两亲分子设计在抗静电聚烯烃材料与防水抗菌纸中的应用
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摘要
论文以研究高分子材料表面功能化理论为核心,以解决聚烯烃抗静电问题、纸质包装材料防水抗菌问题等为应用背景,在研究材料抗静电原理、聚合物接枝原理以及材料抗菌原理基础上设计并合成了多种具有亲水疏水结构的两亲分子,包括可交联型表面活性剂、抗菌表面活性剂、功能化聚乙烯蜡、功能化聚丙烯蜡和梳状两亲聚合物等,将具有两亲结构的表面活化物与聚丙烯、聚乙烯熔融共混,制备了永久型抗静电聚丙烯和聚乙烯；将抗菌功能化聚乙烯蜡制备成乳液用于造纸,制备了具有防水抗菌性能的纸材料,具体工作如下：
为克服传统小分子抗静电剂容易流失、不耐水等缺点,本文选用具有一个疏水臂、三个亲水臂的吐温类表面活性剂为研究对象,首先将不同疏水臂长、亲水臂长的吐温与司盘和聚丙烯熔融共混制备了抗静电聚丙烯,对试样抗静电性能的影响因素,包括添加量、加工条件、大气湿度等进行了全面的研究,挑选出具有最快迁移速率和抗静电性能最好的抗静电剂吐温40(T40)。并将T40与阳离子聚丙烯(CPP)复配,发现了两者之间存在一定的协同效应。此外,对T40进行双键化改性,得到三双键吐温40(TDB-T40),发现添加TDB-T40的聚丙烯样品经过表面紫外照射后具有一定的耐水洗能力。研究表明,基于T40的抗静电体系能有效地降低PP的表面电阻率,添加量为0.5%时,PP样品的表面电阻率达到1010Ω/sq,水接触角为57°,表面能达到49.5mN/m,即便经超声水洗后表面电阻率也只升高至1011～1012Ω/sq。
论文研究了一类抗静电效果显著,效果持久的高分子类抗静电剂。将与聚丙烯相容性好的聚烯烃蜡(PEW、PPW)和具有抗静电功能的丙烯酸钠(AAS)通过接枝方法键合在一起,制备了本征体积电导率为105Ω-cm和106Ω·cm的PEW-g-AAS和PPW-g-AAS两种两亲性大分子,将两者分别与聚丙烯熔融共混,制备了PEW-g-AAS/PP和PPW-g-AAS/PP两种抗静电材料。集中研究了它们在不同处理条件下的表面电阻率(ρs)、水接触角、分散效果、介电常数和介电损耗等。结果表明,该类抗静电剂以微米级的片或颗粒形式均匀分散在基体中,通过在聚丙烯内形成导电网络而使电荷流通,当两种抗静电剂添加量为15%时,聚丙烯表面电阻率和体积电阻率分别降为4.7×109Ω/sq,1.5×109Ω·cm和2.5×1010Ω/sq,4.9×109Q·cm,而且该类抗静电剂的加入对聚丙烯的力学性能影响不大,尤为突出的是使聚丙烯抗静电性能具有耐水洗性优点。
论文在主链阳离子聚合物中引入不同长度的疏水侧链,得到具有梳状结构的两亲聚合物C-ionene。采用电荷密度、FTIR、H-NMR、TGA、最低抑菌浓度(MIC)、抗霉性、粒径及分布、Zeta电位、表面张力等方法对C-ionene进行了研究。结果表明,侧链长度为4个碳原子(即4I)时具有最好的抗菌性能,对大肠杆菌的最低抑菌浓度达到7.8μg/mL,是通过破坏细菌细胞膜令细菌在几秒钟内致死而实现抗菌效果的。
将C-ionene与低密度聚乙烯(LDPE)混合制备了LDPE/ionene复合材料,采用ATR-FTIR.水接触角、SEM以及采用贴膜法等对其抗静电性能的影响因素(包括C-ionene侧链长度、添加量、大气湿度、耐水洗性等)以及抗菌性能进行了详细的研究。结果表明,侧链长度为12个碳原子(即12I)是最佳的抗静电剂,添加5%时,复合材料表面电阻率降到2.3×109Ω/sq,而且抗静电效果具有持久性和耐水洗性能；LDPE/4I和LDPE/121复合材料具有良好的抗菌效果,其中LDPE/4I (5%)对大肠杆菌的抑菌率达到99.9%以上。
最后,论文制备了四种乳化性和抗菌性良好的复合的阳离子表面活性剂(S121,S122,S181和S182),用其对PEW和蜂蜡(BEW)进行乳化,得到抗菌的蜡乳液。另一方面将疏水的PEW和具有抗菌性能的PHGH键合在一起,制备了具有两亲性结构的多功能大分子PEW-g-PHGH,然后直接乳化制成抗菌乳液。然后将蜡乳液通过湿部、涂布、浸渍法用于造纸,制备了具有一定的防水、抗菌性能的纸。结果表明,BEW乳液比PEW乳液防水效果好,接枝法制备的蜡乳液不仅抗菌、防水效果显著,而且以化学键与PEW连接的抗菌剂,不易使抗菌剂渗出,具有抗菌长效性和安全性。
The thesis aims to prepare antistatic polyolefin and hydrophobic paper-based material with antimicrobial properties based on the surface modification of polymers. According to the electrostatic dissipative mechanism, principle of polymer grafting and antimicrobial theories, several amphiphilic moceluces with hydrophobic and hydrophilic segments were prepared including crosslinkable surfactants, antimicrobial surfactants, functional polyethylene wax, functional polypropylene wax and comb-like cationic polymers. The antistatic agents with amphiphilic structures were blended with polypropylene (PP) and polyethylene (PE) to fabricate permanent antistatic polyolefin materials, while the polyethylene wax (PEW) and bees wax (BEW) were made into antimicrobial emulsions with the help of antimicrobial surfactants or being modified with antimicrobial agent, and then applied to paper to obtain hydrophobic and antimicrobial paper.
The traditional antistatic agents were easy to wear out thus losing antistatic properties. To fabricate the permanent antistatic PP materials, Tween surfactants with one hydrophobic arm and three hydrophilic arms were investigated as inner antistatic agents of PP. Firstly, a cluster of nonnionic surfactants with different hydrophile-lipophile balance (HLB) were blended with PP to produce antistatic sheet samples. Then, the influence factors of antistatic performance including addition amount, processing conditions and the atmosphere humidity were investigated in detail, and Tween40(T40) was verified as the best antistic agent. Finally, two methods were applied to improve the water endurance of antistatic performance, including combination of T40and cationic PP (CPP) and surface crossliking of modified T40. The results show that T40based antistatic agents were effective to dissipative the electrostatic. The PP/T40(0.5%) sample revealed surface resistivity of1010Ω2/sq, water contact angle of57°and surface energy of49.5mN/m, and the treated sample had surface resistivity of1011～1012Ω/sq after umtrosound cleaning.
The thesis also focused on a type of polymeric antistatic agents with exerellent antistatic properties. Polyethylene wax grafted with sodium acrylate (PEW-g-AAS) and polypropylene wax grafted with sodium acrylate (PPW-g-AAS), were prepared using a solution grafting method and applied to polypropylene (PP) to enhance antistatic properties. The grafting degree was determined using back titration method and structures were confirmed by Fourier transform infrared spectroscopy (FTIR). The antistatic properties of PEW-g-AAS/PP blends and PPW-g-AAS/PP blends were characterized by surface resistivities (ρs) and volume resistivities (ρv), and a combination of contact angle measurements, scanning electron microscopy (SEM), permittivity and dielectric loss were used to investigate the surface and inner structures of the blends. Results showed ρs and ρv of PEW-g-AAS/PP blends dropped significantly (4-7orders of magnitudes) above a critical addition at10%, where an electrostatic dissipative network formed; PPW-g-AAS revealed an inferior antistatic performance than PEW-g-AAS due to its better compatibility and smaller content of dispersed phase in the matrix. Furthermore, the antistatic blends treated in80℃water,80℃air and room temperature were investigated and the results were interpreted from surface energy. Moreover, the addition of antistatic agent had little impact on tensile strength of the PP matrix.
The thesis investigated a type of amphiphilic polymers with comb-like structures. The prepared comb-like ionenes (C-ionene) were characterized by charge density, FTIR, H-NMR and TGA, and their antimicrobial properties were investagited via the measurement of the minimal inhibitory concentration (MIC) against the escherichia coli (E. coli) and the anti-mound tests against Aspergillus niger and Chaetomium globosum. Besides, the solution properties including the morphology of the ionene molecular chain and surface tension of ionene solutions were studied by measuring the paticle size, Zeta potential and suface tension. Results showed that the C-ionene with butyl as side chains (41) had the best antimicrobial property, and its MIC reached7.8μg/mL. The C-ionenes inhibited the growth of bacteria by destroying the membranes of bacteria and causing the cytoplasm leaking.
The LDPE/C-ionene composites were prepared by blending C-ionenes and LDPE, and the antistatic influence including the length of side chain, the addition amount, the atomosphere humidity and water durability were discussed in detail. The surface and inner structures of the composites were characterized by ATR-FTIR, water contact angles and SEM. In addition, the antimicrobial properties of the composites were investigated by growth inhibition of E. coli with membrane adhering-colony counting method. Result showed that the C-ionene with dodecyl as side chains (121) revealed the best antistatic properties. The LDPE/121(5%) composite had permanent antistatic performance with surface resistivitity of2.3×109Ω/sq. The LDPE/4I (5%) composite revealed99.9%growth inhibition of E. coli.
In order to prepare the waterproof and antimicrobial paper, the antimicrobial PEW and bees wax (BEW) emulsions were prepared and applied to paper using wet end method, roll coating and dip coating method. The antimicrobial wax emulsions were prepared by being emulsified with antimicrobial surfactants (S121, S122, S181and S182) or grafted of polyhexamethylene guanidine hydrochloride (PHGH), and characterized by particle size, Zeta potential and AFM. The hydrophobic and antimicrobial of active paper were investigated by water contact angles, inhibition zone, and growth inhibition against Aspergillus niger and Chaetomium globosum. Results showed BEW emulsions had better effect on waterproof improvement, and the emulsions prepared by grafting method showed significant superiority than the surfactant assistance.
为克服传统小分子抗静电剂容易流失、不耐水等缺点,本文选用具有一个疏水臂、三个亲水臂的吐温类表面活性剂为研究对象,首先将不同疏水臂长、亲水臂长的吐温与司盘和聚丙烯熔融共混制备了抗静电聚丙烯,对试样抗静电性能的影响因素,包括添加量、加工条件、大气湿度等进行了全面的研究,挑选出具有最快迁移速率和抗静电性能最好的抗静电剂吐温40(T40)。并将T40与阳离子聚丙烯(CPP)复配,发现了两者之间存在一定的协同效应。此外,对T40进行双键化改性,得到三双键吐温40(TDB-T40),发现添加TDB-T40的聚丙烯样品经过表面紫外照射后具有一定的耐水洗能力。研究表明,基于T40的抗静电体系能有效地降低PP的表面电阻率,添加量为0.5%时,PP样品的表面电阻率达到1010Ω/sq,水接触角为57°,表面能达到49.5mN/m,即便经超声水洗后表面电阻率也只升高至1011～1012Ω/sq。
论文研究了一类抗静电效果显著,效果持久的高分子类抗静电剂。将与聚丙烯相容性好的聚烯烃蜡(PEW、PPW)和具有抗静电功能的丙烯酸钠(AAS)通过接枝方法键合在一起,制备了本征体积电导率为105Ω-cm和106Ω·cm的PEW-g-AAS和PPW-g-AAS两种两亲性大分子,将两者分别与聚丙烯熔融共混,制备了PEW-g-AAS/PP和PPW-g-AAS/PP两种抗静电材料。集中研究了它们在不同处理条件下的表面电阻率(ρs)、水接触角、分散效果、介电常数和介电损耗等。结果表明,该类抗静电剂以微米级的片或颗粒形式均匀分散在基体中,通过在聚丙烯内形成导电网络而使电荷流通,当两种抗静电剂添加量为15%时,聚丙烯表面电阻率和体积电阻率分别降为4.7×109Ω/sq,1.5×109Ω·cm和2.5×1010Ω/sq,4.9×109Q·cm,而且该类抗静电剂的加入对聚丙烯的力学性能影响不大,尤为突出的是使聚丙烯抗静电性能具有耐水洗性优点。
论文在主链阳离子聚合物中引入不同长度的疏水侧链,得到具有梳状结构的两亲聚合物C-ionene。采用电荷密度、FTIR、H-NMR、TGA、最低抑菌浓度(MIC)、抗霉性、粒径及分布、Zeta电位、表面张力等方法对C-ionene进行了研究。结果表明,侧链长度为4个碳原子(即4I)时具有最好的抗菌性能,对大肠杆菌的最低抑菌浓度达到7.8μg/mL,是通过破坏细菌细胞膜令细菌在几秒钟内致死而实现抗菌效果的。
将C-ionene与低密度聚乙烯(LDPE)混合制备了LDPE/ionene复合材料,采用ATR-FTIR.水接触角、SEM以及采用贴膜法等对其抗静电性能的影响因素(包括C-ionene侧链长度、添加量、大气湿度、耐水洗性等)以及抗菌性能进行了详细的研究。结果表明,侧链长度为12个碳原子(即12I)是最佳的抗静电剂,添加5%时,复合材料表面电阻率降到2.3×109Ω/sq,而且抗静电效果具有持久性和耐水洗性能；LDPE/4I和LDPE/121复合材料具有良好的抗菌效果,其中LDPE/4I (5%)对大肠杆菌的抑菌率达到99.9%以上。
最后,论文制备了四种乳化性和抗菌性良好的复合的阳离子表面活性剂(S121,S122,S181和S182),用其对PEW和蜂蜡(BEW)进行乳化,得到抗菌的蜡乳液。另一方面将疏水的PEW和具有抗菌性能的PHGH键合在一起,制备了具有两亲性结构的多功能大分子PEW-g-PHGH,然后直接乳化制成抗菌乳液。然后将蜡乳液通过湿部、涂布、浸渍法用于造纸,制备了具有一定的防水、抗菌性能的纸。结果表明,BEW乳液比PEW乳液防水效果好,接枝法制备的蜡乳液不仅抗菌、防水效果显著,而且以化学键与PEW连接的抗菌剂,不易使抗菌剂渗出,具有抗菌长效性和安全性。
The thesis aims to prepare antistatic polyolefin and hydrophobic paper-based material with antimicrobial properties based on the surface modification of polymers. According to the electrostatic dissipative mechanism, principle of polymer grafting and antimicrobial theories, several amphiphilic moceluces with hydrophobic and hydrophilic segments were prepared including crosslinkable surfactants, antimicrobial surfactants, functional polyethylene wax, functional polypropylene wax and comb-like cationic polymers. The antistatic agents with amphiphilic structures were blended with polypropylene (PP) and polyethylene (PE) to fabricate permanent antistatic polyolefin materials, while the polyethylene wax (PEW) and bees wax (BEW) were made into antimicrobial emulsions with the help of antimicrobial surfactants or being modified with antimicrobial agent, and then applied to paper to obtain hydrophobic and antimicrobial paper.
The traditional antistatic agents were easy to wear out thus losing antistatic properties. To fabricate the permanent antistatic PP materials, Tween surfactants with one hydrophobic arm and three hydrophilic arms were investigated as inner antistatic agents of PP. Firstly, a cluster of nonnionic surfactants with different hydrophile-lipophile balance (HLB) were blended with PP to produce antistatic sheet samples. Then, the influence factors of antistatic performance including addition amount, processing conditions and the atmosphere humidity were investigated in detail, and Tween40(T40) was verified as the best antistic agent. Finally, two methods were applied to improve the water endurance of antistatic performance, including combination of T40and cationic PP (CPP) and surface crossliking of modified T40. The results show that T40based antistatic agents were effective to dissipative the electrostatic. The PP/T40(0.5%) sample revealed surface resistivity of1010Ω2/sq, water contact angle of57°and surface energy of49.5mN/m, and the treated sample had surface resistivity of1011～1012Ω/sq after umtrosound cleaning.
The thesis also focused on a type of polymeric antistatic agents with exerellent antistatic properties. Polyethylene wax grafted with sodium acrylate (PEW-g-AAS) and polypropylene wax grafted with sodium acrylate (PPW-g-AAS), were prepared using a solution grafting method and applied to polypropylene (PP) to enhance antistatic properties. The grafting degree was determined using back titration method and structures were confirmed by Fourier transform infrared spectroscopy (FTIR). The antistatic properties of PEW-g-AAS/PP blends and PPW-g-AAS/PP blends were characterized by surface resistivities (ρs) and volume resistivities (ρv), and a combination of contact angle measurements, scanning electron microscopy (SEM), permittivity and dielectric loss were used to investigate the surface and inner structures of the blends. Results showed ρs and ρv of PEW-g-AAS/PP blends dropped significantly (4-7orders of magnitudes) above a critical addition at10%, where an electrostatic dissipative network formed; PPW-g-AAS revealed an inferior antistatic performance than PEW-g-AAS due to its better compatibility and smaller content of dispersed phase in the matrix. Furthermore, the antistatic blends treated in80℃water,80℃air and room temperature were investigated and the results were interpreted from surface energy. Moreover, the addition of antistatic agent had little impact on tensile strength of the PP matrix.
The thesis investigated a type of amphiphilic polymers with comb-like structures. The prepared comb-like ionenes (C-ionene) were characterized by charge density, FTIR, H-NMR and TGA, and their antimicrobial properties were investagited via the measurement of the minimal inhibitory concentration (MIC) against the escherichia coli (E. coli) and the anti-mound tests against Aspergillus niger and Chaetomium globosum. Besides, the solution properties including the morphology of the ionene molecular chain and surface tension of ionene solutions were studied by measuring the paticle size, Zeta potential and suface tension. Results showed that the C-ionene with butyl as side chains (41) had the best antimicrobial property, and its MIC reached7.8μg/mL. The C-ionenes inhibited the growth of bacteria by destroying the membranes of bacteria and causing the cytoplasm leaking.
The LDPE/C-ionene composites were prepared by blending C-ionenes and LDPE, and the antistatic influence including the length of side chain, the addition amount, the atomosphere humidity and water durability were discussed in detail. The surface and inner structures of the composites were characterized by ATR-FTIR, water contact angles and SEM. In addition, the antimicrobial properties of the composites were investigated by growth inhibition of E. coli with membrane adhering-colony counting method. Result showed that the C-ionene with dodecyl as side chains (121) revealed the best antistatic properties. The LDPE/121(5%) composite had permanent antistatic performance with surface resistivitity of2.3×109Ω/sq. The LDPE/4I (5%) composite revealed99.9%growth inhibition of E. coli.
In order to prepare the waterproof and antimicrobial paper, the antimicrobial PEW and bees wax (BEW) emulsions were prepared and applied to paper using wet end method, roll coating and dip coating method. The antimicrobial wax emulsions were prepared by being emulsified with antimicrobial surfactants (S121, S122, S181and S182) or grafted of polyhexamethylene guanidine hydrochloride (PHGH), and characterized by particle size, Zeta potential and AFM. The hydrophobic and antimicrobial of active paper were investigated by water contact angles, inhibition zone, and growth inhibition against Aspergillus niger and Chaetomium globosum. Results showed BEW emulsions had better effect on waterproof improvement, and the emulsions prepared by grafting method showed significant superiority than the surfactant assistance.
引文
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