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Preparation method of gallium trichloride granules

A technology of gallium trichloride and particles, applied in chemical instruments and methods, inorganic chemistry, gallium/indium/thallium compounds, etc., can solve the problem of easy adhesion on the container wall, poor control of the addition amount, inconvenient operation, etc. problems, to achieve the effect of cheap raw materials, convenient operation, and guaranteed purity

Inactive Publication Date: 2016-07-06
清远先导材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the poor fluidity of needle-like or powdered gallium trichloride, it is easy to adhere to the container wall, and it is very inconvenient to operate during transfer and application; and it needs to be heated before application, which will also cause temperature High, difficult to control the amount of addition and other issues

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Weigh 40g of gallium trichloride needle-like powder crystals and put them into a borosilicate glass bottle, put the borosilicate glass bottle into a glove box, control the water and oxygen content in the glove box to be less than 5ppm, and adjust it to 150°C through a heating mantle. The borosilicate glass bottle is heated to melt the gallium trichloride in the bottle. Transfer the molten gallium trichloride to a constant pressure dropping funnel. Open the constant pressure dropping funnel and drop the gallium trichloride liquid into the degree tile tank filled with liquid nitrogen, settle for five to fifteen minutes, pour out the upper layer of liquid nitrogen, and wait for the remaining liquid nitrogen to evaporate completely Dozens of spherical gallium trichloride particles were obtained at the bottom of the tank.

Embodiment 2

[0038] Weigh 100g of gallium trichloride needle-like powder crystals and put them in a borosilicate glass bottle, put the borosilicate glass bottle into the glove box, control the water and oxygen content in the glove box to be less than 5ppm, and then put the trichloride in the bottle Gallium was transferred to a constant pressure dropping funnel. The gallium trichloride in the constant pressure dropping funnel is heated to melt by a heating temperature control device, the heating temperature is controlled to be 90-150° C., and the gallium trichloride is not solidified during the subsequent dropping process. Open the constant pressure dropping funnel and drop the gallium trichloride droplet into the crock pot filled with liquid nitrogen at a rate of one to two drops per second, settle for about ten minutes, pour out the upper layer of liquid nitrogen, and wait for the remaining liquid nitrogen to volatilize After complete, obtain the spherical gallium trichloride particle of ...

Embodiment 3

[0040] Weigh 200g of gallium trichloride needle-like powder crystals and put them in a borosilicate glass bottle, put the borosilicate glass bottle into the glove box, control the water and oxygen content in the glove box to be less than 5ppm, and then put the trichloride in the bottle Gallium was transferred to a constant pressure dropping funnel. The gallium trichloride in the constant-pressure dropping funnel is heated to melt by a heating temperature control device, and the gallium trichloride is kept from solidifying during the next dropping process. Open the constant pressure dropping funnel to drop the gallium trichloride liquid into the earthen jar filled with liquid nitrogen, settle for about ten minutes, pour out the upper layer of liquid nitrogen, and wait for the remaining liquid nitrogen to evaporate completely, pour it on the bottom of the earthen jar 180 g of spherical gallium trichloride particles were obtained. The obtained granules were sieved in a glove box...

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Abstract

The invention relates to the technical field of gallium trichloride synthesis and discloses a preparation method of gallium trichloride granules. The preparation method includes the steps of: 1) moving gallium trichloride in a glove box, controlling the contents of water and oxygen in the glove box to be lower than 5 ppm, and increasing the temperature to melt the gallium trichloride; 2) adding the molten gallium trichloride dropwisely in liquid nitrogen in the glove box; 3) solidifying the molten gallium trichloride to obtain spherical or spherical-like gallium trichloride granules. The preparation method is simple in process steps, employs low-cost and easy-to-obtain raw materials, is free of introduction of impurities and can prepare regular spherical granules. These regular spherical granules have strong flowability, are not adhered on wall of a container, are very easy to move and apply, and are very easy to control in addition amount.

Description

technical field [0001] The invention relates to the technical field of gallium trichloride synthesis, in particular to a preparation method of gallium trichloride particles. Background technique [0002] Molecular formula of aqueous gallium trichloride: GaCl 3 , Properties: colorless needle crystals, density: 2.47g / cm 3 (25°C), melting point: 78°C, boiling point: 201.3°C, easy to deliquescence, easy to oxidize, easily soluble in water, soluble in benzene, carbon tetrachloride and carbon disulfide. Gallium trichloride is generally prepared by the direct reaction of gallium and chlorine, or by the reaction of hydrogen chloride and gallium trioxide at 200°C. Gallium trichloride is a catalyst for spectroscopic analysis and organic reactions, and is an important raw material for the synthesis of organic gallium reagents. [0003] When gallium trichloride is prepared, it is a colorless needle-like crystal. Its preparation and post-treatment need to be operated under anhydrous a...

Claims

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Application Information

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IPC IPC(8): C01G15/00
Inventor 曾小东童培云朱刘胡智向
Owner 清远先导材料有限公司
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