葛萍,安秋凤,谷江东,卢攀,黄良仙.杀菌性纳米杂化氟硅树脂的合成及成膜形貌[J].表面技术,2022,51(8):418-426, 434.
GE Ping,AN Qiu-feng,GU Jiang-dong,LU Pan,HUANG Liang-xian.Synthesis, Morphology and Antibacterial Properties of Bactericidal Nano-hybrid Fluorosilicone Resin[J].Surface Technology,2022,51(8):418-426, 434 |
| 杀菌性纳米杂化氟硅树脂的合成及成膜形貌 |
| Synthesis, Morphology and Antibacterial Properties of Bactericidal Nano-hybrid Fluorosilicone Resin |
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| DOI：10.16490/j.cnki.issn.1001-3660.2022.08.038 |
| 中文关键词: 氟硅树脂 杀菌性 季铵盐 纳米粒 杂化涂层 |
| 英文关键词:fluorosilicon resin bactericide quaternary ammonium salt nano particle hybrid coating |
| 基金项目:陕西省重点研发计划项目(2020ZDLGY13-11);国家科技部重点研发计划项目(2017YFB0307700) |
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| Author | Institution |
| GE Ping | Key Laboratory of Auxiliary Chemistry and Technology for Light Chemical Industry, Shaanxi Provincial, Shaanxi University of Science and Technology, Xi'an 710021, China |
| AN Qiu-feng | Key Laboratory of Auxiliary Chemistry and Technology for Light Chemical Industry, Shaanxi Provincial, Shaanxi University of Science and Technology, Xi'an 710021, China |
| GU Jiang-dong | Key Laboratory of Auxiliary Chemistry and Technology for Light Chemical Industry, Shaanxi Provincial, Shaanxi University of Science and Technology, Xi'an 710021, China |
| LU Pan | Key Laboratory of Auxiliary Chemistry and Technology for Light Chemical Industry, Shaanxi Provincial, Shaanxi University of Science and Technology, Xi'an 710021, China |
| HUANG Liang-xian | Key Laboratory of Auxiliary Chemistry and Technology for Light Chemical Industry, Shaanxi Provincial, Shaanxi University of Science and Technology, Xi'an 710021, China |
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| 中文摘要: |
| 目的 合成一种具有拒水、拒油与抗菌一体的防护材料。方法 在酸催化下，将全氟己基乙基三甲氧基硅烷(FTMS)与有机硅杀菌剂——(三甲氧基硅丙基)十八烷基二甲基氯化铵 (TMSPQ)及正硅酸乙酯(TEOS)进行水解，次序共聚，制得一种兼具良好拒水、拒油和杀菌性能的长链氟烃基/季铵基共改性的氟硅树脂(QFS)。用FT-IR、TEM、AFM、XPS等仪器表征研究了QFS的结构、成膜形貌和性能。结果 新合成的QFS为典型的无机-有机纳米杂化树脂，且在透明状QFS体系中存在大量球状、纳米组分且平均粒径约为164.2 nm。受此球状结构及长链氟烃基的影响，QFS在基材表面呈现出一种凹凸不平、微观结构相对粗糙的形貌，同时在AFM扫描范围为5 μm×5 μm内QFS膜表面的均方粗糙度Ra达1.273 nm，且从FESEM可看出QFS涂膜微观表面由微纳米结构组成。在QFS合成时，当FTMS的加入量为25 % 时，QFS涂膜的水接触角(θWCA)可达145.0°，滚动角最小为12°，耐油笔性最高为79次。通过抑菌圈试验，QFS对金黄色葡萄球菌和大肠杆菌均有良好的杀菌抑菌效果，其抑菌圈大小分别可达到18.1 mm和15.8 mm。同时，分别通过一锅共聚和次序共聚法合成QFS，最后从涂膜的水接触角、膜的厚度、平均粒径和粒径范围等综合考虑，选择次序共聚法合成。结论 含有低表面能长链氟烃基和杀菌性季铵基的QFS制备的涂膜可从拒水、拒油和抗菌3个方面对基材起到良好的防护作用。 |
| 英文摘要: |
| In recent years, with the deterioration of the environment and the breeding and spread of highly pathogenic bacteria and viruses, how to inhibit bacteria and kill bacteria has become a topic of great concern. The antibacterial and bactericidal properties of silicone quaternary ammonium salt have the advantages of broad spectrum, low toxicity, high efficiency, and resistance to pH changes. After the positively charged long carbon chain quaternary ammonium group is adsorbed on the surface of negatively charged bacteria, it can be It restrains the activity of bacteria, inhibits the respiratory function of bacteria, penetrates the cell membrane and enters the bacterial cells, destroys the metabolism of intracellular enzymes and makes them die, thereby achieving the antibacterial and bactericidal effect; long-chain fluorocarbon groups can increase the water repellency of the resin. Oil repellent performance, and make it difficult for bacteria, viruses or bacteria-carrying microorganisms to adhere to the surface of the substrate after the resin treatment, and then easy to fall off and remove. Purpose to synthesize a protective material with integrated water repellent, oil repellent and antibacterial. In the presence of acid catalysis, the hydrolytic copolymerization of perfluorohexyl ethyl trimethoxysilane (FTMS) with organosilicon fungicide, (trimethoxysilpropyl)octadecyldimethyl ammonium chloride (TMSPQ) and ethyl orthosilicate (TEOS) undergoes hydrolysis and sequential copolymerization, a long chain fluoroalkyl/quaternary ammonium commodified fluorosilicone resin (QFS) with good water-repellent, oil-repellent and bactericidal properties has been prepared. The chemical structure, film morphology and performance of QFS were characterized by FT-IR, TEM, AFM, XPS and other instruments. The experiment results show that the newly synthesized QFS is a typical inorganic-organic nano hybrid resin. There are a large number of spherical and nano components in the transparent QFS system, and the average particle size is about 164.2 nm. Because of the influence of the spherical structure and the long chain fluoroalkyl group, the surface of QFS is uneven and the microstructure is relatively rough. At the same time, the mean square roughness (Ra) of the QFS film surface in the AFM scanning range of 5 μm×5 μm reaches 1.273 nm; and FESEM can see that the microscopic surface of QFS coating film is composed of micron-nano structure，When the amount of FTMS added is 25%, the water contact angle (θWCA) of the coating film can reach 145°, the minimum rolling angle is 12°, and the oil pen resistance can reach 79 times; In addition, the inhibition zone experiment indicates that QFS showed good bactericidal and antibacterial properties for staphylococcus aureus and escherichia coli. Thus, the inhibition zone of QFS reached 18.1 mm for staphylococcus aureus and 15.8 mm for escherichia coli, respectively; At the same time, QFS was synthesized by one-pot copolymerization and sequential copolymerization respectively, and finally, the sequential copolymerization method was selected from the comprehensive consideration of the water contact angle of the coating film, the thickness of the film, the average particle size and the particle size range. The coating film prepared by QFS containing low surface energy long-chain fluorocarbon groups and bactericidal quaternary ammonium groups can protect the substrate from three directions:water repellency, oil repellency and antibacterial. |
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