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A method for separating and purifying ammonium paratungstate in ammonium tungstate solution

A technology of ammonium paratungstate and ammonium tungstate, applied in the field of separation of ammonium paratungstate, can solve the problems of many impurities, large particle size and low purity in ammonium paratungstate products, and achieve the effect of improving crystallization effect, uniform particle size and improving purity

Active Publication Date: 2017-07-28
NANCHANG HANGKONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the ammonium paratungstate (APT) production process, the WO in the APT crystallization mother liquor (ammonium tungstate solution) 3 The content generally accounts for 5% to 15% of the whole process. In addition, it also contains impurities such as Mo, P, and As. The ammonium paratungstate products obtained by existing crystallization have more impurities, low purity, and large particle size.

Method used

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  • A method for separating and purifying ammonium paratungstate in ammonium tungstate solution
  • A method for separating and purifying ammonium paratungstate in ammonium tungstate solution

Examples

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Effect test

Embodiment 1

[0021] A method for separating and purifying ammonium paratungstate in ammonium tungstate solution, the specific steps are:

[0022] (1) Put the ammonium tungstate solution in an open container and place it in a dark place, and at the same time pass nitrogen into the solution, keep it for 8 hours and then filter to obtain the filtrate;

[0023] (2) Add the composite active reagent to the filtrate, the mass ratio of the filtrate and the composite active reagent is 10:1.3, heat it in a water bath to 70° C., and stir for 50 minutes to obtain a composite solution;

[0024] (3) Cool down the composite solution after stirring, stir with a graphite stirring rod while cooling down, the rotating speed is 50r / min, cool down to 40°C and keep for 30 minutes, precipitate crystals, filter to obtain crystal a and filtrate a;

[0025] (4) Continue to cool the filtrate a to 20°C, keep it for 10 minutes, precipitate crystals, filter to obtain crystals b;

[0026] (5) Combine crystal a and crys...

Embodiment 2

[0032] A method for separating and purifying ammonium paratungstate in ammonium tungstate solution, the specific steps are:

[0033] (1) Put the ammonium tungstate solution in an open container and place it in a dark place, and at the same time pass nitrogen into the solution, keep it for 9 hours and then filter to obtain the filtrate;

[0034] (2) Add the composite active reagent to the filtrate, the mass ratio of the filtrate to the composite active reagent is 10:1.5, heat it in a water bath to 75° C., and stir for 60 minutes to obtain a composite solution;

[0035] (3) After stirring, cool down the composite solution, stir with a graphite stirring rod while cooling down, the rotating speed is 100r / min, cool down to 45°C and keep for 40 minutes, precipitate crystals, filter to obtain crystal a and filtrate a;

[0036] (4) Continue to cool the filtrate a to 25° C., keep it for 20 minutes, precipitate crystals, filter to obtain crystal b;

[0037] (5) Combine crystal a and cr...

Embodiment 3

[0041] A method for separating and purifying ammonium paratungstate in ammonium tungstate solution, the specific steps are:

[0042] (1) Put the ammonium tungstate solution in an open container and place it in a dark place, and at the same time pass nitrogen into the solution, keep it for 9 hours and then filter to obtain the filtrate;

[0043] (2) Add the composite active reagent to the filtrate, the mass ratio of the filtrate to the composite active reagent is 10:1.6, heat the water bath to 70° C., and stir for 70 minutes to obtain a composite solution;

[0044] (3) Cool down the composite solution after stirring, stir with a graphite stirring rod while cooling down, the rotating speed is 80r / min, cool down to 50°C and keep for 40 minutes, precipitate crystals, filter to obtain crystal a and filtrate a;

[0045] (4) Continue to cool the filtrate a to 25° C., keep it for 20 minutes, precipitate crystals, filter to obtain crystal b;

[0046] (5) Combine crystal a and crystal ...

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Abstract

The invention discloses a method for separating and purifying ammonium paratungstate in an ammonium tungstate solution. The ammonium tungstate solution is fed with nitrogen gas for pretreatment, then a composite active reagent is added, stirred with a graphite stirring rod, and the temperature is lowered in stages to obtain ammonium paratungstate The crystal has high purity, small particle size, regular hexahedral crystal structure, less impurities such as WO3, Mo, As, etc., and has significant social and economic benefits.

Description

technical field [0001] The invention relates to a method for separating ammonium paratungstate, in particular to a method for separating and purifying ammonium paratungstate in an ammonium tungstate solution. Background technique [0002] Ammonium paratungstate (APT) is an important intermediate compound for the production of tungsten powder, tungsten wire, tungsten-based alloy and all tungsten materials, and it is also a bulk export commodity in my country. Due to the genetic relationship, the crystal characteristics of APT, such as crystal morphology, lattice parameters, average particle size and particle size distribution, bulk specific gravity and fluidity, have a great influence on the material properties of subsequent powder metallurgy products tungsten powder, tungsten wire and tungsten alloy, so The development of high-performance tungsten materials has put forward higher and higher requirements on the characteristics of the crystallized product from solution, that i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G41/00
CPCC01G41/00C01P2004/61C01P2006/80
Inventor 曾桂生罗胜联肖民罗旭彪隋幸桢关乾黄盛魏栖梧
Owner NANCHANG HANGKONG UNIVERSITY