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Method for preparing iron phosphide and carbon composite structure by utilizing carbothermic reaction

A carbothermal reaction and iron phosphide technology, which is applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve problems such as high cost, high chemical activity, and high price, and achieve easy operation, The effect of simple process and low cost

Inactive Publication Date: 2014-10-08
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, the use of phosphorus-containing organic compounds P(SiMe 3 ) 3 Synthesized phosphide nanomaterials with TOP, and obtained very ideal results. However, P(SiMe 3 ) and TOP have high chemical activity, the air is unstable, the price is expensive, and it is difficult to put into production
And it is recognized as the simplest and most effective method for synthesizing metal phosphides and catalysts - temperature-programmed reduction of metal phosphates in a hydrogen atmosphere (TPR method) - the synthesis process requires the introduction of hydrogen at high temperatures, which is more dangerous , and the cost is high, which is difficult to achieve in the process of industrial mass production

Method used

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  • Method for preparing iron phosphide and carbon composite structure by utilizing carbothermic reaction
  • Method for preparing iron phosphide and carbon composite structure by utilizing carbothermic reaction
  • Method for preparing iron phosphide and carbon composite structure by utilizing carbothermic reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] FeCl 3 .6H 2 O, NH 4 h 2 PO 4 and C 3 N 6 h 6 The masses are 0.1g, 0.0213g and 4g respectively, FeCl 3 .6H 2 O and NH 4 h 2 PO 4 Dissolve in 1.2mL deionized water, drop into C by dipping method 3 N 6 h 6 , after drying, at N 2 (Flow rate 100sccm) at 3°C / min to 800°C, keep warm for 30min and then cool naturally.

[0025] X-ray diffraction (XRD) showed that the obtained product was pure Fe 2 P crystal phase.

Embodiment 2

[0027] FeCl 3 .6H 2 O, NH 4 h 2 PO 4 and C 3 N 6 h 6 The masses are 0.5g, 0.1065g and 4g respectively, FeCl 3 .6H 2 O and NH 4 h 2 PO 4 Dissolve in 1.2mL, drop into C by dipping method 3 N 6 h 6 , after drying, at N 2 (Flow rate 100sccm) at 3°C / min to 800°C, keep warm for 30min and then cool naturally.

[0028] X-ray diffraction (XRD) showed that the obtained product was pure Fe 2 P crystal phase.

Embodiment 3

[0030] The difference from Example 1 is:

[0031] FeCl 3 .6H 2 O, NH 4 h 2 PO 4 and C 3 N 6 h 6 The masses are 1g, 0.213g and 4g respectively, FeCl 3 .6H 2 O and NH 4 h 2 PO 4 Dissolve in 1.2mL, drop into C by dipping method 3 N 6 h 6 , after drying, at N 2 (Flow rate 100sccm) at 3°C / min to 800°C, keep warm for 30min and then cool naturally.

[0032] X-ray diffraction (XRD) showed that the obtained product was pure Fe 2 P crystal phase.

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Abstract

The invention relates to a method for preparing an iron phosphide and carbon composite structure by utilizing carbothermic reaction, and particularly relates to a simple and easy method for preparing the iron phosphide and carbon composite structure. The method is suitable for preparing a composite structure of iron phosphide, other metal phosphides and carbon in large scale. The method comprises the following steps: soaking melamine by a mixed solution of ferric chloride hexahydrate and ammonium dihydrogen phosphate by adopting a soaking method in which the ferric chloride hexahydrate, the ammonium dihydrogen phosphate and the melamine are used as raw materials, then carrying out high-temperature pyrolysis on melamine under inert gas by adopting a high-temperature pyrolysis method, reducing metal phosphates into metal phosphides, thereby obtaining the iron phosphide and carbon composite structure. According to the method, the uniform refining of the iron phosphide and carbon composite structure can be achieved by changing the ratio of the ferric chloride hexahydrate to the melamine and conditions of the pyrolysis reduction, such as warming velocity, holding temperature, temperature holding time, so that the iron phosphide and carbon composite structure which is uniform in granule and excellent in catalytic performance can be obtained.

Description

technical field [0001] The invention relates to a method for preparing a composite structure of iron phosphide and carbon by using carbon heat reaction, belonging to the field of energy and catalytic materials. Background technique [0002] Metal phosphides are a type of interstitial compounds formed by interstitial insertion of phosphorus atoms into the metal lattice. Metal phosphides have a series of physical and chemical properties such as semiconducting, superconducting, ferromagnetic, magnetocaloric and magnetoresistance effects, excellent catalytic activity and Li ion insertion / release capacity, etc., and are widely used in optoelectronic devices, magnetic memories, etc. Components, magnetic refrigeration systems, industrial catalysis and battery materials and other fields. [0003] Due to the high activity and stability of transition metal phosphides in the reaction of oil HDS and HDN, exploring new methods to synthesize transition metal phosphides has become a hot...

Claims

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Application Information

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IPC IPC(8): B01J27/185
Inventor 黄智鹏吕存财
Owner JIANGSU UNIV
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