高效纳米银抗菌剂制备及其在棉麻织物中应用研究
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摘要
纳米银抗菌纤维是新兴的抗菌纺织品,它能保护皮肤、祛除异味,阻断疾病传播,有卫生保洁的功能,同时可防止微生物对纤维制品的损害,能应用于日常生活用品,包括制服、便装、衬衫、内衣、睡衣、床上用品和手帕等,拥有十分广阔的市场前景。基于抗菌功能性纺织品的社会需求,本论文选择“高效纳米银抗菌剂制备及其在棉麻织物中应用”作为研究方向,从以下几个方面开展了工作：
1.以聚乙二醇为软模板制备了单分散的纳米TiO2/Ag胶体,TiO2和Ag粒子成球状,纳米TiO2的平均粒径在50 nm, Ag的平均粒径在20nm。X射线衍射分析表明TiO2晶型为锐钛矿型。纳米TiO2/Ag胶体具有很强的紫外屏蔽效果,复合TiO2/Ag胶体在浓度为0.29 mg/mL时就达到了最小防护紫外光效果,在1.19 mg/mL浓度时可以完全防护紫外线照射。纳米TiO2/Ag对大肠杆菌和霉菌具有极好的抑菌效果,Ag浓度10 ppm对大肠杆菌抑菌率为99.9%,对霉菌抑菌率为97.9%。
2.以聚乙二醇软模板制备了单分散的纳米Ag胶体。1)不同方法制备的纳米银粒子都为球状,不加助还原剂和加入抗坏血酸的纳米Ag粒径分布在10-20 nm,加入单宁酸作为助还原剂粒径分布在3-50 nm。2)在反应温度为60℃,硝酸银浓度为20 mg/mL,硝酸银与抗坏血酸质量比值为4：1.25时,银离子转化率可达94.1%。3)纳米银胶体具有极强的抗菌效果,对大肠杆菌最低抑菌浓度5 ppm,对霉菌最低抑菌浓度16 ppm。
3.纳米Ag胶体对棉织物进行了抗菌整理。XPS测试表明,纳米银以单质Ag形式负载到棉织物上。在浴比为1：50时,纳米银浓度为100ppm,整理时间1 min,对大肠杆菌抑菌圈达到6 mm,在250 mm时,整理时间30 min,对大肠杆菌抑菌圈达到10mm。100 ppm纳米Ag整理1 min后的抗菌棉布经过50次洗涤后,对金黄色葡萄球菌和大肠杆菌抑菌圈都≥1 mm,对金黄色葡萄球菌抑菌率≥80％,对大肠杆菌抑菌率≥70%,达到AAA级标准。
4.溶液聚合法制备了聚甲基丙烯酸羟乙酯,合成了聚甲基丙烯酸羟乙酯包覆的纳米Ag胶体。TEM分析表明纳米银被聚甲基丙烯酸羟乙酯包覆,平均粒径为20 nm；利用红外光谱研究了高聚物与纳米银的结合机理,采用抑菌圈法初步研究了它的抗菌性能。
Nano-silver antimicrobial fibers are emerging antimicrobial textiles. It can protect the skin, eliminate the offensive smell, and prevent the spread of disease, which has the function of cleaning and hygiene. Meanwhile, it can prevent fiber products from microbial damage. It can be used in daily necessities, including uniforms, clothes, shirts, underwear, pajamas, bedding and a handkerchief and so on. Thus, it has a very broad market prospects. Considering the above reasons, our research focused on preparation of Ag colloidal dispersions and preparation of durable and permanent antibacterial cotton products using a new finishing process, inserting nanometer-like silver particles to cotton fibers and the thesis consists of the following contents:
1. TiO2/Ag colloidal dispersions was prepared by using PEG as template.1) TiO2 and Ag nanoparticles are both spherical, the average particle size of TiO2 among these nanomaterials was around 50 nm, and the average particle size of nano-silver was around 20 nm. X-ray diffraction (XRD) reveals that the formation of metallic silver particles crystallized in the face centered cubic (fcc) structure and the TiO2 samples exhibit well-crystallized anatase phase.2) TiO2/Ag has excellent anti-UV effect, complex colloidal solution has smallest UV protective effect with concentration at 0.29 mg/mL, folly protective ultraviolet radiation effect as the concentration is 1.19 mg/mL.3) TiO2/Ag has strong antibacterial effect. The growth inhibition rates of 10 ppm TiO2/Ag against Escherichia coli and Staphylococcus aureus are 99.9% and 97.9% respectively.
2. Nano-Ag colloidal dispersions were prepared by using PEG as template. The effect of reaction temperature and ratio of AgNO3 to ascorbic acid on conversion rate of silver ion were determined by Volhard law.1) Transmission electron microscopy (TEM) analysis showed that stable spherical metal particles 3-50 nm in diameter with a well-crystallized structure were obtained by using tannic acid as co-reducing agent, and particles 10-20 nm in diameter were gained by using ascorbic acid as co-reducing agent.2) Conversion rate of silver ion can exceed 94.1% under the following condition:temperature was fixed at 60℃, concentration of AgNO3 is 20 mg/mL, the initial ratio between AgNO3 and ascorbic acid is 4:1.25. However, the Ag colloidal solution would become unstable with the increase of ascorbic acid.3) MIC against E.coli of Ag-nanoparticles reduced by ascorbic acid and tannic acid are 5 ppm, comparing to 16 ppm against Streptomyces. All of them were significantly lower than the values obtained for the Ag metal particles.
3. The bacterial inactivation of E.coli and S. aureus on Ag-cotton textiles were investigated under different experimental conditions with novel stable Ag colloids fixed on cotton textiles. X-ray photoelectron spectroscopy (XPS) results indicated that only one states of silver were present on the surface of the antimicrobial textile. The antimicrobial test results showed that the treated textile has an excellent antimicrobial effect and laundering durability. Bacterial inhibition ring of antimicrobial textile reached 6 mm, which was treated by 100 ppm nano-silver at bath ratio of 1:50 for 1 min,10 mm(treated by 250 ppm nano-silver at bath ratio of 1:50 for 30 min).The bacterial inhibition ring of antimicrobial cotton finished by 100 ppm nano-Ag for 1 min against E. coli and S. aureus are more than 1 mm as the antibacterial fabric was washed for 50 times. Growth inhibition rates against S. aureus is higher than 80%, and E. coli higher than 70%. Thus, antibacterial finished products can reach AAA result.
4. Silver nano-particles coated by poly (hydroxyethyl methacrylate) using N, N-dimethylformamide (DMF) as a medium has been performed successfully using solution polymerization method. Transmission electron microscopy(TEM) analysis showed that stable Ag spherical metal particles, coated by PHEMA,20 nm in diameter with a well-crystallized structure were obtained. Antimicrobial properties of Ag/PHEMA nano-composite was studied primarily.
1.以聚乙二醇为软模板制备了单分散的纳米TiO2/Ag胶体,TiO2和Ag粒子成球状,纳米TiO2的平均粒径在50 nm, Ag的平均粒径在20nm。X射线衍射分析表明TiO2晶型为锐钛矿型。纳米TiO2/Ag胶体具有很强的紫外屏蔽效果,复合TiO2/Ag胶体在浓度为0.29 mg/mL时就达到了最小防护紫外光效果,在1.19 mg/mL浓度时可以完全防护紫外线照射。纳米TiO2/Ag对大肠杆菌和霉菌具有极好的抑菌效果,Ag浓度10 ppm对大肠杆菌抑菌率为99.9%,对霉菌抑菌率为97.9%。
2.以聚乙二醇软模板制备了单分散的纳米Ag胶体。1)不同方法制备的纳米银粒子都为球状,不加助还原剂和加入抗坏血酸的纳米Ag粒径分布在10-20 nm,加入单宁酸作为助还原剂粒径分布在3-50 nm。2)在反应温度为60℃,硝酸银浓度为20 mg/mL,硝酸银与抗坏血酸质量比值为4：1.25时,银离子转化率可达94.1%。3)纳米银胶体具有极强的抗菌效果,对大肠杆菌最低抑菌浓度5 ppm,对霉菌最低抑菌浓度16 ppm。
3.纳米Ag胶体对棉织物进行了抗菌整理。XPS测试表明,纳米银以单质Ag形式负载到棉织物上。在浴比为1：50时,纳米银浓度为100ppm,整理时间1 min,对大肠杆菌抑菌圈达到6 mm,在250 mm时,整理时间30 min,对大肠杆菌抑菌圈达到10mm。100 ppm纳米Ag整理1 min后的抗菌棉布经过50次洗涤后,对金黄色葡萄球菌和大肠杆菌抑菌圈都≥1 mm,对金黄色葡萄球菌抑菌率≥80％,对大肠杆菌抑菌率≥70%,达到AAA级标准。
4.溶液聚合法制备了聚甲基丙烯酸羟乙酯,合成了聚甲基丙烯酸羟乙酯包覆的纳米Ag胶体。TEM分析表明纳米银被聚甲基丙烯酸羟乙酯包覆,平均粒径为20 nm；利用红外光谱研究了高聚物与纳米银的结合机理,采用抑菌圈法初步研究了它的抗菌性能。
Nano-silver antimicrobial fibers are emerging antimicrobial textiles. It can protect the skin, eliminate the offensive smell, and prevent the spread of disease, which has the function of cleaning and hygiene. Meanwhile, it can prevent fiber products from microbial damage. It can be used in daily necessities, including uniforms, clothes, shirts, underwear, pajamas, bedding and a handkerchief and so on. Thus, it has a very broad market prospects. Considering the above reasons, our research focused on preparation of Ag colloidal dispersions and preparation of durable and permanent antibacterial cotton products using a new finishing process, inserting nanometer-like silver particles to cotton fibers and the thesis consists of the following contents:
1. TiO2/Ag colloidal dispersions was prepared by using PEG as template.1) TiO2 and Ag nanoparticles are both spherical, the average particle size of TiO2 among these nanomaterials was around 50 nm, and the average particle size of nano-silver was around 20 nm. X-ray diffraction (XRD) reveals that the formation of metallic silver particles crystallized in the face centered cubic (fcc) structure and the TiO2 samples exhibit well-crystallized anatase phase.2) TiO2/Ag has excellent anti-UV effect, complex colloidal solution has smallest UV protective effect with concentration at 0.29 mg/mL, folly protective ultraviolet radiation effect as the concentration is 1.19 mg/mL.3) TiO2/Ag has strong antibacterial effect. The growth inhibition rates of 10 ppm TiO2/Ag against Escherichia coli and Staphylococcus aureus are 99.9% and 97.9% respectively.
2. Nano-Ag colloidal dispersions were prepared by using PEG as template. The effect of reaction temperature and ratio of AgNO3 to ascorbic acid on conversion rate of silver ion were determined by Volhard law.1) Transmission electron microscopy (TEM) analysis showed that stable spherical metal particles 3-50 nm in diameter with a well-crystallized structure were obtained by using tannic acid as co-reducing agent, and particles 10-20 nm in diameter were gained by using ascorbic acid as co-reducing agent.2) Conversion rate of silver ion can exceed 94.1% under the following condition:temperature was fixed at 60℃, concentration of AgNO3 is 20 mg/mL, the initial ratio between AgNO3 and ascorbic acid is 4:1.25. However, the Ag colloidal solution would become unstable with the increase of ascorbic acid.3) MIC against E.coli of Ag-nanoparticles reduced by ascorbic acid and tannic acid are 5 ppm, comparing to 16 ppm against Streptomyces. All of them were significantly lower than the values obtained for the Ag metal particles.
3. The bacterial inactivation of E.coli and S. aureus on Ag-cotton textiles were investigated under different experimental conditions with novel stable Ag colloids fixed on cotton textiles. X-ray photoelectron spectroscopy (XPS) results indicated that only one states of silver were present on the surface of the antimicrobial textile. The antimicrobial test results showed that the treated textile has an excellent antimicrobial effect and laundering durability. Bacterial inhibition ring of antimicrobial textile reached 6 mm, which was treated by 100 ppm nano-silver at bath ratio of 1:50 for 1 min,10 mm(treated by 250 ppm nano-silver at bath ratio of 1:50 for 30 min).The bacterial inhibition ring of antimicrobial cotton finished by 100 ppm nano-Ag for 1 min against E. coli and S. aureus are more than 1 mm as the antibacterial fabric was washed for 50 times. Growth inhibition rates against S. aureus is higher than 80%, and E. coli higher than 70%. Thus, antibacterial finished products can reach AAA result.
4. Silver nano-particles coated by poly (hydroxyethyl methacrylate) using N, N-dimethylformamide (DMF) as a medium has been performed successfully using solution polymerization method. Transmission electron microscopy(TEM) analysis showed that stable Ag spherical metal particles, coated by PHEMA,20 nm in diameter with a well-crystallized structure were obtained. Antimicrobial properties of Ag/PHEMA nano-composite was studied primarily.
引文
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