is not suitable for large-scale preparation; in addition, this preparation process is limited to metal nickel substrates and is not suitable for other substrate materials. 2 The self-supporting preparation of P, the application range is also limited

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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

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Experimental program
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Effect test

Embodiment 1

[0059] 1) Weigh 1g of nickel foam, ultrasonically treat it in 20mL of industrial alcohol for 30 minutes, wash it with distilled water and treat it with 1M dilute nitric acid for 2 minutes, wash it with distilled water and immerse it in a hydrothermal reaction kettle containing nickel nitrate and ammonium chloride aqueous solution, The concentration of nickel nitrate is 0.01M, the concentration of ammonium chloride is 0.04M, the hydrothermal temperature is 100°C, and the hydrothermal time is 3 hours. After the reaction is completed, it is washed with distilled water and dried at 100°C. a self-supporting nickel phosphide catalyst precursor grown with a nickel hydroxide crystalline layer;

[0060] 2) Place the prepared self-supporting nickel phosphide catalyst precursor in the reaction tube, after purging with 50mL / min nitrogen for 30 minutes, pass it into the atmosphere of phosphine, and start the temperature-raising phosphating treatment: treat at 300°C 0.5 hour, and finally pu...

Embodiment 2

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

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

[0075] Figure 5 It is the X-ray diffraction spectrum figure of the self-supporting nickel phosphide catalyst prepared by the present embodiment, by Figure 5 It can be seen that the se...

Embodiment 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 ammonium phosphate aqueous solution (1 g of ammonium phosphate dissolved in 0.7 g of water), perform an equal volume impregnation on it, and ultrasonically treat it for 10 minutes after impregnation, and place it in an oven at 100 ° C , dried for 6 hours, and then placed in a reaction tube for temperature-programmed reduction treatment at 20-650°C: the reducing gas is hydrogen, and the hydrogen flow rate is 10mL / min; in the temperature range of 20-250°C, the heating rate is 10°C / min , 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, to obtain the self-supporting nickel phosphide catalyst.

[0082] Figure 6 It is the X-ray diffraction spectrum figure of the self-supporting nickel phosphide catalyst prepared by the present embodimen...

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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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