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Preparation method of high-purity ammonium fluoroberyllate and application thereof

Ammonium fluoroberyllate, high-purity technology, applied in chemical instruments and methods, beryllium compounds, inorganic chemistry, etc., can solve problems such as inconsistent metal impurity ion content, unavoidable sulfate ion, etc.

Active Publication Date: 2014-02-26
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Usually, the raw material beryllium hydroxide used to prepare beryllium fluoride is prepared from beryllium ore by sulfuric acid leaching process, which inevitably contains a large amount of sulfate ions (analysis results show that the sulfate ion content in industrial beryllium hydroxide More than 2000ppm), resulting in beryllium fluoride prepared by conventional methods using industrial beryllium hydroxide as raw material also contains a large amount of sulfate ions, and the content of various metal impurity ions does not meet the requirements of molten salt preparation

Method used

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Examples

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Effect test

preparation example Construction

[0067] Preparation of ammonium fluoroberyllate

[0068] The invention uses industrial grade beryllium hydroxide as raw material. First, a mixed suspension of beryllium hydroxide and water is provided, hydrofluoric acid is slowly added dropwise into the mixed suspension, the turbidity in the mixed suspension gradually disappears, and a transparent solution is formed. At this time, the pH value of the detection solution is about 2 to 3, and the reaction of beryllium hydroxide is complete. Then add ammonia water dropwise to the transparent solution until a precipitate occurs in the transparent solution to form a precipitate suspension. The above-mentioned precipitate is non-high-purity ammonium fluoroberyllate, and the precipitate is used as the recrystallization raw material in the purification step.

[0069] The beryllium hydroxide used as raw material in the present invention can be selected as industrial-grade beryllium hydroxide commonly used as a chemical raw material, an...

Embodiment 1

[0101] The preparation of embodiment 1 ammonium fluoroberyllate

[0102]It uses industrial beryllium hydroxide (98%), hydrofluoric acid (42%), and ammonia water (25%) as raw materials. Take 100g of beryllium hydroxide and place it in 400mL of deionized water to form a suspension. Slowly add hydrofluoric acid dropwise to the suspension to adjust the pH value to 2-3, at this time the suspension gradually becomes a transparent solution. Slowly add ammonia water dropwise to the transparent solution to adjust the pH value to 8-9, and at this time, white flocculent precipitates appear in the solution. The precipitate was suction filtered, washed with ethanol, and dried in a box-type atmosphere furnace at 120°C. The resulting precipitate weighed 158 g.

Embodiment 2

[0103] Embodiment 2 Preparation of high-purity ammonium fluoroberyllate (No.1)

[0104] Weigh 50 g of the precipitate, stir and dissolve it with 75 mL of deionized water in a heating water bath at 90° C., and stop stirring until the precipitate is fully dissolved. The solution was left to stand, and the cooling device control program was manually set to slowly cool down. After cooling to room temperature, a large amount of white precipitates precipitated out. Continue cooling in an ice-water bath, and precipitation increases. The precipitated precipitate was suction-filtered, washed with ethanol, and dried at 120°C to obtain a recrystallized product. The primary recrystallized product was stirred and dissolved with 75 mL of deionized water in a heating water bath at 90° C., and the stirring was stopped after the precipitate was fully dissolved. The solution was left to stand, and the cooling device control program was manually set to slowly cool down. After cooling to room...

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Abstract

The invention provides a preparation method of high-purity ammonium fluoroberyllate and application thereof, and in particular relates to a method of preparing high-purity ammonium fluoroberyllate; purity of the high-purity ammonium fluoroberyllate is greater than 99.95%, and the method comprises the following steps: (i), providing a mixture a of beryllium hydroxide and water; (ii), adding hydrofluoric acid into the mixture a to form a transparent mixture b; (iii), adding ammonia water into the transparent mixture b to form a mixture c containing precipitates; and (iv), carrying out recrystallization for at least twice onto the precipitates to obtain a recrystallization product, i.e., the high-purity ammonium fluoroberyllate. According to the preparation method disclosed by the invention, material requirements are low, preparation needs can be satisfied by only needing industrial beryllium hydroxide; and moreover, the obtained product contains extremely few impurities, and therefore, the preparation method can be conveniently applied to preparing the high-purity ammonium fluoroberyllate.

Description

technical field [0001] The invention belongs to the fields of nuclear energy industry technology and chemical technology, and in particular relates to a high-purity ammonium fluoroberyllate for preparing a beryllium fluoride intermediate and a preparation method thereof. Background technique [0002] Molten Salt Reactor (Molten Salt Reactor, MSR) is a reactor that uses molten salt dissolved in fissile material and in a molten state as nuclear fuel. It is a reactor commonly used in nuclear power generation technology. The molten salt nuclear reactor is a liquid nuclear fuel obtained by directly dissolving nuclear fuel into molten salt in a molten state. Molten salt nuclear reactor has many advantages such as extremely high neutron economy, high power density, inherent load control, large negative temperature coefficient, high conversion ratio, high reliability, low fuel combination consumption, and value-added. At the International Symposium on Generation IV Nuclear Reactors...

Claims

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Application Information

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IPC IPC(8): C01F3/00
Inventor 肖吉昌宗国强陈伟李晓东陈博张龙王正能
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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