Bis(trimethoxysilylpropyl)amine synthesis

Yield:82985-35-1 461 g

Reaction Conditions:

at 60; for 2 h;Inert atmosphere;

Steps:

1 Example 1.
1. Under a nitrogen atmosphere, add 1100 g of aminopropyltrimethoxysilane to a 2L three-necked flask, raise the temperature to 60 ° C, add 413 g of chloropropyltrimethoxysilane dropwise for 2 hours,After the dropwise addition, the reaction was incubated for 3 hours, and the chlorine content was 46213ppm, which was close to the theoretical value, indicating that the basic reaction was complete. 2. Add 257g of diethylenetriamine to the reaction system and stir at 60 ° C for 1 hour to remove chlorine. 3. After the chlorine removal reaction is completed, cool to 30 ° C and separate out the precipitated diethylenetriamine hydrochloride.A total of 1326g of filtrate was obtained. The chlorine content in the filtrate was 198.65ppm. 4. Ammonia gas was bubbled into the filtrate for 1 hour, and the temperature was controlled at 40 .The ammonium chloride salt was removed by filtration to obtain a bis [(3-trimethoxysilyl) -propyl] amine reaction solution, weighing a total of 1278 g, and detecting the total chlorine content of 17.23 ppm. 5. Distillation of the reaction solution of bis [(3-trimethoxysilyl) -propyl] amine under reduced pressure, when the pressure is controlled to -0.1MPa, and the kettle temperature is 182 ,The finished product of bis [(3-trimethoxysilyl) -propyl] amine is taken out and distilled to a kettle temperature of 205 ° C to stop. A total of 461 g of the finished product of bis [(3-trimethoxysilyl) -propyl] amine was obtained, with a detection purity of 98.65% and a chlorine content of 10.22 ppm.

References:

Zhangjiagang Cathay Huarong Chemical New Materials Co., Ltd.;Liu Lei;Shi Erbo;Chang Nan;Lu Yunlong;Chen Xiaohua;Zhou Mingke CN110835355, 2020, A Location in patent:Paragraph 0028-0029