Method for preparing high-purity ammonium tetramolybdate mainly by using ammonium molybdate transformation process

A technology of ammonium tetramolybdate and ammonium molybdate, applied in chemical instruments and methods, molybdenum compounds, inorganic chemistry, etc., to achieve the effects of small total loss, reduced production cost, and stable product quality

Inactive Publication Date: 2012-01-25
西部鑫兴金属材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods have many advantages, but there are many deficiencies in the purification process and purification effect. Therefore, there is no ammonium molybdate purification and impurity removal method that can obtain ammonium tetramolybdate with a purity of ≥99.998%.

Method used

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  • Method for preparing high-purity ammonium tetramolybdate mainly by using ammonium molybdate transformation process
  • Method for preparing high-purity ammonium tetramolybdate mainly by using ammonium molybdate transformation process
  • Method for preparing high-purity ammonium tetramolybdate mainly by using ammonium molybdate transformation process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Weigh 300g of the raw material ammonium tetramolybdate, the quality of W in the raw material ammonium tetramolybdate is 40μg / g, put it into a reactor with a heating mantle and a stirring device filled with 300mL industrial pure water, and gradually add 150mL concentrated Ammonia, mixed solution 1 is obtained after stirring and dissolving completely, and the density of mixed solution 1 is adjusted to 1.36g / cm with pure water 3 , and filtered to remove the solid mechanical impurities contained in the mixed solution 1 to obtain the filtrate 1.

[0027] Under constant stirring at room temperature, the pH value of the filtrate 1 was adjusted to 7.2 with concentrated nitric acid, and 6 g of FeCl 3 The solid powder was added to filtrate 1, stirred at room temperature for 2 h, and filtered to obtain filtrate 2.

[0028] Evaporate and crystallize the filtrate 2, and filter after evaporating 1 / 3 of its total volume to obtain crystals to obtain the filtrate 3 and filter cake 1, w...

Embodiment 2

[0039]Weigh 600g of raw material ammonium tetramolybdate, the quality of W in the raw material ammonium tetramolybdate is 30μg / g, put it into a reactor with heating mantle and stirring device filled with 630mL industrial pure water, add 300mL concentrated Ammonia, mixed solution 1 is obtained after stirring and dissolving completely, and the density of mixed solution 1 is adjusted to 1.38g / cm with pure water 3 , and filtered to remove the solid mechanical impurities contained in the mixed solution 1 to obtain the filtrate 1.

[0040] Under constant stirring at room temperature, the pH value of filtrate 1 was adjusted to 7.5 with concentrated nitric acid, and 14.5g FeCl 3 The solid powder was added to filtrate 1, stirred at room temperature for 2.5 h, and filtered to obtain filtrate 2.

[0041] Evaporate and crystallize the filtrate 2, and filter after evaporating 1 / 3 of its total volume to obtain crystals to obtain the filtrate 3 and filter cake 1, wherein the filter cake 1 i...

Embodiment 3

[0052] Weigh 900g of the raw material ammonium tetramolybdate, the quality of W in the raw material ammonium tetramolybdate is 50μg / g, put it into a reactor with a heating mantle and a stirring device filled with 990mL industrial pure water, and gradually add 450mL of it under stirring at room temperature Concentrated ammonia water, stir and dissolve completely to obtain mixed solution 1, adjust the density of mixed solution 1 to 1.40g / cm with pure water 3 , and filtered to remove the solid mechanical impurities contained in the mixed solution 1 to obtain the filtrate 1.

[0053] Under constant stirring at room temperature, the pH value of filtrate 1 was adjusted to 7.8 with concentrated nitric acid, and 45g FeCl 3 The solid powder was added to filtrate 1, stirred at room temperature for 3 h, and filtered to obtain filtrate 2.

[0054] Evaporate and crystallize the filtrate 2, and filter after evaporating 1 / 3 of its total volume to obtain crystals to obtain the filtrate 3 and...

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Abstract

The invention relates to a method for preparing high-purity ammonium tetramolybdate, which comprises the steps of: mixing raw ammonium tetramolybdate with pure water and concentrated ammonia water to dissolve the raw ammonium tetramolybdate, then using pure water to adjust density and filtering to obtain filtrate 1; using concentrated nitric acid to adjust the density of the filtrate 1 at room temperature, then adding FeCl3, agitating and filtering to obtain filtrate 2; conducting evaporation and crystallization and filtering to obtain filtrate 3 and a filter cake 1; after the filtrate 3 is cooled, filtering to obtain a filter cake 2; after the filter cake 1 and the filter cake 2 are mixed with pure water, are agitated and are dissolved, adding concentrated nitric acid to obtain solution with H+ concentration being 3-8 mol / L, agitating, heating, preserving heat, cooling and filtering to obtain a filter cake 3, and using nitric acid aqueous solution to wash the filter cake 3 to obtain ammonium dodecamolybdate; adding pure water and concentrated ammonia water to mix and dissolve, heating, evaporating, regulating pH, cooling and then using pure water to adjust density; and adding concentrate nitric acid to regulate pH, agitating, heating, preserving heat, filtering to obtain a filter cake 4, washing the filter cake 4 and drying the filter cake 4 to an extent with the water content being less than or equal to 1.0g / cm<3> to obtain ammonium tetramolybdate with the purity being more than or equal to 99.998 percent. Therefore, the content of impurities in the raw ammonium tetramolybdate is effectively reduced.

Description

technical field [0001] The present invention relates to a method for preparing high-purity ammonium tetramolybdate mainly by ammonium molybdate transformation process, in particular, it relates to a method for further removing impurities by mainly using ammonium molybdate transformation process to prepare ammonium tetramolybdate with a purity ≥ 99.998 % of the preparation method of ammonium tetramolybdate. Background technique [0002] Molybdenum is a refractory metal with high boiling point and high melting point. It has good thermal conductivity and electrical conductivity, low thermal expansion coefficient, excellent wear resistance and corrosion resistance. It is widely used in aerospace, energy and power, micro Electronics, VLSI components, biomedicine, machining, medical equipment, lighting, glass fiber, and national defense construction. Ammonium molybdate is the primary raw material for preparing metal molybdenum powder and various alloys of molybdenum. Ammonium mol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/00
Inventor 冯宝奇白宏斌马高峰王子川王炳旭郭金亮谢亚宁雷宁董永王伟薛丽颖
Owner 西部鑫兴金属材料有限公司
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