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Synthesis And Application Of Polyether Block/lons Chain Alkyl Amino Modified Silicone Oil

Posted on:2014-08-26Degree:MasterType:Thesis
Country:ChinaCandidate:J P SunFull Text:PDF
GTID:2251330428463034Subject:Chemical processes
Abstract/Summary:PDF Full Text Request
Amino-modified silicone oil (ASO) has been widely used. Applied in the field of textile finishing, it can impart a unique soft, smooth and comfortable sensation for various kinds of fabrics. However, the fabric treated by ASO is hydrophobic, easy to turn yellow, poor in anti-electrostatic property, and the dyed fabric is difficult to re-work and redye. Introducing the polyether segment into ASO molecules, the hydrophilicity and anti-yellowing capability of treated fabric can be effectively improved.Nowadays, as demands for multifunctional fabric increases, the research has focused on the development of silicone oil with complex function in the field of textile auxiliary. The long chain alkyl and amino co-modified silicone oil can not only render fabrics soft and smooth handle, but also improve the hydrophilic property and increase the fluffy and full sence for treated fabrics.The synthesis and characterization of [AB]nA-type polyether block amino silicone oil were studied in the first part of this thesis. With octamethylcyclo-tetrasiloxane (D4) and tetramethyldisiloxane (TMDS) as raw materials, emathlite as catalyst, hydrogen-terminated polydimethylsiloxane (PHMS) was prepared via equilibrium polymerization in nitrogen atmosphere, and the reaction temperature was60℃, the reaction time was24hrs. The PHMS with four different molecular weight were prepared by adjusting the molar ratio of D4and TMDS. It was found that Si-H had been introduced into two terminals of polydimethysiloxane skeleton by FTIR and.’H NMR analysis. The molecular weight of PHMS was investigated by the ways of hydrogen content tritration,1H NMR and gel permeation chromatography (GPC). The results showed that the molecular weight calculated by tritration and1H NMR was closer to the design of molecular weight, and molecular weight distribution was1.4-1.7by GPC analysis. Then with the chloroplatinic acid/isopropyl alchohol as catalyst, toluene as solvent, epoxy-terminated polydimethylsiloxane was prepared via hydrosilylation reaction of PHMS with allyl glycidyl ether (AGE). The IR absorption peak and’H NMR peak of Si-H in the corresponding spectrums were absolutely disappeared. The product structure was identified by1H NMR and13C NMR, which showed that the PEMS with established structure was synthesized. The molecular weight of PEMS was investigated by the ways of expoxy content tritration,:H NMR and13C NMR. It was showed that Mw of PEMS was slightly higher than PHMS. Finally, twelve [AB]nA-type polyether block amino silicone oil were prepared via ring-opening reaction of PEMS and amino-terminated polyether with different molecular weight.The emulsification process and application performance of homemade polyether block amino silicone oil (PEBASO) were investigated in the second part of this thesis. AB-67-13was emulsified using six kinds of commercially available nonionic surfactants and two self-made emulsifier with HLB≈10.5, respectively. It was found that the emulsion was uniform transparent, and had adequate blue light and good stability using XL-449as emulsifier. Meanwhile, the effect of process conditions including the emulsion method, the emulsifier dosage, pH value of emulsion and emulsification time on the emulsion appearance, stability and appilication performance were also discussed. The results showed that the different process parameters had great impact on the emulsion appearance and stability. The emulsion with uniform transparent appearance and good stability was obtained with the first method,4wt%emulsifier dosage, pH=6and5min in phase inversion emulsification.100%cotton fabric and100%polyether fabric were treated by above-mentioned PEBASO emulsion using optimum emulsifying conditions. The most suitable PEBASO and emulsion concentration were screened by comparing the bending rigidity, crease revovery angle, whiteness and hydrophilic properties treated by different block silicone oil and emulsion concentration, the best choices were AB-69-9(10%) for cotton fabric and AB-137-13(15%) for polyether fabric. The treated fabric feels soft, smooth and comfortabele, the whiteness had little change and the hydrophilic property of fabrics was greatly improved. Finally, the effect of different PEBASO on the color fastness and color shading of dyed cotton fabric was studied. The results indicated that the color fastness had little change, the color strength decreased. The treated fabric was lighter, more green and blue in color, the total aberration was between0.53and1.12.The preparation and application performance of long chain alkyl and amino co-modified silicone oil were researched. With D4, concentrate hydrosilicone oil and hexamethyldisiloxane (MM) as raw metarials, emathlite as the catalyst, the low-hydro silicone oil was prepared via telomerization. Then the epoxy group and long chain alkyl co-modified silicone oil intermediate was synthesized by hydroslylation of low-hydro silicone oil with allyl glycidyl ether and α-olefins (1-octene,1-decene and1-dodecene). At last, the long chain alkyl and amino co-midified silicone oil was synthesized by ring-opening reaction of above-me ntioned intermediate and N,N-dimethyl-1,3-propanediamine. The product structure of each step were identified by FTIR,1H NMR and13C NMR analysis, which indicated that the products with established structure were synthesized.. Then the octyl, decyl or dodecyl and amino co-modified silicone oil (LASO-8, LASO-10and LASO-12) were emulsified, and the emulsion were applied in the finishing process of100%cotton fabric. The observation of field emission scanning electron microscopy (FESEM) showed that the surface of cotton fabric treated by dodecyl and amino co-modified silicone oil changed smooth, and the groove and gap in the surface disappeared or shallowed. It was indicated that the fabric softness slightly decreased. The properties of fabric treated by LASO-12with different amino value and different alkyl value were also discussed. It turned out that the fabric became more soft as the amino value increased, less soft and more fluffy with the alkyl value increased.
Keywords/Search Tags:polyether block amino silicone oil, long chain alkyl, hydrolilylation, silicone oil emulsion, textile finishing, bending rigidity, creasy recovery angle
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