Preparation method of ammonium octamolybdate

A technology of ammonium dimolybdate and ammonium molybdate, applied in chemical instruments and methods, molybdenum compounds, inorganic chemistry, etc., can solve problems such as poor operation and operator injury, and achieve complete structure, low energy consumption, and uniform crystal form Effect

Inactive Publication Date: 2007-09-19
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of operation, aqua regia is easy to caus

Method used

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  • Preparation method of ammonium octamolybdate
  • Preparation method of ammonium octamolybdate
  • Preparation method of ammonium octamolybdate

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0047] Example 1

[0048] 1. Prepare the mixed solution

[0049] Take 2.54g ammonium heptamolybdate (NH 4 ) 6 Mo 7 O 24 ·4H 2 O and 2.10 g ammonium dimolybdate (NH 4 ) 2 Mo 2 O 7 Mixing, that is, the molar ratio of ammonium heptamolybdate and ammonium dimolybdate is 1:3, and dissolved in distilled water to a mixed solution of 5.69% ammonium heptamolybdate and 4.70% ammonium dimolybdate by weight.

[0050] 2. Preparation of ammonium dodecamolybdate precursor

[0051] The device containing the mixed solution was fixed in a digital display constant temperature water bath, the reaction temperature was 60 ° C, and 14.53 g of perchloric acid was slowly added under stirring, and the mol ratio of ammonium heptamolybdate, ammonium dimolybdate and perchloric acid was 1 : 3: 70.36, carry out chemical reaction, its ionic reaction equation is as follows:

[0052] Mo 7 O 24 6- +3Mo 2 O 7 2- +10H + =Mo 12 MoO 40 2- +5H 2 O

[0053] A precursor of ammonium dodecamolybdate...

Example Embodiment

[0058] Example 2

[0059] In the process step 1 of preparing the mixed solution, take 2.14 g of ammonium heptamolybdate (NH 4 ) 6 Mo 7 O 24 ·4H 2 O and 1.77g ammonium dimolybdate (NH 4 ) 2 Mo 2 O 7 Mixing, that is, the molar ratio of ammonium heptamolybdate to ammonium dimolybdate is 1:3, and dissolved in distilled water to a mixed solution of 4.87% ammonium heptamolybdate and 4.03% ammonium dimolybdate by weight. In the process step 2 of preparing the ammonium dodecamolybdate precursor, the device containing the mixed solution was fixed in a digital display constant temperature water bath, the reaction temperature was 60°C, and 10.62g of perchloric acid, ammonium heptamolybdate and ammonium heptamolybdate were slowly added under stirring. , the molar ratio of ammonium dimolybdate and perchloric acid is 1:3:61.02 for chemical reaction. The aging time in process step 3 is 1 hour. Other process steps are the same as in Example 1. The scanning electron microscope image...

Example Embodiment

[0060] Example 3

[0061] In the process step 1 of preparing the mixed solution, 3.38 g of ammonium heptamolybdate (NH 4 ) 6 Mo 7 O 24 ·4H 2 O and 2.79 g ammonium dimolybdate (NH 4 ) 2 Mo 2 O 7 Mixing, that is, the molar ratio of ammonium heptamolybdate to ammonium dimolybdate is 1:3, and dissolved in distilled water to a mixed solution with a weight concentration of 7.32% ammonium heptamolybdate and 6.04% ammonium dimolybdate. In the process step 2 of preparing the ammonium dodecamolybdate precursor, the device containing the mixed solution was fixed in a digital display constant temperature water bath, the reaction temperature was 60°C, and 14.16g of perchloric acid, ammonium heptamolybdate and ammonium heptamolybdate were slowly added under stirring. , the molar ratio of ammonium dimolybdate and perchloric acid is 1:3:51.54 for chemical reaction. The aging time in process step 3 is 1 hour. Other process steps are the same as in Example 1. The scanning electron mi...

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Abstract

The present invention relates to a preparation method of dedoammonium molybdate, which comprises the steps of preparing mixted solution, preparing the precursor of dedoammonium molybdate, preparing dedoammonium molybdate and scrubbing and drying. The present invention uses perchloric acid to prepare high purity dedoammonium molybdate at a lower temperature, and overcomes the disadvantage of that the conventional method adopts the strong oxidation and acidity conditions of aqua regia to prepare dedoammonium molybdate. Observing by scanning electron microscopy, the obtained dedoammonium molybdate has even crystal form, complete structure and the typical crystal form of hexagonal bar; testing by X ray diffractometer, the diffraction pattern conforms with the standard X ray diffraction pattern of dedoammonium molybdate, which validates that the obtained product is dedoammonium molybdate crystal. The present invention has the advantages of safe operation, low energy consumption, greatly improved crystallinity and purity.

Description

technical field [0001] The invention belongs to the technical field of ammonium dodecamolybdate, and in particular relates to using perchloric acid instead of aqua regia to provide a strong oxidizing and acidic medium. Background technique [0002] Ammonium molybdate is a type of molybdate composed of ammonium cations and various isopolymolybdate anions, and is one of the molybdenum compounds. The industrial production of metal molybdenum is generally made of ammonium molybdate as raw material. Molybdenum bar is a typical representative of molybdenum products. The quality of its products is closely related to the process conditions and production environment. It is directly related to the structure and performance of molybdenum products such as molybdenum billet and molybdenum wire. The traditional ammonium molybdate, such as ammonium dimolybdate, has the chemical formula (NH 4 ) 2 Mo 2 o 7 , Mo%=56.47%; Ammonium heptamolybdate, chemical formula (NH 4 ) 6 Mo 7 o 24 ...

Claims

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Application Information

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IPC IPC(8): C01G39/00
Inventor 陈亚芍赵丽芳
Owner SHAANXI NORMAL UNIV
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