Method for industrially preparing trimethyl gallium
A technology of trimethyl gallium and methyl tetrahydrofuran, which is applied in the field of trimethyl gallium preparation, can solve the problems of filling and transfer safety hazards, low reaction conversion efficiency, and high price of trimethyl aluminum, and is suitable for large-scale industrialization. Production, easy to industrialize, easy to control effect
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Embodiment 1
[0016] In a reactor filled with nitrogen, put 580g of gallium-magnesium alloy into it, add 2100g of anhydrous ether, and gradually add methyl iodide (CH 3 I) 2050g, by controlling iodomethane (CH 3 1) The speed of addition controls the solvent reflux speed, after the reaction is completed, continue to keep reflux for 4 hours, then the solvent is steamed, and then under reduced pressure (vacuum degree is between 1~100mmgH) to obtain the mixture of trimethylgallium and ether The complex is finally decomposed (the decomposed temperature is between 70°C and 140° C.) to obtain 370 g of trimethylgallium, with a yield of 90% (calculated as metal gallium).
Embodiment 2
[0018] In a reactor filled with nitrogen, put 580g of gallium-magnesium alloy into it, add 1600g of anhydrous ether, and gradually add methyl iodide (CH 3 I) 2050g, by controlling iodomethane (CH 3 1) The speed of addition controls the solvent reflux speed, after the reaction is completed, continue to keep reflux for 4 hours, then the solvent is steamed, and then under reduced pressure (vacuum degree is between 1~100mmgH) to obtain the mixture of trimethylgallium and ether The complex was finally decomposed (the decomposed temperature was between 70 and 140° C.) to obtain 341 g of trimethylgallium, with a yield of 83% (calculated as metal gallium).
Embodiment 3
[0020] In a reactor filled with nitrogen, put 580g of gallium-magnesium alloy into it, add 2100g of anhydrous ether, and gradually add methyl iodide (CH 3 1) 1550g, by controlling iodomethane (CH 3 1) The speed of addition controls the solvent reflux speed, after the reaction is completed, continue to keep reflux for 4 hours, then the solvent is steamed, and then under reduced pressure (vacuum degree is between 1~100mmgH) to obtain the mixture of trimethylgallium and ether The complex was finally decomposed (the decomposed temperature was between 70°C and 140° C.) to obtain 325 g of trimethylgallium, with a yield of 79% (calculated as metal gallium).
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