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A kind of preparation method and equipment of gallium trichloride

A technology of gallium trichloride and equipment, applied in the field of preparation of gallium trichloride, which can solve the problems of high impurity content and low purity

Active Publication Date: 2022-02-22
昆明先导新材料科技有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of the prior art is that a large amount of gallium monochloride impurity will be produced when chlorine gas is directly introduced into the liquid gallium metal for reaction, and a large amount of chlorine gas will be dissolved in the liquid gallium trichloride solution produced by the reaction, so the existing The liquid gallium trichloride produced by the technical reaction has the disadvantages of high impurity content and low purity

Method used

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  • A kind of preparation method and equipment of gallium trichloride
  • A kind of preparation method and equipment of gallium trichloride

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preparation example Construction

[0022] According to the first aspect of the present invention, a preparation method of gallium trichloride is provided, comprising the following steps: preheating the temperature of liquid metal gallium to 40-70°C, and preheating the initial temperature of the reaction vessel to 100-150°C First, liquid metal gallium is added to the reaction kettle, then chlorine gas after sulfuric acid drying is passed into the liquid metal gallium, and the chlorine gas is directly passed into the bottom of the metal gallium solution to ensure that the reaction can be completely complete; the synthesis reaction of the present invention consists of Two stages. In the first stage, the main product is gallium monochloride. By adjusting the temperature of the reactor, the temperature of the reactor is controlled at 200-400 ° C. After the first preset time period, the main product is gallium monochloride and gallium trichloride. Product, wherein, the gallium trichloride of by-product is liquid galli...

Embodiment 1

[0031] The gallium metal is preheated to 40°C, and the reactor is preheated to 100°C. Add liquid metal gallium into the reactor, pass chlorine gas into the bottom of the metal gallium liquid after being dried by sulfuric acid, control the reaction temperature at 200°C in the first stage of the reaction process, and control the reaction temperature at 100°C in the second stage, the reaction process The gallium trichloride in the medium is boiled and evaporated to the fractionating tube, and the fractionating tube cools the gaseous gallium trichloride to obtain liquid gallium trichloride which flows into the storage tank; after the reaction is complete, keep the reactor temperature at 150 ° C, and pass through the protective gas (It can be nitrogen or inert gas) to take away the chlorine gas dissolved in the gallium trichloride solution, and the purity of the dechlorinated gallium trichloride product can reach 99.999% after testing.

Embodiment 2

[0033]The difference from Example 1 is that the metal gallium is preheated to 60°C, the reactor is preheated to 120°C, the reaction temperature is controlled to be 300°C in the first stage of the reaction process, and the reaction temperature is controlled to be 200°C in the second stage. The temperature of the reactor is controlled at 200°C when the protective gas is used, and the purity of the dechlorinated gallium trichloride product can reach 99.999% after testing.

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Abstract

The invention discloses a preparation method of gallium trichloride, which comprises the following steps: firstly adding liquid metal gallium into a reactor, and then feeding chlorine gas into the liquid metal gallium; controlling the temperature of the reactor at 200-400 °C, after the first preset time period, the main product-gallium monochloride and the by-product-gallium trichloride are obtained; by adjusting the temperature of the reactor at 100-300 °C, the liquid state is obtained after the second preset time period Gallium trichloride and gaseous gallium trichloride; the obtained gaseous gallium trichloride is evaporated into the fractionating tube, and then the gaseous gallium trichloride becomes liquid gallium trichloride and flows into the storage device through cooling. A preparation method of gallium trichloride provided by the present invention can effectively solve the prior art problem of directly feeding chlorine gas into liquid metal gallium by setting two-stage reactions and setting different reaction temperatures in the two stages Carrying out the reaction creates technical problems with large quantities of gallium monochloride and chlorine gas impurities.

Description

technical field [0001] The invention relates to the technical field of fine chemical production, in particular to a preparation method and equipment of gallium trichloride. Background technique [0002] The molecular formula of gallium trichloride is GaCl 3 , is a colorless needle-like crystal that is easy to deliquesce, easy to oxidize, and easily soluble in water. Gallium trichloride can be dissolved in benzene, carbon tetrachloride and carbon disulfide, and can be directly reacted by metal gallium and chlorine gas, or at 200 ° C It is prepared by the action of hydrogen chloride and gallium trioxide, used for spectroscopic analysis and organic reaction catalyst, and is an important raw material for the synthesis of organic gallium reagents. [0003] The method for preparing gallium trichloride in the prior art: firstly, liquid metal gallium is added into a reactor, and then chlorine gas is directly introduced into the liquid metal gallium, and the liquid gallium trichlori...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G15/00B01J3/00B01J3/04
CPCC01G15/00B01J3/002B01J3/04
Inventor 刘华胜徐成朱刘周声万
Owner 昆明先导新材料科技有限责任公司
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