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A kind of method of sulfide separation molybdenum in tungstate solution

A technology of tungstate and molybdenum tungstate, which is used in the field of molybdenum removal from tungstate solution and extraction and separation of quaternary ammonium extractant, which can solve the problem of high concentration of primary amine extractant, high price of thiocyanate, and vulcanization reaction. Long time and other problems, to achieve good vulcanization effect, easy stripping, good separation effect of tungsten and molybdenum

Active Publication Date: 2021-01-08
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Li Jia (Research on new technology for separation of tungsten and molybdenum based on new vulcanizing agent [D]. Central South University, 2019.) Using new vulcanizing agent trimeric thiocyanate sulfomolybdate ion, and extracting and separating tungsten and molybdenum with primary amine extractant N1923, separation The effect is good, the vulcanization rate of molybdate ions has reached over 99.5%, and the molybdenum in the feed liquid can be reduced to below 5mg / L through 4-stage countercurrent extraction, tungsten is hardly extracted, and the stripping effect is good, using dissociation-precipitation -Three-step conversion method can recover thiocyanic acid, the recovery rate is more than 95%, but this method has long vulcanization reaction time, high temperature, high price of thiocyanic acid, resulting in increased vulcanization cost, the primary amine used for extraction The concentration of the solvent is high, the saturation capacity is low, the extraction efficiency is low, and the recovery process needs to consume more acid and alkali, resulting in more waste water, and the overall cost needs to be reduced

Method used

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  • A kind of method of sulfide separation molybdenum in tungstate solution
  • A kind of method of sulfide separation molybdenum in tungstate solution
  • A kind of method of sulfide separation molybdenum in tungstate solution

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The feed liquid is a molybdenum-containing ammonium tungstate solution prepared in the laboratory: the feed liquid contains Mo 1g / L, WO 330g / L. The original pH of the feed solution was 7.5. The amount of vulcanizing agent added is 1:4, 1:10, 1:20, 1:30, 1:40, 1:50, 1:60 according to the molar ratio of molybdenum and ethyl thioglycolate vulcanizing agent. Mix and stir and heat to 40°C. Insulation reaction 4h. The vulcanization rate of molybdenum under various conditions is measured in the following table.

[0032] Table 1 The effect of the amount of vulcanizing agent added on the vulcanization effect of molybdenum

[0033]

[0034] 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

[0036] The composition of the feed liquid is exactly the same as that in Example 1. Add the vulcanizing agent according to the molar ratio of molybdenum to ethyl mercaptoacetate vulcanizing agent is 1:20, and control the reaction temperature to be 20°C, 30°C, 40°C, 50°C, and 60°C respectively. , 70 ℃, heat preservation reaction 2h, feed liquid pre-adjusted pH = 7 or so, the vulcanization rate of molybdenum measured under each condition is shown in the table below.

[0037] Table 2 Effect of reaction temperature on molybdenum vulcanization effect

[0038]

[0039] 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 cause oxidation of vulcanizing agent to ether.

Embodiment 3

[0041] The composition of the feed liquid is exactly the same as that in Example 1. Add the vulcanizing agent according to the molar ratio of molybdenum to ethyl thioglycolate vulcanizing agent is 1:20, control the reaction temperature to 40°C, and pre-adjust the pH of the feed liquid to about 7.5, only changing the reaction Time, the reaction time is 0.5h, 1h, 2h, 3h, 4h, 5h respectively. Table 3 shows the vulcanization rate of molybdenum under various conditions.

[0042] 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.

[0043] The influence of table 3 reaction time on molybdenum vulcanization effect

[0044]

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Abstract

The invention discloses a method for vulcanizing and separating molybdenum in a tungstate solution. Add ethyl thioglycolate to the solution containing molybdenum tungstate to carry out the sulfuration reaction of molybdate, the sulfide molybdate is extracted and separated with the organic phase containing quaternary ammonium extractant, and the organic phase loaded with sulfide molybdate is reacted with alkaline solution extraction and separation to obtain a molybdenum-containing solution. The method has fast vulcanization speed, high efficiency, high selectivity, and mild conditions, and the vulcanized product can be extracted with quaternary ammonium salt, and has the characteristics of low extraction agent concentration, high saturation capacity, high extraction efficiency and low reaction acid and alkali consumption.

Description

technical field [0001] The invention relates to a method for removing molybdenum from a tungstate solution, in particular to a method in which an organic sulfide is used to selectively sulfide a small amount of molybdate in a molybdenum-containing tungstate solution, and then extracted and separated by a quaternary ammonium extractant, which belongs to the wet method field of metallurgical technology. Background technique [0002] Due to the similar properties of tungsten and molybdenum in the metallurgical process, the separation of the two has always been a difficult technical problem in tungsten metallurgy. With the mining of ore, the grade of tungsten and molybdenum ore is getting lower and lower. People are interested in tungsten and molybdenum metal and its alloys. The requirements are getting higher and higher, and new requirements are also put forward for tungsten and molybdenum products. To solve this worldwide problem, the existing methods of precipitation, extrac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B3/28C22B3/44C22B34/34C22B34/36
CPCC22B3/44C22B34/34C22B34/36C22B3/288Y02P10/20
Inventor 曹佐英杜佳炜李嘉张贵清曾理巫圣喜李青刚关文娟肖连生
Owner CENT SOUTH UNIV
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