A method for separating molybdenum in tungstate solution by ion exchange

An ion exchange method and tungstate technology, applied in the field of rare metal metallurgy, can solve problems such as adverse effects of the process, complex mineral raw materials, deterioration of the production environment, etc., and achieve the effects of good desorption separation effect, easy desorption process, and safe and convenient measurement.

Active Publication Date: 2020-04-21
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Although many scholars have done a lot of research on the separation of tungsten and molybdenum, and some of them have realized industrialization, the problem they are currently facing is that the grade of tungsten and molybdenum concentrates is gradually decreasing, and people have put forward more new requirements for metal materials. The mineral raw materials to be processed by enterprises will also become more and more complex. For example, in the Shizhuyuan Mine, a comprehensive polymetallic mine in my country, m(Mo) / m(WO 3 ) is about 2%, m(Mo) / m(WO 3 ) up to 5% or more
In industry, if traditional vulcanizing agents such as Na 2 S and (NH 4 ) 2 S, etc. have the problem of high cost, and there will be toxic gas hydrogen sulfide emissions in the production process, which will deteriorate the production environment, and the environmental friendliness is poor, and hydrogen sulfide gas recovery facilities need to be added; the ion exchange method is used to separate tungsten and molybdenum. During the process, thiomolybdate cannot be desorbed from the resin with an alkaline solution, and oxidants such as hydrogen peroxide and sodium hypochlorite must be added for desorption. The heat released during the oxidation process and the oxidant itself will affect the resin, shorten the service life of the resin, and return it to the subsequent process bring adverse effects

Method used

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  • A method for separating molybdenum in tungstate solution by ion exchange
  • A method for separating molybdenum in tungstate solution by ion exchange
  • A method for separating molybdenum in tungstate solution by ion exchange

Examples

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Effect test

Embodiment 1

[0033]The feed liquid is a prepared ammonium molybdenum tungstate solution, which is vulcanized in advance with a vulcanizing agent. The vulcanization conditions are: prepare 5L containing WO 3 100g / L, Mo1g / L simulated feed liquid, add 148g trimeric thiocyanate as vulcanizing agent. The vulcanization temperature was 70°C, and the pH of the feed solution was adjusted to 9.5 after thiolation. The thiolation rate was 99.5% tested by extraction method. Take 20ml of feed solution each time, 5ml of HBDM-1 resin in a beaker, and adsorb at room temperature for 1 hour. From the adsorption results, it can be seen that the adsorption rate of tungsten and molybdenum varies greatly with pH. When the pH is 9.25 to 9.5, the adsorption of molybdenum The tungsten adsorption rate reached the maximum, reaching 78.79%, while the adsorption rate of tungsten increased with the decrease of pH. It can be known by calculation that the separation coefficient of tungsten and molybdenum can reach 3.28 ...

Embodiment 2

[0035] The feed liquid is the thiolated ammonium molybdenum tungstate solution prepared in Example 1. Each time, 20 ml of the feed liquid is taken, and 5 ml of HBDM-1 resin is adsorbed in a beaker for 1 hour, and the adsorption temperature is controlled to be normal temperature (25° C.)~ 60°C. It can be seen from the experimental results that the adsorption rate of tungsten and molybdenum keeps increasing with the increase of temperature, and the calculation shows that the separation coefficient is continuously increasing. At room temperature, the adsorption rates of tungsten and molybdenum are 27.19% and 60.63% respectively. According to the actual economic factors and experimental results, it can meet the requirements of tungsten and molybdenum separation at room temperature.

Embodiment 3

[0037] The feed solution is the thiolated ammonium molybdenum tungstate solution prepared in Example 1. 20ml feed solution and 5ml HBDM-1 resin are taken each time and adsorbed at room temperature. The adsorption time is 5min~2h respectively. It can be seen from the results It can be seen that with the extension of adsorption time, the adsorption rate of tungsten and molybdenum increases continuously, and the calculation shows that the separation coefficient increases continuously, indicating that the longer the adsorption time, the better the separation effect of tungsten and molybdenum. After 2 hours, the adsorption rate of tungsten and molybdenum tended to be stable and reached an equilibrium state.

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Abstract

The invention discloses a method for separating molybdenum from a tungstate solution through ion exchange. The method includes the steps that trithiocyanuric acid is added into the molybdenum-containing tungstate solution to carry out vulcanization reaction, so that a tungstate solution containing thiomolybdate is obtained; the tungstate solution containing the thiomolybdate is subjected to ion exchange by adopting weak-base anion-exchange resin so as to adsorb the thiomolybdate, and a tungstate solution is obtained; and the weak-base anion-exchange resin loaded with the thiomolybdate is desorbed by an alkaline desorption solution, so that a molybdate solution is obtained. According to the method, the separating effect of molybdenum in the high-tungsten low-molybdenum solution is good, tungsten loss is little, operation is simple, no hydrogen sulfide is released in the vulcanization process, a hydrogen sulfide recovery facility is not needed, no oxidant is used in the desorption process, molybdenum is easy to recover, the service life of the resin is prolonged, and industrial application is facilitated.

Description

technical field [0001] The invention relates to a method for removing molybdenum from a tungstate solution, in particular to a method of vulcanizing a small amount of molybdenum in a molybdenum-containing tungstate solution through a special vulcanizing agent, and then removing and recovering it through ion exchange, which belongs to the metallurgical technology of rare metals field. Background technique [0002] Tungsten and molybdenum belong to the same subgroup in the periodic table of elements, and due to the contraction of the lanthanide series, the tungsten and molybdenum ions and atomic radii are similar, making the chemical properties of tungsten and molybdenum similar, and it is difficult to separate, so the separation of tungsten and molybdenum has always been tungsten Difficulties in metallurgical processes. The existing separation methods of tungsten and molybdenum include chemical precipitation method, solvent extraction method, ion exchange method and so on. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G41/00
CPCC01G41/003
Inventor 曹佐英杜佳炜李嘉张贵清李青刚曾理关文娟
Owner CENT SOUTH UNIV
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