CN113621835A - Method for efficiently removing molybdenum based on extraction-precipitation combination - Google Patents
Method for efficiently removing molybdenum based on extraction-precipitation combination Download PDFInfo
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Abstract
The invention discloses a method for efficiently removing molybdenum based on extraction-precipitation combination, which comprises the steps of taking trioctylmethylammonium chloride as an extracting agent, taking tributyl phosphate as a cosolvent and sulfonated kerosene as a diluent to form an extraction organic phase, and simultaneously transforming the organic phase extracting agent, so that tungsten in an acid system or tungsten in a molybdenum-containing sodium tungstate solution can be extracted, separated sulfuric acid and phosphoric acid are returned for use, and a negative tungsten organic phase is reversely extracted by ammonia water to obtain a high-concentration ammonium tungstate solution, so that the transformation of cations is realized.
Description
Technical Field
The invention relates to a method for efficiently removing molybdenum based on extraction-precipitation combination, belonging to the field of wet-process tungsten metallurgy.
Background
Tungsten is an insoluble nonferrous metal and has the characteristics of high melting point, high hardness, strong ductility, wear resistance, corrosion resistance and the like. Metallic tungsten and various tungsten alloys are widely used in modern technology, among which alloy steels, tungsten carbide based cemented carbides, wear and heat resistant alloys are the most important. Tungsten metallurgy is the traditional dominant industry in China, and the reserve of tungsten metallurgy accounts for about half of the world reserveThe tungsten market worldwide has irreplaceable dominance. In the series products of tungsten, molybdenum is a strictly controlled impurity element, and the molybdenum content is required to be less than 20 multiplied by 10 according to the APT-0 grade requirement of ammonium tungstate GB10116-2007 in the national standard-6. With the consumption of high-quality tungsten resources, the content of impurities such as molybdenum in the mined preserved resources is higher and higher, and qualified products cannot be produced without separate molybdenum removal treatment.
Because the physicochemical properties of the tungsten and the molybdenum, such as the atomic radius, the chemical valence state, and the like, are very similar, the efficient separation and the deep separation of the tungsten and the molybdenum become the bottleneck of the urgent research of the current tungsten metallurgy. For a long time, the separation of tungsten and molybdenum has been studied by technicians, and almost all separation methods such as precipitation, solvent extraction, ion exchange, activated carbon adsorption, liquid membrane separation, etc. have been used in the research of tungsten and molybdenum separation. At present, a mature selective precipitation method, an ion exchange molybdenum removal method, a molybdenum trisulfide precipitation method, a hydrogen peroxide complexing system extraction and separation tungsten-molybdenum method and the like have various characteristics, and have a good tungsten-molybdenum separation effect under a suitable environment, but the processes have applicable conditions and pH ranges, and for an ammonium tungstate solution with low impurity content except for high molybdenum concentration, the methods have different problems of high cost, low purity, large repeated smelting energy consumption, poor molybdenum removal effect or serious environmental pollution and the like.
The patent with publication number CN 113073212A discloses a flotation type tungsten raw material extraction full-wet smelting process, and particularly discloses a process for producing an ammonium paratungstate product by leaching, solid-liquid separation, purification, sulfuration acid adjustment and molybdenum removal, extraction, back extraction and crystallization procedures, wherein a defoaming agent and oxygen-enriched gas are added in the leaching procedure, so that the influence of a surfactant in a sodium tungstate solution on the production process is inhibited, and the quality of the ammonium paratungstate product is effectively improved; the invention discloses a method for extracting and separating tungsten and molybdenum, and particularly discloses a method for extracting and separating ammonium tungstate solution by using an N263-sec-octanol-kerosene system, firstly preparing a vulcanized organic phase, and then extracting and removing molybdenum.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for efficiently removing molybdenum based on extraction-precipitation combination, which combines solvent extraction and chemical precipitation to efficiently and stably separate tungsten and molybdenum, thereby achieving the purpose of removing molybdenum.
The technical scheme of the invention is as follows:
the invention discloses a method for efficiently removing molybdenum based on extraction-precipitation combination, which comprises the following steps:
(1) preparing an organic phase: mixing trioctylmethylammonium chloride as an extracting agent, tributyl phosphate as a cosolvent and sulfonated kerosene as a diluent, and uniformly stirring to form an extracted organic phase;
(2) transforming an organic phase; subjecting the organic phase to transformation treatment with H2SO4Treating the organic phase with a solution several times, treating the organic phase with NaOH solution at least 1 time, and subsequently with NaHCO3Treating the solution for several times, and treating the solution with NaOH solution for at least 1 time, wherein the Cl in the water phase-The concentration is less than 0.1g/L, the organic phase transformation is complete, and the CO is obtained3 2-A type of extractant;
(3) and (3) extraction: contacting the tungstate solution to be treated with an extractant at room temperature for 8-10min under the conditions that the O/A ratio is 1:3 and the pH value is less than or equal to 2, extracting at least two stages, and back-extracting the organic phase at room temperature by using an ammonia water solution as a back-extraction agent to obtain a back-extraction solution (NH) with low molybdenum concentration4)2WO4；
(4) Precipitating and removing molybdenum: stripping solution (NH)4)2WO4With (NH)4)2S is directly vulcanized in S2-Standing and vulcanizing for at least 4 hours at room temperature when the free content is more than 8 g/L; then adding metal sulfide, uniformly stirring for 5-10min, standing and clarifying the feed liquid, and filtering to obtain filtrate, namely the tungstate purified liquid after molybdenum removal.
Further, the volume ratio of the extracting agent, the cosolvent and the diluent in the organic phase in the step (1) is 1:1: 3.
Further, H in the step (2)2SO4Treating the organic phase for 3-5 times, wherein the concentration of the solution is 3 mol/L; NaHCO 23Treating the organic phase for 3-5 times, wherein the concentration of the solution is 1 mol/L; NaOH solution with concentration of 2mol/L, and treating the organic phase for 3-5 times.
Further, H in the step (2)2SO4Solution, NaOH solution and NaHCO3The phase ratio during solution treatment of the organic phase was 2/1.
Further, in the step (3), the concentration of hydrogen peroxide is 1mol/L, and the dosage of hydrogen peroxide is 10% of tungstate solution.
Further, the concentration of the stripping agent ammonia water solution in the step (3) is 0.5-4 mol/L.
Further, in the step (4), the metal sulfide is CuS.
Further, the addition amount of the metal sulfide in the step (4) is at least the amount of strip liquor (NH)4)2WO4The content of molybdenum is 5 times of that of molybdenum.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention provides the method for efficiently removing molybdenum based on extraction-precipitation, which has wide adaptability, is suitable for molybdenum removal treatment of tungstate solutions obtained by treating different tungsten ore raw materials by different decomposition methods, has no limit on the content of molybdenum impurities in the tungstate solution, has good impurity removal effect and is suitable for Mo/WO3The recovery rate of the feed liquid which is approximately equal to 1 percent is more than 99.8 percent.
2. The molybdenum removing method provided by the invention does not adopt sec-octanol as a polarity improver and a trioctylmethylammonium chloride compatible organic phase, but adopts tributyl phosphate as a cosolvent and trioctylmethylammonium chloride compatible organic phase, and the tributyl phosphate not only can assist dissolution, but also is a good extracting agent and can be used for extracting metals such as cobalt, iridium, manganese, molybdenum, palladium, platinum, rhodium, technetium, uranium, tungsten and the like, and experiments show that the extraction rate of a low-concentration tungsten solution is up to more than 99% when the pH of the solution is less than or equal to 2.
3. The organic phase is treated for a plurality of times,the transformation of organic phase is realized, and in the extraction process, the obtained CO is transformed3 2-The extraction agent can extract tungsten in an acid system, the separated sulfuric acid and phosphoric acid can be returned for use, the negative tungsten organic phase is back-extracted by ammonia water to obtain a high-concentration ammonium tungstate solution, and the transformation of cations is realized, the extraction of the invention has no ion exchange process, and the back-extracted organic phase does not need a saponification transformation process, so that anions with equal molar number do not enter production wastewater, thereby reducing the production cost and the water pollution risk and reducing the difficulty of wastewater treatment, and through the treatment of the method, the single-stage tungsten extraction can reach more than 90 percent, and the extraction rate can be further improved after more than two-stage extraction; meanwhile, the molybdenum is removed by combining precipitation, so that the content of molybdenum in the purified liquid after molybdenum removal can be ensured to be less than 20 multiplied by 10-6And the quality requirement that the ammonium paratungstate obtained by subsequent evaporation and crystallization meets 0-grade APT (ammonium paratungstate) of GB10116-2007 is met.
Drawings
FIG. 1 is a flow chart of the method for removing molybdenum based on extraction-precipitation.
Detailed Description
The invention will be further described with reference to preferred embodiments and the accompanying drawings.
Example 1
A method for efficiently removing molybdenum based on extraction-precipitation combination comprises the following steps:
(1) preparing an organic phase: mixing and uniformly stirring trioctylmethylammonium chloride serving as an extracting agent, tributyl phosphate serving as a cosolvent and sulfonated kerosene serving as a diluent to form an extraction organic phase, wherein the volume ratio of the extracting agent to the cosolvent to the diluent is 1:1: 3;
(2) transforming an organic phase; the organic phase is subjected to a transformation treatment, first with 3mol/L of H2SO4Treating the organic phase with the solution 3-5 times, treating the organic phase with 2mol/L NaOH solution 3-5 times, and then with 1mol/L NaHCO3Treating the solution for 3-5 times, and treating with 2mol/L NaOH solution for 3-5 times to obtain water phase Cl-The concentration is less than 0.1g/L, the organic phase transformation is complete, and the CO is obtained3 2-A type of extractant; wherein H2SO4Solution, NaOH solution and NaHCO3The phase ratio in the process of treating the organic phase by the solution is 2/1;
(3) and (3) extraction: taking 10L of mixed sulfuric-phosphoric acid solution containing tungsten, adding 1mol/L hydrogen peroxide solution 1L, stirring and heating to 80 ℃, and keeping the temperature for 1 h; adjusting the concentration of tungsten trioxide to be less than or equal to 150g/L, the concentration of sulfuric acid to be less than 2mol/L and the pH to be less than or equal to 2, extracting by using the prepared transformed organic phase extracting agent, keeping the reaction pH to be less than or equal to 2 when the ratio of O/A is 1:3, enabling the tungstate solution to be treated to be in contact with the extracting agent for 8min at room temperature, extracting the organic phase at room temperature by using an ammonia water solution as a stripping agent after more than two-stage extraction, wherein the concentration of the ammonia water solution is 0.5-2mol/L, the phase flow rate is 0.5-1L/min, and obtaining a stripping solution (NH) with low molybdenum concentration4)2WO4；
(4) Precipitating and removing molybdenum: stripping solution (NH)4)2WO4With (NH)4)2S is directly vulcanized in S2-Standing and vulcanizing for at least 4 hours at room temperature when the free content is more than 8 g/L; then adding CuS, wherein the addition amount of CuS is at least the amount of stripping solution (NH)4)2WO4The molybdenum content is 5 times of that of the medium molybdenum, and the mixture is uniformly stirred for 5-8min to be preferentially mixed with MoS4 2-Function, MoS after the reaction has reached a plateau4 2-Is precipitated, and WO4 2-The solution is still kept, the solution is filtered after the feed liquid is kept stand and clarified, the filtrate is tungstate purified liquid after molybdenum is removed, and the molybdenum is absorbed in slag; besides CuS, the metal sulfide may also be selected from NiS, CoS, and PbS.
In the present example, the mixed sulfuric-phosphoric acid solution containing tungsten is a solution obtained by decomposing tungsten ore using mixed sulfuric-phosphoric acid.
Example 2
Example 2 differs from example 1 in the extraction process and precipitation molybdenum removal process:
and (3) extraction: taking 10L of molybdenum-containing sodium tungstate solution, adding 1mol/L of hydrogen peroxide, stirring and heating to 80 ℃, and keeping the temperature for 1 h; adjusting the concentration of tungsten trioxide to be less than or equal to 150g/L, the concentration of sulfuric acid to be less than 2mol/L and the pH to be less than or equal to 2, extracting by using the prepared transformed organic phase extracting agent, and keeping the reaction pH to be less than or equal to 2 when the ratio of O/A is 1:3 so as to wait forContacting the treated tungstate solution with an extractant at room temperature for 10min, extracting at least two stages, and back-extracting the organic phase at room temperature with ammonia water solution of 2-4mol/L and phase flow rate of 1-2L/min to obtain back-extraction solution (NH) with low molybdenum concentration4)2WO4；
Precipitating and removing molybdenum: stripping solution (NH)4)2WO4With (NH)4)2S is directly vulcanized in S2-Standing and vulcanizing for at least 4 hours at room temperature when the free content is more than 8 g/L; then adding CuS, wherein the addition amount of CuS is at least the amount of stripping solution (NH)4)2WO4The molybdenum content is 5 times of that of the molybdenum, and the mixture is uniformly stirred for 8-10min to be preferentially mixed with MoS4 2-Function, MoS after the reaction has reached a plateau4 2-Is precipitated, and WO4 2-The solution is still kept, the solution is filtered after the feed liquid is kept stand and clarified, the filtrate is tungstate purified liquid after molybdenum is removed, and the molybdenum is absorbed in slag;
in the embodiment, the molybdenum-containing sodium tungstate solution is obtained by dissolving molybdenum-containing sodium tungstate crystals in water or decomposing tungsten ore with alkali.
In addition to the sulfuric-phosphoric mixed acid solution containing tungsten obtained by decomposing tungsten ore with sulfuric-phosphoric mixed acid and the sodium tungstate solution containing molybdenum obtained by dissolving sodium tungstate crystals in water or decomposing tungsten ore with alkali described in the above examples, the method of the present invention is also applicable to the treatment of tungstate solutions obtained by other different treatment methods, and is not limited to the above two solutions.
The molybdenum removal efficiency according to the methods described in examples 1 and 2 above is shown in the following table;
TABLE 1 shows the molybdenum removal rate for different W/Mo ratios
TABLE 2 tungsten losses for different W/Mo ratios
As can be seen from tables 1 and 2, the method provided by the invention has the advantages of high molybdenum removal efficiency, less tungsten loss in the molybdenum removal process and WO in molybdenum slag3The ratio of Mo to Mo is less than 0.1, i.e. WO caused by precipitation of 1kg of molybdenum3The loss is less than 0.1kg, the tungsten loss rate is less than 0.1 percent, and the recovery rate is more than 99.9 percent.
The above examples of the present invention are merely examples provided for clearly illustrating the present invention and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. Not all embodiments are exhaustive. All obvious changes and modifications of the present invention are within the scope of the present invention.
Claims (8)
1. A method for efficiently removing molybdenum based on extraction-precipitation combination is characterized by comprising the following steps:
(1) preparing an organic phase: mixing trioctylmethylammonium chloride as an extracting agent, tributyl phosphate as a cosolvent and sulfonated kerosene as a diluent, and uniformly stirring to form an extracted organic phase;
(2) transforming an organic phase; subjecting the organic phase to transformation treatment with H2SO4Treating the organic phase with a solution several times, treating the organic phase with NaOH solution at least 1 time, and subsequently with NaHCO3Treating the solution for several times, and treating the solution with NaOH solution for at least 1 time, wherein the Cl in the water phase-The concentration is less than 0.1g/L, the organic phase transformation is complete, and the CO is obtained3 2-A type of extractant;
(3) and (3) extraction: oxidizing the tungstate solution to be treated with hydrogen peroxide, contacting the tungstate solution to be treated with an extractant at room temperature for 8-10min under the conditions that the ratio of O/A is 1:3 and the pH value is less than or equal to 2, extracting the organic phase at room temperature by taking an ammonia water solution as a stripping agent after more than two-stage extraction, and obtaining a stripping solution (NH) with low molybdenum concentration4)2WO4；
(4) Precipitation ofRemoving molybdenum: stripping solution (NH)4)2WO4With (NH)4)2S is directly vulcanized in S2-Standing and vulcanizing for at least 4 hours at room temperature when the free content is more than 8 g/L; then adding metal sulfide, uniformly stirring for 5-10min, standing and clarifying the feed liquid, and filtering to obtain filtrate, namely the tungstate purified liquid after molybdenum removal.
2. The method for efficiently removing molybdenum based on extraction-precipitation combination as claimed in claim 1, wherein the volume ratio of the extracting agent, the cosolvent and the diluent in the organic phase in the step (1) is 1:1: 3.
3. The method for removing molybdenum based on extraction-precipitation combination with high efficiency as claimed in claim 1, wherein H in the step (2)2SO4Treating the organic phase for 3-5 times, wherein the concentration of the solution is 3 mol/L; NaHCO 23Treating the organic phase for 3-5 times, wherein the concentration of the solution is 1 mol/L; NaOH solution with concentration of 2mol/L, and treating the organic phase for 3-5 times.
4. The method for removing molybdenum based on extraction-precipitation combination with high efficiency as claimed in claim 1, wherein H in the step (2)2SO4Solution, NaOH solution and NaHCO3The solution treatment of the organic phase was carried out at 2/1 for the O/A ratio.
5. The method for efficiently removing molybdenum based on extraction-precipitation combination as claimed in claim 1, wherein the concentration of hydrogen peroxide in the step (3) is 1mol/L, and the amount of hydrogen peroxide is 10% of tungstate solution.
6. The method for removing molybdenum with high efficiency based on the combination of extraction and precipitation as claimed in claim 1, wherein the concentration of the stripping agent aqueous ammonia solution in the step (3) is 0.5-4 mol/L.
7. The method for removing molybdenum with high efficiency based on the combination of extraction and precipitation as claimed in claim 1, wherein the metal sulfide in the step (4) is CuS.
8. The method for removing molybdenum based on extraction-precipitation combination with high efficiency as claimed in claim 1, wherein the amount of the metal sulfide added in the step (4) is at least the amount of strip liquor (NH)4)2WO4The content of molybdenum is 5 times of that of molybdenum.
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| CN114349143A (en) * | 2021-12-23 | 2022-04-15 | 扬州大学 | Complex coacervate phase system and preparation method and application thereof |
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