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Preparation method of gallium chloride

A technology of gallium chloride and ammonium chloride, applied in chemical instruments and methods, inorganic chemistry, gallium/indium/thallium compounds, etc., can solve the problems of high degree of gas drying, high preparation cost, toxicity, etc., and avoid potential safety hazards , cost reduction effect

Pending Publication Date: 2021-07-09
SHENHUA ZHUNNENG RESOURCE COMPREHENSIVE DEV COMPANY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the disadvantages of the above method are that the reaction of hydrogen chloride gas or chlorine gas with metal gallium requires a high degree of dryness of the gas, low utilization rate of the gas, certain toxicity of the exhaust gas, and high preparation cost.
In addition, the storage of hydrogen chloride gas or chlorine gas presents a huge safety hazard

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Use high-purity reagents (that is, the purity is not less than 99.99%, the same below) for raw material preparation, put ammonium chloride and gallium into the reaction kettle at a molar ratio of 6:1, pass a protective gas for a period of time, and remove the reaction kettle The air in the air; the reactor is heated to about 350°C to decompose the ammonium chloride into ammonia and hydrogen chloride, and fully react the generated hydrogen chloride with metal gallium to form gaseous gallium chloride;

[0029] Then control the temperature of the reactor at 220°C, so that the ammonium chloride generated by the reaction of ammonia gas and excess hydrogen chloride recrystallizes to form solid ammonium chloride to precipitate, and keep the gallium chloride in a gaseous state; open the outlet valve of the reactor, and continuously feed the protective gas Drive the gas in the reactor into a sealed container through the outlet valve and filter screen of the reactor, and gaseous g...

Embodiment 2

[0031] Use high-purity reagents for raw material preparation, put ammonium chloride and gallium into the reactor at a molar ratio of 5:1, pass through a protective gas for a period of time, and remove the air in the reactor; heat the reactor to 360°C Left and right, ammonium chloride is decomposed into ammonia and hydrogen chloride, and the generated hydrogen chloride and metal gallium are fully reacted to form gaseous gallium chloride;

[0032] Then control the temperature of the reactor at 240°C, so that the ammonium chloride generated by the reaction of ammonia gas and excess hydrogen chloride recrystallizes to form solid ammonium chloride to precipitate, and keep the gallium chloride in a gaseous state; open the outlet valve of the reactor, and continuously feed the protective gas Drive the gas in the reactor into a sealed container through the outlet valve and filter screen of the reactor, and gaseous gallium chloride is cooled and solidified in the sealed container; rehea...

Embodiment 3

[0034] Use high-purity reagents for raw material preparation, put ammonium chloride and gallium into the reactor at a molar ratio of 7:1, pass through a protective gas for a period of time, and remove the air in the reactor; heat the reactor to 400°C Left and right, ammonium chloride is decomposed into ammonia and hydrogen chloride, and the generated hydrogen chloride and metal gallium are fully reacted to form gaseous gallium chloride;

[0035] Then control the temperature of the reactor at 250°C, so that the ammonium chloride generated by the reaction of ammonia gas and excess hydrogen chloride recrystallizes to form solid ammonium chloride to precipitate, and keep the gallium chloride in a gaseous state; open the outlet valve of the reactor, and continuously feed the protective gas Drive the gas in the reactor into a sealed container through the outlet valve and filter screen of the reactor, and gaseous gallium chloride is cooled and solidified in the sealed container; rehea...

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Abstract

The invention discloses a preparation method of gallium chloride, wherein the preparation method comprises the steps: adding anhydrous ammonium chloride and gallium which are used as reaction raw materials into a reaction kettle, wherein the molar ratio of anhydrous ammonium chloride to gallium is more than 3:1; raising the temperature of the reaction kettle to 320-500 DEG C, decomposing ammonium chloride into ammonia gas and hydrogen chloride, and reacting the hydrogen chloride with metal gallium to generate gaseous gallium chloride; cooling the reaction kettle, recrystallizing ammonium chloride obtained by reaction of ammonia gas and residual hydrogen chloride to generate solid ammonium chloride, separating out the solid ammonium chloride, and keeping gallium chloride in a gaseous state; replacing gas in the reaction kettle with protective gas and storing the gas in a sealed container; and cooling the gaseous gallium chloride in the sealed container to obtain a gallium chloride solid product. Anhydrous ammonium chloride and gallium are used as raw materials, gaseous gallium chloride is generated from hydrogen chloride and gallium obtained by ammonium chloride decomposition through heating, and the gaseous gallium chloride is packaged and stored after being cooled, crystallized and separated, so that the cost of synthesizing gallium trichloride is remarkably reduced, and the potential safety hazard problem existing in gas synthesis is avoided.

Description

technical field [0001] The invention belongs to the technical field of inorganic chemical synthesis and relates to a preparation method of gallium trichloride. Background technique [0002] Gallium chloride, also known as gallium trichloride, has the molecular formula GaCl 3 , with a density of 2.47g / cm 3 (25°C), with a melting point of 78°C and a boiling point of 201.3°C. It is a white needle-like crystal that is easily deliquescent, oxidizable, and soluble in water. It is hydrolyzed by moisture in the air and emits white smoke. As an important inorganic salt derivative of gallium, gallium trichloride is an important raw material for the synthesis of organic gallium reagents, especially an indispensable raw material for the synthesis of organic gallium compounds such as trialkylgallium and alkoxygallium compounds. It can be used as a catalyst in organic reactions, and can also be used as a reagent for spectral analysis. It has a wide range of uses. [0003] The current m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G15/00
CPCC01G15/00C01P2006/80
Inventor 赵飞燕徐靓李超陈东陈荐郭志峰马越李小燕彭卓寅任延杰杜春雷
Owner SHENHUA ZHUNNENG RESOURCE COMPREHENSIVE DEV COMPANY
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