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Transition metal phosphide hydrogen-evolution composite material as well as preparation method and application thereof

A transition metal and composite material technology, applied in chemical instruments and methods, physical/chemical process catalysts, electrolysis processes, etc., can solve the problems of complex transition metal phosphide methods, large consumption, dangerous operation, etc. The effect of large-scale production, improved application value and low price

Inactive Publication Date: 2019-04-09
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] For the preparation of transition metal phosphides in the prior art is complex, high energy consumption, dangerous operation, consumes a large amount of phosphorus source and releases pH 3 Toxic gas and other defects, the first purpose of the present invention is to provide a method for preparing a transition metal phosphide hydrogen evolution composite material, aiming at preparing phosphorus and transition metal elements complexed on the hydrogel in situ, and further Composite materials with high hydrogen production performance and high stability obtained by calcination

Method used

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  • Transition metal phosphide hydrogen-evolution composite material as well as preparation method and application thereof
  • Transition metal phosphide hydrogen-evolution composite material as well as preparation method and application thereof
  • Transition metal phosphide hydrogen-evolution composite material as well as preparation method and application thereof

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Effect test

Embodiment 1

[0063] Step (1): Synthesis of polyvinylphosphonic acid: Polyvinylphosphonic acid was synthesized according to the method reported by Millaruelo et al. Weigh 5g of vinylphosphonic acid monomer and 0.15g of azobisisobutyronitrile into a 100ml round bottom flask, then add 28ml of ethyl acetate as a solvent into the flask, cover with a rubber stopper, and quickly place the system in liquid nitrogen , the reaction system was evacuated under the condition of liquid nitrogen freezing, the temperature was raised to room temperature and filled with dry nitrogen, and after repeated operations for 3-5, the temperature of the reaction system was raised to 60° C. for 6 hours of reaction. After the reaction, the reaction solvent was spin-dried, and then an appropriate amount of water was added to dissolve the sample, and then dialyzed in water, changing the water every 2 hours, dialyzed for two days, and freeze-dried to obtain polyvinylphosphonic acid (white solid).

[0064] Step (2): Prepa...

Embodiment 2

[0071] Compared with Example 1, the only difference is that in step (2), the transition metal salt is copper nitrate trihydrate, and the dosage is 1.18g (P / Cu element molar ratio is 1:1). The dual network hydrogel diagram is shown in figure 1 . After calcining in the step (3), the copper phosphide / carbon in-situ composite material is obtained. The obtained Co 2 The morphology of P hydrogen evolution composites is not a carbon framework structure. The XRD spectrum pattern of the product that this case obtains is attached figure 2 As shown, by comparing with the standard map, it shows that Cu was successfully prepared 3 p. When the current density is 10mAcm -2 , the material has an overpotential of 512mV and a Tafel slope of 220mV dec -1 .

Embodiment 3

[0073] Compared with Example 1, the only difference is that in step (2), the transition metal salt is nickel chloride hexahydrate, and the dosage is 1.09g (P / Ni element molar ratio is 1:1). The dual network hydrogel diagram is shown in figure 1 . After calcining in the step (3), the nickel phosphide / carbon in-situ composite material is obtained. The obtained Co 2 The morphology of P hydrogen evolution composites is not a carbon framework structure. The XRD spectrum pattern of the product that this case obtains is attached figure 2 As shown, the overpotential of the material is 336mV, and the Tafel slope is 122mV dec -1 .

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Abstract

The invention belongs to the hydrogen-evolution material field and particularly discloses a transition metal phosphide hydrogen-evolution composite material as well as a preparation method and application thereof. The preparation method comprises the following steps: dissolving a phosphorus source into water, and adding a certain amount of an organic amine alkali compound, so as to obtain a solution A, wherein the phosphorus source is at least one of a polymer containing phosphonic acid groups and a monomer containing phosphonic acid groups; adding a transition metal source into the solution A, and stirring to obtain dispersion liquid B; adding agar into the dispersion liquid B, and stirring, so as to obtain double-network hydrogel; cooling the double-network hydrogel, and drying, so as toobtain dried gel; and calcining the dried gel at 750-1000 DEG C in a protective atmosphere, so as to obtain the transition metal phosphide hydrogen-evolution composite material. The preparation method is wide in raw material source and low in cost, obtained transition metal phosphide has excellent electro-catalytic property, and the preparation method is hopefully applied to the industrial production.

Description

technical field [0001] The invention belongs to the field of hydrogen-producing materials, and relates to a double-network hydrogel, in particular to a metal phosphide hydrogen-evolution composite material prepared by using the double-network hydrogel and a preparation method thereof. Background technique [0002] In recent years, transition metal phosphides (TMPs) have attracted intense interest in catalyzing the hydrogen evolution reaction (HER) due to their high activity and low cost. However, there are currently two main strategies for the preparation of TMP, namely, solution-phase reaction and solid-phase reaction. Considering the strong coordination effect, trioctylphosphine (TOP) is a common phosphorus source for most solution-phase reactions. However, observing the demand for high-temperature organic solvents on the reaction system indicates that solution-phase reactions are highly corrosive and flammable. by NaH 2 PO 2 The PH produced by thermal decomposition 3...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/185B01J35/10B01J35/04C25B1/04
CPCC25B1/04B01J27/1853B01J35/33B01J35/56B01J35/61Y02E60/36
Inventor 孙晓毅王丛森李娟
Owner CENT SOUTH UNIV
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