Device and method for preparing gallium chloride

A technology of gallium chloride and ammonium chloride, applied in chemical instruments and methods, chemical/physical processes, chemical/physical/physical chemical processes, etc., can solve the problem of low gas utilization rate, high degree of gas dryness, hydrogen chloride gas or chlorine gas Safety hazards and other issues

Pending Publication Date: 2021-07-06
SHENHUA ZHUNNENG RESOURCE COMPREHENSIVE DEV COMPANY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 util

Method used

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  • Device and method for preparing gallium chloride

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Experimental program
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Effect test

Embodiment 1

[0045] 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;

[0046] Then, the temperature of the reactor is controlled at 220° C., so that the ammonium chloride generated by the reaction of ammonia gas and excess hydrogen chloride is recrystallized to form solid ammonium chloride, and the gallium chloride is kept in a gaseous state;

[0047] Introduce protective gas through the second protective gas inlet to replace the sealed container, and use a vacuum tube to vacuumize the sealed container; after vacuuming the sealed container, cl...

Embodiment 2

[0049] 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 in a molar ratio of 5:1 into the reaction kettle, 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 360°C to decompose ammonium chloride into ammonia and hydrogen chloride, and fully react the generated hydrogen chloride with metal gallium to form gaseous gallium chloride;

[0050] Then the temperature of the reactor is controlled at 240°C, so that the ammonium chloride generated by the reaction of ammonia and excess hydrogen chloride is recrystallized to form solid ammonium chloride and precipitated, and the gallium chloride is kept in a gaseous state;

[0051] Introduce protective gas through the second protective gas inlet to replace the sealed container, and use a vacuum tube to vacuumize the sealed container; after vacuuming the sealed contain...

Embodiment 3

[0053] 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 in a molar ratio of 7:1 into the reactor, pass a period of protective gas, and remove the reactor The air in the air; the reactor is heated to about 400°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;

[0054] Then the temperature of the reactor is controlled at 250°C, so that the ammonium chloride generated by the reaction of ammonia and excess hydrogen chloride is recrystallized to form solid ammonium chloride and precipitates, and the gallium chloride is kept in a gaseous state;

[0055] Introduce protective gas through the second protective gas inlet to replace the sealed container, and use a vacuum tube to vacuumize the sealed container; after vacuuming the sealed container, close the first val...

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Abstract

The invention discloses a device and a method for preparing gallium chloride. The device comprises a reaction kettle, a surge flask and a sealed container. The reaction kettle is provided with a feed port, a first shielding gas inlet and a discharge port. The surge flask is provided with openings in both ends, the opening in one end is connected to the discharge port of the reaction kettle through a pipeline, and the opening in the other end is connected to the sealed container through a pipeline. The sealed container is provided with a second shielding gas inlet and a communication port connected with the opening in the other end of the surge flask. 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 device and a preparation method for preparing gallium trichloride. Background technique [0002] Gallium chloride, also known as gallium trichloride, has a molecular formula of GaCl3, a density of 2.47g / cm3 (25°C), a melting point of 78°C, and a boiling point of 201.3°C. White needle-like crystal, it will be hydrolyzed with moisture in the air and emit 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 method for preparing gallium trichloride is mainly t...

Claims

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Application Information

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IPC IPC(8): B01J19/18B01J19/00
CPCB01J19/18B01J19/0066B01J19/0013
Inventor 赵宇航任延杰张云峰王永旺崔永杰高进高莹熊中义石尔
Owner SHENHUA ZHUNNENG RESOURCE COMPREHENSIVE DEV COMPANY
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