Method for preparing tertiary amine silane
A technology of tertiary aminosilane and secondary amine, which is applied in the purification of tertiary aminosilane and the preparation of organosilicon compounds, can solve the problems of inability to industrialize production, low efficiency, low product yield, etc., and achieves mild reaction conditions and high energy efficiency. Low consumption and high product purity
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Embodiment 1
[0043] 1) Mix 10 kg of anhydrous diethylamine with chlorohydrocarbyl silane (CH 3 O) 2 CH 3 Si(CH 2 ) 3 Cl 10kg is added in the reactor and stirred and mixed, (CH 3 O) 2 CH 3 Si(CH 2 ) 3 Cl and HN(CH 2 CH 3 ) 2 The molar ratio is 1:2.5, protected by nitrogen, heated to 100 ° C for 18 hours, cooled, filtered, and filtered to remove diethylamine hydrochloride HN (CH 2 CH 3 ) 2 HCl, the filtrate is processed in the next step;
[0044] 2) The filtrate of step 1) is distilled to remove excess diethylamine and then cooled to 10°C, according to the product (CH 3 O) 2 CH 3 Si(CH 2 ) 3 N(CH 2 CH 3 ) 2 85% of the molar weight is slowly fed into dry hydrogen chloride gas, keeping the reaction temperature at 10°C, and filtering after completion of the reaction to obtain tertiary aminosilane (CH 3 O) 2 CH 3 Si(CH 2 ) 3 N(CH 2 CH 3 ) 2 The hydrochloride solid, the conversion rate of reaction is about 95%;
[0045] 3) Slowly add anhydrous diethylamine dropwise t...
Embodiment 2
[0047] 1) 10 kg of anhydrous diethylamine, chlorohydrocarbyl silane (CH 2 CH 3 O) 2 CH 3 Si(CH 2 ) 3 Cl 8kg adds in the reactor, (CH 3 CH 2 O) 2 CH 3 Si(CH 2 ) 3 Cl and HN(CH 2 CH 3 ) 2 The molar ratio is 1: 3, nitrogen protection, 120 ℃ reaction 20 hours, after the reaction is completed, filter off diethylamine hydrochloride HN (CH 2 CH 3 ) 2 HCl, the filtrate is processed in the next step;
[0048] 2) After distilling excess diethylamine from the filtrate of step 1), cool down to 5°C, and then press the product (CH 3 CH 2 O) 2 CH 3 Si(CH 2 ) 3 N(CH 2 CH 3 ) 2 80% of the molar weight is passed into dry hydrogen chloride gas, and the reaction temperature is maintained at 5 ° C. After the reaction is completed, filter to obtain tertiary aminosilane (CH 3 CH 2 O) 2 CH 3 Si(CH 2 ) 3 N(CH 2 CH 3 ) 2 The hydrochloride, the reaction conversion rate reaches about 98%;
[0049] 3) Slowly add anhydrous diethylamine dropwise to the salt obtained in step...
Embodiment 3
[0051] 1) Chloroalkylsilane (CH 3 O) 3 Si(CH 2 ) 3 Cl 8kg was added in the reactor, passed into dry dimethylamine 6kg, the temperature was raised to 110°C, and the reaction time was 10 hours, (CH 3 O) 3 Si(CH 2 ) 3 Cl and HN(CH 3 ) 2 The molar ratio is 1: 3.3, after the reaction is completed, filter off dimethylamine hydrochloride HN (CH 3 ) 2 HCl, the filtrate is processed in the next step;
[0052] 2) After the filtrate of step 1) is distilled off excessive dimethylamine, press product (CH 3 O) 3 Si(CH 2 )3 N(CH 3 ) 2 90% of the molar weight is fed into dry hydrogen chloride gas, and the reaction temperature is 20° C. After the reaction is completed, filter to obtain tertiary aminosilane (CH 3 O) 3 Si(CH 2 ) 3 N(CH 3 ) 2 hydrochloride;
[0053] 3) Slowly add anhydrous diethylamine dropwise to the salt obtained in step 2), diethylamine and (CH 3 O) 3 Si(CH 2 ) 3 N(CH 3 ) 2 The molar ratio of hydrochloride is 2:1, the reaction temperature is 10°C, an...
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