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Method for preparing high-purity dimethyl zinc by preparing trimethylgallium by-product

A technology of dimethyl zinc and trimethyl gallium, applied in the direction of zinc organic compounds, etc., can solve the problems of secondary pollution, gallium pollution, low yield, etc.

Active Publication Date: 2017-12-26
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There are roughly two existing synthetic methods, one is to use ZnCl 2 and TMA or methylmagnesium iodide, the disadvantage of this method is mainly that ZnCl 2 It is a solid, so the reaction is not carried out in a homogeneous phase, the yield is not high and it is not conducive to large-scale production, and when using methylmagnesium iodide as a reactant, ethers need to be used as solvents, and ethers are easily mixed with dimethyl magnesium iodide. Zinc coordination, resulting in secondary contamination
The second is to use dimethylaluminum chloride and diethylzinc to prepare by exchanging alkyl groups. Since dimethylaluminum chloride is a by-product of preparing trimethylgallium, the raw materials are easy to obtain and the cost is relatively low, but The biggest disadvantage of using this method is that it is easy to cause gallium pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Install dropping and cooling devices on the 500mL three-necked bottle respectively, and install a thermometer. Now pour 185 grams of MeAlCl into the bottle 2 , heat the reaction bottle to 90°C and start adding diethylzinc (247g) dropwise. When the heating temperature reaches 100°C, start to distill dimethyl zinc. The temperature of the distillation head is 46°C. Stop heating when the temperature of the reaction bottle reaches 180°C . Obtain about 162 grams of product, yield 85%. ICP sampling analysis, which contains 20,000 ppm of trimethylgallium.

[0013] Add 150 grams of dimethyl zinc into a 250 mL round bottom flask, install a rectification device, remove 10 grams of the front fraction, take 120 grams of the middle fraction, and take a sample for ICP. The impurity content is: Cu: 6.2ppm; Ga: 2000ppm, Product purity is unqualified.

Embodiment 2

[0015] Install dropping and cooling devices on the 500mL three-necked bottle respectively, and install a thermometer. Now pour 203 grams of MeAlCl into the bottle 2 , heat the reaction bottle to 90°C and start adding diethylzinc (247g) dropwise. When the heating temperature reaches 100°C, start to distill dimethyl zinc. The temperature of the distillation head is 46°C. Stop heating when the temperature of the reaction bottle reaches 180°C . About 174 grams of product were obtained, and the yield was 91%. ICP sampling analysis, which contains 20,000 ppm of trimethylgallium.

[0016] Add 100 grams of tri-n-butylamine to a 250 mL round-bottomed flask, add 5 grams of sodium metal, keep stirring at 150 ° C for two hours, change to a distillation device, take about 10 grams of the front fraction, 30 grams of the rear fraction, and obtain 60 grams of Anhydrous tri-n-butylamine.

[0017] Add 150 grams of dimethyl zinc and 20 grams of tri-n-butylamine in a 250mL round bottom flask,...

Embodiment 3

[0019] Install dropping and cooling devices on the 500mL three-necked bottle respectively, and install a thermometer. Now pour 213 grams of MeAlCl into the bottle 2 , heat the reaction bottle to 90°C and start to add diethylzinc (247g) dropwise. When the heating temperature reaches 100°C, start to distill the crude dimethyl zinc. The temperature of the distillation head is 46°C, and stop when the temperature of the reaction bottle reaches 180°C heating. About 179 grams of the product were obtained, with a yield of 94%. ICP sampling analysis, which contains 20,000 ppm of trimethylgallium.

[0020] Add 100 grams of tri-n-butylamine to a 250 mL round-bottomed flask, add 5 grams of sodium metal, keep stirring at 150 ° C for two hours, change to a distillation device, take about 10 grams of the front fraction, 30 grams of the rear fraction, and obtain 60 grams of Anhydrous tri-n-butylamine.

[0021] In an inert atmosphere, add 150 grams of crude dimethyl zinc and 20 grams of an...

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Abstract

The invention provides a method for preparing high-purity dimethylzine by utilizing a prepared trimethyl gallium by-product. The method comprises the steps of heating to prepare the ethyl gallium by-product Me2AlCl, dropwise adding Et2Zn, and continuously heating a reaction system, distilling to obtain the crude dimethylzine; in inert atmosphere, adding the crude dimethylzine and anhydrous tri-n-butylamine into a reactor with a rectification device; heating, keeping reflux of the dimethylzine at the bottom of a rectifying column without steaming out, rectifying after the reflux, removing the front and back distillate, wherein the obtained middle distillate is the hyperpure dimethylzine. By utilizing a synthesized trimethyl gallium byproduct, the cost is reduced, meanwhile, due to the fact that the activity of Et2AlCl is far lower than that of Me2AlCl, post-processing waste liquid is favorable to treat. A solvent is not needed during reaction, and pollution brought is avoided. Meanwhile, the Me2AlCl and the Et2Zn both are liquid, a homogeneous reaction is achieved, test operation is facilitated, and the improvement of yield is improved.

Description

technical field [0001] The invention relates to a method for purifying metal organic compounds in the chemical field, in particular to a method for preparing high-purity dimethyl zinc by using a by-product of preparing trimethylgallium. Background technique [0002] Dimethyl zinc is a commonly used raw material for chemical synthesis. It is often used to prepare methyl-containing organic compounds or to prepare methyl metal compounds, and its most important use is to prepare II-VI compounds on MOCVD. In recent years, II-VI compound semiconductors and their solid solutions have attracted more and more attention, because II-VI compounds have great potential in optoelectronics. Their bandgaps cover the entire visible, near-infrared, and mid-infrared regions. On the other hand, the development of molecular beam extension and MOCVD technology has opened up a new way to manufacture high-quality II-VI compounds and their solid solution films. With dimethyl zinc (DMZ) and in situ ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F3/06
CPCC07F3/06
Inventor 孔令宇潘毅虞磊王晓晨韩建林
Owner NANJING UNIV