Process for preparing diethyl zinc

A diethyl zinc and preparation technology, applied in the direction of zinc organic compounds, etc., can solve the problems of high production cost and high price of diethyl zinc, and achieve the effects of low production cost, reduced production cost, high yield and high purity

Inactive Publication Date: 2006-09-06
INNER MONGOLIA MENG XI HIGH TECH GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Yet because the preparation cost of producing diethyl zinc at home and abroad is very high at present, cause its price very high

Method used

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  • Process for preparing diethyl zinc

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Effect test

Embodiment 1

[0017] Add 8% of its volume of 40 mesh copper-zinc alloy powder in a sealed stainless steel reactor with a stirrer, and use CO 2 Gas replaces the air in the reactor twice, seals the reactor, and starts the stirrer. The stirring paddle is in the form of an anchor-rake compound. After rising to 80°C, add ethyl iodide and ethyl bromide dropwise at the same time. The mass ratio of ethyl iodide and ethyl bromide is 1:2. After the reaction is triggered, stop adding ethyl iodide and continue to add ethyl bromide dropwise. , the dropping speed is inversely proportional to the reflux speed during the dropping process. The temperature of the reaction process is controlled at 80°C to make the reactant reflux smoothly. After the reflux is completed, close the reflux system of the reactor, control the temperature at 120°C, and continue to stir and react at this temperature After 1 hour, the vacuum system of the reactor was opened, diethyl zinc was recovered by distillation under reduced pr...

Embodiment 2

[0019] Add 12% of the volume of 80 mesh copper-zinc alloy powder in a sealed stainless steel reactor with a stirrer, replace the air in the reactor with nitrogen for 3 times, seal the reactor, start the reactor to stir, stir The form is an anchor-rake compound form. After the temperature inside the reactor is raised to 150°C within 60 minutes, ethyl iodide and ethyl bromide with a mass ratio of 1:1 are added dropwise at the same time, and the dropwise addition is stopped after the reaction is initiated. Ethyl iodide, continue to add ethyl bromide dropwise, the dropping rate during the dropping process is inversely proportional to the reflux rate, and the temperature in the reaction process is controlled at 100°C to make the reactant reflux smoothly. After the reflux is completed, close the reflux system of the reactor, control the temperature at 100°C, continue to stir and react at this temperature for 1.5 hours, open the vacuum system of the reactor, and recover diethyl zinc b...

Embodiment 3

[0021] Add 10% of the volume of 120-mesh copper-zinc alloy powder into a sealed stainless steel reactor with a stirrer, replace the air in the reactor with nitrogen for 3 times, seal the reactor, start the reactor to stir, stir The form is an anchor-rake composite form. After raising the temperature of the reactor to 60°C within 50 minutes, add iodoethane and bromoethane with a mass ratio of 1:1.5. After the reaction is initiated, stop adding iodine Ethane, continue to add bromoethane dropwise. During the dropwise addition, the drop rate is inversely proportional to the reflux rate. The temperature in the reaction process is controlled at 45° C. to make the reactant reflux smoothly. After the reflux is completed, close the reflux system of the reactor, control the temperature at 110°C, continue to stir and react at this temperature for 1.2 hours, open the vacuum system of the reactor, recover diethyl zinc after vacuum distillation, and obtain diethyl zinc with a purity of more ...

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Abstract

The invention relates to a method for preparation of compounds and especially to a method for preparation of zinc diethyl. The preparation technology of the said method includes the following steps: a. adding powdered copper-zinc alloy into a reactor with an agitator, of which the powdered copper-zinc alloy occupies 8-12 % of the reactor, replacing the air in the reactor with inert gas, afterwards, beginning to stir; b. heating the temperature of the reactor to 40-150 DEG C while stirring, simultaneously, dripping iodoethane and bromoethane, after the reaction is initiated, gradually dripping bromoethane continuously, and controlling the temperature at 40-100 DEG C to stably reflux the reactants; c.after the reflux, controlling the temperature of the reactor at 100-120 DEG C, continuously stirring the reactants for 0.5-2 hours, and then beginning to distill in reduced pressure state to obtain high-purity zinc diethyl. The technical project of this invention is characterized in that it is of simple process, low cost, and high yield rate and purity of the obtained product.

Description

technical field [0001] The invention relates to a method for preparing a compound, in particular to a method for preparing diethylzinc. Background technique [0002] Diethylzinc ((CH 3 CH 2 ) 2 Zn) is one of the most important catalyst monomers used in the research and production of carbon dioxide-based fully degradable plastic resins. At the same time, diethyl zinc is also an MO source for MOCVD, an important growth method for compound semiconductor thin film materials. It is an important dopant for materials, and it can also be used to prepare materials such as ZnSe and ZnS. In the MOCVD process, the purity requirement of diethyl zinc is very high. If it contains a lot of impurities, it will directly affect the photoelectric performance of the prepared material. It can also be used to protect and restore paper cultural relics and prolong the life of books and periodicals; it can be used in asymmetric addition, enantioselective addition and stereoselective addition of a...

Claims

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Application Information

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IPC IPC(8): C07F3/06
Inventor 毛国玉张明赵晓江向辉张广军牛丽刚海山
Owner INNER MONGOLIA MENG XI HIGH TECH GRP CO LTD
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