Method for preparing 1,1,3,3-tetramethyldisiloxane
A technology of tetramethyldisiloxane and silicochlorosilane, which is applied in chemical instruments and methods, compounds of group 4/14 elements of the periodic table, silicon organic compounds, etc., and can solve production stoppage, storage blockage, limited production capacity, etc. problems, to achieve the effect of comprehensive cost of environmental protection, simple process and low flash point
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Embodiment 1
[0062] Add 500g of organic silicochlorosilane low boilers to a dry 1000mL four-necked flask, and when the temperature of the ice machine is controlled to drop to 0°C, add 55g of methanol into the dropping bottle, and add dropwise when the temperature in the flask is cooled to 10°C. The tail gas is discharged into the acid water pool for absorption, the dripping flow rate is controlled at 300g / h, the heating device is turned on and the temperature is raised to rapidly rectify and extract fractions less than 40°C, M 2 The H utilization rate was 92.3%. . Weigh 300g of water and add it to a dry 1000mL four-necked bottle. When the temperature of the ice machine drops to 3°C, pour 168g of the distillate fraction below 40°C into the dripping bottle and start adding fractions. The flow rate of the addition is controlled. At 472g / h, control the reaction temperature at 8°C, balance for 0.5h after the dropwise addition, let it stand for 5min to remove the acid water in the lower layer, ...
Embodiment 2
[0071] Add 500g of organic silicochlorosilane low boilers to a dry 1000mL four-necked flask, and when the temperature of the ice machine is controlled to drop to 0°C, add 55g of methanol into the dropping bottle, and add dropwise when the temperature in the flask is cooled to 10°C. The tail gas is discharged into the acid water pool for absorption, the dripping flow rate is controlled at 300g / h, the heating device is turned on and the temperature is raised to rapidly rectify and extract fractions less than 40°C, M 2 The H utilization rate was 93.9%. . Weigh 300g of water and add it to a dry 1000mL four-necked bottle. When the temperature of the ice machine drops to 3°C, pour 168g of the distillate fraction below 40°C into the dripping bottle and start adding fractions. The flow rate of the addition is controlled. At 472g / h, control the reaction temperature at 8°C, balance for 0.5h after the dropwise addition, let it stand for 5min to remove the acid water in the lower layer, ...
Embodiment 3
[0073] Add 600g of organic silicon chlorosilane low boilers to a dry 1000mL four-necked flask, and when the temperature of the ice machine is controlled to drop to 0°C, add 50g of ethanol to the dropwise addition bottle, and add dropwise when the temperature in the flask is cooled to 10°C. The tail gas is discharged into the acid water pool for absorption, the dripping flow rate is controlled at 250g / h, the heating device is turned on and the temperature is raised to rapidly rectify and extract fractions less than 40°C, M 2 The H utilization rate was 95.1%. . Weigh 300g of water and add it to a dry 1000mL four-necked bottle. When the temperature of the ice machine drops to 3°C, pour 150g of fractions less than 40°C into the dropping bottle and start adding fractions. At 490g / h, control the reaction temperature at 8°C at the same time, after the dropwise addition, balance for 0.5h, let it stand for 5min to remove the acid water in the lower layer, collect the oil phase in a gl...
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