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Method for preparing carbon supported transition metal phosphide material

A transition metal and phosphide technology, applied in the field of carbon-supported phosphide preparation, can solve problems such as no occurrence, and achieve the effect of simplifying the preparation steps and high purity

Active Publication Date: 2009-12-30
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The metal phosphide-modified gel carbon prepared by the one-pot method adopted in the present invention has not appeared in previous reports

Method used

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  • Method for preparing carbon supported transition metal phosphide material
  • Method for preparing carbon supported transition metal phosphide material
  • Method for preparing carbon supported transition metal phosphide material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 3.17g resorcinol (R) into 4.0g deionized water (W) and stir to dissolve, then add 0.35g Ni(NO 3 ) 2 ·6H 2 O, add 0.08g (NH 4 ) 2 HPO 4 , at this time, phosphate precipitates are formed, and concentrated HNO is added dropwise 3 Dissolve the precipitate, adjust the pH to 2-3 at the same time, and add 4.67g of 37wt% formaldehyde (F) solution dropwise under stirring condition. After the formaldehyde is added, the mixed solution will quickly gel into a solid polymer. The resulting polymer was transferred to a vacuum drying oven, and dried at 85° C. for 5 to 7 days to obtain a xerogel. Under the protection of nitrogen (75ml / min), the xerogel was raised to 800°C at a heating rate of 2°C / min, and calcined at this temperature for 3 hours to prepare metal nickel phosphide-modified gel carbon. Using the same method, we also prepared cobalt phosphide and iron phosphide modified gel carbon, and different metals were used in the same molar amount in the preparation process....

Embodiment 2

[0032] Preparation of transition metal phosphide-supported gel carbon materials by a step-by-step method. The method is as follows: first, according to the method in Example 1, under the situation of not introducing phosphide and metal ion salt, in N 2 Under roasting, the gelled carbon is prepared. Get 1.0g of this gelled carbon in a beaker, put 0.148g Ni(NO 3 ) 2 ·6H 2 O or Co(NO 3 ) 2 ·6H 2 O or 0.216g Fe(NO 3 ) 2 9H 2 O was dissolved in 1.5 ml of water, and 0.1 g of concentrated HNO was added dropwise to the water 3 , and then add 0.034g (NH 4 ) 2 HPO 4 After stirring and dissolving, the solution was added dropwise to the gel carbon, dried at 120°C, and dried at 800°C N 2 Under protection, calcined for 3 hours to obtain gel carbon supported by transition phosphide.

Embodiment 3

[0034] XRD diffraction test showed that in N 2 The crystal forms of the transition metal phosphides modified by roasting in the atmosphere are Fe 2 P, Co. 2 P, Ni 12 P 5 . See figure 2 .

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Abstract

The invention relates to a method for preparing a novel carbon supported transition metal phosphide (Fe2P, Co2P, Ni12P5) material, which comprises the steps: 1) adding soluble VIII metal salt into hydroxyphenol solution, and stirring the mixed solution to dissolve the metal salt; 2) adding diammonium phosphate into the solution according to certain proportion to form a precipitate, and dripping proper amount of concentrated nitric acid until the precipitate is exactly dissolved; and 3) dripping formaldehyde solution in the stirring state, making the solution form gel, and obtaining metal phosphide modified gel carbon through drying and high-temperature roasting in inert atmosphere. The invention adopts a method of roasting a polymer containing metal ions, phosphate and phenolic aldehyde to perform one-step preparation of the metal phosphide modified gel carbon under the protection of inert gas of N2.

Description

technical field [0001] The invention relates to a preparation method of carbon-supported phosphide, specifically a new method for preparing phosphide-modified gel carbon material. Background technique [0002] In 1989, Pekala et al. used resorcinol and formaldehyde as carbon sources for the first time, and alkali (NaOH or Na 2 CO 3 ) as catalyst, carbon gel was prepared by organic sol-gel method. Resorcinol and formaldehyde first undergo an addition reaction under the action of a catalyst, and the addition product is further polycondensed under heating to form a macromolecular organic compound, and the macromolecular polymer is decomposed at a high temperature to obtain gel carbon. The gel carbon prepared by this method has unique physical and chemical properties, and can be widely used in adsorption separation, catalyst carrier, super insulation material, supercapacitor electrode material and fuel cell electrode material, so this material has attracted people's attention ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02
Inventor 王辉舒玉瑛郑明远王爱琴王晓东张涛
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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