A kind of linear tin phosphide compound and its preparation method

A technology of tin phosphide and compound, applied in the field of preparation of linear tin phosphide compound, can solve the problems of short reaction time, low phosphide yield, low yield, complicated process, etc., so as to shorten the production time and improve the The effect of reducing productivity and activation ability

Inactive Publication Date: 2019-06-11
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to provide a method for preparing a linear tin phosphide compound in view of the complex process and low yield in the synthesis process of tin phosphide, which is simple and easy to control and does not require high-pressure reactors Instruments, and the reaction time is short, the output rate of phosphide is high, and there is no by-product pollution

Method used

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  • A kind of linear tin phosphide compound and its preparation method
  • A kind of linear tin phosphide compound and its preparation method
  • A kind of linear tin phosphide compound and its preparation method

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Experimental program
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Embodiment 1

[0028] The synthesis of embodiment 1 linear tin phosphide

[0029] (1) Prepare the ball milling powder according to the mass ratio of tin powder and phosphorus powder at 2:1, prepare the corresponding grams of aluminum powder according to 1 / 10 of the total mass of the two, put the three kinds of powder into the stainless steel ball milling tank, and The ball-to-material ratio was set at 10:1. Vacuum the ball mill tank and inject nitrogen protective gas. This process is repeated three times to ensure that the atmosphere in the ball mill tank is well protected.

[0030] (2) Fix the ball mill jar on the high-energy ball mill, set its rotational speed at 280rpm, and ball milling time at 30h. During the ball milling process, the machine was stopped for 10 minutes every 30 minutes of ball milling. The ball mill product is taken out, and the powder is collected after passing through a 200-mesh sieve.

[0031] (3) Put the obtained powder into a vacuum tube furnace for calcination, ...

Embodiment 2

[0032] The synthesis of embodiment 2 linear tin phosphide

[0033] (1) Prepare the ball milling powder according to the mass ratio of tin powder and phosphorus powder at 5:1, and prepare the corresponding grams of aluminum powder according to 1 / 30 of the total mass of the two, and put the three kinds of powder into a stainless steel ball milling tank. This ball to material ratio was set at 15:1. Vacuum the ball mill tank and inject nitrogen protective gas. This process is repeated three times to ensure that the atmosphere in the ball mill tank is well protected.

[0034] (2) Fix the ball mill jar on the high-energy ball mill, set its rotation speed to 400rpm, and ball milling time to 20h. During the ball milling process, the machine was stopped for 10 minutes every 30 minutes of ball milling. The ball mill product is taken out, and the powder is collected after passing through a 200-mesh sieve.

[0035] (3) The obtained powder is put into a vacuum tube furnace for calcinati...

Embodiment 3

[0038] Example 3 Form of tin phosphide

[0039] The sample obtained in embodiment 1, embodiment 2 and comparative example 1 is carried out scanning electron microscope observation, and photo is as Figure 1-3 Shown: The powder particles of S1 are covered with Sn with a length ranging from 0.31 μm to 10.65 μm and a width ranging from 190.3 nm to 305.7 nm. 4 P 3 Line; the powder particles of S2 are covered with Sn with a length ranging from 0.17 μm to 1.51 μm and a width ranging from 88.5nm to 195.7nm 4 P 3 Line; the powder particles of C1 are nearly spherical particles.

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Abstract

The invention discloses a linear tin phosphide compound. A chemical formula of the linear tin phosphide compound is Sn4P3; the linear tin phosphide compound has a linear shape and has the length of 0.1mu m to 12mu m and the length-width ratio is 1 to (1.82 to 35.7). The linear tin phosphide compound is prepared by adopting the following steps: carrying out high-energy ball milling on red phosphorus, tin powder and aluminum powder; carrying out calcination on the obtained powder in a vacuum tubular furnace to obtain the linear tin phosphide compound. According to a preparation method of the linear tin phosphide compound, disclosed by the invention, the production cost is reduced, a generation procedure is greatly simplified, the production time is shortened and the yield is improved. Meanwhile, harsh reaction conditions including a toxic phosphorus source, high pressure and the like are also avoided. A prepared phosphide has a linear structure so that the specific surface area is greatly improved, hydrodesulfurization (HDS), hydrodenitrogenation (HDN) and hydrodeoxygenation (HDO) activity and photocatalysis performance of the phosphide are improved and application performance of the phosphide in a lithium-ion battery material is improved.

Description

technical field [0001] The invention relates to a transition metal phosphide synthesis technology, in particular to a preparation method of a linear tin phosphide compound. Background technique [0002] Transition metal phosphides refer to binary or multi-component compounds with a triangular prism structure composed of metal and non-metal element phosphorus, and interstitial compounds formed by filling phosphorus atoms with larger atomic radius in the lattice of metal atoms. Compared with other catalysts (sulfides, nitrides, etc.), due to its special composition structure, it has high catalytic activity and high stability in catalysis. The current research focus is on the hydrodesulfurization of petroleum (HDS ) and hydrodenitrogenation (HDN) above. At the same time, compared with traditional negative electrode materials, transition metal phosphides have the advantages of good cycle stability, large theoretical capacitance, and small polarization, because this material has...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/08
CPCC01B25/08C01P2004/03C01P2004/61C01P2004/62
Inventor 左敏宋丽娇李嘉赵德刚王艳
Owner UNIV OF JINAN
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