反应详情

温度

70 °C

A 500 ml 5-neck round-bottom flask, rendered inert with nitrogen and equipped with paddle stirrer, dropping funnel, thermometer, and water separator with reflux condenser, is charged with 70 g (0.5 mol) of methyl-trimethoxysilane (available commercially from Wacker Chemie AG), 6 g (0.05 mol) of trimethylmethoxysilane (prepared in the laboratory by reacting trimethyl-chlorosilane with methanol), and 98.6 g of Isopar E (isoparaffinic hydrocarbon mixture having a boiling range of 113-143° C., available commercially from ExxonMobil). The water separator is filled to the brim with Isopar E. Accompanied by stirring at 300 rpm, a solution of 40.5 g of 50% strength aqueous potassium hydroxide solution (0.36 mol of potassium hydroxide) and 3.2 g of demineralized water is metered in over 6 minutes. During this metered addition, the mixture heats up to 63° C. The mixture is heated to boiling temperature (70° C.). The distillate separates out as the bottom phase in the water separator. Up to a boiling temperature of 118° C., 60.3 g of colorless, slightly turbid distillate are accumulated, and—according to analysis by gas chromatography—contains 84 area % of methanol, 10.8 area % of water, 3.3 area % of Isopar E, and 0.8 area % of trimethylmethoxysilane. The suspension which remains is subsequently evaporated to dryness with stirring under a full oil-pump vacuum (5 hPa) to 70° C. This gives 55.9 g of fine, white, free-flowable powder with a solids content of 99.9% (determined using the HR73 halogen moisture analyzer from Mettler Toledo at 160° C.). A 50% strength aqueous solution prepared with this powder exhibits no precipitation even after being stored at room temperature for two weeks in the absence of air.

1. customA 500 ml 5-neck round-bottom flask, rendered inert with nitrogen
2. customequipped with paddle stirrer
3. temperaturewith reflux condenser
4. customprepared in the laboratory
5. customis metered in over 6 minutes
6. additionDuring this metered addition
7. customheats up to 63° C
8. customThe suspension which remains is subsequently evaporated to dryness
9. stirringwith stirring under a full oil-pump vacuum (5 hPa) to 70° C
10. customat 160° C.
11. customA 50% strength aqueous solution prepared with this powder
12. customno precipitation even
13. waitafter being stored at room temperature for two weeks in the absence of air