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: 2009-07-01
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 cause injury to the operator, and it is not easy to operate

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

Embodiment 1

[0048] 1. Prepare mixed solution

[0049] Get 2.54g ammonium heptamolybdate (NH 4 ) 6 Mo 7 o 24 4H 2 O and 2.10g 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 with a weight concentration of 5.69% ammonium heptamolybdate and 4.70% ammonium dimolybdate.

[0050] 2. Preparation of ammonium dodecamolybdate precursor

[0051] Fix the device with the mixed solution in a digital constant temperature water bath, the reaction temperature is 60°C, slowly add 14.53g perchloric acid under stirring, the molar ratio of ammonium heptamolybdate, ammonium dimolybdate and perchloric acid is 1 :3:70.36, carry out chemical reaction, its ion 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] Generate ammonium dodecamolybdate precursor.

[0054] 3. Preparation of ammonium dodecamoly...

Embodiment 2

[0059] In preparation mixed solution process step 1, get 2.14g ammonium heptamolybdate (NH 4 ) 6 Mo 7 o 24 4H 2 O and 1.77g ammonium dialuminate (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 with a weight concentration of 4.87% ammonium heptamolybdate and 4.03% ammonium dimolybdate. In step 2 of the process for preparing the ammonium dodecamolybdate precursor, the device containing the mixed solution is fixed in a digital display constant temperature water bath, the reaction temperature is 60°C, and 10.62g of perchloric acid and ammonium heptamolybdate are slowly added under stirring. , ammonium dimolybdate, and perchloric acid in a molar ratio of 1:3:61.02 for chemical reaction. The aging time in process step 3 is 1 hour. Other processing steps are identical with embodiment 1. The scanning electron microscope picture of prepared ammonium dodecamolyb...

Embodiment 3

[0061] In preparation mixed solution process step 1, get 3.38g ammonium heptamolybdate (NH 4 ) 6 Mo 7 o 24 4H 2 O and 2.79g 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 with a weight concentration of 7.32% ammonium heptamolybdate and 6.04% ammonium dimolybdate. In step 2 of the process for preparing the ammonium dodecamolybdate precursor, the device containing the mixed liquid is fixed in a digital display constant temperature water bath, the reaction temperature is 60°C, and 14.16g of perchloric acid and ammonium heptamolybdate are slowly added under stirring. , ammonium dimolybdate, and perchloric acid in a molar ratio of 1:3:51.54 for chemical reaction. The aging time in process step 3 is 1 hour. Other processing steps are identical with embodiment 1. The scanning electron microscope picture of prepared ammonium dodecamolybda...

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PUM

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Abstract

A method for preparing ammonium dodecamolybdate, comprising the steps of preparing a mixed solution, preparing an ammonium dodecanolybdate precursor, preparing ammonium dodecamolybdate, and washing and drying. The invention overcomes the disadvantages of the traditional method for preparing ammonium dodecamolybdate by using aqua regia to provide strong oxidation and acidic conditions, and prepares high-purity ammonium dodecamolybdate by using perchloric acid at a relatively low temperature. The prepared ammonium dodecamolybdate was observed with a scanning electron microscope. The crystal form was uniform and the structure was complete. It had a typical hexagonal rod-shaped crystal form of ammonium dodecamolybdate. It was tested with an X-ray diffractometer. The X-ray diffraction patterns are consistent and belong to ammonium dodecyl molybdate crystals. The invention has the advantages of safe operation, less energy consumption, can significantly improve the crystallinity and purity of the ammonium dodecamolybdate, and can be used for preparing the ammonium dodecamolybdate.

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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Patent Type & Authority Patents(China)
IPC IPC(8): C01G39/00
Inventor 陈亚芍赵丽芳
Owner SHAANXI NORMAL UNIV
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