Short-flow preparation method of rare earth doped modified ammonium paratungstate powder

A kind of ammonium paratungstate, rare earth doping technology, applied in chemical instruments and methods, tungsten compounds, inorganic chemistry, etc., can solve the problems of APT particle size is not uniform, lengthy process, labor-intensive, etc., to inhibit the growth of APT particles, shorten Process flow, the effect of reducing labor intensity

Active Publication Date: 2018-12-18
INST OF APPLIED PHYSICS JIANGXI ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high pressure required for the decomposition reaction, usually 8 to 18 atmospheres, there are major safety hazards, and the process is a single-pot intermittent operation, with high labor intensity, harsh working environment, and low production efficiency.
Since these two processes are to obtain the crude sodium tungstate solution first, and then divide the impurities in multiple passes, then convert the sodium tungstate solution int

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0037] Example 1

[0038] Put 300g of scheelite concentrate powder, 0.7g of yttrium nitrate powder, and 0.7g of lanthanum nitrate powder into a planetary ball mill for wet grinding for 4 hours, put it into a boat, and put the boat into a vacuum drying box at 80 °C for heating and drying for 2 hours. Put the mixed powder into the polytetrafluoroethylene reaction kettle, and then pour 338.5ml of hydrochloric acid with a concentration of 31-38% preheated in the constant temperature water bath into the reaction kettle, stir until fully mixed, and tighten the upper cover of the kettle body. Put it into a homogeneous reactor, the temperature of the homogeneous reactor is set to 80 °C, and the reaction time is 1 h. During the reaction process, the mixture is continuously stirred, and the stirring speed is 60 rad / min. After the reaction is completed, the stirring is stopped, and the residual temperature is used to make The solution was allowed to stand for 0.5h at not lower than 60°C,

Example Embodiment

[0039] Example 2

[0040] Put 300g of scheelite concentrate powder, 6.8g of yttrium nitrate powder, and 34.1g of lanthanum nitrate powder into a planetary ball mill for wet grinding for 6 hours, put them into a boat, and put the boat into a vacuum drying box at 90 °C for heating and drying for 3 hours. Put the mixed powder into the polytetrafluoroethylene reaction kettle, then pour 300ml of preheated concentrated hydrochloric acid in the constant temperature water bath into the reaction kettle, stir until fully mixed, tighten the upper cover of the kettle body, and put it into the homogeneous reactor, The temperature of the homogeneous reactor was set to 90°C, and the reaction time was 2h. During the reaction, the mixture was continuously stirred, and the stirring speed was 70 rad / min. After the reaction was completed, the stirring was stopped, and the residual temperature was used to make the solution no lower than 60°C. Let stand for 2 hours, discard the upper layer waste liq

Example Embodiment

[0041] Example 3

[0042] Put 300g of scheelite concentrate powder, 5.5g of yttrium nitrate powder and 6.2g of lanthanum nitrate powder into a planetary ball mill for wet grinding for 12 hours, put them into a boat, put the boat into a vacuum drying box and heat and dry at 100 °C for 4 hours. Put the mixed powder into the polytetrafluoroethylene reaction kettle, then pour 389.5ml of preheated concentrated hydrochloric acid in the constant temperature water bath into the reaction kettle, stir until fully mixed, tighten the upper cover of the kettle body, and put it into the homogeneous reactor , the temperature of the homogeneous reactor is set to 120 ° C, the reaction time is 3 h, the mixture is continuously stirred during the reaction, and the stirring speed is 70 rad / min. Let stand at ℃ for 2h, pour out the upper layer waste liquid, pour the obtained crude tungstic acid into a polytetrafluoroethylene reaction kettle, add 1503.3ml of ammonia water with a concentration of 28.0-

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PUM

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Abstract

The invention provides a short-flow preparation method of rare earth doped modified ammonium paratungstate (APT) powder. The short-flow preparation method comprises ammonia dissolving treatment of crude tungstic acid and crystallization of an ammonium tungstate solution. According to the method, yttrium nitrate powder and lanthanum nitrate powder are added into scheelite concentrate powder, and the powder is subjected to efficient wet grinding to obtain mixed powder, so that the scheelite concentrate powder is refined and homogenized; the mixed powder is treated by adopting concentrated hydrochloric acid to obtain crude tungstic acid particles. The method comprises the following steps: (1) mixing materials; carrying out wet grinding on the yttrium nitrate powder, the lanthanum nitrate powder and the scheelite concentrate powder, and mixing to prepare the mixed powder; (2) drying the mixed powder; (3) preparing the crude tungstic acid; (4) preparing an ammonium tungstate solution; (5) evaporating and crystallizing ammonium tungstate. According to the short-flow preparation method provided by the invention, two rare earth elements including yttrium and lanthanum are compounded and added into the scheelite concentrate powder in a soluble rare earth nitrate form and are not independently added, and a synergistic effect is formed; compared with APT powder obtained by a traditional acid decomposition technology, the APT powder prepared by the method has the advantages that the particles are smaller, the grain diameter distribution is more uniform and the dispersity is more excellent.

Description

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Claims

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Application Information

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Owner INST OF APPLIED PHYSICS JIANGXI ACADEMY OF SCI
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