纤维素基抗菌复合材料的制备与性能研究
摘要
纤维素基抗菌纳米复合材料以纤维素为基体相,银、氯化银、二氧化钛等无机抗菌材料为增强相,结合了纤维素和无机抗菌材料的优点,具有生物可降解性、生物适应性和抗菌性,在组织工程、生物医用等领域具有潜在的利用前景。目前,纤维素基抗菌纳米复合材料存在制备方法繁琐、增强相在基体相中分散性差等问题。本论文针对这些科学问题,利用绿色环保的方法快速制备一系列纤维素基抗菌纳米复合材料,实现无机抗菌材料与纤维素均匀复合,对其物相、形态、分散性和性能进行全面表征和系统研究,探讨其复合机理。
以微晶纤维素为基体相,乙二醇为溶剂、微波吸收剂和还原剂,硝酸银为银源,通过微波辅助加热法原位快速制备纤维素/银纳米复合材料。研究结果表明,在140℃反应10min就获得纤维素/银纳米复合材料；通过优化制备参数,可以实现银纳米颗粒均匀稳定的分布在纤维素表面；与单体-微晶纤维素比较,所得纤维素/银纳米复合材料热稳定性能显著提高；制备出的复合材料对大肠杆菌以及金黄色葡萄球菌具有明显的抗菌特性。
以微晶纤维素为基体相,通过LiC1/DMAc预处理纤维素,DMAc为溶剂,抗坏血酸为还原剂,通过微波辅助加热法制备纤维素/氯化银-银和纤维素/银纳米复合材料。研究表明,通过调节抗坏血酸浓度,可以制备纤维素/氯化银-银、纤维素/银-氯化银以及纤维素/银等一系列纳米复合材料；与油浴加热相比较,微波辅助加热有利于氯化银相向银相的转变；与油浴加热相比较,微波辅助加热有利于提高纤维素/银纳米复合材料中银的比例。抗菌实验说明,与纤维素/银纳米复合材料相比,制备出的纤维素/氯化银-银纳米复合材料对大肠杆菌和金黄色葡萄球菌具有更好的抗菌效果。
以微晶纤维素为基体相,通过LiC1/DMAc预处理纤维素,DMAc为溶剂,不添加任何还原剂,通过微波辅助加热法制备纤维素/氯化银纳米复合材料。研究结果表明,氯化银纳米晶体的形成与纤维素的再生几乎同时发生；较高的微波加热温度以及较长的微波加热时间对于复合材料中氯化银纳米颗粒的成核生长是至关重要的；制备出的纤维素/氯化银纳米复合材料对大肠杆菌和金黄色葡萄球菌有比较好的抗微生物活性。
以棉秆综纤维素为基体相,通过NaOH/尿素体系预处理综纤维素,采用水热法制备棉秆综纤维素／银纳米复合材料。研究表明,与硼氢化钠和葡萄糖作还原剂相比较,采用果糖处理水热反应制备的复合材料其表面分布有大量的片状结构纳米银；较长的水热反应时间更有利于银的晶化,但不利于银纳米颗粒的均匀分布；与微晶纤维素制备的复合材料相比较,农林生物质棉秆综纤维素作为银纳米颗粒的载体,更有利于提高其分散性；经NaOH/尿素体系预处理棉秆综纤维素,其纤维形态分布较好,更有利于提高银的分散性。
以棉秆纤维为基体相,通过NaOH/尿素体系预处理棉秆纤维,采用超声波法制备棉秆纤维／银纳米复合材料。研究结果表明,硼氢化钠作还原剂,超声波反应40min时,复合材料表面生成线状纳米银；添加葡萄糖作还原剂,更有利于片状纳米银的生成；超声波反应时间增加导致棉秆纤维结晶度下降；硼氢化钠作还原剂制备的复合材料其热稳定性能有很大提高。
以微晶纤维素为基体相,分别采用LiC1/DMAc体系和NaOH/尿素体系预处理纤维素,再利用水热法将纤维素与二氧化钛进行复合。研究表明,不同的纤维素溶解体系制备的复合材料其形态有较大差别；NaOH/尿素体系预处理纤维素制备的复合材料无论是在物相、热稳定性还是抗菌性能上都优于LiC1/DMAc体系预溶解纤维素制备的复合材料。复合材料通过煅烧处理最终获得金红石相二氧化钛。
以微晶纤维素为基体相,乙酸锰和六次甲基四胺为原料,二甲基甲酰胺为溶剂,通过微波法制备纤维素/锰氧化物纳米复合材料。研究结果表明,加热时间增加导致纤维素结晶度降低；通过煅烧处理纤维素/锰氧化物纳米复合物获得三氧化二锰材料。以微晶纤维素为基体相,乙酸锰为锰源,采用超声波法制备纤维素／四氧化三锰纳米复合材料。研究表明,超声波反应90min,尿素、六次甲基四胺、氢氧化钠和氢氧化钾四种碱制备的复合材料其基体相表面的四氧化三锰颗粒形态有所不同；强碱氢氧化钠有利于无机颗粒形成具有长薄片状的形态；与尿素和六次甲基四胺相比较,氢氧化钠和氢氧化钾制备的纤维素/四氧化三锰纳米复合材料其热稳定性能更佳。通过煅烧处理纤维素/锰氧化物纳米复合材料获得具有尖晶石结构的四氧化三锰材料。
Combined with the advantages of the cellulose and inorganic antibacterial materials, the cellulose-based antimicrobial nanocomposites were synthesized by using cellulose as the matrix, and silver, silver chloride, titanium dioxide, other inorganic antimicrobial materials as the reinforcing phase, which had potential applications in the field of tissue engineering and biomedical owing to its unique properties such as biodegradation, biocompatibility, and antibacterial activities. Currently, there had been problems about the cellulose-based antimicrobial nanocomposites, such as the tedious preparation method and poor dispersion of the reinforcing phase in the matrix. This thesis focused on the above scientific issues, used green method to fabricate series of cellulose-based antimicrobial nanocomposites, characterized their phase, shape, dispersion, and explored the mechanism of the composites.
The cellulose/silver nanocomposites were in-situ synthesized by fast microwave-assisted heating method by using microcrystalline cellulose (MCC) as the matrix, ethylene glycol as the solvent, microwaves absorbers and reducing agent, and silver nitrate as reactant. The results showed that cellulose-silver nanocomposites were synthesized by microwave heating at140℃for only10min. By optimized the preparation parameters, it can be achieved uniform and stable distribution of silver nanoparticles on the cellulose matrix. Compared to the monomer-MCC, the thermal stability of the cellulose/silver nanocomposites had significantly improved. The prepared composites had obvious antibacterial properties against Escherichia coli and Staphylococcus aureus.
The cellulose/AgCl-Ag nanocomposites and cellulose/Ag nanocomposites were synthesized via microwave-assisted heating method by LiCl/DMAc pretreatment of cellulose using MCC as the matrix, DMAc as the solvent, and ascorbic acid as a reducing agent. The results indicated that series of cellulose/AgCl-Ag, cellulose/Ag-AgCl, and cellulose/Ag nanocomposites were synthesized by adjusted the concentration of ascorbic acid. Compared with the oil bath heating, microwave-assisted heating method was much more favor of the phase transition from silver chloride to silver and also conducive to improve the proportion of silver in nanocomposites. Compared to the cellulose/Ag nanocomposites, the antibacterial experiment demonstrated that the cellulose/AgCl-Ag nanocomposites had better antimicrobial effect against Escherichia coli and Staphylococcus aureus.
The cellulose/AgCl nanocomposites were synthesized via microwave-assisted heating method by LiCl/DMAc pretreatment of cellulose without any reducing agent using MCC as the matrix and DMAc as the solvent. The novel preparation method was based on the simultaneous formation of the AgCl nanoparticles and precipitation of the cellulose. The high heating temperature and long heating time are favorable for the complete formation of AgCl nanoparticles in the cellulose/AgCl nanocomposites. The cellulose/AgCl nanocomposites had good antibacterial activities against both E. coli (Gram-negative) and S. aureus (Gram-positive).
The holocellulose/Ag nanocomposites were synthesized via hydrothermal method by NaOH/urea pretreatment of holocellulose using holocellulose as the matrix from cotton stalk. Compared with the reductants of sodium borohydride and glucose, there had been a large number of silver nanosheets dispersed on the surface of composites prepared using fructose as reducing agent by hydrothermal method. The long hydrothermal reaction time is conducive to the crystallization of silver, but not favorable for the uniform distribution of silver nanoparticles. Holocellulose from cotton stalk as the carrier for silver nanoparticles, are much more conducive to improve the dispersion of silver nanoparticles in the cellulose matrix compared with the composites prepared by MCC. It has been well distributed for cotton stalk holocellulose fiber by NaOH/urea pretreatment, which were much more conducive to improve the dispersion of silver nanoparticles.
The cotton stalk fiber/Ag nanocomposites were synthesized via ultrasonic treatment by NaOH/urea pretreatment of cotton stalk fiber. It was generated linear nano-silver on the surface of the composites by using sodium borohydride as reducing agent via ultrasonic treatment for40min. It was much more conducive to the generation of the chip-like nano-silver using glucose as reducing agent. The crystallinity of cotton stalk fiber decreased with the increasing ultrasonic treatment time. The thermal stability was greatly improved by using sodium borohydride as reducing agent.
The cellulose/TiO2nanocomposites were synthesized via hydrothermal method by LiCl/DMAc pretreatment and NaOH/urea pretreatment of Cellulose, respectively, which were used MCC as the matrix. The morphology of the composites was different by using different cellulose dissolution systems. The composites prepared by NaOH/urea pretreatment were superior to the composites pretreated by LiCl/DMAc solution either in phase, thermal stability and antibacterial properties. The TiO2crystals were obtained by calcination the composites.
The cellulose/manganese oxide nanocomposites were synthesized via microwave-assisted heating method using MCC as the matrix, manganese acetate and hexamethylenetetramine (HMT) as raw materials, dimethylformamide (DMF) as a solvent. The crystallinity of cellulose decreased with the increasing microwave heating time. The Mn2O3materials were obtained by calcination the nanocomposites. The cellulose/Mn3O4nanocomposites were synthesized via ultrasonic treatment using MCC as the matrix, manganese acetate as manganese source. The particle morphology of the manganese tetroxide on the matrix of composites synthesized by ultrasonic treatment for90min were different using four kinds of alkalis——urea, HMT, sodium hydroxide and potassium hydroxide. Sodium hydroxide is conducive to the formation of inorganic particles having a long thin sheet-like morphology. Compared with urea and HMT, the thermal stability of the cellulose/Mn3O4nanocomposites prepared by sodium hydroxide and potassium hydroxide were much better. The Mn3O4materials with spinel structure were obtained by calcination the nanocomposites.
以微晶纤维素为基体相,乙二醇为溶剂、微波吸收剂和还原剂,硝酸银为银源,通过微波辅助加热法原位快速制备纤维素/银纳米复合材料。研究结果表明,在140℃反应10min就获得纤维素/银纳米复合材料；通过优化制备参数,可以实现银纳米颗粒均匀稳定的分布在纤维素表面；与单体-微晶纤维素比较,所得纤维素/银纳米复合材料热稳定性能显著提高；制备出的复合材料对大肠杆菌以及金黄色葡萄球菌具有明显的抗菌特性。
以微晶纤维素为基体相,通过LiC1/DMAc预处理纤维素,DMAc为溶剂,抗坏血酸为还原剂,通过微波辅助加热法制备纤维素/氯化银-银和纤维素/银纳米复合材料。研究表明,通过调节抗坏血酸浓度,可以制备纤维素/氯化银-银、纤维素/银-氯化银以及纤维素/银等一系列纳米复合材料；与油浴加热相比较,微波辅助加热有利于氯化银相向银相的转变；与油浴加热相比较,微波辅助加热有利于提高纤维素/银纳米复合材料中银的比例。抗菌实验说明,与纤维素/银纳米复合材料相比,制备出的纤维素/氯化银-银纳米复合材料对大肠杆菌和金黄色葡萄球菌具有更好的抗菌效果。
以微晶纤维素为基体相,通过LiC1/DMAc预处理纤维素,DMAc为溶剂,不添加任何还原剂,通过微波辅助加热法制备纤维素/氯化银纳米复合材料。研究结果表明,氯化银纳米晶体的形成与纤维素的再生几乎同时发生；较高的微波加热温度以及较长的微波加热时间对于复合材料中氯化银纳米颗粒的成核生长是至关重要的；制备出的纤维素/氯化银纳米复合材料对大肠杆菌和金黄色葡萄球菌有比较好的抗微生物活性。
以棉秆综纤维素为基体相,通过NaOH/尿素体系预处理综纤维素,采用水热法制备棉秆综纤维素／银纳米复合材料。研究表明,与硼氢化钠和葡萄糖作还原剂相比较,采用果糖处理水热反应制备的复合材料其表面分布有大量的片状结构纳米银；较长的水热反应时间更有利于银的晶化,但不利于银纳米颗粒的均匀分布；与微晶纤维素制备的复合材料相比较,农林生物质棉秆综纤维素作为银纳米颗粒的载体,更有利于提高其分散性；经NaOH/尿素体系预处理棉秆综纤维素,其纤维形态分布较好,更有利于提高银的分散性。
以棉秆纤维为基体相,通过NaOH/尿素体系预处理棉秆纤维,采用超声波法制备棉秆纤维／银纳米复合材料。研究结果表明,硼氢化钠作还原剂,超声波反应40min时,复合材料表面生成线状纳米银；添加葡萄糖作还原剂,更有利于片状纳米银的生成；超声波反应时间增加导致棉秆纤维结晶度下降；硼氢化钠作还原剂制备的复合材料其热稳定性能有很大提高。
以微晶纤维素为基体相,分别采用LiC1/DMAc体系和NaOH/尿素体系预处理纤维素,再利用水热法将纤维素与二氧化钛进行复合。研究表明,不同的纤维素溶解体系制备的复合材料其形态有较大差别；NaOH/尿素体系预处理纤维素制备的复合材料无论是在物相、热稳定性还是抗菌性能上都优于LiC1/DMAc体系预溶解纤维素制备的复合材料。复合材料通过煅烧处理最终获得金红石相二氧化钛。
以微晶纤维素为基体相,乙酸锰和六次甲基四胺为原料,二甲基甲酰胺为溶剂,通过微波法制备纤维素/锰氧化物纳米复合材料。研究结果表明,加热时间增加导致纤维素结晶度降低；通过煅烧处理纤维素/锰氧化物纳米复合物获得三氧化二锰材料。以微晶纤维素为基体相,乙酸锰为锰源,采用超声波法制备纤维素／四氧化三锰纳米复合材料。研究表明,超声波反应90min,尿素、六次甲基四胺、氢氧化钠和氢氧化钾四种碱制备的复合材料其基体相表面的四氧化三锰颗粒形态有所不同；强碱氢氧化钠有利于无机颗粒形成具有长薄片状的形态；与尿素和六次甲基四胺相比较,氢氧化钠和氢氧化钾制备的纤维素/四氧化三锰纳米复合材料其热稳定性能更佳。通过煅烧处理纤维素/锰氧化物纳米复合材料获得具有尖晶石结构的四氧化三锰材料。
Combined with the advantages of the cellulose and inorganic antibacterial materials, the cellulose-based antimicrobial nanocomposites were synthesized by using cellulose as the matrix, and silver, silver chloride, titanium dioxide, other inorganic antimicrobial materials as the reinforcing phase, which had potential applications in the field of tissue engineering and biomedical owing to its unique properties such as biodegradation, biocompatibility, and antibacterial activities. Currently, there had been problems about the cellulose-based antimicrobial nanocomposites, such as the tedious preparation method and poor dispersion of the reinforcing phase in the matrix. This thesis focused on the above scientific issues, used green method to fabricate series of cellulose-based antimicrobial nanocomposites, characterized their phase, shape, dispersion, and explored the mechanism of the composites.
The cellulose/silver nanocomposites were in-situ synthesized by fast microwave-assisted heating method by using microcrystalline cellulose (MCC) as the matrix, ethylene glycol as the solvent, microwaves absorbers and reducing agent, and silver nitrate as reactant. The results showed that cellulose-silver nanocomposites were synthesized by microwave heating at140℃for only10min. By optimized the preparation parameters, it can be achieved uniform and stable distribution of silver nanoparticles on the cellulose matrix. Compared to the monomer-MCC, the thermal stability of the cellulose/silver nanocomposites had significantly improved. The prepared composites had obvious antibacterial properties against Escherichia coli and Staphylococcus aureus.
The cellulose/AgCl-Ag nanocomposites and cellulose/Ag nanocomposites were synthesized via microwave-assisted heating method by LiCl/DMAc pretreatment of cellulose using MCC as the matrix, DMAc as the solvent, and ascorbic acid as a reducing agent. The results indicated that series of cellulose/AgCl-Ag, cellulose/Ag-AgCl, and cellulose/Ag nanocomposites were synthesized by adjusted the concentration of ascorbic acid. Compared with the oil bath heating, microwave-assisted heating method was much more favor of the phase transition from silver chloride to silver and also conducive to improve the proportion of silver in nanocomposites. Compared to the cellulose/Ag nanocomposites, the antibacterial experiment demonstrated that the cellulose/AgCl-Ag nanocomposites had better antimicrobial effect against Escherichia coli and Staphylococcus aureus.
The cellulose/AgCl nanocomposites were synthesized via microwave-assisted heating method by LiCl/DMAc pretreatment of cellulose without any reducing agent using MCC as the matrix and DMAc as the solvent. The novel preparation method was based on the simultaneous formation of the AgCl nanoparticles and precipitation of the cellulose. The high heating temperature and long heating time are favorable for the complete formation of AgCl nanoparticles in the cellulose/AgCl nanocomposites. The cellulose/AgCl nanocomposites had good antibacterial activities against both E. coli (Gram-negative) and S. aureus (Gram-positive).
The holocellulose/Ag nanocomposites were synthesized via hydrothermal method by NaOH/urea pretreatment of holocellulose using holocellulose as the matrix from cotton stalk. Compared with the reductants of sodium borohydride and glucose, there had been a large number of silver nanosheets dispersed on the surface of composites prepared using fructose as reducing agent by hydrothermal method. The long hydrothermal reaction time is conducive to the crystallization of silver, but not favorable for the uniform distribution of silver nanoparticles. Holocellulose from cotton stalk as the carrier for silver nanoparticles, are much more conducive to improve the dispersion of silver nanoparticles in the cellulose matrix compared with the composites prepared by MCC. It has been well distributed for cotton stalk holocellulose fiber by NaOH/urea pretreatment, which were much more conducive to improve the dispersion of silver nanoparticles.
The cotton stalk fiber/Ag nanocomposites were synthesized via ultrasonic treatment by NaOH/urea pretreatment of cotton stalk fiber. It was generated linear nano-silver on the surface of the composites by using sodium borohydride as reducing agent via ultrasonic treatment for40min. It was much more conducive to the generation of the chip-like nano-silver using glucose as reducing agent. The crystallinity of cotton stalk fiber decreased with the increasing ultrasonic treatment time. The thermal stability was greatly improved by using sodium borohydride as reducing agent.
The cellulose/TiO2nanocomposites were synthesized via hydrothermal method by LiCl/DMAc pretreatment and NaOH/urea pretreatment of Cellulose, respectively, which were used MCC as the matrix. The morphology of the composites was different by using different cellulose dissolution systems. The composites prepared by NaOH/urea pretreatment were superior to the composites pretreated by LiCl/DMAc solution either in phase, thermal stability and antibacterial properties. The TiO2crystals were obtained by calcination the composites.
The cellulose/manganese oxide nanocomposites were synthesized via microwave-assisted heating method using MCC as the matrix, manganese acetate and hexamethylenetetramine (HMT) as raw materials, dimethylformamide (DMF) as a solvent. The crystallinity of cellulose decreased with the increasing microwave heating time. The Mn2O3materials were obtained by calcination the nanocomposites. The cellulose/Mn3O4nanocomposites were synthesized via ultrasonic treatment using MCC as the matrix, manganese acetate as manganese source. The particle morphology of the manganese tetroxide on the matrix of composites synthesized by ultrasonic treatment for90min were different using four kinds of alkalis——urea, HMT, sodium hydroxide and potassium hydroxide. Sodium hydroxide is conducive to the formation of inorganic particles having a long thin sheet-like morphology. Compared with urea and HMT, the thermal stability of the cellulose/Mn3O4nanocomposites prepared by sodium hydroxide and potassium hydroxide were much better. The Mn3O4materials with spinel structure were obtained by calcination the nanocomposites.
引文
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