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A kind of method for extracting and separating molybdenum from tungstate solution

A technology of tungstate and molybdenum tungstate, which is applied in the direction of improving process efficiency, can solve the problems of complex tungsten metallurgical raw materials, difficulty in controlling the amount of oxidant, and increased production costs, so as to improve the production environment, eliminate the generation of H2S, and eliminate The effect of harmful gas release

Active Publication Date: 2019-09-27
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 the thiomolybdate to achieve stripping during the stripping process. The production cost is greatly increased, and the amount of oxidant is also difficult to control.

Method used

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  • A kind of method for extracting and separating molybdenum from tungstate solution
  • A kind of method for extracting and separating molybdenum from tungstate solution
  • A kind of method for extracting and separating molybdenum from tungstate solution

Examples

Experimental program
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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, and 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 vulcanizin...

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 for extracting and separating molybdenum from a tungstate solution. In this method, thiocyanuric acid (also known as 2,4,6-trimercapto-S-triazine, TTCA) is added to the molybdenum-containing tungstate solution for vulcanization reaction, and the mixed solution obtained from the vulcanization reaction is extracted with primary amines. The organic phase of the molybdenum is extracted and separated, and the negative molybdenum organic phase is washed, and then back-extracted and separated with an alkaline solution to obtain a molybdate solution. This method realizes the high-efficiency separation of tungsten and molybdenum, and can directly obtain high-purity tungstate solution and molybdate solution, and no harmful gas such as hydrogen sulfide is released during the vulcanization reaction using thiocyanuric acid, which is safe and environmentally friendly, and the vulcanization products It is easy to achieve extraction and stripping, and no oxidizing agent is added in the stripping stage, which solves the problem that MoS2‑4 generated by the general vulcanizing agent molybdate sulfide is difficult to strip after quaternary ammonium salt extraction.

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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Patent Type & Authority Patents(China)
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