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    PROCESS FOR THE COUPLED PREPARATION OF POLYSILAZANES AND TRISILYLAMINE
    2.
    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

    申请人： Carl-Friedrich Hoppe ,  Christian Goetz ,  Hartwig Rauleder ,  Goswin Uehlenbruck

    发明人： Carl-Friedrich Hoppe ,  Christian Goetz ,  Hartwig Rauleder ,  Goswin Uehlenbruck

    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。

    Process for the coupled preparation of trisilylamine and polysilazanes having a molar mass of up to 500 g/mol
    3.
    发明授权
    Process for the coupled preparation of trisilylamine and polysilazanes having a molar mass of up to 500 g/mol 有权
    具有摩尔质量高达500g / mol的三甲胺和聚硅氮烷的偶联制备方法

    公开(公告)号：US09446954B2

    公开(公告)日：2016-09-20

    申请号：US14345587

    申请日：2013-06-05

    申请人： Carl-Friedrich Hoppe ,  Christian Goetz ,  Goswin Uehlenbruck ,  Hartwig Rauleder

    发明人： Carl-Friedrich Hoppe ,  Christian Goetz ,  Goswin Uehlenbruck ,  Hartwig Rauleder

    IPC分类号： C01B21/087 ,  B01D3/14 ,  C08G77/62 ,  B01J19/24

    CPC分类号： C01B21/087 ,  B01D3/143 ,  B01J19/24 ,  B01J2219/24 ,  C08G77/62

    摘要： The invention relates to a process for preparing trisilylamine and polysilazanes in the liquid phase, in which ammonia is introduced in a superstoichiometric amount relative to 5 monochlorosilane which is present in an inert solvent. Here, a reaction in which trisilylamine and polysilazanes are formed proceeds. TSA is subsequently 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. The bottom product mixture is conveyed from the reactor through a filter unit in which solid ammonium chloride is separated off to give a liquid mixture of polysilazanes and solvent. This is fed to a further distillation to recover solvent. As a result of the NH3 being introduced in a superstoichiometric amount relative to monochlorosilane, monochlorosilane is completely reacted in the reactor. This completely prevents the reaction of monochlorosilane with additional disilylamine formed in small amounts to form solid ammonium chloride in the downstream plant parts for purification of the TSA. The solutions filtered downstream of the reactor are accordingly completely free of solids.

    摘要翻译： 本发明涉及一种在液相中制备三甲胺和聚硅氮烷的方法，其中相对于存在于惰性溶剂中的5个一氯硅烷，以超化学计量的量引入氨。 这里，形成三甲基胺和聚硅氮烷的反应。 TSA随后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。 底部产物混合物从反应器通过过滤器单元输送，其中分离固体氯化铵以得到聚硅氮烷和溶剂的液体混合物。 将其进料进一步蒸馏以回收溶剂。 作为相对于一氯硅烷以超化学计量量引入NH 3的结果，一氯硅烷在反应器中完全反应。 这完全防止一氯甲硅烷与少量形成的另外的二甲硅烷的反应在下游的植物部分中形成固体氯化铵，用于纯化TSA。 因此，在反应器下游过滤的溶液完全不含固体。