Process for preparing metal alkyl compounds

Abstract

A method for preparing metal alkyl compounds, the raw materials for the manufacture of trialkylgallium and trialkylindium include metal indium or metal gallium, at least one alkyl donor, reducing agent and solvent; the alkyl donor is selected from alkyl halides; MR2 In ‑4, R represents an alkyl group, and 2‑4 R groups are independently selected from the same or different alkyl groups; M is especially aluminum, gallium or indium; gallium or indium or aluminum use high purity; use Sesquialkane aluminum chloride is used as a co-reactant, and metal gallium or metal indium can react with alkyl donor alkyl chloride at low temperature and low pressure to generate sesquialkyl gallium chloride or sesquialkyl indium chloride; reducing agent When reducing sesquialkylgallium chloride or sesquialkane indium chloride to trialkylgallium or trialkylindium, metal gallium or metal indium must be simultaneously generated; the newly generated metal gallium or metal indium is combined with chlorine in situ Methane (b) ethane reaction, so that the starting materials are fully utilized. The two-step yields are almost complete. This new synthetic route is an environmentally friendly green process.

Description

technical field [0001] The invention relates to the preparation of an alkyl metal compound, and belongs to the technical field of chemical industry. Background technique [0002] Group III-A organometallic compounds such as trialkylgallium and trialkylindium are used in the production of semiconductor layers in metal organic chemical vapor deposition (MOCVD) or metal organic vapor phase epitaxy (MOVPE). Monomers, commonly known as MO sources, their purity directly affects the optoelectronic properties of the semiconductors produced. The quality of such MO sources requires ultra-high purity, and the production process is complicated. Although the price is expensive, the market demand is still increasing. For more than half a century, people have been studying the preparation of trialkylgallium and trialkylindium. [0003] E. Wiberg at al, Z. Anorg. Chem. 251, 114 (1943) and G. E. Coates, J. Chem. Soc. 2003, 2011 (1951), heating methylmercury with a small amount of mercury c...

AI Technical Summary

Problems solved by technology

[0045] WO2015136049 (2014 Umicore) reacted 12.5mmol (1.94g) of methylgallium dichloride with equimolar sesquimethylaluminum chloride 12.5mmol (2.56g), added sodium chloride and potassium chloride without solvent Form an ionic liquid, and finally the utilization rate of gallium is very high, but in this case, sesquimethylaluminum chloride CH 3 AlCl 2 ·(CH 3 ) 2 AlCl contains two aluminum atoms, only half of which is used, the highly active components remain in the ionic liquid, and the residual liquid treatment is a big problem

[0046] So far, all the methods for preparing trimethylgallium or indium are not simple, some have potential safety hazards, the cost is generally high, and there are residues or residues, which are not friendly to the environment, and there is no atom economy.

Sesquite method is not yet mature