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Method for separating tungsten and molybdenum from tungsten and molybdenum acid salt solution

A technology of tungsten molybdate and solution, which is applied in the field of selective separation of rare metals, can solve the problems of complex separation process of tungsten and molybdenum, low cation depolymerization rate, and reduced separation effect, etc. It is easy to achieve industrialization and has a good application prospect , the effect of shortening the reaction time

Active Publication Date: 2020-05-15
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Molybdenum is a rare strategic resource with a high melting point. With the rapid development of high-end manufacturing, automobile lightweight, nuclear power, weaponry, high-performance steel and other fields, the demand for molybdenum resources is increasing day by day; however, primary molybdenum ore and molybdenum secondary resources It is often accompanied by tungsten element. According to YST235-2007, WO in molybdenum concentrate 3 The content shall not be greater than 0.05wt%, and the content control of tungsten in molybdenum products is very strict, but due to the shrinkage effect of lanthanide elements, molybdenum and tungsten have similar atomic radii and similar electronic structures, making it difficult to separate the two
[0003] The process of separating tungsten and molybdenum by solvent extraction and ion exchange is complicated and the cost is relatively high
[0004] The Chinese invention patent application with publication number CN106435181A (publication date 2017.2.22) discloses a synergistic extractant containing primary amine extractant and pyridine carboxylate for extracting and separating tungsten from molybdate solution. When it is 7.5-8.5, use primary amine extractant and pyridine carboxylate to extract tungsten synergistically, but it will be affected by tungsten molybdenum heteropolyacid ion
[0005] The Chinese invention patent (disclosure date 1987.5.27) with the publication number CN85108533 discloses a method for solvent extraction and separation of molybdenum in tungsten. Under strong acid conditions, molybdenum and polyacid ions are depolymerized into cationic forms, and tungsten is Extraction with the difference in the form of polyacid ions, but the amount of acid used is too large and the depolymerization rate of cations is not high
[0006] The chemical precipitation method is applied to the separation of tungsten and molybdenum due to its simple process, short process, easy operation and less secondary pollution. 3 Precipitates out, tungsten stays in solution and separates, but releases H in separation methods using sulfidation treatment 2 S gas, pollutes the environment
[0007] The Chinese invention patent with the publication number CN1033978 (publication date 1989.7.19) discloses a production method of ammonium paratungstate or sodium tungstate with high molybdenum removal effect. Guanidine salt is used as a precipitant to precipitate tungsten, while molybdenum remains in the solution However, under neutral conditions, tungstate ions and molybdate ions will polymerize to form tungsten-molybdenum heteropolyacid ions, resulting in reduced separation effect
[0008] The Chinese invention patent application with the publication number CN108425011A (publication date 2018.8.21) discloses a method for extracting tungsten and molybdenum from high-molybdenum scheelite. The peroxytungstic acid is thermally decomposed into tungstic acid precipitation, and the molybdenum remains in the solution. And separation, high energy consumption and excessive acid consumption
[0009] The Chinese invention patent with the publication number CN101565778 (publication date 2009.10.28) discloses a method for precipitating and separating tungsten and molybdenum from a mixed solution of tungstomolybdate. In a suitable pH range, a manganese divalent compound is used as a precipitant Adding it to the mixed solution and heating and stirring, the obtained solid-liquid mixture is separated from the solid-liquid to realize the separation of tungsten and molybdenum, but this method will inevitably cause the loss of molybdenum, and only a single precipitant has not been able to achieve an environmentally friendly solution. High efficiency separation of tungsten and molybdenum

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] The embodiment of the present invention provides a method for separating tungsten and molybdenum from tungstomolybdate solution, specifically as follows:

[0046] S1. Take 0.911g of cetyltrimethylammonium bromide (CTAB), that is, n(CTAB)=n(Mo), add it to c(Mo): c(W)=1:1, metal ion concentration The sum is 0.1mol / L 50ml tungstomolybdate solution, put it in a 30°C water bath environment and mix, stir for 10min until the solution is clear;

[0047]S2. Use 1mol / L sulfuric acid solution and 1mol / L sodium hydroxide solution to adjust the mixed clear solution obtained in step S1 to a pH value of 9.5, put it in a water bath environment at 50°C to keep it warm, and set it aside;

[0048] S3. Add 2.5ml of 1mol / L manganese sulfate precipitant to the solution in the water bath environment in step S2 and stir the reaction at a speed of 250r / min, and the reaction time is 1h;

[0049] S4, performing solid-liquid separation on the solid-liquid mixture in step S3.

[0050] It was dete...

Embodiment 2

[0052] The embodiment of the present invention provides a method for separating tungsten and molybdenum from tungstomolybdate solution, specifically as follows:

[0053] S1. Take 0.455g of cetyltrimethylammonium bromide (CTAB), that is, n(CTAB)=0.5n(Mo), add it to c(Mo):c(W)=5:1, metal ion Put in 50ml tungstomolybdate solution whose sum of concentration is 0.05mol / L, mix in 50℃ water bath environment, stir for 10min until the solution is clear;

[0054] S2. Use 3mol / L sulfuric acid solution and 3mol / L sodium hydroxide solution to adjust the mixed clear solution obtained in step S1 to a pH value of 9.5, put it in a water bath environment at 40°C to keep it warm, and set it aside;

[0055] S3. Add 2.5ml of 1mol / L manganese sulfate precipitant to the solution in the water bath environment in step S2 and stir the reaction at a speed of 250r / min. The reaction time is 20min;

[0056] S4, performing solid-liquid separation on the solid-liquid mixture in step S3.

[0057] It was det...

Embodiment 3

[0059] The embodiment of the present invention provides a method for separating tungsten and molybdenum from tungstomolybdate solution, specifically as follows:

[0060] S1. Take 0.455g of cetyltrimethylammonium bromide (CTAB), that is, n(CTAB)=0.5n(Mo), add it to c(Mo):c(W)=10:1, metal ion Put in 50ml tungstomolybdate solution whose sum of concentration is 0.05mol / L, mix in 50℃ water bath environment, stir for 10min until the solution is clear;

[0061] S2. Use 3mol / L sulfuric acid solution and 3mol / L sodium hydroxide solution to adjust the mixed clear solution obtained in step S1 to a pH value of 11, put it in a water bath environment at 50°C to keep it warm, and set it aside;

[0062] S3. Add 1.25ml of 2mol / L manganese sulfate precipitant to the solution in the water bath environment in step S2 and stir the reaction at a speed of 250r / min. The reaction time is 60min;

[0063] S4, performing solid-liquid separation on the solid-liquid mixture in step S3.

[0064] It was de...

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Abstract

The invention discloses a method for separating tungsten and molybdenum from a tungsten and molybdenum acid salt solution. The method comprises the steps that quaternary ammonium salt is added in thetungsten and molybdenum acid salt solution to serve as a stabilizer, the pH value is adjusted to be 8-11, then, divalent manganese salt is added to serve as a precipitator, and solid-liquid separationis conducted after the reaction. Through introduction of the stabilizer, the function of stabilizing molybdenum acid radical ions in the tungsten and molybdenum acid salt solution can be achieved, the efficiency of the precipitator is improved, and then the tungsten and molybdenum separation efficiency is improved; in the process of selective separation of tungsten through introduction of the stabilizer and the precipitator, toxic and harmful gas generation is avoided, the raw material cost is low, the operation environment is good, the equipment requirement is low, and industrial achieving is easy; and the conditions of the tungsten and molybdenum separating process are moderate, usage of strong acid, strong base, high temperature and high pressure is avoided, and compared with a traditional method, the reaction time is shortened, energy consumption is reduced, economic benefits are high, and the actual application prospects are good.

Description

technical field [0001] The invention belongs to the technical field of selective separation of rare metals, and in particular relates to a method for separating tungsten and molybdenum from a tungstomolybdate solution. Background technique [0002] Molybdenum is a rare strategic resource with a high melting point. With the rapid development of high-end manufacturing, automobile lightweight, nuclear power, weaponry, high-performance steel and other fields, the demand for molybdenum resources is increasing day by day; however, primary molybdenum ore and molybdenum secondary resources It is often accompanied by tungsten element. According to YST235-2007, WO in molybdenum concentrate 3 The content should not be greater than 0.05wt%. The content of tungsten in molybdenum products is very strictly controlled. However, due to the shrinkage effect of lanthanides, molybdenum and tungsten have similar atomic radii and similar electronic structures, making it difficult to separate them...

Claims

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Application Information

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IPC IPC(8): C22B34/34C22B34/36C22B3/44
CPCC22B34/34C22B34/36C22B3/44
Inventor 马立文蔡圆圆席晓丽聂祚仁
Owner BEIJING UNIV OF TECH
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