Study On The Synthesis Of Several Functional Silane Compounds And Their Gas-Liquid Equilibrium

Organosilane compounds and the silicone materials have many excellent properties,such as high and low temperature resistance,air permeability,water repellency,physiological inertness and oxidation resistance.Therefore,organic silicon materials are widely used in the transportation,electronic information,medical and health,aerospace,light industrial textiles and other fields.Although the new silicone materials have many superior properties as described above,there are still some shortcomings,such as poor oil resistance,poor solvent resistance,strong water absorption,and poor mechanical properties.Using other organic functional groups to completely or partially replace the methyl functional groups of the side groups or end groups of the polysiloxane molecular segment is an effective way to improve the performance defects mentioned above.Organochlorosilane is one of the most important raw materials for the preparation of various silicone polymers and various silicon functional silanes.The Si-Cl bond in organochlorosilane has the properties of both ionic and covalent bonds,and it can react with almost all polar reagents.Therefore,organochlorosilane is often used to synthesize other functional silane compounds.Using organochlorosilane as a raw material,various silicon-functional silanes such as organoalkoxysilane,organosilazane,organosilanol,acyloxysilane,amidosilane,and cyanosilane,can be prepared effectively.In this thesis,the synthetic methods and processes for preparing several functional organosilane compounds initiatiated from chlorosilanes were inveatigated.The gas-liquid phase equilibrium data of prepared silane compounds and other functional compounds are measured with inclined ebulliometer at reduced pressures.The research work conducted in this thesis is listed below:1.A feasibility study of synthesis of ethenyltris(2,2,2-trifluoroethoxy)silane by transesterification method with ethenyltrimethoxysilane and trifluoroethanol as raw materials was explored but no good result was achieved.When alcoholysis reaction between vinyltrichlorosilane and trifluoroethanol was conducted,ethenyltris(2,2,2-trifluoroethoxy)silane with good yield could be obtained.The effects of various factors like the oil bath temperature,feed rate,feed ratio and condensation temperature,on the yield were investigated.Theorthogonal experiment method was further designed to determine the optimal reaction conditions.By means of distillation method,high purity ethenyltris(2,2,2-trifluoroethoxy)silane was acquired.2.The saturated temperature of three fluorine-containing silane compounds,namely,ethenyltris(2,2,2-trifluoroethoxy)silane(tris F-ES),dimethoxymethyl(3,3,3-trifluoropropyl)silane(F-Di MOMS)and trimethoxy(3,3,3-trifluoropropyl)silane(F-Tri MOS),were determined using an inclined ebulliometer from 3.00 to 100.00 k Pa.The experimental data were fitted with the Antoine equation and the Clarke-Glew equation by a weighted least-squares regression method.The critical properties of tris F-ES,F-Di MOMS and F-Tri MOS,including critical temperature,pressure,and volume,were estimated by the group contribution method.3.1,1,3,3-Tetramethyldisilazane was obtained through the reaction of dimethylchlorosilane and ammonia gas at a low temperature.Tris(dimethylsilyl)amine was prepared by 1,1,3,3-tetramethyldisilazane and dimethylchlorosilane under the action of n-butyllithium.These two compounds were separated and purified by distillation.The saturated temperature of 1,1,3,3-tetramethyldisilazane and tris(dimethylsilyl)amine were determined using an inclined ebulliometer from 10.0 to 100.0 k Pa and 5.0 to 100.0 k Pa,respectively.The experimental data were fitted with the Antoine equation and the Clarke-Glew equation by a weighted least-squares regression method.The critical properties and acentric factors were estimated by the group contribution method.4.Tris(methylethylketoxime)phenylsilane were prepared by phenyltrichlorosilane and 2-butanoneoxime.The effects of the solvent type,the amount of solvent and the feed ratio on the synthesis yield were investigated.The refractive index data and the density data of the mixed solutions of 2-butanoneoxime and tris(methylethylketoxime)phenylsilane at different concentrations have been measured.The dependence of density and refractive index on concentration of the pseudo-binary system have been deteremined by nonlinear regression methdo.The purity of the prepared tris(methylethylketoxime)phenylsilane product was further determined by these equations.