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Liquid phase reaction preparing method for V-Ti-Fe hydrogen storage alloy powder

A technology of hydrogen storage alloy powder and liquid phase reaction, which is applied to electrical components, battery electrodes, circuits, etc., can solve the problems of high production cost and excessive impurities, achieve low reaction temperature, ensure uniformity, and reduce oxygen content Effect

Active Publication Date: 2017-11-17
XI'AN UNIVERSITY OF ARCHITECTURE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the defects and insufficiencies of the existing preparation technology, the purpose of the present invention is to provide a liquid phase reaction preparation method of V-Ti-Fe hydrogen storage alloy powder, which solves the problems that the existing preparation method introduces too many impurities and the preparation cost is high

Method used

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Examples

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Effect test

preparation example Construction

[0019] The liquid-phase reaction preparation method of V-Ti-Fe hydrogen storage alloy powder of the present invention specifically comprises:

[0020] Liquid VCl 4 , liquid TiCl 4 and FeCl 3 Mix the powders, add a reducing agent to the mixture for reaction, filter the solid product after the reaction, remove the remaining reducing agent and chloride salt impurities in the product, and obtain V-Ti-Fe hydrogen storage alloy powder.

[0021] Specifically, VCl 4 、TiCl 4 and FeCl 3 The mixing process of mixing is: first VCl 4 solution and TiCl 4 solution mixed, and then FeCl 3 powder dissolved in VCl 4 and TiCl 4 in the mixture.

[0022] Specifically, the reaction temperature of the mixture and the reducing agent is 350-850° C., and the reaction process is carried out under a protective atmosphere.

[0023] Specifically, the reducing agent is metal sodium or metal magnesium.

[0024] Specifically, in the V-Ti-Fe series hydrogen storage alloy, by mole percentage: V is 40...

Embodiment 1

[0029] VCl 4 、TiCl 4 , FeCl 3 Dosing according to the molar ratio of 5:4.5:0.5, the VCl 4 and TiCl 4 Stir to mix, FeCl 3 Slowly add the powder into the mixture and stir well to make the FeCl 3 dissolved in the mixture. Through the flow control valve, the mixed chloride liquid is slowly introduced into the reactor protected by a high-purity argon atmosphere. The reactor is filled with liquid metal sodium, and the dosage is twice the theoretical requirement of the reaction. The reaction temperature is controlled at 700°C . After the reaction, the liquid metal sodium and the solid product were separated by filtration, and the solid product was vacuum distilled at a vacuum degree of 0.01 Pa, at a temperature of 850° C., and for 2 hours. The solid product obtained after distillation was rod-milled for 1 min, then placed in an ultrasonic environment, and immersed in water for 5 hours to dissolve sodium chloride into water, and then centrifuged to obtain a V-Ti-Fe hydrogen sto...

Embodiment 2

[0033] VCl 4 、TiCl 4 , FeCl 3 Dosing according to the molar ratio of 6.0:3.8:0.2, the VCl 4 and TiCl 4 Stir to mix, FeCl 3 Slowly add the powder into the mixture and stir well to make the FeCl 3 dissolved in the mixture. Through the flow control valve, the mixed chloride liquid is slowly passed into the reactor protected by a high-purity argon atmosphere. The reactor is filled with liquid metal sodium, and the amount is 3 times the theoretical requirement of the reaction. The reaction temperature is controlled at 800 ° C. . After the reaction, the liquid metal sodium and the solid product were separated by filtration, and the solid product was vacuum distilled at a vacuum degree of 0.01 Pa, at a temperature of 800° C., and for 2 hours. The solid product obtained after distillation was rod-milled for 1 min, then placed in an ultrasonic environment, and immersed in water for 5 hours to dissolve sodium chloride into water, and then centrifuged to obtain V-Ti-Fe hydrogen st...

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Abstract

The invention discloses a liquid phase reaction preparing method for V-Ti-Fe series hydrogen storage alloy powder. VCl4, TiCl4 and FeCl3 are mixed, a reducing agent is added into the mixture for a reaction, a solid product is filtered after the reaction is over, the residual reducing agent and chlorine salt impurities in the product are removed, and the V-Ti-Fe hydrogen storage alloy powder is obtained. Compared with a traditional pure-metal mixing smelting method or an oxide metal thermal reduction method, the VCl4, the TiCl4 and the FeCl3 are used as the raw materials to prepare a V-Ti-Fe series hydrogen storage alloy, the raw materials are mixed in a liquid manner and are sufficiently mixed, uniformity of the alloy components can be ensured, the prepared product is directly in an alloy powder manner, and the influences of breaking conditions on the alloy performance can be reduced. The reaction temperature of the preparing process of the method is low, and the oxygen content of the alloy can be effectively reduced.

Description

technical field [0001] The invention belongs to the field of hydrogen storage alloy preparation, in particular to a liquid-phase reaction preparation method of V-Ti-Fe hydrogen storage alloy powder. Background technique [0002] As a clean and efficient clean energy, hydrogen energy is one of the current research hotspots. The key technology of hydrogen energy utilization is the safe storage and transportation of hydrogen, and hydrogen storage alloy technology is one of the more efficient storage and transportation methods. The V-Ti-Fe hydrogen storage alloy has a large theoretical hydrogen storage capacity, good kinetics of hydrogen absorption and desorption at room temperature, and has a good application prospect. At present, its preparation method generally uses pure metal as raw material, and adopts high-temperature mixed melting. Due to the high melting point of each metal, the melting temperature is also high. Excessively high melting temperature is easy to introduce ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24H01M4/38
CPCB22F9/24H01M4/383Y02E60/10
Inventor 王斌杜金晶俞娟方钊武小雷
Owner XI'AN UNIVERSITY OF ARCHITECTURE AND TECHNOLOGY
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