Preparation process of diethyl zinc

Abstract

A process for preparing diethyl zinc includes such steps as activating and drying Zn powder, adding it along with cuporous iodide and a quarter of the mixture of iodoethane and bromoethane into reactor, adding finished diethyl zinc as trigger, heating, adding rest of said mixture, heating, stirring while reacting, vacuum distilling and collecting product at a temp lower than -35 deg.C.

Description

technical field [0001] The invention belongs to the technical field of synthesis of metal organic compounds, in particular to a preparation method of diethylzinc. Background technique [0002] Known preparation method - use zinc powder (Zn), bromoethane (EtBr) and iodoethane (EtI) to react in the presence of copper salt and catalyst and heat to make the generated Et Zn X (X=Br, I) Converted to DEZn, and then separated by distillation to obtain a transparent diethyl zinc solution. [0003] Due to the different requirements for the purity of the product diethyl zinc, the purity of the zinc powder used in the reaction is also different. Taking the preparation of high-purity 5.5N diethyl zinc as an example, although the purity of the zinc powder used for the reaction is 5N~6N, due to the influence of packaging, storage and other factors, even if the reaction is dried before the reaction, the reaction time is generally It will also be around 1.5 hours, sometimes even as long as...

AI Technical Summary

Problems solved by technology

Taking the preparation of high-purity 5.5N diethyl zinc as an example, although the purity of the zinc powder used for the reaction is 5N~6N, due to the influence of packaging, storage and other factors, even if the reaction is dried before the reaction, the reaction time is generally It will also be around 1.5 hours, sometimes even as long as 6~7 hours, which increases the uncertainty of the reaction and the reaction yield is also unstable

In addition, because the reaction is a one-time feed intake, and the boiling point of the solution is low (bromoethane 36.5 ℃ and iodoethane 73 ℃), so before and after the initiation, the loss of a large amount of exothermic solvent is very large. If the control is not good, the bromoethane And the loss of iodoethane even reaches more than half, so the actual reaction yield is very low and unstable (generally at 45% ~ 70%)