Preparation method of indium trichloride

A technology of indium trichloride and chlorine gas, which is applied in chemical instruments and methods, inorganic chemistry, gallium/indium/thallium compounds, etc., can solve the problems of insufficient chlorination, containing, difficult to control the reaction, etc., and achieve high utilization rate of raw materials , short process time and low production cost

Inactive Publication Date: 2017-10-24
FIRST RARE MATERIALS CO LTD
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AI Technical Summary

Problems solved by technology

The content of other metal impurities in the product prepared by this method is low, but the reaction is difficult to control in this method, and it is prone to insufficient chlorination, resulting in the problem that the product contains indium chloride impurities

Method used

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preparation example Construction

[0016] The preparation method of a kind of indium trichloride of the present invention comprises the following steps: primary chlorination: passing protective gas into the first reactor to replace the air in the first reactor, placing the raw material indium in the first reactor and heating to The first heating temperature makes the raw material indium melt, and the dry chlorine gas is passed into the liquid indium at a flow rate of 60~600L / h during the first aeration time to react. The first aeration time is proportional to the mass of the raw material indium, and then the aeration is stopped. Dry the chlorine gas, cool to room temperature to obtain solid indium chloride, and demold the indium chloride for use.

[0017] Secondary chlorination: put solid indium monochloride into a second reactor, pass through protective gas to replace the air in the second reactor, then stop feeding protective gas and change to dry chlorine gas, dry chlorine gas to The ventilation flow rate of...

Embodiment 1

[0026] Primary chlorination: Take 2kg of 4N indium, melt it in an indium melting furnace, transfer it to an indium chloride reactor, feed dry nitrogen at a certain flow rate to discharge the oxygen in the reactor, heat to 230°C, and turn off the nitrogen , feed dry chlorine gas at a rate of 60 L / h for 200 minutes, transfer indium monochloride to a graphite mold after the reaction, and cool to room temperature.

[0027] Secondary chlorination: put 2.6kg of indium chloride into the heating end of the quartz chlorination sublimation reactor, feed dry nitrogen at a certain flow rate to discharge the air in the reactor, close the nitrogen gas and feed dry chlorine gas, the flow rate is 60L / h , the temperature was raised to 300° C., and the indium chloride at the heating end was completely reacted. After cooling down to room temperature, 3.8 kg of anhydrous indium trichloride was collected at the collecting end. Sampling test shows that the product has a purity of 99.999% and a wate...

Embodiment 2

[0029] Primary chlorination: take 2kg of 4N indium, melt it in an indium melting furnace, transfer it to an indium chloride reactor, feed dry nitrogen at a certain flow rate to discharge the oxygen in the reactor, heat to 400°C, and turn off the nitrogen , feed dry chlorine gas at a rate of 300 L / h for 40 minutes, transfer indium monochloride to a graphite mold after the reaction, and cool to room temperature.

[0030] Secondary chlorination: put 2.6kg of indium chloride into the heating end of the quartz chlorination sublimation reactor, feed dry nitrogen at a certain flow rate to discharge the air in the reactor, close the nitrogen gas and feed dry chlorine gas, the flow rate is 300L / h , the temperature was raised to 500° C., and the indium chloride at the heating end was completely reacted. After cooling down to room temperature, 3.8 kg of anhydrous indium trichloride was collected at the collecting end. Sampling test shows that the product has a purity of 99.999% and a wat...

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Abstract

The invention relates to a preparation method of indium trichloride, which is divided into a primary chlorination process and a secondary chlorination process. The invention adopts the secondary chlorination sublimation method to prepare indium trichloride, and the product prepared by the method has high purity, short process time, less equipment required, high raw material utilization rate and low production cost.

Description

technical field [0001] The invention relates to a preparation method of indium chloride, in particular to a preparation method of indium trichloride. Background technique [0002] High-purity anhydrous indium trichloride is the main raw material for ITO thin films, III-IV semiconductors, and organic indium series compounds (MO sources), and is widely used in organic reaction catalysts, organic synthesis, and electronics industries. [0003] The synthesis method of high-purity anhydrous indium trichloride currently reported is generally divided into two steps. First, the reaction of elemental indium and hydrochloric acid synthesizes InCl 3 • 4H 2 O, and then calcination, organic solvent substitution and other methods to remove the water of crystallization. Chinese patent CN101254942B discloses a synthesis method of high-purity anhydrous indium trichloride, in which InCl is prepared by reacting 4~5N indium with hydrochloric acid 3 • 4H 2 O, using organic solvents n-butanol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G15/00
CPCC01G15/00C01P2006/80C01P2006/82
Inventor 王波朱刘康冶
Owner FIRST RARE MATERIALS CO LTD
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