CN111183979A - 一种高效复合无机抗菌剂及其制备方法 - Google Patents
一种高效复合无机抗菌剂及其制备方法 Download PDFInfo
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- CN111183979A CN111183979A CN202010077615.XA CN202010077615A CN111183979A CN 111183979 A CN111183979 A CN 111183979A CN 202010077615 A CN202010077615 A CN 202010077615A CN 111183979 A CN111183979 A CN 111183979A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/80—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with zinc, cadmium or mercury
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8906—Iron and noble metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8933—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/8953—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with zinc, cadmium or mercury
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plant Pathology (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Dentistry (AREA)
- Wood Science & Technology (AREA)
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Abstract
一种高效复合无机抗菌剂及其制备方法,属于纳米材料制备技术领域。按重量份组成为:坡缕石100份,光催化材料30~50份,石墨烯3~5份,金属氧化物和/或金属盐2~8份,聚季铵盐0.5~2份。以多孔道结构的坡缕石为载体,将其与石墨烯进行微观纳米复合,使坡缕石载体和石墨烯均能够在加工和使用过程中保持高度分散状态,同时加入了具有抗菌作用的光催化材料、金属氧化物和金属盐类,制备成具有光催化作用、电子迁移破壁、金属离子抗菌多种功能协同增效的新型复合无机抗菌材料。可以通过其良好的分散性,提高抗菌活性成分与细菌接触面积,通过各抗菌成分协同发挥抗菌作用,从而达到杀灭细菌以及高效抑制细菌繁殖的作用。
Description
技术领域
本发明涉及一种无机抗菌剂及其制备方法,属于纳米材料制备技术领域,具体是涉及一种坡缕石-石墨烯复合型高效无机抗菌剂及其制备方法。
背景技术
众所周知,当今世界已步入医疗技术高度发达、健康促进行业多元发展的时代,但是,由于接触环境中的病原菌感染仍然是人类面临的重要威胁之一,导致每年数以百万计的感染患者出现,而细菌抗药性的出现与扩散已严重威胁全球公共卫生安全,因此,发展新型抗菌药物是解决细菌抗药性的关键策略之一。目前国内外抗菌材料分为天然、有机和无机三大系列。天然系抗菌剂品种不多,目前尚未规模化,有机系抗菌剂主要包括有机酸/酯、醇和酚类物质,是最早商品化的抗菌剂,但由于其对人体和环境有一定危害,同时因其耐热性差、易水解、使用寿命短等问题而无法推广应用到塑料、橡胶、陶瓷、化纤、涂料等制品中。
近年来,无机抗菌剂发展迅速,无机抗菌剂以其广谱、耐热、安全、高效和持久的抗菌效果而越来越受到广泛的重视,无机抗菌材料又可分为银系无机抗菌剂、氧化物光催化系无机抗菌剂和氧化物天然矿物类无机抗菌剂。纳米无机抗菌剂报道较多,大多是在无机载体材料(如分子筛、蒙脱土、碳酸钙等)上负载纳米级银、锌、铜、稀土元素等,其缺点是载体材料的团聚导致吸附性弱、比表面积小,从而使抗菌有效成分负载少,抗菌剂用量大。
坡缕石是一种以镁、铝为主的纤维状硅酸盐矿物,其具有发达的孔道结构,被称为“千土之王”,目前世界上仅有中国、美国、俄罗斯、西班牙、墨西哥等极少数国家或地区产出该类矿床。坡缕石矿物已成为世界性稀缺资源,它具有优良的胶体性能、吸附性能和催化性能。长期以来,我国坡缕石主要用作钻井泥浆,其内在价值未得到充分体现。因其无毒无害,在环境和健康领域具有广阔的应用前景。
自从2004年英国曼彻斯特大学的物理学家安德烈·盖姆和康斯坦丁·诺沃肖洛夫发现石墨烯以来,各国研究人员对其进行了大量的应用研究,发现其具有高导电性、高稳定性、高比表面积等优异特性,有研究表明,氧化石墨烯表面含有各种含氧官能团,这些含氧官能团具有较高的反应活性,当其黏附于细菌细胞表面时可以通过电子转移破坏其细胞壁与细胞膜的完整性导致细菌死亡。石墨烯抗菌性能的发挥取决于其良好的分散状态,而目前对于石墨烯在使用中保持分散状态仍是相当困难的。但其用于抗菌剂的制备方面至今几乎是空白的。
同时,目前的无机抗菌剂多以人工合成的具有层状或网状的无机材料为载体,以银、铜、锌为抗菌有效成分,还有部分以纳米二氧化钛为载体,辅助以光催化材料、银等制备得到了具有良好的抗菌特性的无机抗菌材料。这些抗菌材料的载体都是人工合成的氧化物,其成本高、抗菌活性成分单一、载体和抗菌成分难于分散导致用量大、抗菌效率低、速度慢,无法发挥载体与多种抗菌成分的协同作用。
本发明采用了以多孔道结构的坡缕石为载体,将其与石墨烯进行微观纳米复合,使坡缕石载体和石墨烯均能够在加工和使用过程中保持高度分散状态,同时加入了具有抗菌作用的光催化材料、金属氧化物和金属盐类,制备成新型高效复合无机抗菌剂。
发明内容
本发明针对已有无机抗菌剂中所存在的不足之处,提供一种具有光催化作用、电子迁移破壁、金属离子抗菌功能多种功能协同增效的新型高效复合无机抗菌剂。本发明的另一目的是提供该高效复合无机抗菌剂的制备方法。
为了实现上述目的,本发明所采用的技术方案为:一种高效复合无机抗菌剂,按重量份组成为:坡缕石100份,光催化材料30~50份,石墨烯3~5份,金属氧化物和/或金属盐2~8份,聚季铵盐0.5~2份。
一种高效复合无机抗菌剂的制备方法,包括如下步骤:
1)改性:将坡缕石和聚季铵盐按配比进行混合;
2)制备坡缕石水悬浮液:将坡缕石-聚季铵盐混合粉体加入到去离子水中,按重量比为1:20~40配成水悬浮液,并采用超声处理2~4小时;
3)制备石墨烯水悬浮液:将石墨烯粉体加入到去离子水中,按重量比为1:10~50配成水悬浮液,并采用超声处理2~4小时;
4)制浆:将所得到的坡缕石水悬浮液和石墨烯水悬浮液进行混合,并进行搅拌0.5~2小时;加入光催化材料、金属氧化物和/或金属盐混合均匀,过滤后将其调制成含水50~70%的浆料;
5)湿研磨:把配制好的浆料在高能行星球磨机中,在300~500转/分钟的速率下高速研磨12~48小时;
6)烘干:把经过研磨的粉体料浆在100~200℃烘干,脱去料浆中的水分;
7)焙烧:将烘干后的产物在温度400~700℃下焙烧2~5小时;
8)干研磨:将焙烧后产物在高能行星球磨机上研磨至粒度≤5μm;
9)包装:将最后产物分级、包装,即得到高效复合无机抗菌剂。
本发明的高效复合无机抗菌剂的组分中:
1、坡缕石
坡缕石黏土呈青灰色、灰色,致密块状,塑性大,呈层状,显微镜下呈泥质结构,矿物组成主要由坡缕石和石英组成。在电镜下观察,坡缕石单体呈细长的纤维状、针状、集合体呈球状、干稻草堆状。矿石具有抗盐造浆性能好、胶质价高。坡缕石黏土的化学成分以SiO2、MgO和Al2O3为主,并含有一定的Fe2O3。其晶体化学式为:(Mg,Al,Fe)5Si8O20(OH)24(H2O)·nH2O。坡缕石具有表面颠覆性吸附及微孔分子筛吸附的物化吸附作用,其孔道结构赋予了坡缕石具有大比表面积和微孔体积,其于国内外已被广泛地应用于石油钻井工业的抗盐泥浆。
本发明中所采用的坡缕石为2:1型层链状结构的针棒状坡缕石、纤维状坡缕石、绒状坡缕石、土状坡缕石,更优选为95~100%纯度的纤维状坡缕石。
2、光催化材料
光催化材料可选用n型半导体材料,如纳米TiO2、纳米ZnO、纳米CdO、纳米SnO2,其中优选为锐钛型纳米TiO2,其具有活性高,稳定性好,且对人体无害。TiO2本身并非抗菌材料,其禁带宽度为3.2eV,当用波长一定的光照射时,产生的高活性电子和空穴能使空气中的氧分子、水分子形成反应活性极强的羟基自由基,羟基自由基能有效的分解细菌的有机物,使细菌蛋白质变异,从而抑制了细菌的繁殖功能
3、石墨烯
石墨烯具有高导电性、高稳定性、高比表面积等优异特性,氧化石墨烯表面含有丰富的含氧官能团,这些含氧官能团具有较高的反应活性,当其黏附于细菌细胞表面时可以通过电子转移破坏其细胞壁与细胞膜的完整性导致细菌死亡。石墨烯与坡缕石进行纳米尺度的复合后,可使石墨烯处于分散状态,从而能够较充分地发挥石墨烯的表面抗菌活性,同时,由于其可以将易于堆垛的坡缕石进行分隔,使坡缕石能够更多地负载银离子和金属氧化物,因此,其在抗菌剂中可起协同促进作用。
本发明中所采用的石墨烯为1~4层的少片层氧化石墨烯,它自身作为抗菌活性成分并同时作为抗菌剂的协同促进剂。
4、金属氧化物、金属盐
无机化合物、金属离子或金属氧化物接触微生物后,在金属离子催化作用下会产生活性氧,在活性氧的作用下会发生阻碍微生物呼吸、电子转移、阻碍酶的作用、破坏蛋白质、损伤细胞膜以及干扰DNA的合成,通过这些作用达到杀菌和抑菌的效果。
本发明所采用的金属氧化物为MgO,ZnO,CaO,Al2O3,优选为MgO、ZnO。
本发明所采用的金属盐的金属离子为:Ag,Co,Fe,Sn,Al,Zn,Cu,Ni,金属盐是这些金属离子的硝酸盐、硫酸盐、磷酸盐、碳酸盐或有机酸盐。优选为AgNO3。
本发明高效复合无机抗菌剂的抗菌机理为:
以二氧化钛作为光催化材料为例,复合无机抗菌剂组分中,坡缕石、石墨烯和二氧化钛三者协同作用,可显著提高TiO2的光催化活性,TiO2受到能量大于带隙能的光激发时,价带上的电子受激发越过禁带进入导带,并在价带上留下空穴。TiO2表面羟基俘获光生空穴羟基自由基(·OH),羟基自由基能迅速发生夺氢反应:光生电子与O2反应形成过氧化物自由基(O2 2-),具有强氧化能力的·OH和O2 2-自由基可与细菌的细胞壁发生生化反应,使细胞壁发生代谢障碍从而导致细菌死亡。但在价带电子吸收光子跃迁到导带的同时,还会有相当部分光生电子回迁至价带与空穴复合。由于银离子自身具有优越的抗菌性能,同时其具有复杂的电子结构,其电子容易激发,银的掺入减少了TiO2表面光生电子e-和光生空穴的h+复合,这种异质结使TiO2表面产生更多的·OH,提高了光催化剂的活性。
在自然光和天然辐射条件下产生:
TiO2+hν→e-+h+
上述作用效果是永久循环的,凡是在自然光条件下都可以应用。
与现有技术相比,本发明的有益效果表现在:
1)、本发明的无机抗菌剂具有光催化作用、电子迁移破壁、金属离子抗菌功能,活性成分高分散状态,是多种功能协同增效的新型复合无机抗菌材料。该抗菌材料可以通过其良好的分散性,提高抗菌活性成分与细菌接触面积,通过各抗菌成分协同发挥抗菌作用,从而达到杀灭细菌以及高效抑制细菌繁殖的作用。
2)、本发明的无机抗菌剂性能优异,具有无毒、快速、高效、长效、广谱、不产生耐药性等优点,特别是其优异的耐热性、化学稳定性,解决了普通无机抗菌剂杀菌效率低、速度慢的特点。可在纤维、塑料、陶瓷、涂料、橡胶领域内使用,抗菌效果良好。具有良好的市场前景,值得推广。
附图说明
图1为本发明高效复合无机抗菌剂制备方法流程框图。
图中,1、坡缕石,2、聚季铵盐,3、改性坡缕石水悬液,4、石墨烯水悬液,5、光催化材料,6、金属氧化物和/或金属盐,7、原料混合料浆,8、研磨后粉体,9、干燥、焙烧、研磨后粉体。
具体实施方式
请参阅图1所示,本发明的无机抗菌剂是以天然高纯坡缕石纳米矿物为载体,对其进行改性后与石墨烯进行插层复合制成纳米复合粉体,再在其中加入纳米光催化材料、金属氧化物和/或金属盐类,通过过滤、研磨、干燥、焙烧等工艺方法制备成高效复合无机抗菌剂。下面结合实施例对本发明作进一步详细的表述:
实施例1
把纯度为95%的针棒状坡缕石粉末100g和聚季铵盐1g混合,加入去离子水500g,混合均匀后,再加入2500g去离子水,用超声波处理器处理2小时。另在3g氧化石墨烯中加入100g去离子水,超声处理2小时,将所得的悬浮液缓慢加入到前述所调制的坡缕石改性水悬液中,进行搅拌同时超声处理1小时,随后加入40g锐钛型纳米TiO2、3g硝酸银,混合均匀,过滤多余的去离子水,调制成含水60%的浆料。把配制好的浆料用高能行星球磨机在300转/分钟的速率高速研磨12小时。把经过研磨的粉体料浆在100℃下烘干,脱去料浆中的水分。在温度600℃焙烧4小时,使纳米TiO2和Ag离子负载在坡缕石上。在高能行星球磨机上研磨至粒度≤5μm,然后分级,检验,包装,即得到高效复合无机抗菌剂。
实施例2
把纯度为96%的绒状坡缕石粉末100g和聚季铵盐1g混合,加入去离子水500g,混合均匀后,再加入2000g去离子水,用超声波处理器处理2.5小时。另在3g氧化石墨烯中加入100g去离子水,超声处理2.5小时,将所得的悬浮液缓慢加入到前述所调制的坡缕石改性水悬液中,进行搅拌同时超声处理1小时,随后加入37g锐钛型纳米TiO2、4g金属氧化物ZnO,混合均匀,过滤多余的去离子水,调制成含水50%的浆料。把配制好的浆料用高能行星球磨机在350转/分钟的速率高速研磨12小时。把经过研磨的粉体料浆在150℃下烘干,脱去料浆中的水分。在温度600℃焙烧4小时,使纳米TiO2和ZnO负载在坡缕石上。在高能行星球磨机上研磨至粒度≤5μm,然后分级,检验,包装,即得到高效复合无机抗菌剂。
实施例3
把纯度为96%的纤维状坡缕石粉末100g和聚季铵盐1g混合,加入去离子水500g,混合均匀后,再加入3000g去离子水,用超声波处理器处理3小时。另在3g氧化石墨烯中加入100g去离子水,超声处理2.5小时,将所得的悬浮液缓慢加入到前述所调制的坡缕石改性水悬液中,进行搅拌同时超声处理1小时,随后加入35g锐钛型纳米TiO2、6g硝酸银,混合均匀,过滤多余的去离子水,调制成含水70%的浆料。把配制好的浆料用高能行星球磨机在400转/分钟的速率高速研磨15小时。把经过研磨的粉体料浆在120℃下烘干,脱去料浆中的水分。在温度500℃焙烧4小时,使纳米TiO2和Ag离子负载在坡缕石上。在高能行星球磨机上研磨至粒度≤5μm,然后分级,检验,包装,即得到高效复合无机抗菌剂。
实施例4
把纯度为96%的土状坡缕石粉末100g和聚季铵盐1g混合,加入去离子水500g,混合均匀后,再加入3500g去离子水,用超声波处理器处理2.5小时。另在4g氧化石墨烯中加入100g去离子水,超声处理2.5小时,将所得的悬浮液缓慢加入到前述所调制的坡缕石改性水悬液中,进行搅拌同时超声处理1小时,随后加入38g纳米ZnO(作为光催化材料),4g硝酸铁,混合均匀,过滤多余的去离子水,调制成含水55%的浆料。把配制好的浆料用高能行星球磨机在450转/分钟的速率高速研磨15小时。把经过研磨的粉体料浆在140℃下烘干,脱去料浆中的水分。在温度600℃焙烧5小时,使纳米ZnO和Fe离子负载在坡缕石上。在高能行星球磨机上研磨至粒度≤5μm,然后分级,检验,包装,即得到高效复合无机抗菌剂。
实施例5
把纯度为97%的纤维状坡缕石粉末100g和聚季铵盐1.5g混合,加入去离子水500g,混合均匀后,再加入3000g去离子水,用超声波处理器处理3小时。另在4g氧化石墨烯中加入100g去离子水,超声处理3小时,将所得的悬浮液缓慢加入到前述所调制的坡缕石改性水悬液中,进行搅拌同时超声处理1小时,随后加入35.5g锐钛型纳米TiO2、3g金属氧化物ZnO、3g硝酸银,混合均匀,过滤多余的去离子水,调制成含水60%的浆料。把配制好的浆料用高能行星球磨机在500转/分钟的速率高速研磨18小时。把经过研磨的粉体料浆在180℃下烘干,脱去料浆中的水分。在温度550℃焙烧4小时,使纳米TiO2、ZnO和Ag离子负载在坡缕石上。在高能行星球磨机上研磨至粒度≤5μm,然后分级,检验,包装,即得到高效复合无机抗菌剂。
实施例6
把纯度为97%的针棒状坡缕石粉末100g和聚季铵盐1.3g混合,加入去离子水500g,混合均匀后,再加入2200g去离子水,用超声波处理器处理2.5小时。另在3.6g氧化石墨烯中加入100g去离子水,超声处理3小时,将所得的悬浮液缓慢加入到前述所调制的坡缕石改性水悬液中,进行搅拌同时超声处理1.5小时,随后加入37.5g纳米SnO2、4g金属氧化物Al2O3、3g磷酸铁,混合均匀,过滤多余的去离子水,调制成含水60%的浆料。把配制好的浆料用高能行星球磨机在350转/分钟的速率高速研磨18小时。把经过研磨的粉体料浆在180℃下烘干,脱去料浆中的水分。在温度500℃焙烧4小时,使纳米SnO2、Al2O3和Fe离子负载在坡缕石上。在高能行星球磨机上研磨至粒度≤5μm,然后分级,检验,包装,即得到高效复合无机抗菌剂。
实施例7
把纯度为98%的绒状坡缕石粉末100g和聚季铵盐1.2g混合,加入去离子水500g,混合均匀后,再加入2400g去离子水,用超声波处理器处理3小时。另在4.5g氧化石墨烯中加入100g去离子水,超声处理3小时,将所得的悬浮液缓慢加入到前述所调制的坡缕石改性水悬液中,进行搅拌同时超声处理1.5小时,随后加入36.5g纳米CdO、3g金属氧化物ZnO、2.5g硫酸铜,混合均匀,过滤多余的去离子水,调制成含水60%的浆料。把配制好的浆料用高能行星球磨机在350转/分钟的速率高速研磨18小时。把经过研磨的粉体料浆在180℃下烘干,脱去料浆中的水分。在温度550℃焙烧4小时,使纳米CdO、ZnO和Cu离子负载在坡缕石上。在高能行星球磨机上研磨至粒度≤5μm,然后分级,检验,包装,即得到高效复合无机抗菌剂。
抗菌性能检测:
将已灭菌的琼脂培养基倒入培养皿中,制成平板,然后取混合菌液1mL于平板上,用刮刀涂布均匀。把抑菌材料制成片剂(直径10mm,厚度5mm),置于平板中央(每种材料分别做出3个试样,放到不同的培养皿中),再将培养皿置于37℃的恒温培养箱中,24h后测定试样周围抑菌环的大小,以抑菌环直径的平均值作为评价材料抗菌性能的依据。
实施例1-7制备无机抗菌剂的性能检测结果
实施例 | 1 | 2 | 3 | 4 | 5 | 6 | 7 |
抑菌环大小(mm) | 13.87 | 14.21 | 15.17 | 11.88 | 12.30 | 10.01 | 10.55 |
从上表可以看出:本发明制备的抗菌剂的抗菌效果较好,其中实施例3制备的复合无机抗菌的抗菌性能最佳。
以上内容仅仅是对本发明的构思所作的举例和说明,所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,只要不偏离发明的构思或者超越本权利要求书所定义的范围,均应属于本发明的保护范围。
Claims (9)
1.一种高效复合无机抗菌剂,其特征在于,按重量份组成为:坡缕石100份,光催化材料30~50份,石墨烯3~5份,金属氧化物和/或金属盐2~8份,聚季铵盐0.5~2份。
2.如权利要求1所述的高效复合无机抗菌剂,其特征在于,所述坡缕石为2:1型层链状结构的针棒状坡缕石、纤维状坡缕石、绒状坡缕石、土状坡缕石。
3.如权利要求2所述的高效复合无机抗菌剂,其特征在于,所述坡缕石为95~100%纯度的纤维状坡缕石。
4.如权利要求1所述的高效复合无机抗菌剂,其特征在于,所述光催化材料为纳米TiO2、纳米ZnO、纳米CdO、纳米SnO2。
5.如权利要求1所述的高效复合无机抗菌剂,其特征在于,所述石墨烯为1~4层的少片层氧化石墨烯。
6.如权利要求1所述的高效复合无机抗菌剂,其特征在于,所述金属氧化物为MgO,ZnO,CaO,Al2O3。
7.如权利要求1所述的高效复合无机抗菌剂,其特征在于,所述金属盐的金属离子为:Ag,Co,Fe,Sn,Al,Zn,Cu,Ni,金属盐是这些金属离子的硝酸盐、硫酸盐、磷酸盐、碳酸盐或有机酸盐。
8.如权利要求7所述的高效复合无机抗菌剂,其特征在于,所述金属盐为AgNO3。
9.制备如权利要求1~8任一项所述高效复合无机抗菌剂的方法,其特征在于,包括如下步骤:
1)改性:将坡缕石和聚季铵盐按配比进行混合;
2)制备坡缕石水悬浮液:将坡缕石-聚季铵盐混合粉体加入到去离子水中,按重量比为1:20~40配成水悬浮液,并采用超声处理2~4小时;
3)制备石墨烯水悬浮液:将石墨烯粉体加入到去离子水中,按重量比为1:10~50配成水悬浮液,并采用超声处理2~4小时;
4)制浆:将所得到的坡缕石水悬浮液和石墨烯水悬浮液进行混合,并进行搅拌0.5~2小时;加入光催化材料、金属氧化物和/或金属盐混合均匀,过滤后将其调制成含水50~70%的浆料;
5)湿研磨:把配制好的浆料在高能行星球磨机中,在300~500转/分钟的速率下高速研磨12~48小时;
6)烘干:把经过研磨的粉体料浆在100~200℃烘干,脱去料浆中的水分;
7)焙烧:将烘干后的产物在温度400~700℃下焙烧2~5小时;
8)干研磨:将焙烧后产物在高能行星球磨机上研磨至粒度≤5μm;
9)包装:将最后产物分级、包装,即得到高效复合无机抗菌剂。
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