• 专利标题:   Continuously producing silazane comprises adding normal-hexane, saturating and passing ammonia gas, dripping trimethylsilyl chloride, adding reaction solution into sodium hydroxide aqueous solution, washing obtained upper layer liquid with hot water and separating organic layer.
  • 专利号:   CN114507253-A
  • 发明人:   ZHANG W
  • 专利权人:   HANGZHOU SIMA CHEM TECHNOLOGY CO LTD
  • 国际专利分类:   B01D067/00, B01D069/10, B01D071/38, C01B032/198, C07F007/10, C07F007/20
  • 专利详细信息:   CN114507253-A 17 May 2022 C07F-007/10 202283 Chinese
  • 申请详细信息:   CN114507253-A CN10065739 20 Jan 2022
  • 优先权号:   CN10065739

▎ 摘  要

NOVELTY - Continuously producing silazane comprises (i) adding normal-hexane into reaction kettle, saturating and passing ammonia gas after three dryings, dripping trimethylsilyl chloride, reacting at 30°C for 4 hours to generate reaction solution, and controlling mol ratio of normal-hexane and trimethylsilyl chloride to be 1.5-1.8:1, where the inlet rate of ammonia is 0.35 l/minute, and (ii) adding reaction solution into a 15% sodium hydroxide aqueous solution, stirring at a constant speed while adding, allowing the solution to stand for separation to remove the lower supernatant, washing the obtained upper layer liquid with hot water at 60-80°C and separating the organic layer, subjecting organic layer to ultrafiltration through an ultrafiltration membrane, and crystallizing the obtained clear liquid after ultrafiltration to obtain silazane. USE - The method is useful for continuously producing silazane. ADVANTAGE - The method: produces silazane having a small degree of hydrolysis in alkaline solution, which can significantly inhibit the progress of the second side reaction; prevents ammonium chloride crystals produced by the first side reaction from depositing on the surface of trimethylsilyl chloride by dropping the reaction material, which affects the reaction process; and increases the yield.