Synthesis Of Modified Silicone Oil With Amino-Polyether Terminal And Pendant Group And Preparation Of Its Emulsion

Silicone oil is widely applied to the fields of the agriculture, the military and everyday life. In recent years, the modified silicone oil has become a highlight of auxiliary industry development.Introducing the organic groups such as hydroxyl, amino, epoxy group, polyether chain, carboxyl into silicone oil can improve its physical and chemical properties including hydrophilic, adsorption, softness and reaction activity etc.Because of the high reaction activity, epoxy-modified silicone oil can synthesize the other modified silicone oils as an intermediate production, eg, athe reaction of epoxy-modified silicone with polyether amine can introduce amino-polyether chain in silicone oil. Amino-polyether modified silicone oil has adsorption, compatibility and gives the flexibility and softness to the textile fabrics and fibers as the fourth generation of organic silicone softener. Silicone oil has hydrophilic and self-emulsifying properties owing to introducing polyether chain, which lays the foundation for the later emulsion of modified silicone oil and promoting the forming of microemulsion. In this work, we study the synthesis and properties of the emulsion which on the end-side basing of amino polyether modified silicone oil.(1) 1,3-diglycidylether oxygen radical propyl-1,1,3,3-tetramethyldisiloxane with double-terminated containing epoxy group was prepared, which used tetramethyldisiloxane(HMM) and allylglycidylether(AGE) as raw material, and H2PtCl6-isopropanol as catalyzes(Speier catalysts) by hydrosilylation reaction. With this as the capping agent, epoxy-modified silicone oil with terminal and pendant group was prepared, which used octamethylcyclotetrasiloxane(D4) and 3-glycidylpropyl(dimethoxy) methyl silane as raw material, and the (CH)4NOH as catalyst by the bulk polymerization reaction. Amino-polyether modified silicone oil was obtained by the amination ring-opening of epoxy and amino, through introducing polyether amine. Then the chemical structure of production was characterized by 1HNMR and IR, the above characteristic methods proved the product was prepared.The optimum conditions were: hydrosilylation reaction HMM:AGE molar ratio was 1:2.5, Speier catalyst was lOppm, the reaction temperature was 55℃, and reaction time was 4h; bulk polymerization catalyst was 0.5%, the reaction temperature was 70℃, and reaction time was 4h; amino epoxy ring-opening reaction was in the amount of 50% isopropyl alcohol, epoxy:polyether amine molar ratio was 1:1.2, the reaction temperature was 75℃, and reaction time was 6h.(2)Wih the condition of a series of nonionic surfactant AEO as emulsifier, 2-ethoxyethanol as emulsifier assistant studied the effect of the dosage of emulsifier, ratio and water content on microemulsion of amino-polyether modified silicone oil. Microemulsion was colorless transparent and relatively stable. Emulsion formulations for optimum (silicone oil content 20%):amino polyether-modified silicone oil was 100%-emulsifier was 20%, AEO-3:AEO 9 ratio was 1:1.5, the early stage of the water consumption was 35%, the late water consumption was 345%, and adjust emulsion pH was 6.The above emulsion, and dimethyl silicone oil and amino-polyether modified silicone emulsion in side chain applied to PAN carbon fibers precursor, respectively. And the preoxidation treating was carried out to investigate the surface morphology, and the result of application showed that amino-polyether silicone applied to the surface of fibers could form the better protective layer and improve the defects on the surface of the fibers, therefore, the emulsion was superior to the other two emulsions.