碳基抗菌复合材料的制备与性能研究
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摘要
本论文中,我们研究了四种不同类型的多孔碳基材料,通过物理或化学的方法将银、铜等金属(或其离子)负载在碳基材料上制得系列无机复合抗菌材料,并采用各种测试方法对其结构与性能进行了表征与分析。具体内容总结如下：
(1)以TiO2为核、蔗糖为碳源,采用水热法制备了TiO2@C核壳结构材料,然后通过在AgNO3溶液中浸渍后,将Ag+固定在TiO2@C载体上,得到了TiO2@C/Ag核壳复合材料。研究发现,制备TiO2@C载体的最佳条件是600℃、16 h。随着蔗糖/TiO2质量比的增加,炭壳的厚度也随之增加,锐钛矿相的TiO2越来越稳定。抗菌结果表明,由于银和TiO2协同抗菌作用,使得TiO2@C/Ag核壳复合材料具有良好的抗菌活性。
(2)以无水醋酸锌为碳源,在密闭的高温反应釜中600℃反应8 h,得到ZnO@CNTs核壳结构材料,经化学还原法将银吸附在炭壳的表面,制备了ZnO@CNTs/Ag核壳复合抗菌材料。实验过程中,我们发现AgNO3溶液的浓度和超声时间对银的负载影响较大,并得到制备ZnO@CNTs/Ag的最佳条件：AgNO3的浓度为0.1 mol/L,超声搅拌时间为60 min。抗菌结果显示,ZnO@CNTs核壳结构材料具有微弱的抗菌活性,这是由于ZnO的光催化作用所致,而ZnO@CNTs/Ag却表现出了很强的抗菌活性。
(3)以水热法合成的炭微球为原料,经KOH活化制备了活性炭微球,通过在氯化铜溶液中浸渍使铜吸附在活性炭微球上,得到载铜活性炭微球。研究表明,当Cu2+浓度适量,氨水与Cu2+的摩尔比为1：1时,是制备铜负载活性炭微球的最佳条件。活性炭微球表面负载的铜是以+2价形式存在,并且随着溶液中铜离子浓度的增加,载铜量增大,氨水的加入可明显提高铜的负载量。抗菌结果显示,载铜活性炭微球对大肠杆菌(E coil)和金黄色葡萄球菌(S. aureus)具有良好的杀灭能力。
(4)采用独特孔隙结构、高比表面积的有序介孔炭CMK-3为载体,通过直接在CuCl2溶液中浸渍制备了Cu/CMK-3复合抗菌材料。研究表明,负载在CMK-3上的铜是以+2价形式存在,并且单纯的CMK-3是没有抗菌活性的,而Cu/CMK-3却具有良好的抗菌活性。
In this paper, we studied four different types of porous carbon-based materials, and uesd physical or chemical method to load silver or copper metal (Ag+or Cu2+) on the carbon-based materials to obtain series of inorganic antibacterial composites. The structures and properties of as-prepared samples were characterized and analyzed by various methods. The major contents were summarized as follows:
(1) TiO2@C core-shell composite was prepared by a hydrothermal method using TiO2 as core and sucrose as carbon source. Then the synthesized TiO2@C served as a support for the immobilization of Ag by impregnation in AgN03 aqueous solution to obtain TiO2@C/Ag core-shell composite. It found that the optimized synthesis condition was identified at 600℃for 16 h. With the mass ratio of sucrose/TiO2 increasing, the carbon shell became thicker and the anatase TiO2 phase became more stable. The results indicate that the TiO2@C/Ag core-shell composite has excellent antibacterial activity due to the synergistic antibacterial effect of silver and TiO2.
(2) ZnO@CNTs core-shell structure composite was synthesized in a closed reactor at 600℃for 8 h by using anhydrous zinc acetate as carbon source. Silver was absorbed on the surface of ZnO@CNTs core-shell composite by the chemical reduction method, and then the ZnO@CNTs/Ag core-shell composite was obtained. During the experiment, we found that the concentration of AgNO3 aqueous solution and the ultrasonic time have great influence on the loading of silver. When the AgNO3 concentration was 0.1 mol/L and the ultrasonic stirring time was 60 min, the optimal ZnO@CNTs/Ag core-shell composite was prepared. The antibacterial results indicate that ZnO@CNTs core-shell material has weak antibacterial activity owing to the photocatalysis of ZnO. However, the as-prepared ZnO@CNTs/Ag shows strong antibacterial activity.
(3) Carbon microspheres were prepared via a hydrothermal method, and then activated with KOH to form activated carbon microspheres (ACMs). Copper-loaded activated carbon microspheres (Cu/ACMs) were obtained by the direct immersion in aqueous solution. It shows that when in the right concentration of Cu2+, the optimized preparation condition of Cu/ACMs is in the molar ratio of ammonia/Cu2+ =1:1. The experimental results show that the copper valence state of Cu-ACMs samples is Cu2+ion, and the amount of absorbed copper increases with the increase of copper ion concentration in solution. The addition of ammonia can significantly improve the amount of absorbed copper. The antibacterial activities of as-prepared materials were measured. The measured result indicates that the Cu/ACMs have the good activities to kill E. coli and S. aureus.
(4) Cu/CMK-3 composite material was prepared by the direct immension in CuCl2 aqueous solution, using ordered mesoporous carbon (CMK-3) as a carrier, which has ordered pore structure and high specific surface area. The results show that the supported copper on CMK-3 was observed to be the bivalence state. Furthermore, pure CMK-3 has no antibacterial activity, but Cu/CMK-3 has good antibacterial activity.
(1)以TiO2为核、蔗糖为碳源,采用水热法制备了TiO2@C核壳结构材料,然后通过在AgNO3溶液中浸渍后,将Ag+固定在TiO2@C载体上,得到了TiO2@C/Ag核壳复合材料。研究发现,制备TiO2@C载体的最佳条件是600℃、16 h。随着蔗糖/TiO2质量比的增加,炭壳的厚度也随之增加,锐钛矿相的TiO2越来越稳定。抗菌结果表明,由于银和TiO2协同抗菌作用,使得TiO2@C/Ag核壳复合材料具有良好的抗菌活性。
(2)以无水醋酸锌为碳源,在密闭的高温反应釜中600℃反应8 h,得到ZnO@CNTs核壳结构材料,经化学还原法将银吸附在炭壳的表面,制备了ZnO@CNTs/Ag核壳复合抗菌材料。实验过程中,我们发现AgNO3溶液的浓度和超声时间对银的负载影响较大,并得到制备ZnO@CNTs/Ag的最佳条件：AgNO3的浓度为0.1 mol/L,超声搅拌时间为60 min。抗菌结果显示,ZnO@CNTs核壳结构材料具有微弱的抗菌活性,这是由于ZnO的光催化作用所致,而ZnO@CNTs/Ag却表现出了很强的抗菌活性。
(3)以水热法合成的炭微球为原料,经KOH活化制备了活性炭微球,通过在氯化铜溶液中浸渍使铜吸附在活性炭微球上,得到载铜活性炭微球。研究表明,当Cu2+浓度适量,氨水与Cu2+的摩尔比为1：1时,是制备铜负载活性炭微球的最佳条件。活性炭微球表面负载的铜是以+2价形式存在,并且随着溶液中铜离子浓度的增加,载铜量增大,氨水的加入可明显提高铜的负载量。抗菌结果显示,载铜活性炭微球对大肠杆菌(E coil)和金黄色葡萄球菌(S. aureus)具有良好的杀灭能力。
(4)采用独特孔隙结构、高比表面积的有序介孔炭CMK-3为载体,通过直接在CuCl2溶液中浸渍制备了Cu/CMK-3复合抗菌材料。研究表明,负载在CMK-3上的铜是以+2价形式存在,并且单纯的CMK-3是没有抗菌活性的,而Cu/CMK-3却具有良好的抗菌活性。
In this paper, we studied four different types of porous carbon-based materials, and uesd physical or chemical method to load silver or copper metal (Ag+or Cu2+) on the carbon-based materials to obtain series of inorganic antibacterial composites. The structures and properties of as-prepared samples were characterized and analyzed by various methods. The major contents were summarized as follows:
(1) TiO2@C core-shell composite was prepared by a hydrothermal method using TiO2 as core and sucrose as carbon source. Then the synthesized TiO2@C served as a support for the immobilization of Ag by impregnation in AgN03 aqueous solution to obtain TiO2@C/Ag core-shell composite. It found that the optimized synthesis condition was identified at 600℃for 16 h. With the mass ratio of sucrose/TiO2 increasing, the carbon shell became thicker and the anatase TiO2 phase became more stable. The results indicate that the TiO2@C/Ag core-shell composite has excellent antibacterial activity due to the synergistic antibacterial effect of silver and TiO2.
(2) ZnO@CNTs core-shell structure composite was synthesized in a closed reactor at 600℃for 8 h by using anhydrous zinc acetate as carbon source. Silver was absorbed on the surface of ZnO@CNTs core-shell composite by the chemical reduction method, and then the ZnO@CNTs/Ag core-shell composite was obtained. During the experiment, we found that the concentration of AgNO3 aqueous solution and the ultrasonic time have great influence on the loading of silver. When the AgNO3 concentration was 0.1 mol/L and the ultrasonic stirring time was 60 min, the optimal ZnO@CNTs/Ag core-shell composite was prepared. The antibacterial results indicate that ZnO@CNTs core-shell material has weak antibacterial activity owing to the photocatalysis of ZnO. However, the as-prepared ZnO@CNTs/Ag shows strong antibacterial activity.
(3) Carbon microspheres were prepared via a hydrothermal method, and then activated with KOH to form activated carbon microspheres (ACMs). Copper-loaded activated carbon microspheres (Cu/ACMs) were obtained by the direct immersion in aqueous solution. It shows that when in the right concentration of Cu2+, the optimized preparation condition of Cu/ACMs is in the molar ratio of ammonia/Cu2+ =1:1. The experimental results show that the copper valence state of Cu-ACMs samples is Cu2+ion, and the amount of absorbed copper increases with the increase of copper ion concentration in solution. The addition of ammonia can significantly improve the amount of absorbed copper. The antibacterial activities of as-prepared materials were measured. The measured result indicates that the Cu/ACMs have the good activities to kill E. coli and S. aureus.
(4) Cu/CMK-3 composite material was prepared by the direct immension in CuCl2 aqueous solution, using ordered mesoporous carbon (CMK-3) as a carrier, which has ordered pore structure and high specific surface area. The results show that the supported copper on CMK-3 was observed to be the bivalence state. Furthermore, pure CMK-3 has no antibacterial activity, but Cu/CMK-3 has good antibacterial activity.
引文
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