Gallium nitrate preparation method

A technology of gallium nitrate and nitric acid, applied in chemical instruments and methods, gallium/indium/thallium compounds, inorganic chemistry, etc., can solve problems such as long crystallization time, difficult crystallization, and difficult dissolution, so as to accelerate the speed of product precipitation, The effect of shortening the induction period and shortening the seed precipitation time

Inactive Publication Date: 2006-04-26
GUIZHOU BRANCH CHINA ALUMINUM IND
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  • Abstract
  • Description
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Problems solved by technology

[0004] In the above-mentioned acid-dissolving process, when digallium trioxide is dissolved in concentrated nitric acid at room temperature, it is very difficult to dissolve
Metal gallium reacts with nitric acid at room temperature, and a layer of oxide passivation film is formed on the surface, which will prevent the further reaction of gallium and nitric acid, and it is difficult to dissolve in acid
And above-mentioned method crystallization is comparatively difficult, and crystallization time is longer, and preparation cycle is too long

Method used

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  • Gallium nitrate preparation method

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Embodiment 1

[0014] Dissolve metal gallium in hot concentrated nitric acid at 50°C. After the metal gallium is completely dissolved, evaporate the solution, keep the reaction temperature at 100°C, add water after concentration, repeat concentration and evaporation until there is no smell of nitric acid in the solution, cool the solution until -20°C, add seed crystals at the same time, the weight ratio of the added seed crystals to the weight of gallium nitrate in the solution, that is, the seed crystal coefficient is 0.03, carry out stirring and decomposition of the seeds, and obtain hydrated gallium nitrate crystals after separation, and air-dry at 30°C Within 2 days, using ICP-MS analysis and detection technology, the product quality can reach more than 99.99%.

Embodiment 2

[0016] Dissolve metal gallium in hot concentrated nitric acid at 65°C. After the metal gallium is completely dissolved, evaporate the solution, keep the reaction temperature at about 90°C, control the solution to slightly boil, after concentration, add water, and concentrate until there is no smell of nitric acid in the solution. Cool the solution to 0°C, add seed crystals (the seed crystal coefficient is 0.01) at the same time to stir and decompose the seeds, and obtain hydrated gallium nitrate crystals after separation, air-dry at 40°C for 1 day, use ICP-MS analysis and detection technology, product quality It can reach more than 99.99%.

Embodiment 3

[0018] Use high-purity water and high-purity reagents for raw material preparation, and control the appropriate acid-soluble and crystallization conditions: dissolve metal gallium in hot concentrated nitric acid at 85°C, wait until the metal gallium is completely dissolved, evaporate the solution, maintain the reaction temperature at 80°C, and concentrate Finally, add water, concentrate until there is no nitric acid odor in the solution, cool the solution to -10°C, and add seed crystals (the seed crystal coefficient is 0.05) at the same time to carry out stirring and decomposition of the seeds, and the hydrated gallium nitrate crystals can be obtained after separation. Air-dried at 40°C for 2 days, using ICP-MS analysis and detection technology, the product quality can reach more than 99.99%.

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Abstract

The present invention relates to gallium nitrate preparing process. The preparation process includes: dissolving 6N metal gallium in high purity nitric acid at 50-80 deg.c, evaporating the solution at 80-100 deg.c until no bad smell of nitric acid, cooling the solution to -20 deg.c to 0 deg.c, adding gallium nitrate crystal seed into the solution with the weight ratio between the added gallium nitrate crystal seed and gallium nitrate inside the solution being 0.01-0.1, separating crystal, filtering to separate gallium nitrate crystal hydrate, and air drying to obtain gallium nitrate crystal. Owing to the controlled acid dissolving and separation, the process has shortened acid dissolving time and crystal separating time, effectively raised production efficiency, simple operation and easy embodiment. Owing to the high purity of the material, the product has high purity up to 4N.

Description

technical field [0001] The invention relates to a preparation method of gallium nitrate. Background technique [0002] There are few reports on the preparation process of gallium nitrate. In "Handbook of Synthesis of Inorganic Compounds" (edited by the Chemical Society of Japan, translated by An Jiaju and Chen Zhichuan, Chemical Industry Press, 1986), there are two methods for preparing gallium nitrate disclosed. The first method is to dissolve metal gallium or gallium trioxide in nitric acid, evaporate the solution, and add water after concentration. Repeat this operation until there is no smell of nitric acid in the solution. Then dilute the concentrated solution to contain 26g of gallium in 100ml of solution. From this viscous solution Ga(NO 3 ) 3 ·xH 2 O solid. After suction filtration, let stand for a while. The crystals were dried at room temperature in a dry air stream, and then dried at 40° C. for 2 days to obtain anhydrous matter. [0003] Method 2: dissolv...

Claims

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Application Information

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IPC IPC(8): C01G15/00
Inventor 王熙慧吕子剑吴钢张学英黄健龚斌薛祎姝王钧全玉吕元龙张瑜赵镁翼杨群太陈东郑敏
Owner GUIZHOU BRANCH CHINA ALUMINUM IND
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