Preparation method of liquid-state polycarbosilane
A polycarbosilane, liquid technology, applied in the field of preparation of liquid polycarbosilane, can solve the problems of limiting the large-scale preparation and application of liquid polycarbosilane, difficult control of the reaction process, difficult operation, etc. The effect of low carbon content and improved safety
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[0031] Example 1
[0032] (1) Add 184 grams of chloromethyltrichlorosilane and 282 grams of hexamethyldisilazane to a Schlenk reactor filled with an inert gas atmosphere in advance, and stir to make the raw materials evenly mixed, then raise the temperature to 50°C, stir And react for 12 hours;
[0033] (2) Add 28 grams of activated magnesium chips to purified and dried tetrahydrofuran, and use a dropping funnel to add the material obtained in step (1), 7.6 grams of chloropropene and a certain amount of 200 mL of tetrahydrofuran. After stirring for 1 hour, a mixed solution of 16.3 grams of chloromethylmethyldichlorosilane and 100 mL of tetrahydrofuran was added to the system using a dropping funnel, the system was heated to 60°C, stirred and reacted for 12 hours.
[0034] (3) Add 19 grams of sodium borohydride, and the reaction temperature is 60°C. Stir for 12 hours after adding sodium borohydride.
[0035] (4) Add petroleum ether, deionized water and concentrated hydrochloric acid....
Example Embodiment
[0039] Example 2
[0040] (1) Add 184 grams of chloromethyltrichlorosilane and 241.5 grams of hexamethyldisilazane to a Schlenk reactor filled with an inert gas atmosphere in advance, and stir to make the raw materials evenly mixed, then raise the temperature to 50°C, stir And react for 12 hours;
[0041] (2) Add 28 grams of activated magnesium chips to purified and dried tetrahydrofuran, and use a dropping funnel to add the material obtained in step (1), 7.6 grams of chloropropene and a certain amount of 200 mL of tetrahydrofuran. After stirring for 1 hour, a mixed solution of 16.3 grams of chloromethylmethyldichlorosilane and 100 mL of tetrahydrofuran was added to the system using a dropping funnel, the system was heated to 60°C, stirred and reacted for 12 hours.
[0042] (3) Add 19 grams of sodium borohydride, and the reaction temperature is 60°C. Stir for 12 hours after adding sodium borohydride.
[0043] (4) Add petroleum ether, deionized water and concentrated hydrochloric aci...
Example Embodiment
[0045] Example 3
[0046] (1) Add 184 grams of chloromethyltrichlorosilane and 282 grams of hexamethyldisilazane to a Schlenk reactor filled with an inert gas atmosphere in advance, and stir to make the raw materials evenly mixed, then raise the temperature to 50°C, stir And react for 12 hours;
[0047] (2) Add 28 grams of activated magnesium chips to purified and dried tetrahydrofuran, and use a dropping funnel to add the material obtained in step (1), 7.6 grams of chloropropene and a certain amount of 200 mL of tetrahydrofuran. After stirring for 1 hour, a mixed solution of 14 grams of chloromethylmethylchlorosilane and 100 mL of tetrahydrofuran was added to the system using a dropping funnel, the system was heated to 60°C, stirred and reacted for 12 hours.
[0048] (3) Add 19 grams of sodium borohydride, and the reaction temperature is 60°C. Stir for 12 hours after adding sodium borohydride.
[0049] (4) Add petroleum ether, deionized water and concentrated hydrochloric acid. Th...
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