Purification method for removing diethyl ether from trimethyl antimony

A technology of trimethyl antimony and a purification method, applied in the direction of antimony organic compounds and the like, can solve the problems of long time consumption, dangerous processing, unachievable product purity, etc., and achieve the effects of high reaction efficiency, high safety performance and simple operation.

Active Publication Date: 2021-12-24
安徽亚格盛电子新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is little research on the preparation process of trimethyl antimony at home and abroad. Its atmospheric boiling point is 80.6 °C and is similar to that of most solvents and impurities, which makes it difficult to separate trimethyl antimony from solvents, resulting in high-purity Trimethylantimony is very difficult, and now the generally accepted synthetic method is to use diethyl ether as a solvent to prepare Grignard reagent methylmagnesium iodide and react with antimony trichloride to synthesize trimethylantimony crude product. A series of complex post-treatments such as adding liquid bromine, filtering, reducing zinc particles, and drying and rectifying are not only time-consuming, but also very dangerous to handle.
The crude product of trimethyl antimony contains diethyl ether, which needs to be purified by removal of diethyl ether. The existing impurity removal and drying effects are not very satisfactory, and the product purity cannot meet the existing technical requirements.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] This embodiment provides a kind of purification method that trimethyl antimony removes ether, and the steps are as follows:

[0021] S1: Take 1Kg of trimethyl antimony crude product in an anhydrous and oxygen-free environment, and take NMR to detect that ether accounts for 1%, then the ether content is 10g (0.135mol) / 1.0eq;

[0022] S2: With a normal pressure reflux device, take 10.2g (0.14mol) / 1.05eq of trimethylaluminum and add it dropwise to trimethylantimony, stir while adding it, and keep reflux at 60°C for 3h after the addition;

[0023] S3: Cool down after stirring and reflux, and change to an atmospheric distillation device with a barbed fractionation column, and control the temperature at 145°C to receive fractions at 80-85°C;

[0024] S4: Take the S3 fraction and send it to NMR detection for the remaining trimethylaluminum 0.49g (6.8mmol) / 1.0eq, take tri-n-octylamine 2.6g (7.5mmol) / 1.1eq and add it to the trimethylantimony fraction, stir and reflux at 100°C 1...

Embodiment 2

[0030] This embodiment provides a kind of purification method that trimethyl antimony removes ether, and the steps are as follows:

[0031] S1: Take 800g of trimethyl antimony crude product, and take NMR to detect that ether accounts for 12%, then the ether content is 96g (1.3mol) / 1.0eq;

[0032] S2: Set up a normal-pressure reflux device, take 367g (2.34mol) / 1.8eq of triethylgallium and add it dropwise to trimethyl antimony, stir while adding it, and maintain reflux at 55°C for 3 hours after the addition;

[0033] S3: After the stirring and reflux is completed, the temperature is lowered, and an atmospheric distillation device with a barbed fractionation column is used, and the temperature is controlled at 140°C to receive the fraction of 80-85°C;

[0034] S4: Take the fraction received in S3 and send it to nuclear magnetic detection to detect the content of remaining triethylgallium in trimethylantimony: 70.6g (0.45mol) / 1.0eq, take MBDA86.3g (0.34mol) / 1.5eq and add it to San...

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PUM

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Abstract

The invention provides a purification method for removing diethyl ether from trimethyl antimony, the method comprises the following steps: using one of trimethylaluminum, trimethyl indium and triethyl gallium as an additive I, forming a high-boiling-point complex with diethyl ether, distilling and collecting the trimethyl antimony and a small amount of the additive I, then adding one of high-boiling-point tri-n-octylamine, tri-n-butylamine, MBDA and crown ether as an additive II to coordinate with the additive I to form a high-boiling-point coordination compound, and finally rectifying and purifying to obtain the 6N trimethyl antimony product. The method is low in cost, high in reaction efficiency and high in safety performance, diethyl ether can be effectively removed, harsh reaction conditions are not needed, and the operation is simple.

Description

technical field [0001] The invention relates to a method for purifying metal organic compounds, in particular to a method for purifying trimethyl antimony to remove ether. Background technique [0002] Trimethylantimony (TMSb) is one of the MO sources. It burns in the air and does not react with water. It is often used as an N-type dopant for GaAs, GaP, GaAsP and other deposited layers in the manufacture of light-emitting diodes. The prior art patent discloses CN110483580A a kind of high-purity trialkyl antimony and its preparation method and application. First, ether is used as a solvent to rapidly synthesize the Grignard reagent, and then the low-boiling ether in the Grignard reagent is replaced with a high-boiling solvent, as The only solvent for the synthesis of trimethyl antimony reaction system, which greatly reduces the difficulty of trialkyl antimony purification, simplifies the preparation process of trialkyl antimony, shortens the preparation time, and obtains tria...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/90
CPCC07F9/90Y02P10/20
Inventor 姜永要俞冬雷郑锐
Owner 安徽亚格盛电子新材料有限公司
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