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Method for efficiently removing molybdenum based on extraction-precipitation combination

An extraction and high-efficiency technology, applied in the field of wet tungsten metallurgy, can solve the problems of environmental pollution, great impact on the operating environment, odor of sec-octanol, etc., and achieves the effect of wide adaptability and good impurity removal effect.

Pending Publication Date: 2021-11-09
FUJIAN JINXIN TUNGSTEN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the relatively mature selective precipitation method, ion exchange molybdenum removal method, molybdenum trisulfide precipitation method, hydrogen peroxide complex system extraction and separation of tungsten and molybdenum method, etc. all have their own characteristics, and they all have good tungsten and molybdenum in suitable environments. Molybdenum separation effect, but the above-mentioned processes all have their applicable conditions and pH range. For the ammonium tungstate solution with low impurity content except high molybdenum concentration, the above-mentioned methods have high cost, low purity, and repeated smelting energy consumption. Different problems such as large, poor molybdenum removal effect or serious environmental pollution
[0004] The patent with the publication number of CN 113073212A discloses a flotation-type tungsten raw material extraction full-wet smelting process, which specifically discloses the production process including leaching, solid-liquid separation, purification, sulfidation, acid adjustment and molybdenum removal, extraction, stripping and crystallization. The process of ammonium paratungstate product, by adding defoamer and oxygen-enriched gas in the leaching process, suppresses the influence of surfactant in sodium tungstate solution on the production process, and effectively improves the quality of ammonium paratungstate product; the publication number is CN 104120257A The patent discloses a method for extraction and separation of tungsten and molybdenum, specifically discloses the use of N263-sec-octanol-kerosene system to extract and separate ammonium tungstate solution, first prepare the sulfurized organic phase, and then extract and remove molybdenum. Starting with the configuration, vulcanization process, and stripping process, the problem of low efficiency and high cost of molybdenum removal by traditional ammonium tungstate extraction is solved. The operating environment has a great influence

Method used

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  • Method for efficiently removing molybdenum based on extraction-precipitation combination
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  • Method for efficiently removing molybdenum based on extraction-precipitation combination

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Embodiment 1

[0026] A method for efficiently removing molybdenum based on extraction-precipitation, comprising the following steps:

[0027] (1) Prepare organic phase: take trioctylmethyl ammonium chloride as extractant, tributyl phosphate as cosolvent, sulfonated kerosene as diluent mix, stir to form extraction organic phase, wherein extractant, cosolvent and The volume ratio of diluent is 1:1:3;

[0028] (2) organic phase transformation; organic phase is carried out transformation treatment, at first with the H of 3mol / L 2 SO 4 Treat the organic phase with solution for 3-5 times, then treat the organic phase with 2mol / L NaOH solution for 3-5 times, and then use 1mol / L NaHCO 3 The solution was treated for 3-5 times, and finally treated with 2mol / L NaOH solution for 3-5 times, and the aqueous phase was treated with Cl - When the concentration is less than 0.1g / L, the organic phase transformation is complete, that is, CO 3 2- type extractant; where H 2 SO 4 solution, NaOH solution an...

Embodiment 2

[0033] The difference between embodiment 2 and embodiment 1 is that extraction process and precipitation remove molybdenum process:

[0034] Extraction: Take 10L of molybdenum-containing sodium tungstate solution, add 1L of 1mol / L hydrogen peroxide, stir and heat to 80°C, keep the temperature for 1h; adjust the concentration of tungsten trioxide to ≤150g / L, the concentration of sulfuric acid to less than 2mol / L, and pH≤2, Extract with the transformed organic phase extractant prepared above, and keep the reaction pH ≤ 2 at a ratio of O / A of 1:3, so that the tungstate solution to be treated and the extractant are in contact with the extractant for 10 minutes at room temperature, and after two stages After the above extraction, the ammonia solution is used as the stripping agent, and the organic phase is stripped at normal temperature. The concentration of the ammonia solution is 2-4mol / L, and the phase flow rate is 1-2L / min, so as to obtain the stripping solution with low molybde...

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Abstract

The invention discloses a method for efficiently removing molybdenum based on extraction-precipitation combination. The method comprises the following steps that an extraction organic phase is formed by using methyl trioctyl ammonium chloride as an extraction agent, tributyl phosphate as a cosolvent and sulfonated kerosene as a diluent, and meanwhile, the organic phase extraction agent is transformed, so that tungsten in an acid system can be extracted, or the tungsten in a molybdenum-containing sodium tungstate solution can be extracted, the separated sulfuric acid and phosphoric acid are returned for use, the negative tungsten organic phase is subjected to reverse extraction with ammonia water, a high-concentration ammonium tungstate solution can be obtained, and cation transformation is achieved. According to the method provided by the invention, the content of impurity molybdenum can be effectively removed.

Description

technical field [0001] The invention relates to a method based on extraction-precipitation combined with high-efficiency molybdenum removal, which belongs to the field of wet tungsten metallurgy. Background technique [0002] Tungsten is an insoluble non-ferrous metal with high melting point, high hardness, strong ductility, wear resistance and corrosion resistance. Metal tungsten and various tungsten alloys are widely used in modern technology, among which, the most important ones are alloy steel, tungsten carbide-based hard alloy, wear-resistant and heat-resistant alloy. Tungsten metallurgy is a traditional advantageous industry in my country, its reserves account for about half of the world's reserves, and it plays an irreplaceable leading role in the world's tungsten market. In the series of tungsten products, molybdenum is a strictly controlled impurity element. According to the requirements of APT-0 grade product of ammonium tungstate "GB10116-2007" in the national st...

Claims

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Application Information

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IPC IPC(8): C22B34/36C22B3/44C22B3/40
CPCC22B34/36C22B3/44Y02P10/20
Inventor 谢建干庄世明蓝永祥
Owner FUJIAN JINXIN TUNGSTEN
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