Study On Synthesis And Application Of Amino-silicone Oil Modiifed By Polyether

Generally, hydrophilic amino-silicone oil was a kind of polysiloxane modified by amine andpolyether, bringing polyether segments in the structure of amino modified polysiloxane couldeffectively solve problems of hydrophobic of fabric finished with amino-silicone oil and floatingoil of amino-silicone oil emulsion. But the polyether segments would seriously decrease softnessof cotton fabric finished with amino-silicone oil. Some literatures reported that the size ofpolyether segment and its introduction site in the structure of silicone oil would seriously affecthydrophilic and softness of cotton fabric finished with modified amino-silicone oil. Therefore,two kinds of amino-polysiloxanes modified by polyether（linear amino-silicone modified bypolyether and branched amino-silicone oil modified by polyether） with different structures weresynthesized in this paper in order to obtain a satisfactory amino-polysiloxanes modified bypolyether which possessed good hydrophilic and softness. The detailed contents and results ofresearch are as follows:Part one: The synthesis and characterization of polydimethylsiloxane terminated with epoxygroups and polyether-polydimethylsiloxane terminated with epoxy groups. Polydimethylsiloxaneterminated with epoxy groups was synthesized by hydrosilication reaction withpolydimethylsioxane terminated with hydrogen and allyl glycidyl ether as raw materials. Theepoxy value of intermediate product was determined, and its structure was characterized byFT-IR and¹H-NMR. The results indicated that the epoxy value of synthetic product was3.57×10^-2mol/100g, and the product was proved to be polydimethylsiloxane terminated with epoxygroups by FT-IR and¹H-NMR. Polyether-polydimethylsiloxane terminated with epoxy groupswas synthesized by hydrosilication reaction with polydimethylsioxane terminated with hydrogenand allyl-polyether glycidyl ether as raw materials. The effect of reaction factors on conversionrate of the synthetic product were studied, and the conditions of the synthesis reaction wereoptimized, then the epoxy value of intermediate product was determined; at last, its structure wascharacterized by FT-IR and¹H-NMR. The results indicated that the dosage of catalyst was35ppm, the reaction temperature was75℃, the reaction time was3h, and the amounts ofdissolvent was35%wt; in this moment, the epoxy value of synthetic product was5.47×10^-2mol/100g, and it was proved to be polyether-polydimethylsiloxane terminated with epoxygroups by FT-IR and¹H-NMR. Part two: Study on synthesis and application of linear amino-silicone oil modified bypolyether. Linear amino-silicone oil modified by polyether was synthesized by ring-openingreaction of epoxy groups with polydimethylsiloxane terminated with epoxy groups and polyetherterminated with aminopropyl（ED-600） as raw materials, and it was applied on cotton fabric forhydrophilic and softness. The influences of reaction factors on the intrinsic viscosity of productwere studied, and the conditions of the reaction were optimized, and then, the linearamino-silicone oil modified by polyether was characterized by¹H-NMR and GPC. Beyond that,the influence of molecular weight of polydimethylsiloxane terminated with epoxy group on thesoftness and hydrophilic of cotton fabric finished by linear amino-silicone modified by polyetherwere researched. On that basis, the influence of finished factors of linear amino–siliconemodified by polyether on hydrophilic and softness of the finished fabric were studied, and theconditions of finishing process of the product were optimized, at last, it was compared with theapplication performance of linear amino-silicone modified by polyether, amino-silicone oil andother hydrophilic amino-silicone oil in the market. The results indicated that the synthesisoptimum conditions of linear amino-silicone oil modified by polyether were that the molar ratioof polydimethylsiloxane terminated with epoxy groups to ED-600was1.0:1.2, the reactiontemperature was80℃, the reaction time was6h, and the dissolvent was30%wt, then, the productwhose intrinsic viscosity was0.1747dL/g was got, and its Mn was19574g/mol. It was proved tobe the target we wanted by¹H-NMR and GPC; and more, the linear amino-silicone oil modifiedby polyether synthesized with5328molecular weight of polydimethylsiloxane terminated withepoxy groups possessed better softness and hydrophilic. The optimum conditions of padfinishing process of linear amino-silicone modified by polyether were that dosage of finishingagent was8g/L, baking temperature time was130℃, and baking time was30s, in this moment,the integral area value of finished cotton fabric was4.52, and its wetting time was16s; then itwas compared with the application property of linear amino-silicone modified by polyether andamino-silicone oil, the cotton fabric finished with linear amino-silicone modified by polyetherpossessed poorer softness and washing fastness, but better hydrophilicity and whiteness;however, it was compared with the application property of linear amino-silicone modified bypolyether and other hydrophilic amino-silicone oil （SSC）in the market, the cotton fabric finishedwith linear amino-silicone modified by polyether possessed as good as softness and washing fastness, but poorer hydrophilic.Part three: Study on synthesis and application of branched amino-silicone oil modified bypolyether. Branched amino-silicone oil modified by polyether was synthesized withpolyether-polydimethylsiloxane terminated with epoxy groups and diethylenetriamine（DETA） asraw materials. The influence of reaction factors on conversion ratio of epoxy groups and intrinsicviscosity of product were studied, and the conditions of the reaction were optimized. Themolecular weight of the branched amino-silicone was tested by GPC. On that basis, the influenceof finished factors of branched amino-silicone modified by polyether on hydrophilic and softnessof the finished fabric were studied, and the conditions of finishing process of the product wereoptimized, then, it was compared with the application performance of branched amino-siliconeoil modified by polyether, amino-silicone oil and other hydrophilic amino-silicone in the market.The results indicated that the synthesis optimum conditions of the branched amino-silicone oilmodified by polyether were that the molar ratio of polyether-polydimethylsiloxane terminatedwith epoxy groups to DETA was1.5:1, the reaction temperature was75℃, the reaction time was4h, and the dissolvent was35%wt, in this moment, the conversion ratio of epoxy groups was94%, the intrinsic viscosity of product was0.1252dL/g, and the Mn of product was12137g/mol;at last, the optimum conditions of pad finishing process of branched amino-silicone oil modifiedby polyether were that dosage of finishing agent was10g/L, baking temperature was140℃, andbaking time was30s, in this moment, the stiffness value of finished cotton fabric was1.631cm,its wetting time was0.5s. It was compared with the application property of branchedamino-silicone oil modified by polyether and amino-silicone oil, the cotton fabric finished withbranched amino-silicone modified by polyether possessed poorer softness and washing fastness,but better hydrophilicity and whiteness; however, it was compared with the application propertyof branched amino-silicone oil modified by polyether and other hydrophilic amino-siliconeoil（SSC） in the market, the cotton fabric finished with branched amino-silicone oil modified bypolyether possessed as good as softness and hydrophilic, however, better washing fastness andwhiteness.In conclusion, it was compared with the application property of two kinds ofamino-silicone oil modified by polyether, the hydrophilic of the cotton fabric finished withbranched amino-silicone modified by polyether was improved greatly, the softness and washing fastness was improved a little, and the whiteness was as good as that of linear amino-silicone oilmodified by polyether. Therefore, branched amino-silicone modified by polyether could beconsidered as a better organic silicon hydrophilic softener.