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A method for preparing iron phosphide and carbon composite structure by carbothermal reaction

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

Inactive Publication Date: 2016-06-29
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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  • A method for preparing iron phosphide and carbon composite structure by carbothermal reaction
  • A method for preparing iron phosphide and carbon composite structure by carbothermal reaction
  • A method for preparing iron phosphide and carbon composite structure by carbothermal 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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PUM

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Abstract

The invention relates to a method for preparing iron phosphide and carbon composite structure by carbon-thermal reaction, specifically a simple preparation method for iron phosphide and carbon composite structure, which is suitable for preparing iron phosphide and other metal phosphides and carbon in large quantities composite structure. The method uses ferric trichloride hexahydrate, ammonium dihydrogen phosphate and melamine as raw materials, impregnates melamine with a mixed solution of ferric trichloride hexahydrate and ammonium dihydrogen phosphate by impregnation method, and then uses high-temperature pyrolysis method under inert gas Pyrolysis of melamine under high temperature reduces metal phosphate to metal phosphide, thus obtaining a composite structure of iron phosphide and carbon. The present invention realizes the uniform refinement of iron phosphide and carbon composite structure by changing the ratio of ferric chloride hexahydrate and melamine and the conditions during pyrolysis and reduction, such as heating rate, holding temperature and holding time, so as to prepare uniform particles, Iron phosphide and carbon composite structure with excellent catalytic performance.

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 t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/185
Inventor 黄智鹏吕存财
Owner JIANGSU UNIV
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