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    • 9. 发明公开
    • VERFAHREN ZUR GEKOPPELTEN HERSTELLUNG VON TRISILYLAMIN UND POLYSILAZANEN MIT EINER MOLMASSE BIS 500 G/MOL
    • PROCESS FOR PRODUCING耦合三甲硅烷基胺聚硅氮烷的分子量高达500克/摩尔
    • EP3003971A1
    • 2016-04-13
    • EP13727594.7
    • 2013-06-05
    • Evonik Degussa GmbH
    • HOPPE, Carl-FriedrichGÖTZ, ChristianUEHLENBRUCK, GoswinRAULEDER, Hartwig
    • C01B21/087B01D3/14C07F7/02C08G77/62
    • C01B21/087B01D3/143B01J19/24B01J2219/24C08G77/62
    • The invention relates to a method for producing trisilylamine and polysilazanes in the liquid phase by adding ammonia in an overstoichiometric amount in relation to monochlorosilane that is present in an inert solvent. A reaction takes place in which trisilylamine and polysilazanes are produced. TSA is then separated out of the product mixture in gaseous form. The TSA obtained is purified by filtration and distillation and obtained at a high or ultra-high level of purity. The bottom product mixture is conducted out of the reactor through a filter unit, solid ammonium chloride being separated out, and a liquid mixture of polysilazanes and solvent is obtained. Said mixture is fed to a further distillation stage in order to recover solvent. The stoichiometric overdosing of NH
      3 in relation to monochlorosilane means that all the monochlorosilane in the reactor is reacted. This completely prevents the reaction of monochlorosilane with additional disilylamine, which is formed in small amounts, to form solid ammonium chloride in the downstream system parts for purifying the TSA. The solutions filtered downstream of the reactor are correspondingly completely free of solids. The distillation columns used do not contain any solids or deposits at all after the distillation processes are complete.
    • 本发明涉及一种用于在液相中制备三甲硅烷基胺和聚硅氮烷的方法,其中氨在超化学计量相对于量引入至5一氯所有这些是存在于惰性溶剂中。 这里,在这种三甲硅烷基胺和聚硅氮烷的反应形成所得。 TSA随后从产物混合物中分离出来以气态形式。 获得的TSA通过过滤和蒸馏纯化和在高或非常高的纯度得到。 底部产物混合物从反应器通过过滤器单元,其中固体氯化铵被分离出来,得到聚硅氮烷和溶剂的液体混合物输送。 这被馈送到另外的蒸馏以回收溶剂。 由于NH 3的结果在超化学计量相对于量被引入到一氯甲硅烷,一氯硅烷被完全呼叫反应。在反应器中。 这完全阻止一氯硅烷与少量形成,以形成固体氯化铵在下游植物部分用于TSA的纯化附加disilylamine反应。 在反应器下游过滤的溶液是相应不含固体的完全呼叫。