无皂聚丙烯酸酯/纳米SiO_2复合乳液的合成、性能及其聚合机理的研究
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摘要
聚丙烯酸酯是皮革涂饰材料中应用广泛的一类成膜物质。近年来制革工业对涂饰材料各项性能的要求不断提高,如耐水性、耐溶剂性,涂饰后革样的卫生性能、透明度及真皮感等。本课题的研究就是为了满足上述要求而提出来的,期望在两亲性共聚物作为稳定剂的条件下,采用无皂乳液聚合法同时引入无机纳米SiO_2粉体合成聚丙烯酸酯/纳米SiO_2复合乳液;并在此基础上,简化合成工艺,同步采用无皂乳液聚合法和溶胶-凝胶法原位合成性能良好的聚丙烯酸酯/纳米SiO_2复合乳液。
首先合成了二元两亲性共聚物聚丙烯酸丁酯/丙烯酸钠[P(BA/AANa)]和三元两亲性共聚物聚丙烯酸丁酯/醋酸乙烯酯/丙烯酰胺[P(BA/VAc/AM)],并采用红外光谱(FTIR)、差示扫描量热(DSC)和透射电镜(TEM)等检测手段对两种两亲性共聚物的结构进行了表征。分别以P(BA/AANa)和P(BA/VAc/AM)为稳定剂,采用表面带有不饱和双键的纳米SiO_2粉体与丙烯酸酯类单体通过无皂乳液聚合法原位合成了聚甲基丙烯酸甲酯/丙烯酸丁酯/丙烯酸钠[P(MMA/BA/AANa)]/纳米SiO_2复合乳液和聚甲基丙烯酸甲酯/丙烯酸丁酯/醋酸乙烯酯/丙烯酰胺[P(MMA/BA/VAc/AM)]/纳米SiO_2复合乳液;通过单因素实验法优化了这两种纳米复合乳液的合成条件。以P(BA/VAc/AM)为稳定剂,采用正硅酸乙酯(TEOS)和丙烯酸酯类单体通过无皂乳液聚合法和溶胶-凝胶法原位合成了ES-P(MMA/BA/VAc/AM)/纳米SiO_2复合乳液;通过单因素实验法优化了该纳米复合乳液的合成条件。采用FTIR、DSC和TEM等检测手段分别对P(MMA/BA/AANa)/纳米SiO_2复合乳液、P(MMA/BA/VAc/AM)/纳米SiO_2复合乳液和ES-P(MMA/BA/VAc/AM)/纳米SiO_2复合乳液的结构进行了表征。分别将这三种纳米复合乳液应用于皮革涂饰,对涂饰后革样的各项性能进行了检测。最后对ES-P(MMA/BA/VAc/AM)/纳米SiO_2复合乳液的合成过程进行了动力学研究,通过动态激光光散射(DLS)和TEM检测推断出该纳米复合乳液的聚合机理。
二元两亲性共聚物P(BA/AANa)的最优合成条件为:丙烯酸质量分数(以单体总质量计)5%,引发体系过硫酸铵-亚硫酸氢钠。三元两亲性共聚物P(BA/VAc/AM)的最优合成条件为:丙烯酰胺质量分数(以单体总质量计)14%,n(VAc):n(BA)=1:1,反应温度90℃,过硫酸铵-亚硫酸氢钠质量分数(以单体总质量计)6%。
P(MMA/BA/AANa)/纳米SiO_2复合乳液的最优合成条件为:n(BA):n(MMA)=2:1,pH为7,过硫酸钾质量分数(以单体总质量计)2%,反应温度85℃,纳米SiO_2质量分数(以单体总质量计)2%。P(MMA/BA/AANa)/纳米SiO_2复合乳液涂饰后革样与P(MMA/BA/AANa)涂饰后革样相比:透气性增加了376.19%,透水汽性提高了7.78%,吸水率降低了16.31%,耐湿擦性达到3级,耐干擦性均达到4～5级,常温耐屈挠性均达到2万次。
P(MMA/BA/VAc/AM)/纳米SiO_2复合乳液的最优合成条件为:纳米SiO_2粉体为表面带有不饱和双键的纳米SiO_2,纳米SiO_2粉体质量分数(以单体总质量计)1.5%。P(MMA/BA/VAc/AM)/纳米SiO_2复合乳液涂饰后革样与P(MMA/BA/VAc/AM)涂饰后革样相比:透气性增加了109.92%,透水汽性提高了16.49%,吸水率降低了56.19%,耐湿擦性达到2～3级,耐干擦性均达到4～5级,常温耐屈挠性均达到5万次。
同步采用无皂乳液聚合法和溶胶-凝胶法制备的ES-P(MMA/BA/VAc/AM)/纳米SiO_2复合乳液的最优合成条件为:反应温度75℃,反应时间2h,n(BA):n(MMA)=3:2,过硫酸钾质量分数(以单体总质量计)3%,正硅酸乙酯质量分数(以单体总质量计)5%,乙烯基三甲氧基硅烷质量分数(以单体总质量计)4%。
ES-P(MMA/BA/VAc/AM)/纳米SiO_2复合乳液的实验室应用结果表明:与P(MMA/BA/VAc/AM)乳液涂饰后革样相比,透气性提高了285.39%,透水汽性提高了49.01%,吸水率降低了18.47%,动态防水性提高了17.71%,耐湿擦性均达到1级,耐干擦性均达到4～5级,常温耐屈挠性均达到10万次。
ES-P(MMA/BA/VAc/AM)/纳米SiO_2复合乳液的工厂应用结果表明:与厂内大生产用聚丙烯酸酯乳液涂饰后革样相比,涂饰后革样的耐溶剂性有所提高(擦拭20次),柔软度和粘着牢度无明显差异,离板性相近,丰满性较好,粘性略低。
ES-P(MMA/BA/VAc/AM)/纳米SiO_2复合乳液的反应活化能E_a为44.154kJ/mol,聚合反应过程中的反应速率R_p∝[I]~(1.716)[m]~(0.33)。该纳米复合乳液的整个聚合过程遵循了均相成核机理。
Acrylic resin was widely used as the leather finishing materials. Recently,much better properties of acrylic resin, such as better water-resistance,solvent-resistance, hygiene properties and corium feeling, were desirable for theleather finish market. This thesis was mainly focused on the study of acrylicresin/nano-SiO_2 composite emulsion prepared via emulsifier-free emulsionpolymerization, based on the amphiphlic copolymer. Besides, acrylicresin/nano-SiO_2 composite emulsion with the excellent properties systhesized viain-situ emulsifier-free emulsion polymerization and sol-gel method in one step inorder to simplify the systhesis process.
Poly(butyl acrylate/acrylic acid sodium)P(BA/AANa) and Poly(butylacrylate/vinyl acetate/acrylamide)P(BA/VAc/AM) were prepared at first. Thestructures of both amphiphlic copolymers were investigated by FourierTransform Infrared Spectroscopy(FTIR), Differential ScanningCalorimetry(DSC) and Transmission Electron Microscopy (TEM). Poly(methylmethacrylate/butyl acrylate/acrylic acid sodium)P(MMA/BA/AANa)/nano-SiO_2composite emulsion and Poly(methyl methacrylate/butyl acrylate/vinylacetate/acrylamide)P(MMA/BA/VAc/AM)/nano-SiO_2 composite emulsion weresynthesized via in-situ emulsifier-free emulsion polymerization, based onP(BA/AANa)and P(BA/VAc/AM) dividedly. P(MMA/BA/VAc/AM)/nano-SiO_2composite emulsion was obtained via both emulsifier-free emulsionpolymerization and sol-gel method in one step, on the basis of P(BA/VAc/AM). P(MMA/BA/AANa)/nano-SiO_2 composite, P(MMA/BA/VAc/AM)/nano-SiO_2composite and ES-P(MMA/BA/VAc/AM)/nano-SiO_2 composite werecharacterized via FTIR, DSC and TEM. The above three nanocompositeemulsions were applied in leather finish; then the applied properties of thefinished leather were determined in detail. At last, the influence of the syntheticconditions such as the reaction temperature, the monomer concentration and theinitiator concentration on the polymerization dynamics of ES-P(MMA/BA/VAc/AM)/nano-SiO_2 composite emulsion was investigated in detail.The polymerization mechanism of nanocomposite emulsion was also discussed.
The best reaction conditions of P(BA/AANa) were: the use level of AA was5% and ammonium persulphate-sodium bisulfite of the initiator. The bestreaction conditions of P(BA/VAc/AM) were: the use level of AM was 14%,n(VAc): n(BA)=1:1, the reaction temperature was 90℃and the use level ofammonium persulphate-sodium bisulfite was 6%.
The optimized synthesis processes of P(MMA/BA/AANa)/nano-SiO_2composite emulsion were: n(BA): n(MMA)=2:1,pH was 7, the use level of thepotassium persulfate(KPS) was 2%, the reaction temperature was 85℃and theuse level of nano-SiO_2 was 2%. The better properties of the leather finished byP(MMA/BA/AANa)/nano-SiO_2 composite emulsion in contrast to that byP(MMA/BA/AANa) were represented: increasing air permeability by 376.19%and water vapor permeability by 7.78%, decreasing water uptake by 16.31%;besides, wet rubbing fastness was 3class. Dry rubbing fastness was 4～5classand flex resistance was 20000 times.
The best properties of P(MMA/BA/VAc/AM)/nano-SiO_2 compositeemulsion was obtained, when the dosage of nano-SiO_2 with the unsaturatedbonds was 1.5%. The better properties of the leather finished byP(MMA/BA/VAc/AM)/nano-SiO_2 composite emulsion in contrast to that by P(MMA/BA/VAc/AM) were represented: increasing air permeability by109.92% and water vapor permeability by 16.49%, decreasing water uptake by56.19%; besides, wet rubbing fastness was 2-3class. Dry rubbing fastness was4～5class and flex resistance was 50000 times.
When the reaction temperature was 75℃, the reaction time was 2 hours, thedosage of KPS was 3%, the dosage of tetraethoxysilane(TEOS) was 5%, thedosage of vinyl trimethoxy silane was 4% and n(BA): n(MMA)=3: 2, the bestproperties of the emulsifier-free P(BA/VAc/AM)/nano-SiO_2 composite emulsionwas obtained.
The better properties of the leather finished byES-P(MMA/BA/VAc/AM)/nano-SiO_2 composite emulsion in contrast toP(MMA/BA/VAc/AM) were represented: increasing air permeability by285.39% , water vapor permeability by 49.01% and dynamic waterproof by17.71%; besides, decreasing water uptake by 18.47%. Dry rubbing fastness was4～5class, wet rubbing fastness was 1 class and flex resistance was 100000 times.
The solvent resistance and the fullness feeling of the leather finished byES-P(MMA/BA/VAc/AM)/nano-SiO_2 composite emulsion in contrast to that byacrylic resin in the factory were improved. In addition to, the softness andadhesion of finish were indistinguishableness.
The reaction activity energy (E_a) of ES-P(MMA/BA/VAc/AM)/nano-SiO_2composite emulsion was 44.154kJ/mol and the polymerization reaction rate wasR_p∝[I]~(1.716)[m]~(0.33). The polymerization mechanism of nanocomposite emulsion ofthe homogeneous nucleation was concluded.
首先合成了二元两亲性共聚物聚丙烯酸丁酯/丙烯酸钠[P(BA/AANa)]和三元两亲性共聚物聚丙烯酸丁酯/醋酸乙烯酯/丙烯酰胺[P(BA/VAc/AM)],并采用红外光谱(FTIR)、差示扫描量热(DSC)和透射电镜(TEM)等检测手段对两种两亲性共聚物的结构进行了表征。分别以P(BA/AANa)和P(BA/VAc/AM)为稳定剂,采用表面带有不饱和双键的纳米SiO_2粉体与丙烯酸酯类单体通过无皂乳液聚合法原位合成了聚甲基丙烯酸甲酯/丙烯酸丁酯/丙烯酸钠[P(MMA/BA/AANa)]/纳米SiO_2复合乳液和聚甲基丙烯酸甲酯/丙烯酸丁酯/醋酸乙烯酯/丙烯酰胺[P(MMA/BA/VAc/AM)]/纳米SiO_2复合乳液;通过单因素实验法优化了这两种纳米复合乳液的合成条件。以P(BA/VAc/AM)为稳定剂,采用正硅酸乙酯(TEOS)和丙烯酸酯类单体通过无皂乳液聚合法和溶胶-凝胶法原位合成了ES-P(MMA/BA/VAc/AM)/纳米SiO_2复合乳液;通过单因素实验法优化了该纳米复合乳液的合成条件。采用FTIR、DSC和TEM等检测手段分别对P(MMA/BA/AANa)/纳米SiO_2复合乳液、P(MMA/BA/VAc/AM)/纳米SiO_2复合乳液和ES-P(MMA/BA/VAc/AM)/纳米SiO_2复合乳液的结构进行了表征。分别将这三种纳米复合乳液应用于皮革涂饰,对涂饰后革样的各项性能进行了检测。最后对ES-P(MMA/BA/VAc/AM)/纳米SiO_2复合乳液的合成过程进行了动力学研究,通过动态激光光散射(DLS)和TEM检测推断出该纳米复合乳液的聚合机理。
二元两亲性共聚物P(BA/AANa)的最优合成条件为:丙烯酸质量分数(以单体总质量计)5%,引发体系过硫酸铵-亚硫酸氢钠。三元两亲性共聚物P(BA/VAc/AM)的最优合成条件为:丙烯酰胺质量分数(以单体总质量计)14%,n(VAc):n(BA)=1:1,反应温度90℃,过硫酸铵-亚硫酸氢钠质量分数(以单体总质量计)6%。
P(MMA/BA/AANa)/纳米SiO_2复合乳液的最优合成条件为:n(BA):n(MMA)=2:1,pH为7,过硫酸钾质量分数(以单体总质量计)2%,反应温度85℃,纳米SiO_2质量分数(以单体总质量计)2%。P(MMA/BA/AANa)/纳米SiO_2复合乳液涂饰后革样与P(MMA/BA/AANa)涂饰后革样相比:透气性增加了376.19%,透水汽性提高了7.78%,吸水率降低了16.31%,耐湿擦性达到3级,耐干擦性均达到4～5级,常温耐屈挠性均达到2万次。
P(MMA/BA/VAc/AM)/纳米SiO_2复合乳液的最优合成条件为:纳米SiO_2粉体为表面带有不饱和双键的纳米SiO_2,纳米SiO_2粉体质量分数(以单体总质量计)1.5%。P(MMA/BA/VAc/AM)/纳米SiO_2复合乳液涂饰后革样与P(MMA/BA/VAc/AM)涂饰后革样相比:透气性增加了109.92%,透水汽性提高了16.49%,吸水率降低了56.19%,耐湿擦性达到2～3级,耐干擦性均达到4～5级,常温耐屈挠性均达到5万次。
同步采用无皂乳液聚合法和溶胶-凝胶法制备的ES-P(MMA/BA/VAc/AM)/纳米SiO_2复合乳液的最优合成条件为:反应温度75℃,反应时间2h,n(BA):n(MMA)=3:2,过硫酸钾质量分数(以单体总质量计)3%,正硅酸乙酯质量分数(以单体总质量计)5%,乙烯基三甲氧基硅烷质量分数(以单体总质量计)4%。
ES-P(MMA/BA/VAc/AM)/纳米SiO_2复合乳液的实验室应用结果表明:与P(MMA/BA/VAc/AM)乳液涂饰后革样相比,透气性提高了285.39%,透水汽性提高了49.01%,吸水率降低了18.47%,动态防水性提高了17.71%,耐湿擦性均达到1级,耐干擦性均达到4～5级,常温耐屈挠性均达到10万次。
ES-P(MMA/BA/VAc/AM)/纳米SiO_2复合乳液的工厂应用结果表明:与厂内大生产用聚丙烯酸酯乳液涂饰后革样相比,涂饰后革样的耐溶剂性有所提高(擦拭20次),柔软度和粘着牢度无明显差异,离板性相近,丰满性较好,粘性略低。
ES-P(MMA/BA/VAc/AM)/纳米SiO_2复合乳液的反应活化能E_a为44.154kJ/mol,聚合反应过程中的反应速率R_p∝[I]~(1.716)[m]~(0.33)。该纳米复合乳液的整个聚合过程遵循了均相成核机理。
Acrylic resin was widely used as the leather finishing materials. Recently,much better properties of acrylic resin, such as better water-resistance,solvent-resistance, hygiene properties and corium feeling, were desirable for theleather finish market. This thesis was mainly focused on the study of acrylicresin/nano-SiO_2 composite emulsion prepared via emulsifier-free emulsionpolymerization, based on the amphiphlic copolymer. Besides, acrylicresin/nano-SiO_2 composite emulsion with the excellent properties systhesized viain-situ emulsifier-free emulsion polymerization and sol-gel method in one step inorder to simplify the systhesis process.
Poly(butyl acrylate/acrylic acid sodium)P(BA/AANa) and Poly(butylacrylate/vinyl acetate/acrylamide)P(BA/VAc/AM) were prepared at first. Thestructures of both amphiphlic copolymers were investigated by FourierTransform Infrared Spectroscopy(FTIR), Differential ScanningCalorimetry(DSC) and Transmission Electron Microscopy (TEM). Poly(methylmethacrylate/butyl acrylate/acrylic acid sodium)P(MMA/BA/AANa)/nano-SiO_2composite emulsion and Poly(methyl methacrylate/butyl acrylate/vinylacetate/acrylamide)P(MMA/BA/VAc/AM)/nano-SiO_2 composite emulsion weresynthesized via in-situ emulsifier-free emulsion polymerization, based onP(BA/AANa)and P(BA/VAc/AM) dividedly. P(MMA/BA/VAc/AM)/nano-SiO_2composite emulsion was obtained via both emulsifier-free emulsionpolymerization and sol-gel method in one step, on the basis of P(BA/VAc/AM). P(MMA/BA/AANa)/nano-SiO_2 composite, P(MMA/BA/VAc/AM)/nano-SiO_2composite and ES-P(MMA/BA/VAc/AM)/nano-SiO_2 composite werecharacterized via FTIR, DSC and TEM. The above three nanocompositeemulsions were applied in leather finish; then the applied properties of thefinished leather were determined in detail. At last, the influence of the syntheticconditions such as the reaction temperature, the monomer concentration and theinitiator concentration on the polymerization dynamics of ES-P(MMA/BA/VAc/AM)/nano-SiO_2 composite emulsion was investigated in detail.The polymerization mechanism of nanocomposite emulsion was also discussed.
The best reaction conditions of P(BA/AANa) were: the use level of AA was5% and ammonium persulphate-sodium bisulfite of the initiator. The bestreaction conditions of P(BA/VAc/AM) were: the use level of AM was 14%,n(VAc): n(BA)=1:1, the reaction temperature was 90℃and the use level ofammonium persulphate-sodium bisulfite was 6%.
The optimized synthesis processes of P(MMA/BA/AANa)/nano-SiO_2composite emulsion were: n(BA): n(MMA)=2:1,pH was 7, the use level of thepotassium persulfate(KPS) was 2%, the reaction temperature was 85℃and theuse level of nano-SiO_2 was 2%. The better properties of the leather finished byP(MMA/BA/AANa)/nano-SiO_2 composite emulsion in contrast to that byP(MMA/BA/AANa) were represented: increasing air permeability by 376.19%and water vapor permeability by 7.78%, decreasing water uptake by 16.31%;besides, wet rubbing fastness was 3class. Dry rubbing fastness was 4～5classand flex resistance was 20000 times.
The best properties of P(MMA/BA/VAc/AM)/nano-SiO_2 compositeemulsion was obtained, when the dosage of nano-SiO_2 with the unsaturatedbonds was 1.5%. The better properties of the leather finished byP(MMA/BA/VAc/AM)/nano-SiO_2 composite emulsion in contrast to that by P(MMA/BA/VAc/AM) were represented: increasing air permeability by109.92% and water vapor permeability by 16.49%, decreasing water uptake by56.19%; besides, wet rubbing fastness was 2-3class. Dry rubbing fastness was4～5class and flex resistance was 50000 times.
When the reaction temperature was 75℃, the reaction time was 2 hours, thedosage of KPS was 3%, the dosage of tetraethoxysilane(TEOS) was 5%, thedosage of vinyl trimethoxy silane was 4% and n(BA): n(MMA)=3: 2, the bestproperties of the emulsifier-free P(BA/VAc/AM)/nano-SiO_2 composite emulsionwas obtained.
The better properties of the leather finished byES-P(MMA/BA/VAc/AM)/nano-SiO_2 composite emulsion in contrast toP(MMA/BA/VAc/AM) were represented: increasing air permeability by285.39% , water vapor permeability by 49.01% and dynamic waterproof by17.71%; besides, decreasing water uptake by 18.47%. Dry rubbing fastness was4～5class, wet rubbing fastness was 1 class and flex resistance was 100000 times.
The solvent resistance and the fullness feeling of the leather finished byES-P(MMA/BA/VAc/AM)/nano-SiO_2 composite emulsion in contrast to that byacrylic resin in the factory were improved. In addition to, the softness andadhesion of finish were indistinguishableness.
The reaction activity energy (E_a) of ES-P(MMA/BA/VAc/AM)/nano-SiO_2composite emulsion was 44.154kJ/mol and the polymerization reaction rate wasR_p∝[I]~(1.716)[m]~(0.33). The polymerization mechanism of nanocomposite emulsion ofthe homogeneous nucleation was concluded.
引文
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