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Preparation method of ammonium heptamolybdate

A technology of ammonium heptamolybdate and ammonium molybdate, applied in the field of ammonium heptamolybdate preparation

Pending Publication Date: 2021-05-07
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above-mentioned preparation method uses nitric acid to produce a large amount of ammonium nitrate waste water in the process of preparing ammonium tetramolybdate, which needs to be deaminated by adding alkali, and sodium nitrate by-product is generated by evaporation and desalination, so that the environmental protection can reach the standard

Method used

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  • Preparation method of ammonium heptamolybdate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] The preparation method of ammonium heptamolybdate, comprises the following steps:

[0050] (1) Molybdenum calcine water elution of nitrate

[0051] The molybdenum calcine in this example was purchased from Jiangxi Copper Co., Ltd. Dexing Copper Mine, and the molybdenum calcine was acid-washed molybdenum calcine with nitric acid. Therefore, the acid-washed molybdenum calcine contained a certain amount of nitrate (~0.5%). If the acid-washed molybdenum calcine is directly subjected to alkaline oxygen pressure leaching, nitrate radicals will enter the leaching solution, and nitrate radicals will gradually reduce the organic phase extraction capacity of alkaline extraction. root. The slurry is mixed and washed in a steel stirring reaction kettle, and then multi-stage countercurrent washing is carried out by an automatic diaphragm box filter press until the nitrate content in the molybdenum calcine is less than 0.01%. The out-of-stock molybdenum calcine enters the alkaline ...

Embodiment 2

[0078] The preparation method of ammonium heptamolybdate, comprises the following steps:

[0079] (1) Molybdenum calcine water elution of nitrate

[0080] The molybdenum calcine in this example was purchased from Jiangxi Copper Co., Ltd. Dexing Copper Mine, and the molybdenum calcine was acid-washed molybdenum calcine with nitric acid. Therefore, the acid-washed molybdenum calcine contained a certain amount of nitrate (~0.5%). If the acid-washed molybdenum calcine is directly subjected to alkaline oxygen pressure leaching, nitrate radicals will enter the leaching solution, and nitrate radicals will gradually reduce the organic phase extraction capacity of alkaline extraction. root. The slurry is mixed and washed in a steel stirring reaction kettle, and then multi-stage countercurrent washing is carried out by an automatic diaphragm box filter press until the nitrate content in the molybdenum calcine is less than 0.01%. The out-of-stock molybdenum calcine enters the alkaline ...

Embodiment 3

[0093] The preparation method of ammonium heptamolybdate, comprises the following steps:

[0094] (1) Molybdenum calcine water elution of nitrate

[0095] The molybdenum calcine in this example was purchased from Jiangxi Copper Co., Ltd. Dexing Copper Mine, and the molybdenum calcine was acid-washed molybdenum calcine with nitric acid. Therefore, the acid-washed molybdenum calcine contained a certain amount of nitrate (~0.5%). If the acid-washed molybdenum calcine is directly subjected to alkaline oxygen pressure leaching, nitrate radicals will enter the leaching solution, and nitrate radicals will gradually reduce the organic phase extraction capacity of alkaline extraction. root. The slurry is mixed and washed in a steel stirring reaction kettle, and then multi-stage countercurrent washing is carried out by an automatic diaphragm box filter press until the nitrate content in the molybdenum calcine is less than 0.01%. The out-of-stock molybdenum calcine enters the alkaline ...

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Abstract

The invention discloses a preparation method of ammonium heptamolybdate, and relates to the technical field of ammonium heptamolybdate. The preparation method comprises the following steps: (1) mixing molybdenum calcine with a leaching agent, adjusting the pH value to 10-11.5, and keeping the temperature for 2-3 hours under the conditions that the oxygen partial pressure is 0.5-2 MPa and the temperature is 100-220 DEG C to obtain a sodium molybdate solution; (2) adding quaternary ammonium salt into the ammonium molybdate solution obtained in the step (1), extracting molybdenum under an alkaline condition, and then adding ammonium bicarbonate into an extracting solution to obtain an ammonium molybdate solution; (3) carrying out intermittent negative pressure evaporative crystallization on the ammonium molybdate solution under the conditions that the negative pressure is -0.08 to-0.1 MPa and the temperature is 60-75 DEG C to obtain wet ammonium heptamolybdate, and then performing drying to obtain the ammonium heptamolybdate. The method has the beneficial effects that the process is simple, and the recovery rate is high; the whole process is free of acidification, ammonia-nitrogen wastewater discharge is reduced, the process flow is obviously shortened, the cost is reduced, and industrial production is easy to realize.

Description

technical field [0001] The invention relates to the technical field of ammonium heptamolybdate, in particular to a preparation method of ammonium heptamolybdate. Background technique [0002] Ammonium heptamolybdate is mainly used in chemical and petroleum industries and fields such as flowering season, dyes, pigments and micro-fertilizers, and is one of the important molybdates. At present, the production of ammonium heptamolybdate generally uses ammonium tetramolybdate as the raw material. The two-step method is used to prepare ammonium heptamolybdate. The ammonium molybdate solution is added with nitric acid to obtain ammonium tetramolybdate, and the ammonium tetramolybdate is dissolved in ammonia water at 60-80 °C The concentration is 1.42-1.48g / m 3 The ammonium molybdate solution was filtered while hot, crystallized by cooling, centrifugally dehydrated, dried, and screened to obtain the finished product of ammonium heptamolybdate. The preparation process is as follows:...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/00
CPCC01G39/003
Inventor 徐鸿飞徐尊平江来高
Owner CENT SOUTH UNIV
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