Industrial synthesis method for acetoxylpropyltrimethoxysilane
A technology of acetoxypropyltrimethoxysilane and trichlorosilane, applied in chemical instruments and methods, compounds of group 4/14 elements of the periodic table, organic chemistry, etc., can solve the problem of many addition by-products, Eye irritation, environmental pollution and other problems, to achieve the effect of high yield, simple synthesis process, no environmental pollution
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Embodiment 1
[0038] Add a tetrafluoromagnetic stirring bar into a 500 ml four-neck flask, connect the -10~0°C brine reflux condenser at the middle port, and connect the tail gas to the drying tower. Mix 138.2 g (1.02 mol) trichlorosilane and 100.1 g (1.0 mol) ) allyl acetate is mixed evenly and put into a 250 milliliter constant pressure funnel, put 20 milliliters of mixed raw materials in the flask, then add 0.02 milliliters of prepared main catalyst and co-catalyst to the flask mixed material, turn on the magnetic stirring, and slowly The temperature of the kettle rises to 75°C, open the discharge valve of the constant pressure funnel and start to drop the mixed material. Controlled at 75°C. After the dropwise addition, the temperature of the kettle was raised to 85°C for aging for 2 hours, then the reaction equipment was connected to a distillation device, and 2.7 grams of unreacted excess raw material trichlorosilane was distilled out, and the addition product acetoxysilane was contain...
Embodiment 2
[0041] Add a tetrafluoromagnetic stirring bar into a 2000 ml four-neck flask, connect the -10~0°C brine reflux condenser at the middle port, and connect the tail gas to the drying tower, mix 711.4 grams (5.25 mol) of trichlorosilane and 500.5 grams (5.0 mol) ) allyl acetate is mixed evenly and put into a 250 milliliter constant pressure funnel, put 40 milliliters of mixed raw materials in the flask, then add 0.1 milliliters of the prepared main catalyst and co-catalyst to the flask mixed material, turn on the magnetic stirring, and slowly The temperature of the kettle rises to 75°C, open the discharge valve of the constant pressure funnel and start to drop the mixed material. Controlled at 85°C. After the dropwise addition, the temperature of the kettle was raised to 90°C for 2 hours of heat preservation and aging, then the reaction equipment was connected to a distillation device, and 31.8 grams of unreacted excess raw material trichlorosilane was distilled out, and the addit...
Embodiment 3
[0044] Add a PTFE magnetic stirrer in a 2000ml four-neck flask, connect the -10~0°C brine reflux condenser at the middle port, connect the tail gas to the drying tower, and distill out the unreacted excess raw material trichlorosilane in Example 2 31.8 grams and 679.6 grams of new trichlorosilane, a total of 711.4 grams (5.25mol) of trichlorosilane and 500.5 grams (5.0mol) of allyl acetate are mixed evenly, then put into a 250 ml constant pressure funnel, put 20-40 ml and mix Put the raw materials into the flask, then add 0.1 ml each of the prepared main catalyst and co-catalyst to the mixture in the flask, turn on the magnetic stirring, slowly raise the temperature of the kettle to 75°C, open the discharge valve of the constant pressure funnel and start adding the mixture dropwise. During the addition process, the temperature of the kettle will rise, and there will be a small amount of reflux in the reflux condenser pipe. The dropping rate is controlled for 6 hours with the di...
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