Method for preparing high pure ammonium paramolybdate

A technology of pure ammonium paramolybdate and ammonium paramolybdate, which is applied in the field of preparation of high-purity ammonium paramolybdate, can solve the problems of difficulty in meeting the requirements of the development of the electronics industry, long time, reducing the purity of ammonium paramolybdate products, etc. The effect of stirring time, reducing liquid-solid ratio, and shortening crystallization time

Inactive Publication Date: 2005-03-02
ZHUZHOU HARD ALLOY GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Since the liquid-solid ratio of ammonium polymolybdate is relatively large when it is dissolved in ammonium polymolybdate, it takes a long time for evaporation and crystallization. This will cause some impurities, such as iron, to be brought into ammonium paramolybdate due to long-term stirring in the stainless steel tank, reducing the The purity of ammonium paramolybdate products generally can only reach the second level of the national standard (GB3460-82), which is difficult to meet the requirements of the development of the electronics industry

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1: get 1000kg ammonium polymolybdate, technical condition meets national standard two grades, by ammonium polymolybdate (kg): pure water (l): ammoniacal liquor (l)=1: 0.23: 0.6 adds to stainless steel dissolution crystallization tank Pure water 2301, ammonia water 6001, heated to 60°C, to dissolve ammonium polymolybdate, after ammonia dissolved (NH 4 ) 2 MoO 4 The solution density is 1.60g / cm 3 . Evaporation and crystallization were carried out under the condition of constant stirring, and the vapor pressure was kept at 0.1-0.15Mpa to keep the solution in the tank boiling. At the same time, 50g of EDTA was added, and the concentration time was 45 minutes. The measured crystallization mother liquor density was 1.26g / cm 3 Quickly discharge, drain, and centrifuge. The separated ammonium paramolybdate is baked at a temperature of ≤100°C for 4 hours until the water in the ammonium paramolybdate is reduced to 1.0g / cm 3 Below, can make high-purity ammonium para...

Embodiment 2

[0019] Embodiment 2: get 1000kg ammonium polymolybdate, technical condition meets national standard two grades, adds in stainless steel dissolving tank by ammonium polymolybdate (kg): pure water (l): ammoniacal liquor (l)=1: 0.22: 0.6 220l of pure water, 600l of ammonia water, heated to 60°C, dissolving ammonium polymolybdate, after ammonia dissolved (NH 4 ) 2 MoO 4 The solution density is 1.62g / cm 3 . Evaporate and crystallize under constant stirring, keep the vapor pressure at 0.1-0.15MPa to keep the solution in the tank boiling, add 100g of EDTA at the same time, concentrate for 48 minutes, and measure the density of the crystallization mother liquor to be 1.25g / cm 3 Timely discharge, drain, and centrifuge. The separated ammonium paramolybdate is baked for 3 to 4 hours at a temperature of ≤100°C until the water in the ammonium paramolybdate is reduced to 0.85g / cm 3 , can make high-purity ammonium paramolybdate 955kg, crystallization rate reaches 95.5%, and its quality ...

Embodiment 3

[0021] Embodiment 3: get 1000kg ammonium polymolybdate, technical condition meets national standard two grades, adds in stainless steel dissolving tank by ammonium polymolybdate (kg): pure water (l): ammoniacal liquor (l)=1: 0.20: 0.6 200l of pure water, 600l of ammonia water, heated to 60°C, dissolving ammonium polymolybdate, after ammonia dissolved (NH 4 ) 2 MoO 4 The solution density is 1.63g / cm 3 . Evaporate and crystallize under the condition of constant stirring, keep the steam pressure 0.1-0.15Mpa, to keep the solution in the tank boiling, add 120g of EDTA at the same time, the concentration time is 48 minutes, and the measured crystallization mother liquor density is 1.24g / cm 3 Timely discharge, drain, and centrifuge. The separated ammonium paramolybdate is baked for 3 to 4 hours at a temperature of ≤100°C until the water in the ammonium paramolybdate is reduced to 3 , can make high-purity ammonium paramolybdate 956kg, crystallization rate reaches 95.6%, and its qu...

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Abstract

A process for preparing high-purity ammonium paramolybdate from ammonium polymolybdate as raw material includes adding purified water and ammonia water, heating while stirring, stirring under a certain steam pressure for evaporation crystallizing while boiling the solution, concentrating, solid-liquid separation, and baking. Its advantages are high purity and high crystallizing rate (94.5-96%.

Description

Technical field: [0001] The invention relates to a preparation method of high-purity ammonium paramolybdate, in particular to a preparation method of high-purity ammonium paramolybdate required for the production of molybdenum powder and molybdenum alloy. Background technique: [0002] Ammonium paramolybdate can be used to prepare MoO 3 And Mo powder, and then can be processed into aluminum bars, molybdenum electrodes, molybdenum plugs, molybdenum slabs, molybdenum wire, aluminum foil and other molybdenum alloy products, widely used in steel, metal pressure processing, electric light source, electric vacuum, metallurgy, aerospace and military industry and other fields. [0003] At present, the industrial preparation of ammonium paramolybdate mainly adopts the method of dissolving ammonium polymolybdate in ammonia water and recrystallization, that is, ammonium polymolybdate is first dissolved in ammonia in a stainless steel stirring tank, and the reaction formula is [0004...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D9/00C01G39/00
Inventor 申友元吴国根陈和平黄广华李玉清李正林
Owner ZHUZHOU HARD ALLOY GRP CO LTD
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