Green molybdenum smelting ion exchange process

An ion exchange and green technology, applied in the chemical industry, can solve problems such as low recovery rate, easy corrosion of equipment, poor adaptability of raw materials, etc., and achieve the effect of reducing alkali consumption and meeting process requirements

Active Publication Date: 2021-01-05
成都虹波钼业有限责任公司 +1
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Problems solved by technology

[0003] The method for the production of ammonium molybdate by the classic method is a widely used method in China at present. It is characterized by simple equipment, small investment and small processing capacity, but the method has the following disadvantages: (1) The leaching rate of industrial molybdenum oxide is not high during ammonia leaching , the molybdenum in the slag is not easy to recover in this process, resulting in low recovery rate and high cost; (2) the impurity removal effect is poor, and the chemical properties of the product are difficult to meet the national standard requirements; (3) the raw material has poor adaptability and can only be used with high quality (4) The working environment is poor and the equipment is easily corroded; (5) It is difficult to implement automatic control; (6) Environmental protection emissions (such as waste water, waste gas and waste residue, etc.) are difficult to meet the national requirements. During the production process, ammonia leaching consumes a large amount of ammonia, acid precipitation consumes a large amount of nitric acid, and produces a large amount of high-concentration ammonia nitrogen compounds, causing the discharge of ammonia nitrogen to seriously exceed the standard. It is necessary to spend a lot of money to solve the treatment of ammonia nitrogen waste, which is brought by the classic process production. the greatest evil
[0004] The literature on the production of ammonium molybdate by the existing ion exchange method (Chen Zhigang, the author of the paper "Technology Research on the Production of Ammonium Molybdate by Ion Exchange Method") shows that the molybdenum raw material is only a single type of molybdenum calcine with a grade of about 47%. The existing various complex molybdenum raw materials and secondary resources cannot achieve a high level of leaching rate; the key process of ion exchange, the concentration of Mo in the liquid before delivery is lower than 10g / l, and only reaches 8g / l. In other words, every increase of 2g / l in the concentration of liquid Mo before handing over will increase the concentration of liquid Mo after handing in exponentially. Improving the concentration of liquid Mo before handing over will have a strong impact on the direct recovery rate and recovery rate of Mo, and the production efficiency will be greatly reduced; at the same time, the Reducing the Mo concentration of the pre-delivery liquid to 8g / l requires the introduction of a large amount of industrial water for dilution, resulting in a large amount of post-delivery liquid wastewater generated by ion exchange. This process has low production efficiency and is not environmentally friendly.

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0054] The specific implementation steps of this embodiment are as follows:

[0055] 1. Molybdenum calcined sand with a molybdenum grade of 31.4%, according to the molar ratio of the leaching agent required by Mo, 1:1, processing water and sodium carbonate, at a temperature of 90 ° C, compressed air (pressure 0.3 MPa) stirring reaction for 5 hours, carried out The primary filter press, the primary leaching residue contains 14.8% molybdenum, the molybdenum concentration of the filtrate crude sodium molybdate solution is 25.2g / l, P: 0.43g / l, As: 0.34g / l, Si: 0.28g / l. In the following examples, after the initiation of the secondary leaching, this step can use the secondary filtrate (additional leaching agent) to perform primary leaching of the molybdenum raw material.

[0056] 2. The crude sodium molybdate solution is adsorbed by a strong basic anion exchange resin (201 series can be used), the adsorption flow rate is controlled within 3m / h, and the post-transaction liquid contai...

Embodiment 2

[0061] The specific implementation steps of this embodiment are as follows:

[0062] 1. Molybdenum calcine with a molybdenum grade of 31.4% is mixed with the secondary leaching filtrate at a solid-to-liquid ratio of 1:6, and sodium carbonate is added according to the molar ratio of the leaching agent required for Mo at 1:1. At a temperature of 90°C, compressed air (Pressure 0.3MPa) stirring and reacting for 5 hours, performing primary pressure filtration (temperature before pressure filtration is lower than 60° C.), and the primary leaching residue contains 14.8% molybdenum.

[0063] 2. Mix the primary leaching slag obtained in step 1 with the post-transaction liquid obtained by ion exchange adsorption according to the solid-to-liquid ratio of 1:10, and the molar ratio of Mo to leaching agent of 1:4, and add sodium carbonate and sodium hydroxide to make pulp, and react The conditions are: temperature 200°C, oxygen partial pressure 2.0MPa, reaction time 6 hours, secondary leach...

Embodiment 3

[0072] The specific implementation steps of this embodiment are as follows:

[0073] 1. Molybdenum calcined sand with a molybdenum grade of 51.8% is mixed with the secondary leaching filtrate according to the solid-to-liquid ratio of 1:5, and sodium carbonate is added according to the molar ratio of the leaching agent required by Mo at 1:1. At a temperature of 60°C, compressed air (Pressure 0.15MPa) stirring and reacting for 2.5 hours, and carrying out primary pressure filtration, the primary leaching residue contains 5.7% molybdenum.

[0074] 2. The primary leaching slag obtained in step 1 is mixed with sodium carbonate and sodium hydroxide to make pulp according to the solid-to-liquid ratio of 1:5 and the molar ratio of Mo to leaching agent of 1:2 with the ion-exchange adsorption post-transaction liquid, and the reaction The conditions are: temperature 150°C, oxygen partial pressure 1.5MPa, reaction time 3 hours, secondary leaching slag containing 0.18% molybdenum, molybdenu...

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Abstract

The invention discloses a green molybdenum smelting ion exchange process, which adopts mixed alkali two-stage countercurrent leaching to achieve high-level molybdenum metal recovery rate. Zero wastewater is realized through a leaching ion exchange water circulation closed process; post-exchange solution sodium salt extraction is realized through iron exchange, alkali liquor recycling is realized through returning leaching step, and alkali consumption is greatly reduced; the purification and transformation of molybdenum can be synchronously realized by ion exchange adsorption and desorption ofpre-exchange solutions with different Mo concentrations, and various indexes of the obtained ammonium molybdate product meet the highest standard of the national standard.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, in particular to a green molybdenum smelting ion exchange process. Background technique [0002] The raw material for conventional ammonium molybdate production is molybdenite, such as figure 1 As shown, the production process is: molybdenite—roasting—industrial molybdenum oxide—pickling—ammonia leaching—ammonium molybdate solution—magnesium chloride impurity removal—ammonia sulfide impurity removal—acid precipitation— Ammonium tetramolybdate - ammonia solution - evaporation crystallization - ammonium dimolybdate. [0003] The method for the production of ammonium molybdate by the classic method is a widely used method in China at present. It is characterized by simple equipment, small investment and small processing capacity, but the method has the following disadvantages: (1) The leaching rate of industrial molybdenum oxide is not high during ammonia leaching , the molybdenum in the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/00
CPCC01G39/003
Inventor 刘锦锐任倩杨伟高志强易建罗石华刘阳陈炜尹华林
Owner 成都虹波钼业有限责任公司
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