A kind of preparation method of trimethylgallium
A technology of trimethylgallium and methylmagnesium bromide, which is applied in the field of preparation of trimethylgallium, can solve the problems of environmental pollution, complex reaction process, high cost of raw materials, etc., and achieve reduced production costs, high production safety, and high reaction efficiency. high efficiency effect
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Embodiment 1
[0016] Embodiment 1: A kind of preparation method of trimethylgallium. The molar ratio of anhydrous gallium trichloride, magnesium metal and methyl bromide used below was 1 (176 g): 3:3, and the total amount of diisoamyl ether was 1408 g. The method comprises the following steps: 1. Distilling and purifying the diisoamyl ether after being dried through molecular sieves, and the water content of the diisoamyl ether after distillation is 10-40 ppm for use. 2. In a stainless steel reaction kettle filled with nitrogen, add the amount of diisoamyl ether and metal magnesium particles, start stirring, and put the amount of methyl bromide gas at a temperature of 30-100°C and normal pressure for 8 hours Slowly added to the reaction kettle under the condition of generating methylmagnesium bromide solution. After the reaction was completed, the stirring was continued at 50-100° C. for 2 hours, and then lowered to below 40° C. 3. Slowly add the amount of anhydrous gallium trichloride so...
Embodiment 2
[0017] Embodiment 2: A kind of preparation method of trimethylgallium. The molar ratio of anhydrous gallium trichloride, magnesium metal and methyl bromide used below is 1 (176 grams): 3.4: 3.1, and the total amount of diisoamyl ether is 2112 grams. The method comprises the following steps: 1. Distilling and purifying the diisoamyl ether after being dried through molecular sieves, and the water content of the diisoamyl ether after distillation is 10-40 ppm for use. 2. In a stainless steel reaction kettle filled with argon, add the amount of diisoamyl ether and metal magnesium particles, start stirring, and put the amount of methyl bromide gas at a temperature of 30-100 ° C, normal pressure, and a time of 6 Slowly added to the reaction kettle under the conditions of hours to generate methylmagnesium bromide solution. After the reaction was completed, the stirring was continued at 50-100° C. for 3 hours, and then lowered to below 40° C. 3. Slowly add the amount of anhydrous ga...
Embodiment 3
[0018] Embodiment 3: a kind of preparation method of trimethylgallium. The molar ratio of anhydrous gallium trichloride, magnesium metal and methyl bromide used below is 1 (176 grams): 3.5: 3.2, and the total amount of diphenyl ether is 1936 grams. The method comprises the following steps: 1. Diphenyl ether is dried by molecular sieves and then purified by distillation, and the water content of the diphenyl ether after distillation is 10-40 ppm for use. 2. In a stainless steel reaction kettle filled with argon, add the amount of diphenyl ether and metal magnesium particles, start stirring, and put the amount of methyl bromide gas at a temperature of 30-100°C and normal pressure for 5.5 hours Slowly added to the reaction kettle under the condition of generating methylmagnesium bromide solution. After the reaction was completed, the stirring was continued at 50-100° C. for 2.5 hours, and then lowered to below 40° C. 3. Slowly add the amount of anhydrous gallium trichloride sol...
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