Preparation method of high-purity triethyl antimony

A triethyl antimony, high-purity technology, applied in the direction of antimony organic compounds, can solve the problems of explosion, triethyl antimony is easy to burn, reduce production safety accidents, etc., achieve high purity, high yield, safe and efficient production method Effect

Active Publication Date: 2017-01-25
FIRST RARE MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there is little research on the preparation process of triethyl antimony at home and abroad. With the upgrading of semiconductor materials, triethyl antimony is used as an antimony source by enterprises. Triethyl antimony is easy to burn when it meets water and oxygen, and it is easy to cause Explosion, reasonable production process will greatly reduce production safety accidents

Method used

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Examples

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Effect test

preparation example Construction

[0021] The present invention proposes a preparation method of high-purity triethyl antimony. Under the protection of inert gas, the steps are as follows:

[0022] Step S1: drop a monohaloethane solution into the mixture of magnesium scraps and organic solvent, and react to prepare Grignard reagent;

[0023] Step S2: after cooling the Grignard reagent, dropwise add antimony trichloride solution to prepare triethyl antimony solution by reaction;

[0024] Step S3: The triethyl antimony solution is subjected to two atmospheric distillations, two vacuum distillations, and one vacuum rectification to obtain high-purity triethyl antimony with a purity of more than 5N.

[0025] In the present invention, the monohaloethane is one or more of ethyl iodide, ethyl bromide and ethyl chloride. In the case that ethyl iodide is partially or completely replaced, the recovery amount of iodine can be reduced and the amount of iodine recovered can be greatly reduced. Environmental pollution and p...

Embodiment 1

[0027] Under nitrogen protection, using antimony trichloride, magnesium scraps and iodoethane as raw materials and ether as organic solvent, 99.9995% triethyl antimony is obtained after reaction and purification. The following steps are specific operations.

[0028] Preparation of reagents: dry antimony trichloride: vacuum dry antimony trichloride at 50 °C for 24 h, cool, weigh, and then vacuum dry at 50 °C for 3 h until the weight is constant and stop drying; dry ethyl iodide: take 40 g of calcium chloride and add it to In 500ml of iodoethane, heat under reflux for 3h; dry ether: reflux ether with sodium under nitrogen protection, when indicator benzophenone turns dark purple, distill out and collect ether for later use.

[0029] Preparation of Grignard reagent: under the protection of nitrogen gas, add 21g (0.85mol) of magnesium chips and 350ml of diethyl ether to a 1L three-necked flask, heat the three-necked flask to 35°C, and dropwise add 30ml of diethyl ether solution con...

Embodiment 2

[0033] Under argon protection, using antimony trichloride, magnesium scraps, bromoethane as raw materials, and tetrahydrofuran as organic solvent, 99.9995% triethyl antimony is obtained after reaction and purification. The following steps are specific operations.

[0034] Preparation of reagents: dry antimony trichloride: vacuum dry antimony trichloride at 50 °C for 24 h, cool, weigh, and then vacuum dry at 50 °C for 3 h until the weight is constant and stop drying; dry ethyl bromide: take 40 g of calcium chloride and add it to In 500ml of bromoethane, heat under reflux for 3h; dry tetrahydrofuran: reflux tetrahydrofuran with sodium, when the indicator benzophenone turns dark purple, steam out to collect tetrahydrofuran for use.

[0035] Preparation of Grignard reagent: under the protection of argon, add 21g (0.85mol) of magnesium chips and 350ml of tetrahydrofuran to a 1L three-necked flask, heat the three-necked flask to 35°C, and dropwise add 30ml of tetrahydrofuran solution...

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Abstract

The invention provides a preparation method of high-purity triethyl antimony. Under the protection of inert gas, the preparation method of the high-purity triethyl antimony comprises the following steps: S1, adding a monohalogenated ethane solution into a mixture of magnesium chips and an organic solvent to prepare a Grignard reagent; S2, dropwise adding an antimony trichloride solution into the Grignard reagent, and reacting to prepare a triethyl antimony solution; and S3, carrying out atmospheric distillation twice, reduced pressure distillation twice and reduced pressure rectification once on the triethyl antimony solution to obtain the high-purity triethyl antimony with the purity more than 5N. The method for synthesizing triethyl antimony by adopting a Grignard reagent process is carried out under the protection of the inert gas, the yield is high, the purity is high, the operation is safe, and the cost is low.

Description

technical field [0001] The invention belongs to the technical field of preparation of organic antimony compounds, in particular to a preparation method of high-purity triethyl antimony. Background technique [0002] Metal-Organic Chemical Vapor Deposition (MOCVD) is an advanced method for manufacturing semiconductor ultra-thin film materials. Compound semiconductor materials are widely used in laser technology, satellite communications, global positioning systems, solar cells and other fields. High-purity metal-organic compounds (ie, MO sources) are key supporting materials for MOCVD technology. High-purity triethyl antimony provides antimony source for semiconductor materials such as AlSb, GaSb, InSb, etc. It is one of the most important sources for growing optoelectronic materials in metal organic chemical vapor deposition (MOCVD) and chemical beam epitaxy (CBE) processes. [0003] At present, there is little research on the preparation process of triethyl antimony at ho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/90
Inventor 薄福丽朱刘
Owner FIRST RARE MATERIALS CO LTD
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