CN111154991A - Method for separating tungsten and molybdenum from tungsten molybdate solution - Google Patents
Method for separating tungsten and molybdenum from tungsten molybdate solution Download PDFInfo
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- CN111154991A CN111154991A CN202010059970.4A CN202010059970A CN111154991A CN 111154991 A CN111154991 A CN 111154991A CN 202010059970 A CN202010059970 A CN 202010059970A CN 111154991 A CN111154991 A CN 111154991A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/34—Obtaining molybdenum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/36—Obtaining tungsten
Abstract
The invention discloses a method for separating tungsten and molybdenum from a tungsten molybdate solution, which comprises the steps of adding quaternary ammonium salt serving as a stabilizer into the tungsten molybdate solution, adjusting the pH value to be 8-11, then adding bivalent manganese salt serving as a precipitator, and carrying out solid-liquid separation after reaction. By introducing the stabilizer, the method has the function of stabilizing molybdate ions in the tungsten molybdate solution, improves the efficiency of the precipitator and further improves the separation efficiency of tungsten and molybdenum; the process of selectively separating tungsten by introducing the stabilizing agent and the precipitating agent has no generation of toxic and harmful gases, low cost of raw materials, good operating environment, low equipment requirement and easy realization of industrialization; the separation process has mild conditions, avoids the use of strong acid, strong alkali and high temperature and high pressure, shortens the reaction time, reduces the energy consumption, and has higher economic benefit and good practical application prospect compared with the traditional method.
Description
Technical Field
The invention belongs to the technical field of selective separation of rare metals, and particularly relates to a method for separating tungsten and molybdenum from a tungsten molybdate solution.
Background
Molybdenum is used as a rare strategic resource with high melting point, and along with the rapid development of the fields of high-end manufacturing, light weight of automobiles, nuclear power, weaponry, high-performance steel and the like, the demand of molybdenum resources is increasing day by day; however, primary molybdenum ore and secondary molybdenum resources are often accompanied byWith tungsten element, WO in molybdenum concentrate according to specification YST235-20073The content of the tungsten in the molybdenum product is controlled strictly, but the molybdenum and the tungsten have similar atomic radii and similar electronic structures due to the contraction effect of the lanthanide elements, so that the molybdenum and the tungsten are difficult to separate.
The process flow of the solvent extraction method and the ion exchange method for separating tungsten and molybdenum is complex and the cost is relatively high.
Chinese patent application publication No. CN106435181A (published japanese 2017.2.22) discloses a synergistic extractant comprising a primary amine extractant and pyridine carboxylic acid ester for extracting and separating tungsten from a molybdate solution, wherein the primary amine extractant and pyridine carboxylic acid ester are used for synergistically extracting tungsten at a pH of 7.5-8.5, but are affected by tungsten-molybdenum heteropoly acid ions.
Chinese patent application publication No. CN85108533 (published as 1987.5.27) discloses a method for separating molybdenum from tungsten by solvent extraction, which utilizes the difference between the situation that molybdenum is depolymerized into cation form with polyacid ions and tungsten is extracted with the same polyacid ions in strong acid condition, but the acid consumption is too large and the depolymerization rate of cation is not high.
The chemical precipitation method is applied to the separation of tungsten and molybdenum because of the advantages of simple process, short flow, easy operation, less secondary pollution and the like, and the molybdenum is treated by MoS by industrially utilizing the property difference of the thioacid radical ions3The tungsten precipitates out and is separated by remaining in solution, but H is released in the separation process using sulfidation2S gas, which pollutes the environment.
Chinese patent publication No. CN1033978 (published japanese patent No. 1989.7.19) discloses a method for producing ammonium paratungstate or sodium tungstate with high molybdenum removal efficiency, in which guanidine salt is used as a precipitant to precipitate tungsten, while molybdenum remains in the solution, but tungstate ions and molybdate ions are polymerized under neutral conditions to form tungsten-molybdenum heteropoly acid radical ions, resulting in a reduction in separation effect.
The application of the Chinese patent publication No. CN108425011A (published Japanese 2018.8.21) discloses a method for extracting tungsten and molybdenum from high-molybdenum scheelite, which is characterized in that peroxytungstic acid is thermally decomposed into tungstic acid precipitate, molybdenum is left in solution for separation, the energy consumption is high, and the acid consumption is too large.
Chinese patent application publication No. CN101565778 (published japanese 2009.10.28) discloses a method for precipitating and separating tungsten and molybdenum from a mixed solution of tungsten molybdate, in which a divalent compound of manganese is added as a precipitant into the mixed solution and heated and stirred within a suitable pH range, and the obtained solid-liquid mixture is subjected to solid-liquid separation to achieve tungsten and molybdenum separation, but the method cannot avoid molybdenum loss, and cannot achieve efficient separation of environment-friendly tungsten and molybdenum by using only a single precipitant.
In view of this, the present invention is proposed.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for separating tungsten and molybdenum from a tungsten molybdate solution.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for separating tungsten and molybdenum from a tungsten molybdate solution comprises the steps of adding quaternary ammonium salt serving as a stabilizer into the tungsten molybdate solution, adjusting the pH value to be 8-11, then adding bivalent manganese salt serving as a precipitator, and carrying out solid-liquid separation after reaction.
Specifically, in the process of separating tungsten and molybdenum through the reaction, the affinities of tungstate ions, molybdate ions and bivalent manganese ions are obviously different, manganese tungstate can be generated under the conditions from strong acid to strong base, manganese molybdate can be generated only under the conditions from weak acid to weak base, and under the acidic condition, molybdenum and tungsten in the solution are in the form of isopolyate ions and heteropoly acid radical ions and cannot be separated, so that the solution is adjusted to be in a certain alkaline range, and selective separation can be realized; in the separation process, however, molybdate ions and tungstate ions form competitive precipitation to cause a large amount of molybdenum loss, and one of quaternary ammonium salts such as cetyl trimethyl ammonium bromide is introduced to be matched with the molybdate ions, the molybdate ions serve as ligands, oxygen atoms provide lone-pair electrons for coordination atoms, nitrogen atoms in the cetyl trimethyl ammonium bromide provide a valence layer empty orbit, and the two form a matched bond to play a role in stabilizing molybdenum elements in solution, so that the competition with tungsten is reduced in a short time, the precipitation rate of tungsten is increased, and the separation efficiency is improved.
In the above technical scheme, the amount of the stabilizer added is such that the ratio of the nitrogen atoms in the stabilizer to the molar weight of molybdenum ions in the tungsten molybdate solution is controlled to be 0.35-1: 1, preferably 0.5: 1.
when the addition amount of the stabilizer is too large, part of tungstate anions can be prevented from reacting with the divalent manganese salt while the molybdate anions are stabilized, so that the separation effect is poor; when the addition amount of the stabilizer is too small, the stabilizer cannot play a role in stabilizing molybdate anions.
Specifically, in the above technical solution, the stabilizer is one of tetrabutylammonium bromide, hexadecyltrimethylammonium bromide, dodecyldimethylbenzylammonium chloride and dioctadecyldimethylammonium bromide.
In one embodiment, the stabilizer is cetyltrimethylammonium bromide.
Further, in the above technical scheme, the adding process of the stabilizer is specifically that quaternary ammonium salt is added into tungsten molybdate solution, and the mixture is heated and stirred for reaction until the mixture is clear.
When the powdery stabilizer is added, the powdery stabilizer needs to be mixed with the solution until the solution is clear, and the powdery stabilizer is fully matched with molybdate anion to play a stabilizing role.
Specifically, in the above technical solution, the heating temperature is 30 to 50 ℃.
Specifically, in the technical scheme, the stirring reaction time is 10-15 min.
Still further, in the above technical solution, the amount of the precipitant added is such that the ratio of the amount of the divalent manganese ions in the precipitant to the amount of the tungsten ions in the tungsten molybdate solution is controlled to be 1-2: 1.
specifically, in the technical scheme, the precipitant is added in the form of a divalent manganese salt aqueous solution, and the concentration of the divalent manganese salt aqueous solution is 1-3 mol/L.
In a specific embodiment, the precipitant is one or more of manganese sulfate, manganese hydrochloride, and manganese nitrate.
Still further, in the above technical scheme, after the surfactant is added, the pH value is adjusted to 8-11.
Under certain conditions, the pH value has an important influence on the existence form of the tungsten and the molybdenum, and when the pH value is more than 2.5 and less than 5, the tungsten and the molybdenum have main forms of isopoly acid radical ions and heteropoly acid radical ions and are not easy to separate; when the pH value is more than 2.5 and less than 11.5, tungsten is easy to form manganese tungstate precipitate; when the pH value is more than 5 and less than 9, molybdenum is easy to form manganese molybdate precipitate; therefore, when the pH value of the tungsten molybdenum is more than 9 and less than 11.5, manganese tungstate precipitates are easy to form and manganese molybdate precipitates are not easy to form, the tungsten molybdenum has morphological conditions for precipitation separation, and in addition, other solution conditions can change the separation pH value range to a certain extent.
Preferably, in the technical scheme, the pH value is adjusted to be 8-11 by adding a sulfuric acid solution or a sodium hydroxide solution.
In one embodiment, the concentration of the sulfuric acid solution and the sodium hydroxide solution is 1 to 3mol/L, respectively.
Still further, in the above technical scheme, after the precipitant is added, the reaction temperature is 45-55 ℃.
Still further, in the above technical scheme, the reaction time is 10-15min after the precipitant is added.
The sufficient reaction time for separating the tungsten and the molybdenum by using the single divalent manganese salt is at least about 2 hours, and the separation speed is faster when the reaction time for sufficiently separating the tungsten and the molybdenum by using the stabilizer and the precipitator is 1 hour.
Preferably, in the above technical scheme, after the precipitant is added, the stirring rate of the reaction is 200-300 rpm.
In a preferred embodiment of the present invention, the tungsten molybdate solution has a concentration ratio of molybdenum to tungsten ions of 10-1: 1, and the total concentration of molybdenum and tungsten ions is 0.05-0.1 mol/L.
The invention also provides the application of the method in the wet tungsten-molybdenum metallurgical processing.
The invention has the advantages that:
(1) the method for separating tungsten and molybdenum from the tungsten molybdate solution provided by the invention introduces cetyl trimethyl ammonium bromide and the like as the stabilizer, can play a role in stabilizing molybdate ions in the tungsten molybdate solution, improves the efficiency of the precipitator, and thus improves the separation efficiency of tungsten and molybdenum;
(2) the method for separating tungsten and molybdenum from the tungsten molybdate solution introduces cetyl trimethyl ammonium bromide and the like as stabilizing agents, selectively separates tungsten from precipitating agents, generates no toxic and harmful gases in the process, and has the advantages of low cost of used raw materials, good operating environment, low equipment requirement and easy industrial realization;
(3) the method for separating tungsten and molybdenum from the tungsten molybdate solution provided by the invention has the advantages of mild conditions, avoidance of the use of strong acid, strong base and high temperature and high pressure, shortened reaction time compared with the traditional method, reduced energy consumption, higher economic benefit and good practical application prospect.
Detailed Description
The following describes the embodiments of the present invention in further detail with reference to specific examples.
The following examples are intended to illustrate the present invention, but not to limit the scope of the invention, which is defined by the claims.
Unless otherwise specified, the test reagents and materials used in the examples of the present invention are commercially available.
Unless otherwise specified, the technical means used in the examples of the present invention are conventional means well known to those skilled in the art.
Example 1
The embodiment of the invention provides a method for separating tungsten and molybdenum from a tungsten molybdate solution, which comprises the following specific steps:
s1, 0.911g of cetyltrimethylammonium bromide (CTAB), that is, n (CTAB) ═ n (mo), was added to c (mo): c (w) ═ 1: 1. adding 50ml of tungsten molybdate solution with the sum of metal ion concentration of 0.1mol/L into a water bath environment at 30 ℃ for mixing, and stirring for 10min until the solution is clear;
s2, adjusting the mixed clear solution obtained in the step S1 to pH value of 9.5 by using 1mol/L sulfuric acid solution and 1mol/L sodium hydroxide solution, and placing the mixed clear solution into a water bath environment at 50 ℃ for heat preservation for later use;
s3, adding 2.5ml of 1mol/L manganese sulfate precipitator into the solution in the water bath environment in the step S2, and stirring at the speed of 250r/min for reaction for 1 h;
s4, carrying out solid-liquid separation on the solid-liquid mixture in the step S3.
The tungsten precipitation rate was 92.24%, the molybdenum loss was 12.86%, and the separation coefficient was 80.55.
Example 2
The embodiment of the invention provides a method for separating tungsten and molybdenum from a tungsten molybdate solution, which comprises the following specific steps:
s1, 0.455g of cetyltrimethylammonium bromide (CTAB), that is, n (CTAB) 0.5n (mo), was added to c (mo): c (w) ═ 5: 1. adding 50ml of tungsten molybdate solution with the sum of metal ion concentration of 0.05mol/L into a water bath environment at 50 ℃ for mixing, and stirring for 10min until the solution is clear;
s2, adjusting the mixed clear solution obtained in the step S1 to pH value of 9.5 by using 3mol/L sulfuric acid solution and 3mol/L sodium hydroxide solution, and placing the mixed clear solution into a water bath environment at 40 ℃ for heat preservation for later use;
s3, adding 2.5ml of 1mol/L manganese sulfate precipitator into the solution in the water bath environment in the step S2, and stirring at the speed of 250r/min for reaction for 20 min;
s4, carrying out solid-liquid separation on the solid-liquid mixture in the step S3.
The tungsten precipitation rate was 95.05%, the molybdenum loss was 12.64%, and the separation coefficient was 132.96.
Example 3
The embodiment of the invention provides a method for separating tungsten and molybdenum from a tungsten molybdate solution, which comprises the following specific steps:
s1, 0.455g of cetyltrimethylammonium bromide (CTAB), that is, n (CTAB) 0.5n (mo), was added to c (mo): c (w) ═ 10: 1. adding 50ml of tungsten molybdate solution with the sum of metal ion concentration of 0.05mol/L into a water bath environment at 50 ℃ for mixing, and stirring for 10min until the solution is clear;
s2, adjusting the mixed clear solution obtained in the step S1 to pH value of 11 by using 3mol/L sulfuric acid solution and 3mol/L sodium hydroxide solution, and placing the mixed clear solution into a water bath environment at 50 ℃ for heat preservation for later use;
s3, adding 1.25ml of 2mol/L manganese sulfate precipitator into the solution in the water bath environment in the step S2, and stirring at the speed of 250r/min for reaction for 60 min;
s4, carrying out solid-liquid separation on the solid-liquid mixture in the step S3.
The tungsten precipitation rate was found to be 95.54%, the molybdenum loss was found to be 11.29%, and the separation coefficient was found to be 168.32.
Comparative example 1
The invention provides a method for separating tungsten and molybdenum from a tungsten molybdate solution, which comprises the following steps:
s1, arrangement c (mo): c (w) ═ 1: 1. putting 50ml of tungsten molybdate solution with the sum of metal ion concentration of 0.1mol/L into a water bath environment at 30 ℃ for standby;
s2, adjusting the mixed clear solution obtained in the step S1 to pH value of 9.5 by using 1mol/L sulfuric acid solution and 1mol/L sodium hydroxide solution, and placing the mixed clear solution into a water bath environment at 50 ℃ for heat preservation for later use;
s3, adding 2.5ml of 1mol/L manganese sulfate precipitator into the solution in the water bath environment in the step S2, and stirring at the speed of 250r/min for reaction for 3 h;
s4, carrying out solid-liquid separation on the solid-liquid mixture in the step S3.
The tungsten precipitation rate was 89.51%, the molybdenum loss amount was 17.38%, and the separation coefficient was 39.35.
In conclusion, the embodiment of the invention can stabilize molybdate ions in a tungsten molybdate solution by introducing cetyl trimethyl ammonium bromide and the like as the surfactant, thereby improving the efficiency of the precipitator and further improving the separation efficiency of tungsten and molybdenum; the introduced surfactant such as cetyl trimethyl ammonium bromide and the like is used as a surfactant to selectively separate tungsten from a precipitator, no toxic and harmful gas is generated in the process, the used raw materials are low in cost and good in operating environment, the equipment requirement is low, and the industrial implementation is easy; the separation process has mild conditions, avoids the use of strong acid, strong alkali and high temperature and high pressure, shortens the reaction time, reduces the energy consumption, and has higher economic benefit and good practical application prospect compared with the traditional method.
Finally, the above is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for separating tungsten and molybdenum from a tungsten molybdate solution is characterized in that quaternary ammonium salt is added into the tungsten molybdate solution as a stabilizer, the pH value is adjusted to be 8-11, then divalent manganese salt is added as a precipitator, and solid-liquid separation is carried out after reaction.
2. The method of claim 1, wherein the stabilizer is added in an amount such that the ratio of nitrogen atoms in the stabilizer to the molar amount of molybdenum ions in the solution of tungsten molybdate is controlled to be 0.35 to 1: 1, preferably 0.5: 1.
3. the method according to claim 1, wherein the stabilizer is one of tetrabutylammonium bromide, cetyltrimethylammonium bromide, dodecyldimethylbenzylammonium chloride and dioctadecyldimethylammonium bromide, preferably cetyltrimethylammonium bromide.
4. The method according to any one of claims 1 to 3, wherein the stabilizer is added by adding a quaternary ammonium salt to a solution of tungsten molybdate, and heating and stirring the reaction until the solution is clear.
5. The method of claim 4,
the heating temperature is 30-50 ℃;
and/or the stirring reaction time is 10-15 min.
6. The method according to any one of claims 1 to 5,
the addition amount of the precipitant is that the ratio of the divalent manganese ions in the precipitant to the tungsten ions in the tungsten molybdate solution is controlled to be 1-2: 1;
preferably, the precipitant is added in the form of a divalent manganese salt aqueous solution, and the concentration of the divalent manganese salt aqueous solution is 1-3 mol/L;
further preferably, the precipitant is one or more of manganese sulfate, manganese hydrochloride and manganese nitrate.
7. The method according to any one of claims 1 to 5,
after the surfactant is added, the pH value is adjusted to 8-11;
preferably, the pH value is adjusted to 8-11 by adding sulfuric acid solution or sodium hydroxide solution;
further preferably, the concentration of the sulfuric acid solution and the concentration of the sodium hydroxide solution are respectively 1-3 mol/L.
8. The method according to any one of claims 1 to 7,
after the precipitant is added, the reaction temperature is 45-55 ℃, and/or the reaction time is 10-15 min;
preferably, the reaction is stirred at 200-300rpm after the addition of the precipitant.
9. The method of any one of claims 1 to 8, wherein the tungsten molybdate solution has a ratio of molybdenum to tungsten ion concentrations of 10 "1: 1, and the total concentration of molybdenum and tungsten ions is 0.05-0.1 mol/L.
10. Use of the method of any one of claims 1 to 9 in wet tungsten molybdenum metallurgical processing.
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Cited By (4)
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| CN111659535A (en) * | 2020-05-26 | 2020-09-15 | 金堆城钼业股份有限公司 | Molybdenum-tungsten separation method |
| CN113025818A (en) * | 2021-03-19 | 2021-06-25 | 中南大学 | Method for recovering tungsten from molybdate solution through catalytic precipitation separation |
| CN113801997A (en) * | 2020-06-12 | 2021-12-17 | 杭州临安慧尔钼业科技有限公司 | Method for recycling ammonium molybdate and molybdenum precipitation agent from low-molybdenum raffinate molybdenum |
| CN114672670A (en) * | 2022-02-25 | 2022-06-28 | 信丰华锐钨钼新材料有限公司 | Method for efficiently precipitating Mo in low-concentration sodium molybdate solution |
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| CN113801997A (en) * | 2020-06-12 | 2021-12-17 | 杭州临安慧尔钼业科技有限公司 | Method for recycling ammonium molybdate and molybdenum precipitation agent from low-molybdenum raffinate molybdenum |
| CN113025818A (en) * | 2021-03-19 | 2021-06-25 | 中南大学 | Method for recovering tungsten from molybdate solution through catalytic precipitation separation |
| CN114672670A (en) * | 2022-02-25 | 2022-06-28 | 信丰华锐钨钼新材料有限公司 | Method for efficiently precipitating Mo in low-concentration sodium molybdate solution |
| CN114672670B (en) * | 2022-02-25 | 2023-10-10 | 信丰华锐钨钼新材料有限公司 | Method for efficiently precipitating Mo in low-concentration sodium molybdate solution |
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