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Method of extractively separating molybdenum from tungstate solution

A tungstate, molybdenum tungstate technology, applied in the direction of improving process efficiency, can solve the problems of complex tungsten metallurgical raw materials, increased production cost, difficult to control the amount of oxidant, etc., to improve the production environment, no harmful gas release, Eliminate the effect of H2S generation

Active Publication Date: 2018-09-28
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the problem that must be faced at present is: With the continuous reduction of high-quality tungsten resources in my country, the tungsten metallurgical raw materials that tungsten smelting enterprises will deal with will become more and more complex
However, the affinity between quaternary ammonium salt and MoS2-4 is very strong, and it is often necessary to add a certain amount of oxidant to oxidize thiomolybdate in the stripping process to achieve stripping, which greatly increases the production cost, and it is difficult to control the amount of oxidant

Method used

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  • Method of extractively separating molybdenum from tungstate solution
  • Method of extractively separating molybdenum from tungstate solution
  • Method of extractively separating molybdenum from tungstate solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The feed liquid is a molybdenum-containing ammonium tungstate solution prepared in the laboratory: the feed liquid contains Mo 1g / L, WO 3 100g / L. The original pH of the feed solution was 9.5. The amount of vulcanizing agent added is 1:4, 1:8, 1:10, 1:16, 1:20 according to the molar ratio of molybdenum and vulcanizing agent. Mix, stir, and heat to 70°C. Insulate the reaction for 12 hours, and adjust the end point pH to about 8.5 with ammonia water. By the detection method in embodiment 1, record each condition at the vulcanization rate of molybdenum as following table.

[0037] Table 1 The effect of the amount of vulcanizing agent added on the vulcanization effect of molybdenum

[0038]

[0039] It can be seen from Table 1 that when the temperature is constant, the degree of vulcanization of molybdenum increases significantly with the increase of the amount of vulcanizing agent within the same vulcanization time.

Embodiment 2

[0041] The feed liquid composition is exactly the same as that in Example 1, and the amount of adding vulcanizing agent is 5.91g (the molar ratio of molybdenum and vulcanizing agent is 1:16), but the temperature of reaction changes to some extent, and the control reaction temperature is respectively 40 ℃, 50 °C, 60 °C, 70 °C, heat preservation reaction for 12 hours, control the end point pH=8.5 or so. By the detection method in embodiment 1, record each condition at the vulcanization rate of molybdenum as following table.

[0042] Table 2 Influence of reaction temperature molybdenum vulcanization effect

[0043]

[0044] It can be seen from Table 2 that when the amount of vulcanizing agent is constant, as the reaction temperature increases, the vulcanization effect of molybdenum is significantly improved, so an appropriate increase in temperature is beneficial to the sulfidation of molybdenum. But too high temperature may lead to the decomposition of organic vulcanizing ag...

Embodiment 3

[0046] The feed liquid composition is exactly the same as in Example 1, the amount of adding vulcanizing agent is 5.91g (the molar ratio of molybdenum and vulcanizing agent is 1:16), only change the reaction time, the reaction time is respectively 4h, 6h, 8h, 10h, 12h. According to the detection method in Example 1, the vulcanization rate of molybdenum in each condition is recorded as Table 3.

[0047] Table 3 Effect of reaction time molybdenum vulcanization effect

[0048]

[0049] It can be seen from Table 3 that at a certain temperature and under the condition of controlling the amount of curing agent, prolonging the curing time can increase the curing rate of molybdenum, and the effect of curing time is not as significant as the amount of curing agent and reaction temperature.

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Abstract

The invention discloses a method of extractively separating molybdenum from a tungstate solution. The method includes steps of: adding tripolythiocyanic acid (also called as 2,4,6-trithio-S-triazine,TTCA) to a molybdenum-containing tungstate solution to perform a sulfuration reaction to obtain a mixed solution; performing extraction separation to the mixed solution with an organic phase containing a primary amine extract agent; washing the organic phase supporting molybdenum, and performing reverse extraction separation with an alkaline solution to obtain the tungstate solution. The method can high-effectively separate the tungsten and molybdenum and directly prepare high-purity tungstate solution and molybdate solution; in addition, the sulfuration reaction is carried out with the tripolythiocyanic acid and is free of release of harmful gas, such as H2S, so that the method is safe and environment-friendly. The sulfuration product is easy to subject the extraction and reverse extraction. The reverse extraction separation is free of an oxidant, so that a problem that reverse extraction is difficult after extraction by quaternary ammonium salt is carried out to MoS2-4 generated by sulfurating the molybdate ions by a common sulfuration agent can be solved.

Description

technical field [0001] The invention relates to a method for removing molybdenum from a tungstate solution, in particular to a method for extracting and separating a small amount of molybdenum from a molybdenum-containing tungstate solution, and belongs to the fields of chemical extraction technology and rare metal metallurgy. Background technique [0002] Both tungsten and molybdenum are rare strategic metals with unique properties, widely used in civil, industrial and military fields. In the series of tungsten products, molybdenum is a strictly controlled impurity element. Due to the similar properties of tungsten and molybdenum, they are not only closely associated in minerals, but also often show similar chemical properties and the same direction in the process of secondary resource recovery, making them the most difficult elements to remove from their respective products. However, with the continuous advancement of science and technology, people put forward higher requ...

Claims

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Application Information

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IPC IPC(8): C22B3/44C22B3/28C22B34/34C22B34/36
CPCC22B3/44C22B34/34C22B34/36C22B3/28Y02P10/20
Inventor 曹佐英李嘉李嘉豪张贵清李青刚肖连生关文娟曾理
Owner CENT SOUTH UNIV
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