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Preparation method of diethyl zinc

A technology of diethylzinc and diethylaluminum chloride is applied in chemical instruments and methods, zinc organic compounds, compounds containing elements of Group 3/13 of the periodic table, etc. It can not be too high and the cost is high, so as to achieve the effect of easy industrial production, improve yield and purity, and promote the reaction

Active Publication Date: 2013-06-12
SHANGYU HUALUN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because this method involves high temperature and hydrogen, and uses the expensive raw material iodide, the cost is high and the industrialization benefit is not high.
[0005] In the second method, the exchange reaction of various compounds with alkyl zinc, such as iodine-zinc exchange reaction, boron-zinc exchange reaction, mercury-zinc exchange reaction, is mainly used for the synthesis of advanced organozinc compounds and cannot be used for secondary Preparation of ethyl zinc, and industrialization is difficult
The disadvantage of this preparation method is that the purity of the raw materials is relatively high, and the concentration of the hydride contained in it should not be too high, and a special preparation method is required to prepare

Method used

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  • Preparation method of diethyl zinc

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Effect test

Embodiment 1

[0030] 1. The reaction kettle, pipeline, high level tank and receiving tank are replaced by argon 2-3 times. Open the manhole, put in 0.74kg of zirconocene dichloride and 170kg of zinc chloride under the protection of argon, heat up to 90°C, stop the argon, dry under reduced pressure for 2-4 hours, cool to below 25°C for later use;

[0031] 2. Under the protection of argon, press the raw material 292.5kg of triethylaluminum into the triethylaluminum high-level tank, and put the high-level tank triethylaluminum under the protection of argon into a slow-stirring reactor. The reactor system Automatically exothermic and slowly rise to 30-35°C, after the addition is complete, heat up to 40-45°C, and react for 2 hours;

[0032] 3. Cool down to below 30°C, open the diethyl zinc distillation valve, distill the diethyl zinc product under reduced pressure (pressure is -0.08-0.09MPa), slowly raise the temperature of the reactor, and collect diethyl zinc with a gas phase temperature of 30...

Embodiment 2

[0038] 1. The reaction kettle, pipeline, high level tank and receiving tank are replaced by argon 2-3 times. Open the manhole, put in 0.59kg of zirconium chloride and 170kg of zinc chloride under the protection of argon, heat up to 90°C, stop the argon, dry under reduced pressure for 2-4 hours, cool to below 25°C for later use;

[0039] 2. Under the protection of argon, press the raw material 292.5kg of triethylaluminum into the triethylaluminum high-level tank, and put the high-level tank triethylaluminum under the protection of argon into a slow-stirring reactor. The reactor system Automatically exothermic and slowly rise to 30-35°C, after the addition is complete, heat up to 40-45°C, and react for 2 hours;

[0040]3. Cool down to below 30°C, open the diethyl zinc distillation valve, distill the diethyl zinc product under reduced pressure (pressure is -0.08-0.09MPa), slowly raise the temperature of the reactor, and collect diethyl zinc with a gas phase temperature of 30-50°C...

Embodiment 3

[0046] 1. The reaction kettle, pipeline, high level tank and receiving tank are replaced by argon 2-3 times. Open the manhole, put in 6.0kg of zirconocene dichloride and 170kg of zinc chloride under the protection of argon, heat up to 90°C, stop the argon, dry under reduced pressure for 2-4 hours, cool to below 25°C for later use;

[0047] 2. Under the protection of argon, press the raw material 292.5kg of triethylaluminum into the triethylaluminum high-level tank, and put the high-level tank triethylaluminum under the protection of argon into a slow-stirring reactor. The reactor system Automatically exothermic and slowly rise to 30-35°C, after the addition is complete, heat up to 40-45°C, and react for 2 hours;

[0048] 3. Cool down to below 30°C, open the diethyl zinc distillation valve, distill the diethyl zinc product under reduced pressure (pressure is -0.08-0.09MPa), slowly raise the temperature of the reactor, and collect diethyl zinc with a gas phase temperature of 30-...

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Abstract

The invention discloses a preparation method of diethyl zinc, and the preparation method comprises the following steps of: adding aluminum triethyl to zinc chloride under the protection of an inert gas in the presence of a zirconium catalyst for reaction; controlling the reaction temperature to be not higher than 60 DEG C; and after the reaction is completed, decompressing and distilling to obtain the diethyl zinc and distilled mother liquor. The preparation method disclosed by the invention can effectively promote the reaction efficiency of the zinc chloride and the aluminum triethyl, reduce the reaction temperature and reduce the occurrence of secondary reaction and the decomposition of the product diethyl zinc by adding the zirconium catalyst to a reaction system, thereby being favorable to enhance the purity and yield of the product; and in the preparation method disclosed by the invention, the requirement on the concentration of hydride contained in the aluminum triethyl is not so strict after the zirconium catalyst is added, and the commercially available product can be used directly, thereby simplifying the operation steps.

Description

technical field [0001] The invention belongs to the field of organometallic compound synthesis, and in particular relates to a preparation method of diethyl zinc. Background technique [0002] Diethyl zinc is a commonly used organic zinc reagent, which is usually used as a catalyst or reaction reagent for polymerization or drug production, and is widely used in related industries such as polymerization catalysts, drug synthesis, and solar cells. [0003] At present, there are three main methods for the synthesis of dialkyl zinc: (1) the reaction of halides and metal zinc; (2) the exchange reaction of various compounds with alkyl zinc; (3) the use of halide zinc and metal reagents. reaction. [0004] In the first method, iodide and bromide are usually used to react with activated zinc powder, that is, at first the halide of diethyl zinc is obtained by the action of zinc powder with halohydrocarbon, and then the halide is dissociated at high temperature, This produces diethy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F3/06C07F5/06
Inventor 李典正张江林何光明
Owner SHANGYU HUALUN CHEM
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