Purification method for removing diethyl ether from trimethyl antimony

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...

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.