纤维表面聚硅氧烷膜的组装与功能化
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摘要
聚硅氧烷界面性能优异,易成膜,附着于纤维基质表面,有修饰、修复、美化纤维观感及触感、改善其功能的作用。近年来,聚有机硅氧烷整理剂领域的研究热点主要集中在新型结构有机硅新品的开发、氟硅共聚物的合成及其潜在应用、用反电荷聚硅氧烷构筑具有特殊油滑手感效应的整理剂超分子等方面。基于此,本论文进行了下列研究工作：
1以N-β-氨乙基-γ-氨丙基聚二甲基硅氧烷(ASO-1)为低表面能成膜物质制备超疏水织物。
(1)以甲苯为溶剂,以微观粗糙的棉纤维作载膜基质,用静态浸渍法成膜,将N-β-氨乙基-γ-氨丙基聚二甲基硅氧烷附着固载在微米尺寸粗糙的织物表面,制得了一种超疏水性棉织物(ASO-1/Fab),其静态接触角可达到150.50。用场发射扫描电镜(FE-SEM)、全反射傅里叶红外光谱(ATR)和X-射线光电子能谱(XPS)研究了ASO-1/Fab的形貌和表面相组成,探索了影响ASO-1/Fab疏水性能的主要因素。结果表明,ASO-1用量、布样浸渍时间以及交联剂可影响ASO-1/Fab的疏水效果。用γ-氨丙基三甲氧基硅烷对ASO-1交联,能使ASO-1/Fab的接触角上升至154.20。
(2)以荷叶表面微纳米结构为模型,用直径(Φ)为30～280.7nm的硅溶胶对棉纤维进行修饰以增加其表面的粗糙度,再以0.25wt%的ASO-1溶液对纤维进行疏水处理,能使处理后织物表面的接触角达到160.5°以上。其中以Φ为280.7nm的硅溶胶与ASO-1协同处理的织物,接触角最大,0可达到165.2°。
(3)用γ-(2,3-环氧丙氧)丙基硅烷改性的Si02与ASO-1反应、或将γ-氨丙基硅改性Si02与环氧基硅油进行反应合成了两种纳米杂化聚硅氧烷ASO-SiO2和PEMS-SiO2,在IR、XPS对其进行结构分析和表征的基础上,重点对两种杂化聚硅氧烷在纤维表面的成膜性及疏水性进行了研究。结果发现,以0.25wt%的ASO-SiO2和PEMS-SiO2处理的织物,接触角可分别达到155.0°和155.3°。
2利用1,3,5-三甲基-1,3,5-三(3,3,3-三氟丙基)环三硅氧烷(D3F)、八甲基环四硅氧烷(D4)与N-β-氨乙基-γ-氨丙基甲基二甲氧基硅烷等单体的本体聚合反应,合成了新型N-β-氨乙基-γ-氨丙基取代的聚甲基(3,3,3-三氟丙基)-co-二甲基硅氧烷共聚物AFMS和AFSO,用IR、1H NMR对AFMS和AFSO的结构进行了表征,并对其进行了应用。结果表明：经0.03wt%AFSO或AFMS甲苯稀溶液处理的棉布样,其接触角可分别达到151.2°和152.0°。用Φ为313.9nm的Si02溶胶先修饰纤维、再AFMS处理,则能使处理后织物表面的接触角达到161.3°。而用Φ为79.7nm和313.9nm的复合硅溶胶修饰纤维、再用AFMS处理,则接触角可达到161.8°。
3利用三氟丙基含氢聚硅氧烷PFHMS与1,1,2-3H-乙烯基全氟癸烯(PFOE)、烯丙基缩水甘油醚(AGE)等单体的硅氢化反应合成了2种反应性环氧基／氟烃基共改性聚硅氧烷(PPT、PPD)和2种聚醚／环氧／氟烃基共改性聚硅氧烷(PFSEAS、PFEAS),用IR、1H NMR表征了产物的结构,然后用AFM等仪器研究了产物的成膜形态以及疏水性能。结果表明：受氟烃基疏水作用及空间效应的影响,长链氟烃基以直立或平伏的方式排列于聚硅氧烷所形成的硅膜表面,从而使聚硅氧烷表面呈现出参差不齐的粗糙形貌。而在氟烃基聚硅氧烷的侧链进一步引入亲水性聚醚基团,可导致硅膜表面有较大聚醚峰包出现、使硅膜表面更加粗糙,但聚醚基团的存在会导致聚硅氧烷膜疏水性能降低。因此,经PPT、PPD整理的棉织物,其静态接触角可分别达到150.40和151.9°。而PFSEAS、PFEAS处理的棉织物,其静态接触角却只有129.2和134.3°。
4利用顺丁烯二酸酐与-γ-氨丙基聚硅氧烷的开环反应合成γ-(N-羧丙烯酰)氨丙基甲基硅氧烷-co-二甲基硅氧烷共聚物(简称羧基硅CAS-2),用AFM等仪器对CAS-2的结构、成膜性以及膜形貌进行了研究。
在此基础上,以乙酸乙酯作为溶剂,将氨基硅ASO-1和羧基硅CAS-2在溶液中静电自组装,再将其负载在纤维和单晶硅表面,获得了一种自组装ASO/CAS超分子膜。用AFM、FE-SEM等研究了ASO/CAS的膜结构、形貌和性能。结果表明,在乙酸乙酯溶液中,将ASO-1和CAS-2等量共混获得的ASO/CAS,微观形貌呈规则有序的窗棂状,膜厚度为2-3层。将ASO/CAS用于纤维织物整理,能明显改善纤维的柔软性能,并使处理后的纤维织物产生独特的油润感。其中最佳柔软性和油润感可在ASO-1与CAS-2质量比为1：1时获得。
Polysiloxanes are low energy materials with good film-forming capacity. When coated and anchored on hydrophilic fiber/fabric surfaces, polysiloxanes not only modify the surface properties of the treated substrates greatly, but also could provide the treated fiber/fabrics with softness, smoothness, hydrophobicity as well as diversified tactile. These excellent properties make the polysiloxanes have been widely used as softeners, lubricants or waterproofing agents in textile industry.
Functional polysiloxanes have presented in textiles for years, but how to design and synthesis new structure polysiloxanes or the polysiloxanes with outstanding performance such as super-hydrophobicity have still attracted the world attention recently. In addition, architecture of super-molecular polysiloxanes which will give special oily handles from counter-charged polysiloxanes such as amino- and carboxyl-containing polysiloxanes, as well as the preparation of super-hydrophobic textile with fluorinated siloxanes and their derivatives have also been active field in the polymeric material. To correspond with these, we have done the following work in the research:
1. To prepare superhydrophobic cotton textile from N-β-aminoethyl-y-aminopropyl substituted polydimethylsiloxane (ASO-1)
(1) Using N-β-aminoethyl-y-aminopropyl substituted poly dimethyl siloxane (ASO-1) as hydrophobic material and as solvent, a soft but hydrophobic cotton fabrics (ASO-1/Fab) with a water contact angle (CA) of 150.5°was prepared by dipping the fabric, with a rough surface on nano- meter scale, in ASO-1-toluene solution for several seconds, then dried and cured at 170℃. Surface composition and morphology of ASO-1/Fab were characterized and investigated by field emission scanning electron microscope (FESEM), attenuated total reflectance (ATR) infrared spectrum, X-ray photoelectron spectroscopy (XPS), and so on. And the influencing factors on ASO-1/fab superhydrophobic property were also investigated. It was discovered that the dosage of ASO-1, and the immersing time of fabric in ASO-1-toluene solution as well as the amount of cross-linking agent could influence the super-hydrophobicity of ASO-1/Fab. As a result, an optimum CA of ASO-1/Fab was obtained by co-operation of ASO-1 with y-aminopropyltrimethoxysilane.
(2) Water contact angles of treated cotton fabrics could be improved by using ASO-1 and the roughed cotton substrates by SiO2 sols. The experiment results showed the CA, which were more than 160.5°, had been successfully obtained from the cotton fabrics treated by 0.25wt% ASO-1 solution and SiO2 sols with diameters of 30-280.7nm. When the diameter of SiO2 sol increased 280.7nm, the CA of the treated fabrics could reach to 165.2°.
(3) In order to further improve the hydrophobicity of ASO-1 and enhance the fixation of nano-SiO2 on fabrics, two nano-SiO2 hybrid polysiloxanes, ASO-SiO2 (which was prepared from ASO-1 and y-(2,3-epoxypropoxy)propylsilane modified nano-SiO2) and PEMS-SiO2 (which was prepared from ASO-1 and y-aminopropyltrimethoxysilane modified nano-SiO2) were prepared and used to treat cotton fabrics in the experiment. Composition and hydrophobic properties of the two nano-hybrid polysiloxanes were investigated by IR, XPS and other instruments. Experiment results indicated that such hybrid polysiloxanes could impart the treated cotton fabrics with an improved hydrophobicity. The CAs of the treated fabrics were 155.0°for 0.25wt% ASO-SiO2 and 155.3°for 0.25wt% PEMS-SiO2, respectively.
2 Novel N-β-aminoethyl-y-aminopropyl-substituted poly [methyl (3,3,3-trifluoropropyl)]-co-dimethylsiloxane copolymers AFMS and AFSO were prepared by bulk polymerization of 1,3,5-trimethyl-1,3,5-tri(3,3,3-trifluoropropyl) cyclotrisiloxane (D3F) with N-β-aminoethyl-y-aminopropylmethyldimethoxysilane and other monomers. Structure of AFMS and AFSO was characterized by IR and 1H-NMR and performance properties were studied. The results indicated contact angles of the fabrics treated with 0.25wt% AFSO and AFMS in toluene solution could reach to 151.2°and 152.0°, respectively. And moreover, CAs could enhanced to 161.3°nd 161.8°if the cotton fabric was pretreated with SiO2 sol (with a diameter of 313.9nm) or with a mixed silica sol (with diameters of 79.7nm and 313.9nm) before 0.25wt% AFMS solution treatment.
3 Two kinds of reactive epoxy/fluorinated long alkyl modified polysiloxanes (PPT and PPD) and another two reactive polysiloxanes (PFSEAS and PFEAS) with epoxy/polyether/ fluorinated long alkyl groups were prepared by hydrosilylation of poly(hydrogen methylsiloxane-co-trifluoropropyl methylsiloxane) (PFHMS) with 1,1,2-trihydrogen vinyl perfluorodecene (PFOE) and allyl glycidyl ether (AGE) and other monomers. Structure and film morphology as well as hydrophobicity of the synthesized polysiloxanes on cotton fabrics were characterized and investigated by IR,1H-NMR, AFM and so on. Influenced by hydro-/lipo-phobic property as well as the spatial effect of the fluorinated long alkyl groups, and long fluorohydrocarbon groups were distributed on the film surface uprightly or slantingly, resulting in a jagged rough morphology on the treated substrate surface. When polyether groups were introduced in the side chain of fluorinated polysiloxanes, larger aggregates derived from polyether groups were observed on the polysiloxane film, leading to a rougher surface. However, polyether groups could decrease hydrophobicity of the polysiloxane film. As a result, CAs of the fabrics treated with PPT and PPD were 150.4°and 151.9°, while CAs of the fabrics treated with PFSEAS and PFEAS were only 129.2°and 134.3°, respectively.
4 y-(N-carboxylacrylate) aminopropylmethylsiloxane-co-dimethyl-siloxane copolymer(carboxylpolysiloxane for short, CAS) was prepared by ring-opening action of cis-butenedioic anhydride and y-aminopropyl polysiloxane. AFM and other instruments were used to characterize and investigate its structure, film-forming ability and morphology.
On this basis, with ethyl acetate used as solvent, ASO and CAS were assembled through antistatic interaction, then anchored on the fiber and silica substrates and ASO/CAS supermolecular film was obtained, film structure, morphology and performance of which were investigated by AFM, FE-SEM and other instruments. The results indicated that ASO/CAS, formed by blending equivalent amount of ASO and CAS in ethyl acetate solution, showed a highly ordered, window grating-like structure in micro-morphology, with a assembly-layer number of 2～3. When used for cotton fabric finishing, ASO/CAS could improve softness of the fabric obviously, with a unique oily handle exhibited. The optimum softness and unique oily handle can be obtained only when the mass ratio of ASO to CAS is 1:1.
1以N-β-氨乙基-γ-氨丙基聚二甲基硅氧烷(ASO-1)为低表面能成膜物质制备超疏水织物。
(1)以甲苯为溶剂,以微观粗糙的棉纤维作载膜基质,用静态浸渍法成膜,将N-β-氨乙基-γ-氨丙基聚二甲基硅氧烷附着固载在微米尺寸粗糙的织物表面,制得了一种超疏水性棉织物(ASO-1/Fab),其静态接触角可达到150.50。用场发射扫描电镜(FE-SEM)、全反射傅里叶红外光谱(ATR)和X-射线光电子能谱(XPS)研究了ASO-1/Fab的形貌和表面相组成,探索了影响ASO-1/Fab疏水性能的主要因素。结果表明,ASO-1用量、布样浸渍时间以及交联剂可影响ASO-1/Fab的疏水效果。用γ-氨丙基三甲氧基硅烷对ASO-1交联,能使ASO-1/Fab的接触角上升至154.20。
(2)以荷叶表面微纳米结构为模型,用直径(Φ)为30～280.7nm的硅溶胶对棉纤维进行修饰以增加其表面的粗糙度,再以0.25wt%的ASO-1溶液对纤维进行疏水处理,能使处理后织物表面的接触角达到160.5°以上。其中以Φ为280.7nm的硅溶胶与ASO-1协同处理的织物,接触角最大,0可达到165.2°。
(3)用γ-(2,3-环氧丙氧)丙基硅烷改性的Si02与ASO-1反应、或将γ-氨丙基硅改性Si02与环氧基硅油进行反应合成了两种纳米杂化聚硅氧烷ASO-SiO2和PEMS-SiO2,在IR、XPS对其进行结构分析和表征的基础上,重点对两种杂化聚硅氧烷在纤维表面的成膜性及疏水性进行了研究。结果发现,以0.25wt%的ASO-SiO2和PEMS-SiO2处理的织物,接触角可分别达到155.0°和155.3°。
2利用1,3,5-三甲基-1,3,5-三(3,3,3-三氟丙基)环三硅氧烷(D3F)、八甲基环四硅氧烷(D4)与N-β-氨乙基-γ-氨丙基甲基二甲氧基硅烷等单体的本体聚合反应,合成了新型N-β-氨乙基-γ-氨丙基取代的聚甲基(3,3,3-三氟丙基)-co-二甲基硅氧烷共聚物AFMS和AFSO,用IR、1H NMR对AFMS和AFSO的结构进行了表征,并对其进行了应用。结果表明：经0.03wt%AFSO或AFMS甲苯稀溶液处理的棉布样,其接触角可分别达到151.2°和152.0°。用Φ为313.9nm的Si02溶胶先修饰纤维、再AFMS处理,则能使处理后织物表面的接触角达到161.3°。而用Φ为79.7nm和313.9nm的复合硅溶胶修饰纤维、再用AFMS处理,则接触角可达到161.8°。
3利用三氟丙基含氢聚硅氧烷PFHMS与1,1,2-3H-乙烯基全氟癸烯(PFOE)、烯丙基缩水甘油醚(AGE)等单体的硅氢化反应合成了2种反应性环氧基／氟烃基共改性聚硅氧烷(PPT、PPD)和2种聚醚／环氧／氟烃基共改性聚硅氧烷(PFSEAS、PFEAS),用IR、1H NMR表征了产物的结构,然后用AFM等仪器研究了产物的成膜形态以及疏水性能。结果表明：受氟烃基疏水作用及空间效应的影响,长链氟烃基以直立或平伏的方式排列于聚硅氧烷所形成的硅膜表面,从而使聚硅氧烷表面呈现出参差不齐的粗糙形貌。而在氟烃基聚硅氧烷的侧链进一步引入亲水性聚醚基团,可导致硅膜表面有较大聚醚峰包出现、使硅膜表面更加粗糙,但聚醚基团的存在会导致聚硅氧烷膜疏水性能降低。因此,经PPT、PPD整理的棉织物,其静态接触角可分别达到150.40和151.9°。而PFSEAS、PFEAS处理的棉织物,其静态接触角却只有129.2和134.3°。
4利用顺丁烯二酸酐与-γ-氨丙基聚硅氧烷的开环反应合成γ-(N-羧丙烯酰)氨丙基甲基硅氧烷-co-二甲基硅氧烷共聚物(简称羧基硅CAS-2),用AFM等仪器对CAS-2的结构、成膜性以及膜形貌进行了研究。
在此基础上,以乙酸乙酯作为溶剂,将氨基硅ASO-1和羧基硅CAS-2在溶液中静电自组装,再将其负载在纤维和单晶硅表面,获得了一种自组装ASO/CAS超分子膜。用AFM、FE-SEM等研究了ASO/CAS的膜结构、形貌和性能。结果表明,在乙酸乙酯溶液中,将ASO-1和CAS-2等量共混获得的ASO/CAS,微观形貌呈规则有序的窗棂状,膜厚度为2-3层。将ASO/CAS用于纤维织物整理,能明显改善纤维的柔软性能,并使处理后的纤维织物产生独特的油润感。其中最佳柔软性和油润感可在ASO-1与CAS-2质量比为1：1时获得。
Polysiloxanes are low energy materials with good film-forming capacity. When coated and anchored on hydrophilic fiber/fabric surfaces, polysiloxanes not only modify the surface properties of the treated substrates greatly, but also could provide the treated fiber/fabrics with softness, smoothness, hydrophobicity as well as diversified tactile. These excellent properties make the polysiloxanes have been widely used as softeners, lubricants or waterproofing agents in textile industry.
Functional polysiloxanes have presented in textiles for years, but how to design and synthesis new structure polysiloxanes or the polysiloxanes with outstanding performance such as super-hydrophobicity have still attracted the world attention recently. In addition, architecture of super-molecular polysiloxanes which will give special oily handles from counter-charged polysiloxanes such as amino- and carboxyl-containing polysiloxanes, as well as the preparation of super-hydrophobic textile with fluorinated siloxanes and their derivatives have also been active field in the polymeric material. To correspond with these, we have done the following work in the research:
1. To prepare superhydrophobic cotton textile from N-β-aminoethyl-y-aminopropyl substituted polydimethylsiloxane (ASO-1)
(1) Using N-β-aminoethyl-y-aminopropyl substituted poly dimethyl siloxane (ASO-1) as hydrophobic material and as solvent, a soft but hydrophobic cotton fabrics (ASO-1/Fab) with a water contact angle (CA) of 150.5°was prepared by dipping the fabric, with a rough surface on nano- meter scale, in ASO-1-toluene solution for several seconds, then dried and cured at 170℃. Surface composition and morphology of ASO-1/Fab were characterized and investigated by field emission scanning electron microscope (FESEM), attenuated total reflectance (ATR) infrared spectrum, X-ray photoelectron spectroscopy (XPS), and so on. And the influencing factors on ASO-1/fab superhydrophobic property were also investigated. It was discovered that the dosage of ASO-1, and the immersing time of fabric in ASO-1-toluene solution as well as the amount of cross-linking agent could influence the super-hydrophobicity of ASO-1/Fab. As a result, an optimum CA of ASO-1/Fab was obtained by co-operation of ASO-1 with y-aminopropyltrimethoxysilane.
(2) Water contact angles of treated cotton fabrics could be improved by using ASO-1 and the roughed cotton substrates by SiO2 sols. The experiment results showed the CA, which were more than 160.5°, had been successfully obtained from the cotton fabrics treated by 0.25wt% ASO-1 solution and SiO2 sols with diameters of 30-280.7nm. When the diameter of SiO2 sol increased 280.7nm, the CA of the treated fabrics could reach to 165.2°.
(3) In order to further improve the hydrophobicity of ASO-1 and enhance the fixation of nano-SiO2 on fabrics, two nano-SiO2 hybrid polysiloxanes, ASO-SiO2 (which was prepared from ASO-1 and y-(2,3-epoxypropoxy)propylsilane modified nano-SiO2) and PEMS-SiO2 (which was prepared from ASO-1 and y-aminopropyltrimethoxysilane modified nano-SiO2) were prepared and used to treat cotton fabrics in the experiment. Composition and hydrophobic properties of the two nano-hybrid polysiloxanes were investigated by IR, XPS and other instruments. Experiment results indicated that such hybrid polysiloxanes could impart the treated cotton fabrics with an improved hydrophobicity. The CAs of the treated fabrics were 155.0°for 0.25wt% ASO-SiO2 and 155.3°for 0.25wt% PEMS-SiO2, respectively.
2 Novel N-β-aminoethyl-y-aminopropyl-substituted poly [methyl (3,3,3-trifluoropropyl)]-co-dimethylsiloxane copolymers AFMS and AFSO were prepared by bulk polymerization of 1,3,5-trimethyl-1,3,5-tri(3,3,3-trifluoropropyl) cyclotrisiloxane (D3F) with N-β-aminoethyl-y-aminopropylmethyldimethoxysilane and other monomers. Structure of AFMS and AFSO was characterized by IR and 1H-NMR and performance properties were studied. The results indicated contact angles of the fabrics treated with 0.25wt% AFSO and AFMS in toluene solution could reach to 151.2°and 152.0°, respectively. And moreover, CAs could enhanced to 161.3°nd 161.8°if the cotton fabric was pretreated with SiO2 sol (with a diameter of 313.9nm) or with a mixed silica sol (with diameters of 79.7nm and 313.9nm) before 0.25wt% AFMS solution treatment.
3 Two kinds of reactive epoxy/fluorinated long alkyl modified polysiloxanes (PPT and PPD) and another two reactive polysiloxanes (PFSEAS and PFEAS) with epoxy/polyether/ fluorinated long alkyl groups were prepared by hydrosilylation of poly(hydrogen methylsiloxane-co-trifluoropropyl methylsiloxane) (PFHMS) with 1,1,2-trihydrogen vinyl perfluorodecene (PFOE) and allyl glycidyl ether (AGE) and other monomers. Structure and film morphology as well as hydrophobicity of the synthesized polysiloxanes on cotton fabrics were characterized and investigated by IR,1H-NMR, AFM and so on. Influenced by hydro-/lipo-phobic property as well as the spatial effect of the fluorinated long alkyl groups, and long fluorohydrocarbon groups were distributed on the film surface uprightly or slantingly, resulting in a jagged rough morphology on the treated substrate surface. When polyether groups were introduced in the side chain of fluorinated polysiloxanes, larger aggregates derived from polyether groups were observed on the polysiloxane film, leading to a rougher surface. However, polyether groups could decrease hydrophobicity of the polysiloxane film. As a result, CAs of the fabrics treated with PPT and PPD were 150.4°and 151.9°, while CAs of the fabrics treated with PFSEAS and PFEAS were only 129.2°and 134.3°, respectively.
4 y-(N-carboxylacrylate) aminopropylmethylsiloxane-co-dimethyl-siloxane copolymer(carboxylpolysiloxane for short, CAS) was prepared by ring-opening action of cis-butenedioic anhydride and y-aminopropyl polysiloxane. AFM and other instruments were used to characterize and investigate its structure, film-forming ability and morphology.
On this basis, with ethyl acetate used as solvent, ASO and CAS were assembled through antistatic interaction, then anchored on the fiber and silica substrates and ASO/CAS supermolecular film was obtained, film structure, morphology and performance of which were investigated by AFM, FE-SEM and other instruments. The results indicated that ASO/CAS, formed by blending equivalent amount of ASO and CAS in ethyl acetate solution, showed a highly ordered, window grating-like structure in micro-morphology, with a assembly-layer number of 2～3. When used for cotton fabric finishing, ASO/CAS could improve softness of the fabric obviously, with a unique oily handle exhibited. The optimum softness and unique oily handle can be obtained only when the mass ratio of ASO to CAS is 1:1.
引文
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