Invention Grant
US09446954B2 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
- Patent Title: Process for the coupled preparation of trisilylamine and polysilazanes having a molar mass of up to 500 g/mol
- Patent Title (中): 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
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Application No.: US14345587Application Date: 2013-06-05
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Publication No.: US09446954B2Publication Date: 2016-09-20
- Inventor: Carl-Friedrich Hoppe , Christian Goetz , Goswin Uehlenbruck , Hartwig Rauleder
- Applicant: Carl-Friedrich Hoppe , Christian Goetz , Goswin Uehlenbruck , Hartwig Rauleder
- Applicant Address: DE Essen
- Assignee: Evonik Degussa GmbH
- Current Assignee: Evonik Degussa GmbH
- Current Assignee Address: DE Essen
- Agency: Oblon, McClelland, Maier & Neustadt, L.L.P
- Priority: DE102013209802 20130527
- International Application: PCT/EP2013/061541 WO 20130605
- International Announcement: WO2014/191058 WO 20141204
- Main IPC: C01B21/087
- IPC: C01B21/087 ; B01D3/14 ; C08G77/62 ; B01J19/24

Abstract:
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.
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