Preparation method of high-purity molybdenum powder

A molybdenum powder and high-purity technology is applied in the field of preparation of high-purity molybdenum powder, which can solve the problems affecting the purity and application of molybdenum powder, fluctuation of the impurity content of molybdenum powder, etc., and achieve the effect of reducing the impurity content and avoiding the influence.

Active Publication Date: 2012-08-15
湖南顶立科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the purification process, hydrometallurgical technology cannot completely separate various impurity elements, such as tungsten, sulfur, tin and calcium, etc., and when the ore sources are different,

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0025] The invention provides a preparation method of high-purity molybdenum powder, which includes the following steps: A) chlorination reaction of molybdenum dioxide ore powder and chlorine gas, and obtain MoO after condensation 2 Cl 2 solid; B) the MoO 2 Cl 2 Ammonia leaching reaction between the solid and ammonia water to obtain ammonium paramolybdate and HCl gas; C) Roasting the ammonium paramolybdate to obtain MoO 3 ; D) the MoO 3 Perform reduction reaction with reducing gas to obtain high-purity molybdenum powder.

[0026] In order to clearly illustrate the present invention, the experimental processes of steps A, B, C and D are described in detail below.

[0027] According to the present invention, the step A is specifically: the excess Cl 2 Pass it into the reactor equipped with raw material industrial grade molybdenum dioxide, heat it to 220~500°C, preferably 320°C, and react at a stirring rate of 20~160r / min, preferably 55~60r / min. 50~240min, preferably 90~100...

Embodiment 1

[0047] 1.1 Chlorination reaction purification

[0048] Put the raw material industrial grade molybdenum dioxide into the reaction vessel, pass through excess Cl 2 , heated to 320°C, reacted at a stirring speed of 60r / min for 90min and then cooled, the cooling temperature was controlled at 40°C to obtain MoO with extremely low impurity content 2 Cl 2 Crystalline, this is because other elements hardly participate in the reaction, so the impurity content is greatly reduced.

[0049] 1.2 Ammonia leaching to obtain high-purity ammonium paramolybdate

[0050] The MoO obtained in 1.1 2 Cl 2 The crystals and ammonia water are subjected to ammonia leaching treatment in the ammonia immersion tank. The ammonia water is configured according to the volume ratio of ammonia gas and water 1:4 to ensure excess ammonia water. The stirring rate is 60r / min, and the ammonia immersion time is 4h. After the reaction is completed, filter and wash , After being filtered and dried, ammonium paramo...

Embodiment 2

[0058] 2.1 Chlorination reaction purification

[0059] Put the raw material industrial grade molybdenum dioxide into the reaction vessel, pass through excess Cl 2 , heated to 400°C, reacted at a stirring speed of 55r / min for 80min and then cooled, the cooling temperature was controlled at 40°C to obtain MoO with extremely low impurity content 2 Cl 2 Crystals.

[0060] 2.2 Ammonia leaching to obtain high-purity ammonium paramolybdate

[0061] Prepared in the same manner as in Example 1.2.

[0062] 2.3MoO 3 preparation of

[0063] Add the ammonium paramolybdate obtained in 2.2 into a corrosion-resistant and high-temperature-resistant 316L boat, and then put the boat into a roasting furnace for roasting at a roasting temperature of 260°C and a roasting time of 350 minutes to obtain high-purity MoO 3 .

[0064] 2.4 Preparation of high-purity molybdenum powder

[0065] The MoO obtained in 2.3 3 React with hydrogen, the dew point of hydrogen is controlled above -50°C, and t...

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Abstract

The invention provides a preparation method of high-purity molybdenum powder, which comprises the steps: enabling molybdenum dioxide ore powder and chlorine gas to carry out a chlorination reaction; condensing to obtain MoO2C12 solid; then, enabling the MoO2C12 solid and ammonia water to carry out an ammonia leaching reaction to obtain ammonium paramolybdate and HCl gas; further roasting the ammonium paramolybdate to obtain MoO3; and finally, enabling MoO3 and reaction gas to carry out a reduction reaction to obtain high-purity molybdenum powder. Compared with a hydrometallurgical purification method of molybdenum ore sources in the prior art, the preparation method provided by the invention utilizes the molybdenum dioxide ore powder as a raw material to enable the chlorine gas and MoO2 to carry out a selective reaction. As the chlorine gas only reacts with metal Mo, other elements almost do not react; therefore, the content of product impurities is greatly reduced; a high-purity product is obtained; and the effects of the varieties and the contents of the impurities in the molybdenum ore sources of the raw material on the product purity are avoided.

Description

technical field [0001] The invention belongs to the technical field of molybdenum powder preparation, and in particular relates to a preparation method of high-purity molybdenum powder. Background technique [0002] Molybdenum and molybdenum alloys have the characteristics of high high-temperature strength and high-temperature hardness, good thermal and electrical conductivity, and good corrosion resistance. Therefore, they are widely used in metallurgy, chemical industry, electronic information, aerospace and other fields. In recent years, with the rapid development of high-tech, high-tech has put forward higher requirements on the properties of molybdenum and its alloy materials, and at the same time has brought a very broad development space and prospects for the application of molybdenum. Among them, the preparation of molybdenum powder is the primary link in the development of molybdenum industry technology, and the quality of molybdenum powder directly affects the qual...

Claims

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Application Information

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IPC IPC(8): B22F9/22
Inventor 谭兴龙戴煜羊建高
Owner 湖南顶立科技股份有限公司
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