Preparation method of diethyl germanium dihalide

A technology of diethyl germanium dihalide and diethyl germanium dichloride, which is applied in the direction of germanium organic compounds, etc., can solve the problems of not conforming to the concept of green environmental protection, troublesome use and transportation, and complicated tail gas treatment, so as to avoid toxic gases Effects of leakage, less product impurities, and reduction of process burden and cost

Pending Publication Date: 2021-03-30
广东先导微电子科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of this method are that ethyl chloride is a gas, toxic and carcinogenic, has a lot of waste gas, complex tail gas treatment, troublesome use and transportation, strict requirements on equipment sealing, high cost, and many impurities in the product, which does not conform to the concept of green environmental protection.

Method used

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  • Preparation method of diethyl germanium dihalide
  • Preparation method of diethyl germanium dihalide

Examples

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Embodiment 1

[0034] A kind of preparation method of diethylgermanium dichloride as the embodiment of the present invention, described method comprises the following steps:

[0035] (1) Mix ethylmagnesium iodide and germanium tetrachloride in organic solvent A under acidic conditions and react at a temperature not exceeding 10°C to obtain tetraethylgermanium; purify tetraethylgermanium to obtain purified tetraethylgermanium Ethyl germanium; the preparation method of the diethyl germanium dihalide also includes the preparation step of ethyl magnesium iodide, and the preparation step of the ethyl magnesium iodide comprises: under the protective gas atmosphere, magnesium is placed in an organic solvent Reaction system A is obtained in B, heated to 40-60°C, dropwise adding iodoethane solution to the reaction system A under stirring, controlling the reaction temperature to be 40-60°C, stirring reaction 1 after the iodine solution is added dropwise ~2h, the solvent of ethyl iodide solution is org...

Embodiment 2

[0042] As a preparation method of diethylgermanium dichloride in the embodiment of the present invention, the only difference between this embodiment and Example 1 is: under the protection of nitrogen, the tetraethylgermanium in step (II) and 96.3 g of tetraethylgermanium The germanium chloride was mixed evenly in the high-temperature autoclave, and the high-temperature autoclave was transferred to the high-temperature roller heating furnace, and the rolling was started, and the temperature was set at 300°C for 31 hours of reaction.

Embodiment 3

[0044] As a preparation method of diethylgermanium dichloride in the embodiment of the present invention, the only difference between this embodiment and Example 1 is: under the protection of nitrogen, the tetraethylgermanium in step (II) and 96.3 g of tetraethylgermanium The germanium chloride was mixed evenly in the high-temperature autoclave, and the high-temperature autoclave was transferred to the high-temperature roller heating furnace, and the rolling was started, and the temperature was set at 400°C for 31 hours of reaction.

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Abstract

The invention provides a preparation method of diethyl germanium dihalide. The method comprises the following steps: (1) mixing ethyl magnesium iodide and germanium tetrahalide in an organic solvent Aunder an acidic condition, and reacting at the temperature of not more than 10 DEG C to obtain tetraethyl germanium; and (2) reacting the tetraethyl germanium obtained in the step (1) with germaniumtetrahalide at 300-400 DEG C to obtain diethyl germanium dihalide. The preparation method of the diethyl germanium dihalide provided by the invention is a new synthesis process flow of the diethyl germanium dihalide, which does not need to use any toxic gas raw material, especially does not need to use chloroethane and does not need a tail gas treatment step; therefore, toxic gas leakage caused byleakage of reaction equipment is avoided, any toxic gas intermediate product is not generated, the product is less in impurity and high in purity, and a product with stable properties is easier to obtain, so that mass production is facilitated, the yield is high, and the method is green and environment-friendly.

Description

technical field [0001] The invention relates to the field of medical material raw materials, in particular to a preparation method of diethyl germanium dihalide. Background technique [0002] Diethyl germanium dihalide has great application value in the preparation of contact lenses. The EFFICIENTLABORATORY-SCALE GERMANIUM DIRECT SYNTHESIS on the journal Synthesis and Reactivity in Inorganic and Metal-Organic Chemistry discloses a preparation of diethyl germanium dichloride The method is to mix germanium powder and copper powder evenly according to a certain ratio, press them into a cake shape under a certain pressure, and then break them into blocks; the alloy blocks are placed in a high-temperature area in the quartz tube, and when the temperature is raised to a certain temperature, Introduce ethyl chloride, control the gas flow of ethyl chloride, make the molten alloy block in the atmosphere of ethyl chloride, the purpose is to make it fully contact and react completely, ...

Claims

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Application Information

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IPC IPC(8): C07F7/30
CPCC07F7/30
Inventor 曾翼俊陈世栋徐成黄邹松
Owner 广东先导微电子科技有限公司
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