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Acid-alkali combination method for extracting tungsten from tungsten minerals

An acid-base combination and mineral technology, applied in the field of hydrometallurgy, can solve the problems of high equipment safety requirements, complicated operation, and high rate of alkali decomposition of slag and slag, so as to ensure the recovery rate and simplify the process flow.

Active Publication Date: 2019-07-12
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But there are following disadvantages at the same time: (1) the waste hydrochloric acid mother liquor containing calcium chloride is difficult to handle; (2) the production process is carried out under the condition of semi-open and negative pressure, the volatilization loss of hydrochloric acid is serious, and the production environment is poor; (3) the raw material Generally, it can only process high-grade scheelite with low impurity content such as phosphorus and arsenic, and the decomposition rate of wolframite can only reach about 80%.
However, the main disadvantages of this technology are: (1) It needs to work under high temperature and high pressure conditions of 160-220°C and 0.66-2.2MPa, high energy consumption, high equipment safety requirements, and complicated operation; (2) The alkali obtained by decomposition The slag rate of decomposed slag is high, generally 80-90% of the original ore quality; (3) the amount of sodium carbonate is large, generally more than 4 times the theoretical amount; (4) waste water and salt are discharged during the process of ion exchange transformation to ammonium tungstate large

Method used

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Experimental program
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Effect test

Embodiment 1

[0059] The scheelite used contains WO 3 58%, containing P 0.03%, containing Mo 0.1%, particle size less than 150 microns.

[0060] 1) Acid decomposition:

[0061] Weigh 500g of the above-mentioned scheelite, mix it with 1500mL of hydrochloric acid solution with a concentration of 6.0mol / L, stir and react in a closed glass reactor at 95°C for 2 hours, and slowly add 10mL of H 2 o 2 Solution (H 2 o 2 The mass concentration is 30%), after filtration, solid tungstic acid and acid decomposition mother liquor are obtained, and the obtained tungstic acid contains WO 3 81%, the obtained acid decomposes and contains WO in the mother liquor 3 0.22g / L, Mo 0.06g / L, Ca 54g / L, Fe 0.6g / L, Na 0.08g / L, K 0.05g / L, H + 3.0mol / L. The obtained tungstic acid was washed 4 times with 180mL deionized water each time and collected respectively.

[0062] 2) Conversion and purification of acid decomposition mother liquor:

[0063] Add 87g CaCl while stirring in the acid decomposition mother liqu...

Embodiment 2

[0072] The scheelite used contains WO 3 29%, containing P 1.6%, containing Mo 2.3%, particle size less than 150 microns.

[0073] 1) The first level of preprocessing:

[0074] Take 2000g of the above-mentioned scheelite ore, slowly add 6000mL of hydrochloric acid solution with a concentration of 1.5mol / L and start stirring, then continue to stir at room temperature for 1 hour and then filter. The obtained filter cake is the first-stage pretreatment concentrate, which is used for the second-stage pretreatment, and the obtained filtrate is the first-stage pretreatment mother liquor, wherein, the first-stage pretreatment mother liquor contains WO 3 0.34g / L, Mo 0.1g / L, P 0.6g / L, Ca 19g / L, Fe 0.8g / L, K 0.05g / L, Na 0.08g / L, H + 0.46g / L.

[0075] 2) Purification and conversion of pretreatment mother liquor:

[0076] Get 5000mL of the aforementioned first-stage pretreatment mother liquor, add CaCO thereto while stirring 3 powder until the pH of the solution is 4.0, then continue...

Embodiment 3

[0084] The scheelite that adopts is the second grade pretreatment ore that obtains in step 3) in embodiment 2, wherein contains WO 3 50.8%, containing P 0.12%, containing Mo 3.7%.

[0085] 1) Acid decomposition:

[0086] Weigh 600g of the above-mentioned second-stage pretreatment ore, mix it with 4000mL of hydrochloric acid solution with a concentration of 7.0mol / L, stir and react in a closed glass reactor at 95°C for 3 hours, and slowly add 25mL of H 2 o 2 Solution (H 2 o 2 The mass concentration is 30%), solid tungstic acid and acid decomposition mother liquor are obtained after filtration, and the obtained tungstic acid contains WO 3 77%, the resulting acid decomposition mother liquor contains WO 3 0.63g / L, Mo 4.9g / L, Ca 25g / L, Fe 0.8g / L, Na 0.07g / L, K 0.04g / L, H + 5.6mol / L. The obtained tungstic acid was washed 4 times with 250mL deionized water each time and collected respectively.

[0087] 2) Conversion and purification of acid decomposition mother liquor:

[00...

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Abstract

The invention relates to an acid-alkali combination method for extracting tungsten from tungsten minerals. The method comprises the following steps of step 1, decomposing acid, specifically mixing a tungsten ore with a hydrochloric acid solution, adding H2O2 to carry out a stirring reaction to obtain a solid tungstic acid and an acid decomposition mother solution; step 2, dissolving the solid tungstic acid by using sodium carbonate, specifically mixing the solid tungstic acid with a sodium carbonate solution to carry out the stirring reaction, and after the reaction is finished, filtering to obtain dissolved slag and a sodium tungstate solution; step 3, carrying out resin ion exchange treatment on the sodium tungstate solution, specifically neutralizing the sodium tungstate solution obtained in the step 2 with sulfuric acid until the pH value is 3-6 to serve as a pre-exchange solution, adsorbing the tungsten in pre-exchange solution through macroporous weak-alkaline anion exchange resin, washing the macroporous weak-alkaline anion exchange resin adsorbing the tungsten by using deionized water; after washing is completed, carrying out desorption to obtain ammonium tungstate desorption liquid by using ammonia water as a desorption agent, and further, removing impurities, evaporating and crystallizing to obtain ammonium paratungstate. The method has the advantages that the technological process is simplified, and meanwhile, the recovery rate of the tungsten is ensured.

Description

technical field [0001] The invention relates to the field of hydrometallurgy, in particular to a method for extracting tungsten from tungsten minerals through the combination of acid and alkali. Background technique [0002] Tungsten is a rare metal with a high melting point. At present, about two-thirds of its output is used to produce hard alloys. In addition, it is also widely used in the fields of high specific gravity alloys, tungsten wire and steelmaking. The mineral raw materials used to extract tungsten mainly include scheelite, wolframite, black and white tungsten mixed ore, etc. [0003] The main methods of extracting tungsten from tungsten mineral raw materials are acid method and alkali method: the acid method mainly uses hydrochloric acid or a mixed acid of hydrochloric acid and phosphoric acid or a mixed acid of sulfuric acid and phosphoric acid to decompose tungsten minerals under normal pressure to obtain solid tungsten respectively. Acid or phosphotungstic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B34/36C22B3/44C22B3/42C22B3/24
CPCC22B34/36C22B3/44C22B3/42C22B3/24Y02P10/20
Inventor 霍广生曾璐琦易新涛刘洲际卢阳明朱和平
Owner CENT SOUTH UNIV
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