PROCESS FOR THE COUPLED PREPARATION OF POLYSILAZANES AND TRISILYLAMINE
    96.
    发明申请
    PROCESS FOR THE COUPLED PREPARATION OF POLYSILAZANES AND TRISILYLAMINE 审中-公开
    多氯联苯和三甲硅烷偶联制备工艺

    公开(公告)号:US20140341794A1

    公开(公告)日:2014-11-20

    申请号:US14212191

    申请日:2014-03-14

    IPC分类号: C01B21/087

    CPC分类号: C01B21/087 C01C1/164

    摘要: The invention relates to a process for preparing trisilylamine and polysilazanes in the liquid phase, in which ammonia dissolved in an inert solvent is initially introduced in a substoichiometric amount relative to monochlorosilane which is likewise present in an inert solvent. The reaction is carried out in a reactor in which trisilylamine formed according to the following equation 4NH3+3H3SiCl→3NH4Cl+(SiH3)3N and polysilazanes are formed. The reactor is subsequently depressurized and TSA is separated off in gaseous form from the product mixture. The TSA obtained is purified by filtration and distillation and obtained in high or very high purity. Further ammonia dissolved in an inert solvent is subsequently introduced into the reactor, using, together with the previously introduced amount of ammonia, a stoichiometric excess of ammonia relative to the amount of MCS previously present. Excess ammonia is subsequently discharged, inert gas is introduced and the bottom product mixture from the reactor is passed through a filter unit, with solid ammonium chloride being separated off and a liquid mixture of polysilazanes and solvent being obtained.

    摘要翻译: 本发明涉及在液相中制备三甲胺和聚硅氮烷的方法,其中溶解在惰性溶剂中的氨相对于同样存在于惰性溶剂中的一氯硅烷,最初以亚化学计量的量引入。 该反应在其中形成根据下列等式4NH 3 + 3H 3 SiCl→3NH 4 Cl +(SiH 3)3 N和聚硅氮烷形成的三乙胺的反应器中进行。 随后将反应器减压,并将TSA从产物混合物中分离出气态。 通过过滤和蒸馏纯化获得的TSA,得到高纯度或非常高的纯度。 随后将溶解在惰性溶剂中的氨加入到反应器中,与先前导入的氨一起使用相对于先前存在的MCS的量的化学计量过量的氨。 随后排出过多的氨,引入惰性气体,将来自反应器的底部产物混合物通过过滤器单元,分离固体氯化铵,得到聚硅氮烷和溶剂的液体混合物。