Synthetic method of trisilylamine

• Main Authors: CHEN GANG, LI JUN, HUA YONGJIN, YE XIANGRONG, ZHANG XUEGANG, YANG JIANCHENG
• Format: Patent
• Language: Chinese; English
• Published: 28.09.2018
• Subjects: ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAININGELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN,SULFUR, SELENIUM OR TELLURIUM; CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOIDCHEMISTRY; CHEMISTRY; METALLURGY; ORGANIC CHEMISTRY; PERFORMING OPERATIONS; PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL; THEIR RELEVANT APPARATUS; TRANSPORTING

The invention provides a synthetic method of trisilylamine. The preparation method comprises the following steps: using inert gas for purging a catalytic distillation tower with inert gas in advance,respectively, simultaneously and continuously adding chlorosilane and ammonia in the catalytic distillation tower from a rectifying section and a stripping section in a gaseous state for a reaction, wherein the mol ratio of chlorosilane to ammonia is 1:1.2-3, the space velocity of chlorosilane is 0.5-2/h, the reaction pressure is 0.2-1 MPa, and the reaction temperature of the distillation tower is350-420 DEG C, continuously leading the reaction products in the tower bottom out, separating the material to obtain NH4Cl, and using a widely-known impurity-removal refining technology to obtain thehigh purity trisilylamine. 本发明提供了种三甲硅烷基胺的合成方法，其特征在于所述的制备方法包括以下步骤：提前用惰性气体吹扫催化蒸馏塔，分别同时将氯硅烷和氨以气态形式从精馏段和提馏段连续加入催化蒸馏塔进行反应，所述氯硅烷和氨的摩尔比为1∶1.2-3，氯硅烷空速0.5-2/h,反应压力为0.2-1MPa，蒸馏塔反应温度为350℃-420℃，将塔釜反应产物连续引出，分离出NH4Cl，再经过业内公知的脱杂质精制技术，得到高纯的三甲