壳聚糖基膜材料的制备、性能与结构表征
摘要
面对日益严峻的能源危机和“白色污染”等环境问题,壳聚糖凭借其良好的生物分解性,被认为是理想的生物质材料之一。凭借独特的抑菌杀菌作用、优越的成膜性和生物相容性,壳聚糖在食品包装和保鲜方面有着极大的发展前景。但目前壳聚糖膜材料在食品包装和果蔬保鲜方面应用时存在物理机械性能差、生产成本高等缺点。壳聚糖可以通过与其他材料共混改性,来改善其性能,同时降低生产成本。为此,本研究以壳聚糖为主要原料,选用淀粉、纤维素及其衍生物、二氧化钛(TiO2)等添加剂,复合制备了壳聚糖/淀粉可食膜、壳聚糖/纤维素抗菌膜、壳聚糖/TiO2保鲜膜,并研究了膜的性能；采用傅立叶红外光谱、X射线衍射、扫描电镜、热分析、激光粒度分析等现代分析手段,系统研究了壳聚糖基膜材料的结构,讨论了共混材料中各组分相互作用的机理。主要研究结论如下：
(1)羧甲基纤维素钠(CMCNa)能够显著改善壳聚糖/淀粉可食膜的韧性,使膜断裂伸长率增加4.5倍；甲基纤维素(MC)能够增强改性壳聚糖/淀粉可食膜,使膜拉伸强度提高了71%;两种可食膜在碱液中基本不变形,对金黄色葡萄球菌和大肠杆菌的抗菌性都达到90%以上。壳聚糖/淀粉/CMCNa膜中同时存在COO和NH3,能够形成较强的NH3+-COO-离子键连接,生成聚合物电解质。MC能够与壳聚糖和淀粉形成稳固的氢键连接。
(2)功率为50W的超声波处理微晶纤维素(MCC)60min后,与未活化的MCC比较,样品溶解时间减少了87%,溶解度增加了1.3倍。经活化处理后的样品OH缔合强度降低,游离出来的自由OH增加。NaOH尿素-硫脲体系下壳聚糖/纤维素抗菌膜的优化制备工艺是2.5%纤维素完全溶解于氢氧化钠、尿素、硫脲质量分数分别为8%、8%、6.5%的溶液中,与3.6%水溶性壳聚糖共混流延制膜,分别经过5%Na2SO4/5%H2SO,凝固液、0.5%的NaOH溶液、10%甘油浸泡并自然干燥。酸性体系下壳聚糖/纤维素抗菌膜的拉伸强度、断裂伸长率较壳聚糖膜分别提高了16.7%和5倍；碱性体系下壳聚糖/纤维素抗菌膜具有良好的柔软性,柔软度与卫生纸(一等品)接近。两种抗菌膜对金黄色葡萄球菌和大肠杆菌的抗菌性都大于99%。
(3)超声波和阴离子表面活性剂(月桂酸钠)共同改性处理后的TiO2较未处理的原料平均粒径减少了21.4%、亲油化度提高了24%。直接共混法制备的壳聚糖/TiO2保鲜膜的拉伸强度、断裂伸长率较壳聚糖膜分别提高了50.4%和9.6倍；溶胶凝胶膜的拉伸强度又比直接共混膜提高了34%,透氧量下降73.7%,透二氧化碳量下降46.7%。溶胶凝胶膜使西红柿的保鲜时间由6天延长至11天。壳聚糖/TiO2保鲜膜中壳聚糖的-NH2、-CH、-OH与TiO2之间有较强的氢键作用。溶胶凝胶膜中的TiO2以无定形的形式存在,溶胶凝胶膜中的水分,除了结合松散的自由水外,还有与-NH2、-OH等连接的结合水。
论文首次对比研究了CMCNa和MC对壳聚糖/淀粉可食膜特性的不同影响;提出了可用作内缓冲包装材料的NaOH-尿素-硫脲体系下壳聚糖/纤维素抗菌膜的制备工艺；将纳米TiO2溶胶进行改性后用于制备壳聚糖基保鲜膜,延长了果蔬的保鲜期,并发现了TiO2溶胶与壳聚糖的作用机理。
The environmental problems such as energy crisis and white pollution are increasingly serious. Chitosan is considered to be one of ideal biomass materials because of its good biodegradability. With unique antibacterial properties, excellent film-forming properties and biocompatibility, chitosan in food packaging and preservation has great prospects for development.
But chitosan film has some drawbacks such as poor physical and mechanical properties and high cost of production which limit the application in food packaging and preservation. The properties of chitosan can be enhanced and the production cost can be reduced if other materials were introduced into chitosan. In this study, starch, cellulose and its derivatives, titanium dioxide were incorporated into chitosan. Chitosan/starch edible film, chitosan/cellulose antibacterial film and chitosan/titanium dioxide (TiO2) preservative film were then elaborated and properties of films are discussed.The structure of chitosan-based film was assessed through Fourier transform infrared spectroscopy, X-ray deffraction, scanning electron microscopy, thermal analysis and particle laser analyzer. The interaction mechanism of the various components in the blend films was discussed.The main conclusions are as follows:
(1) Sodium carboxymethyl cellulose (CMCNa) significantly improved the toughness of the chitosan/starch edible film and the elongation-at-break of blend film increased by4.5times. The methyl cellulose (MC) enhanced the tensile strength of chitosan/starch edible film which increased by71%. The two edible films Immersed in alkaline solution keep the same shape. The antibacterial rates of the two edible films to bacillus coli and staphylococcus aureus were all more than90%. There was the strong ionic bond connection between NH5+and COO-in chitosan/starch/CMCNa film and polymer electrolyte was generated.The strong hydrogen bonding occurred among MC, chitosan and starch.
(2) Microcrystalline cellulose (MCC) was processed by ultrasonic at50W for60min. Compared with the unactivated MCC, its dissolution time decreased by87%and solubility increased by1.3times. The hydroxy association strength decreases and free hydroxyl increased in the samples after the activation treatment. The optimized preparation process of chitosan/cellulose antimicrobial film in an aqueous solution of sodium hydroxide (NaOH)/urea/thiourea was obtained. Amixture of an aqueous solution was prepared by directly mixed NaOH/urea/thiourea in the ration8.0/8.0/6.5(w/w/w).2.5wt%cellulose was completely dissolved in the solution and then3.6wt%water-soluble chitosan was added. The resulting solution was cast onto a plate to get films which were immersed into5wt%Na2SO4/5wt%H2SO4coagulation liquid,0.5wt%NaOH solution,10%glycerol solution sequentially and were air-dried at room temperature. Compared with chitosan films, the tensile strength and elongation-at-break of chitosan/cellulose antimicrobial films elaborated under the acidic system increased by16.7%and5times respectively. Chitosan/cellulose antimicrobial films elaborated under the alkaline system had good flexibility and softnesses of antimicrobial films and toilet paper (first class) were roughly same. The antibacterial rates of the two antimicrobial films to bacillus coli and staphylococcus aureus were all more than99%.
(3) Titanium dioxide (TiO2) was modified by ultrasonic and anionic surfactant (sodium laurate). Compared to unmodified TiO2, the average particle size decreased by21.4%, the lipophilic degree increased by24%. Compared with chitosan films, the tensile strength and elongation-at-break of chitosan/TiO2preservative films elaborated by direct blending method increased by50.4%and9.6times respectively. The tensile strength of chitosan/TiO2preservative films elaborated by Sol-gel method was higher than that of films by direct blending method, increasing by34%. The oxygen and carbon dioxide transmission rate of sol-gel films were lower than that of direct blending films, decreasing by73.7%and46.7%respectively. The preservative life of tomatoes packed in sol-gel films was extended from6days to11days. There was strong hydrogen bonding among-NH2,-CH,-OH and TiO2in chitosan/TiO2preservative films. TiO2in the sol-gel films was amorphous. In addition to free water, there was bound water connected with-NH2,-OH in the sol-gel films.
The paper firstly comparatively studied the different effects of CMCNa and MC on properties of chitosan/starch edible films. Preparation process of chitosan/cellulose antibacterial film for inner cushioning packaging material in an aqueous solution of NaOH/urea/thiourea is provided. The paper prepared chitosan-based preservative films using TiO2after modification which extend the preservative life of fruits and vegetables and studied the mechanism of action of TiO2and chitosan in the sol-gel films.
(1)羧甲基纤维素钠(CMCNa)能够显著改善壳聚糖/淀粉可食膜的韧性,使膜断裂伸长率增加4.5倍；甲基纤维素(MC)能够增强改性壳聚糖/淀粉可食膜,使膜拉伸强度提高了71%;两种可食膜在碱液中基本不变形,对金黄色葡萄球菌和大肠杆菌的抗菌性都达到90%以上。壳聚糖/淀粉/CMCNa膜中同时存在COO和NH3,能够形成较强的NH3+-COO-离子键连接,生成聚合物电解质。MC能够与壳聚糖和淀粉形成稳固的氢键连接。
(2)功率为50W的超声波处理微晶纤维素(MCC)60min后,与未活化的MCC比较,样品溶解时间减少了87%,溶解度增加了1.3倍。经活化处理后的样品OH缔合强度降低,游离出来的自由OH增加。NaOH尿素-硫脲体系下壳聚糖/纤维素抗菌膜的优化制备工艺是2.5%纤维素完全溶解于氢氧化钠、尿素、硫脲质量分数分别为8%、8%、6.5%的溶液中,与3.6%水溶性壳聚糖共混流延制膜,分别经过5%Na2SO4/5%H2SO,凝固液、0.5%的NaOH溶液、10%甘油浸泡并自然干燥。酸性体系下壳聚糖/纤维素抗菌膜的拉伸强度、断裂伸长率较壳聚糖膜分别提高了16.7%和5倍；碱性体系下壳聚糖/纤维素抗菌膜具有良好的柔软性,柔软度与卫生纸(一等品)接近。两种抗菌膜对金黄色葡萄球菌和大肠杆菌的抗菌性都大于99%。
(3)超声波和阴离子表面活性剂(月桂酸钠)共同改性处理后的TiO2较未处理的原料平均粒径减少了21.4%、亲油化度提高了24%。直接共混法制备的壳聚糖/TiO2保鲜膜的拉伸强度、断裂伸长率较壳聚糖膜分别提高了50.4%和9.6倍；溶胶凝胶膜的拉伸强度又比直接共混膜提高了34%,透氧量下降73.7%,透二氧化碳量下降46.7%。溶胶凝胶膜使西红柿的保鲜时间由6天延长至11天。壳聚糖/TiO2保鲜膜中壳聚糖的-NH2、-CH、-OH与TiO2之间有较强的氢键作用。溶胶凝胶膜中的TiO2以无定形的形式存在,溶胶凝胶膜中的水分,除了结合松散的自由水外,还有与-NH2、-OH等连接的结合水。
论文首次对比研究了CMCNa和MC对壳聚糖/淀粉可食膜特性的不同影响;提出了可用作内缓冲包装材料的NaOH-尿素-硫脲体系下壳聚糖/纤维素抗菌膜的制备工艺；将纳米TiO2溶胶进行改性后用于制备壳聚糖基保鲜膜,延长了果蔬的保鲜期,并发现了TiO2溶胶与壳聚糖的作用机理。
The environmental problems such as energy crisis and white pollution are increasingly serious. Chitosan is considered to be one of ideal biomass materials because of its good biodegradability. With unique antibacterial properties, excellent film-forming properties and biocompatibility, chitosan in food packaging and preservation has great prospects for development.
But chitosan film has some drawbacks such as poor physical and mechanical properties and high cost of production which limit the application in food packaging and preservation. The properties of chitosan can be enhanced and the production cost can be reduced if other materials were introduced into chitosan. In this study, starch, cellulose and its derivatives, titanium dioxide were incorporated into chitosan. Chitosan/starch edible film, chitosan/cellulose antibacterial film and chitosan/titanium dioxide (TiO2) preservative film were then elaborated and properties of films are discussed.The structure of chitosan-based film was assessed through Fourier transform infrared spectroscopy, X-ray deffraction, scanning electron microscopy, thermal analysis and particle laser analyzer. The interaction mechanism of the various components in the blend films was discussed.The main conclusions are as follows:
(1) Sodium carboxymethyl cellulose (CMCNa) significantly improved the toughness of the chitosan/starch edible film and the elongation-at-break of blend film increased by4.5times. The methyl cellulose (MC) enhanced the tensile strength of chitosan/starch edible film which increased by71%. The two edible films Immersed in alkaline solution keep the same shape. The antibacterial rates of the two edible films to bacillus coli and staphylococcus aureus were all more than90%. There was the strong ionic bond connection between NH5+and COO-in chitosan/starch/CMCNa film and polymer electrolyte was generated.The strong hydrogen bonding occurred among MC, chitosan and starch.
(2) Microcrystalline cellulose (MCC) was processed by ultrasonic at50W for60min. Compared with the unactivated MCC, its dissolution time decreased by87%and solubility increased by1.3times. The hydroxy association strength decreases and free hydroxyl increased in the samples after the activation treatment. The optimized preparation process of chitosan/cellulose antimicrobial film in an aqueous solution of sodium hydroxide (NaOH)/urea/thiourea was obtained. Amixture of an aqueous solution was prepared by directly mixed NaOH/urea/thiourea in the ration8.0/8.0/6.5(w/w/w).2.5wt%cellulose was completely dissolved in the solution and then3.6wt%water-soluble chitosan was added. The resulting solution was cast onto a plate to get films which were immersed into5wt%Na2SO4/5wt%H2SO4coagulation liquid,0.5wt%NaOH solution,10%glycerol solution sequentially and were air-dried at room temperature. Compared with chitosan films, the tensile strength and elongation-at-break of chitosan/cellulose antimicrobial films elaborated under the acidic system increased by16.7%and5times respectively. Chitosan/cellulose antimicrobial films elaborated under the alkaline system had good flexibility and softnesses of antimicrobial films and toilet paper (first class) were roughly same. The antibacterial rates of the two antimicrobial films to bacillus coli and staphylococcus aureus were all more than99%.
(3) Titanium dioxide (TiO2) was modified by ultrasonic and anionic surfactant (sodium laurate). Compared to unmodified TiO2, the average particle size decreased by21.4%, the lipophilic degree increased by24%. Compared with chitosan films, the tensile strength and elongation-at-break of chitosan/TiO2preservative films elaborated by direct blending method increased by50.4%and9.6times respectively. The tensile strength of chitosan/TiO2preservative films elaborated by Sol-gel method was higher than that of films by direct blending method, increasing by34%. The oxygen and carbon dioxide transmission rate of sol-gel films were lower than that of direct blending films, decreasing by73.7%and46.7%respectively. The preservative life of tomatoes packed in sol-gel films was extended from6days to11days. There was strong hydrogen bonding among-NH2,-CH,-OH and TiO2in chitosan/TiO2preservative films. TiO2in the sol-gel films was amorphous. In addition to free water, there was bound water connected with-NH2,-OH in the sol-gel films.
The paper firstly comparatively studied the different effects of CMCNa and MC on properties of chitosan/starch edible films. Preparation process of chitosan/cellulose antibacterial film for inner cushioning packaging material in an aqueous solution of NaOH/urea/thiourea is provided. The paper prepared chitosan-based preservative films using TiO2after modification which extend the preservative life of fruits and vegetables and studied the mechanism of action of TiO2and chitosan in the sol-gel films.
引文
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