Synthesis process of hexamethyldisilane
A technology of hexamethyldisilane and a synthesis method, applied in directions such as organic silicon compounds, can solve problems such as unfavorable industrialized production, flammability and explosion, and shortage of raw materials, and achieve the effects of convenient industrialized production, simple process, and easy control.
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example 1
[0014] Pump about 200kg of xylene and 550kg (2.5kmol) of 15-crown-5 into a dry 1500L stainless steel reactor with a condensing reflux system in sequence, and replace the closed system with nitrogen for 3 to 5 times. Add nitrogen to the kettle to a state slightly higher than normal pressure (0.01-0.02Mpa), then open the vent valve, and quickly add 28.8kg (1.25kmol) of metal sodium into the kettle through the manhole under the purging of a slight nitrogen flow , cover the manhole cover, replace the closed system with nitrogen for 5 times, add nitrogen to the kettle for the last time to a state slightly higher than normal pressure (0.01-0.02Mpa), open the open system, so that the entire material and its reaction process are in a state of under the protection of nitrogen atmosphere.
[0015] Heating through the jacket steam, slowly raising the temperature to 95°C-100°C (the heating process takes 1 hour), and keeping it at this temperature for 0.5 hours, after the metallic sodium i...
example 2
[0021] Pump about 300kg of xylene and 440kg (2kmol) of 15-crown-5 into a dry 1500L stainless steel reaction kettle with a condensing reflux system in sequence, and replace the closed system with nitrogen for 3 to 5 times. Supplement nitrogen to the state slightly higher than normal pressure (0.01~0.02Mpa), then open the vent valve, and under the purging of slight nitrogen flow, quickly add 30kg (1.30kmol) of metal sodium into the kettle through the manhole at one time, cover Put on the manhole cover, replace the closed system with nitrogen for 5 times, add nitrogen to the kettle for the last time to a state slightly higher than normal pressure (0.01-0.02Mpa), open the open system, so that the entire material and its reaction process are in a nitrogen atmosphere under the protection of
[0022] Heating through the jacket steam, slowly raising the temperature to 95°C-100°C (the heating process takes 1 hour), and keeping it at this temperature for 0.5 hours, after the metallic so...
example 3
[0027] Pump about 250kg of xylene and 550kg (2.5kmol) of 15-crown-5 into a dry 1500L stainless steel reactor with a condensing reflux system, and replace the closed system with nitrogen for 3 to 5 times. Supplement nitrogen in the kettle to a state slightly higher than normal pressure (0.01-0.02Mpa), then open the vent valve, and quickly add 23kg (1kmol) of metal sodium into the kettle through the manhole under the purging of a slight nitrogen flow, cover Put on the manhole cover, replace the closed system with nitrogen for 5 times, add nitrogen to the kettle for the last time to a state slightly higher than normal pressure (0.01-0.02Mpa), open the open system, so that the entire material and its reaction process are in a nitrogen atmosphere under the protection of
[0028] Heating through the jacket steam, slowly raising the temperature to 95°C-100°C (the heating process takes 1 hour), and keeping it at this temperature for 0.5 hours. First drop a small amount of trimethylch...
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