CN111359642B - 一种半导体广谱杀菌抗病毒复合材料和制备方法和制备方法 - Google Patents
一种半导体广谱杀菌抗病毒复合材料和制备方法和制备方法 Download PDFInfo
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- CN111359642B CN111359642B CN202010189265.6A CN202010189265A CN111359642B CN 111359642 B CN111359642 B CN 111359642B CN 202010189265 A CN202010189265 A CN 202010189265A CN 111359642 B CN111359642 B CN 111359642B
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- semiconductor
- titanium dioxide
- composite material
- black titanium
- antiviral
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Abstract
本发明涉及一种半导体广谱杀菌抗病毒复合材料和制备方法。所述材料是具有能抑制杀灭新冠病毒等病原体的纳米黑色二氧化钛半导体材料和所锚定的多种增效活性物质。所述纳米黑色二氧化钛材料是全光谱响应半导体,能通过光热驱动催化、集热升温杀灭病原体。具体增效活性物质包括:进行“冷火”催化杀灭病原体的寡量金属、可和黑色二氧化钛协同常温催化杀灭病原体的纳米p型半导体、可高效抑制杀灭细菌病毒等病原体的金属离子。因此本发明材料可以通过多种机制协同高效杀灭病菌病毒。这种复合材料适合负载在滤层材料上,工艺简单、价格低廉、无毒副作用,具有高效的广谱杀菌抗病毒功能,可用于抗疫防护。
Description
技术领域
本发明涉及一种半导体广谱杀菌抗病毒复合材料和制备方法,属于日常及医用护理材料领域。
背景技术
近年来,世界范围内不断爆发大规模呼吸道传染疫情,面对传染性极强的病毒和细菌,医护人员和普通居民承担着巨大的感染风险。目前市面上大多数卫生防护用品,如口罩、护目镜、防护服等,都是靠隔离病原体的方式进行防护,没有杀灭病毒细菌的功能。这样的防护用品防护时间和防护能力较为有限,应急时期消耗量巨大,废弃后还会造成二次污染。因此,具备广谱杀菌抗病毒功能的防护材料极为重要。
半导体催化剂由于能实现光催化分解有机物在杀菌抗病毒材料领域有广阔的应用前景。二氧化钛 (TiO2)由于稳定性好、无毒、催化活性好、稳定性强成为其中的代表。但是在实际应用中,普通白色二氧化钛暴露出许多问题,可吸收波长范围窄(紫外光),光转化效率低,因此在商业化应用方面有一定限制,如专利CN108328694A仅能在紫外光中杀菌消毒,必须依靠紫外灯照射才能使用。
一些金属及金属离子虽然也有一定的杀菌、抗病毒潜力,但通常金属用量较大,容易引起潜在健康风险,部分细菌病毒对单一杀灭途径有抗性,其经济成本、杀灭效果、安全性能需要进一步优化。而提升半导体杀菌抗病毒材料性能的关键技术路线在于提升半导体催化剂的光利用率以及能够协同利用多种杀菌机制杀灭细菌病毒。
发明内容
基于上述问题,本发明借助材料学的先进研究成果,利用全光谱响应的纳米黑色二氧化钛通过光热驱动催化反应和集热升温,并锚定多种增效活性物质杀灭新冠病毒等病原体。其中具体增效活性物质包括:基于低温等离子体的常温催化氧化反应(“冷火”催化)能杀灭病原体的寡量金属,与黑色二氧化钛能级匹配并能协同常温催化杀灭病原体的纳米p型半导体,可高效抑制杀灭细菌病毒等病原体的金属离子。本发明材料可以通过协同多种杀菌灭毒机制,实现长效高效广谱抗菌灭毒功能。
本发明中应用的黑色二氧化钛是一种新型全光谱响应材料,克服了传统白色二氧化钛吸收波长范围窄(仅紫外光波段),光转化效率低等缺点,能够非常高效地利用太阳能实现杀菌灭毒功能。普通白色二氧化钛导带和价带之间的禁带宽度过宽,其几种主要晶相带宽都在3.0-3.2eV之间,故只能吸收仅占5%太阳能的紫外光,无法利用可见光和近红外光。而黑色二氧化钛由于引入Ti3+和氧缺陷能够调节材料带隙,存在价带的提升并会形成尾带,同时还会存在大量的中间带(如图4所示)。因此,黑色二氧化钛会发生两种类型的电子激发:一种是电子从价带到导带的激发,另一种是电子从价带到中间带或从中间带到导带的激发,故黑色二氧化钛具有良好的可见光和红外吸收性能,具有比传统二氧化钛更高能量利用率,更好的催化性能。
本发明中的纳米黑色二氧化钛同时是优异的杀菌抗病毒材料和负载材料,其具体作用如下:(1) 纳米黑色二氧化钛本身具有光或热驱动催化氧化降解有机物的作用。(2)该材料也是全光谱响应的高效吸热材料,通过光或热辐射实现温度快速升高,温杀或致残病原体,实现热杀菌。(3)黑色二氧化钛作为高导电载体与氢和氧电位匹配,负载与黑色二氧化钛能级匹配的纳米p型半导体后能协同进行常温催化氧化降解有机物。(4)同时它也是贵金属的优异复载体,能够形成高分散性的寡聚金属原子/氧化物界面,并能通过黑色二氧化钛协调金属原子叠加的局域表面等离子体激元共振效应,提高催化能力,实现“冷火”常温催化分解有机物。(5)其无定型非晶层作为金属离子的载体,可以有效保存金属离子,高效杀灭细菌和病菌等病原体。因此,这种半导体广谱杀菌抗病毒复合材料可以通过多种机制协同杀灭病原体,这样可以避免病单一杀菌抗病毒途径的局限性,可实现长效、高效、广谱、安全的杀菌抗病毒功能。
一方面,本发明提供了一种半导体高效杀菌抗病毒复合材料,其特征在于,具有能抑制杀灭新冠病毒等病原体的纳米黑色二氧化钛半导体以及所锚定的多种增效活性物质,具体增效活性物质包括:基于低温等离子体的常温催化氧化反应(“冷火”催化)能杀灭病原体的寡量金属,包括锰、银、铜、铂、钯、金、铑、钌等;与黑色二氧化钛能级匹配并能协同常温催化杀灭病原体的纳米p型半导体,包括纳米氧化镍、纳米氧化钌、硼掺杂石墨烯等;可高效抑制杀灭细菌病毒等病原体的金属离子,包括银、铜、锌等离子。
所述的纳米黑色二氧化钛,可以光或热驱动催化灭菌灭毒,并高效吸热实现热杀菌灭毒。也可以用含铌、钽、钨、锆、钼等过渡金属的高价态氧化物或含氧酸替代。具体使用中,纳米黑色二氧化钛中可以负载单一增效活性物质,或者同时负载多种增效活性物质,也可以单独使用纳米黑色二氧化钛及其替代物用于杀菌抗病毒。
较佳的,所述纳米黑色二氧化钛具有壳核结构,以二氧化钛为核,缺陷态为壳。较佳的,二氧化钛内核粒径为10-30nm,二氧化钛外壳厚度为1-10nm。
较佳的,所述的寡量金属是指锰、银、铜、铂、钯、金、铑、钌的一种或组合。其中优选锰,银,金。较佳的,原子聚集数为1-1000,尺寸为0.1m-100nm,其中优选原子聚集数为5-10,尺寸为0.3-5nm。
较佳的,所述的纳米p型半导体,包括镍、钌的氧化物,纳米氧化亚铜,硼掺杂石墨烯的一种或组合,其中优选硼掺杂石墨烯。
较佳的,所述的金属离子包括钾、钠、锰、铁、铜、铋、铝、锌、银、镁、钙、稀土离子的一种或组合,其中优选银,锌,钠离子。
所述的半导体高效杀菌抗病毒复合材料,适合负载在滤层材料上,具有抑制或灭杀细菌和病毒的效果,所述滤层材料包含高分子、碳、无机氧化物等材料组成的多孔层状材料,其中优选无纺布或熔喷布、植物纤维织物、石墨烯或者碳管布、氧化物纤维布。
另一方面,本发明还提供一种半导体高效杀菌抗病毒复合材料的制备方法,其特征在于,将前驱体溶液加入到黑色二氧化钛溶液中,通过物理、化学方法一次处理后获得负载有多种增效活性物质物质的黑色二氧化钛材料。
所述物理、化学方法处理包括超声、洗涤、过滤、干燥、水热反应、还原性气体中焙烧、真空焙烧、化学还原等方法。其中优选将各种前驱体溶液加入到黑色二氧化钛溶液中,通过一次水热法,过滤,干燥后获得负载有多种增效活性物质的半导体广谱杀菌抗病毒复合材料。
所述黑色二氧化钛溶液的溶剂选自乙醇、水、异丙醇中的一种或组合,优选为水。所述前驱体溶液包括寡量金属原子的前驱体溶液,纳米半导体的前驱体溶液和金属离子溶液的一种或组合。
又一方面,本发明还提供一种半导体高效杀菌抗病毒复合材料的制备方法,其特征在于,将不同类型的增效活性物质根据上述制备方法,按照一定次序重复多次,获得负载有多种增效活性物质的半导体广谱杀菌抗病毒复合材料。
再者,本发明还提供了半导体高效杀菌抗病毒复合材料的用途,包括制作口罩滤层、防护服、空气净化滤层、喷雾剂、消毒剂、表面防护涂层。
本发明提供了一种半导体广谱杀菌抗病毒复合材料和制备方法。通过纳米黑色二氧化钛负载寡量金属原子,纳米半导体颗粒、金属离子等增效活性物质,协同光热驱动催化灭菌、集热杀菌、“冷火”催化灭菌、复合金属离子灭菌等多种途径实现广谱杀菌抗病毒功能。本发明具有工艺简单、重金属用量小、价格低廉、无毒副作用、能够高效杀菌抗病毒等优势。其应用范围灵活,负载于滤层材料时,可作为市面上非抗病毒口罩、一次性口罩的增效部件,延长口罩使用寿命、增加抗病毒功能;又可以集成于口罩中;还可以直接用于防护服、空气净化滤层、喷雾剂、消毒液、表面防护涂层的制备。可用于医用和民用领域对细菌和病毒的抗疫防护。
附图说明
图1为纳米黑色二氧化钛实物图和电子显微图片。
图2为实施例7中喷涂法制备无纺布负载的半导体广谱杀菌抗病毒复合材料实物图。
图3为实施例11所制备的半导体广谱杀菌抗病毒口罩的实物图。
图4为普通二氧化钛和黑色二氧化钛的能带结构示意图和态密度示意图。
具体实施方式
以下通过下述实施方式进一步说明本发明,应理解,下述实施方式仅用于说明本发明,而非限制本发明。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
以下示例性地说明本发明提供的半导体广谱杀菌抗病毒复合材料的制备方法和负载方式。作为一个半导体广谱杀菌抗病毒复合材料制备方法的示例,该方法主要特征是通过一次水热法在纳米黑色二氧化钛同时负载多种增效活性物质。其具体方法步骤如下:将(1)通过高温还原法制备纳米黑色二氧化钛材料。(2)将金属前驱体溶液、稳定剂、氧化石墨烯,硼氢化钠、纳米黑色二氧化钛在120℃下进行水热反应2小时,过滤、洗涤、干燥后得到负载硼掺杂石墨烯和寡量金属离子的纳米黑色二氧化钛。(3)将(2) 中所得产物放入含有复合金属离子的溶液中浸润得到半导体广谱杀菌抗病毒复合材料分散液。(4)将半导体广谱杀菌抗病毒复合材料分散液喷涂到滤层材料上烘干,完成材料在滤层上的负载。
另外一种制备方法的主要特征是,通过多步物理化学方法,依次负载多种增效活性物质,其具体方法步骤如下:(1)通过高温还原法制备纳米黑色二氧化钛材料。(2)将氧化石墨烯,硼氢化钠和(1) 中制备好的纳米黑色二氧化钛材料在120℃下进行水热反应2小时,得到负载硼掺杂石墨烯的纳米黑色二氧化钛。(3)然后将金属前驱体溶液、稳定剂、还原剂滴加到(2)中所制备的材料,原位完成寡量金属离子负载,洗涤、干燥、过滤后获得,负载硼掺杂石墨烯和寡聚金属离子的纳米黑色二氧化钛。(4)将(3) 中所得产物放入含有复合金属离子的溶液中浸润得到半导体广谱杀菌抗病毒复合材料分散液。(5)将半导体广谱杀菌抗病毒复合材料分散液喷涂到滤层材料上烘干,完成材料在滤层上的负载。
下面进一步举例以详细说明本发明。同样应理解,下述实施方式只用于对本发明进行进一步说明,不能理解为对本发明的限制,本领域技术人员在对本发明做出的非本质的改动和调整都属于本发明保护的范围。下述事例的具体工艺参数等仅是合适范围中的一个示例,即本领域技术人员可以通过文本的说明做合适范围内的选择,而并非要限定于下文示例的具体数值。
所述半导体广谱杀菌抗病毒复合材料抗病毒性能测试是以2014年ISO·18184所规定的抗病毒测试方法进行测试,判断病毒抑制能力以抗病毒活性值作为依据,抗病毒活性值为2.0以上说明病毒减少到百分之一以下的效果。
所述半导体广谱杀菌抗病毒复合材料抗菌性能测试按照GB15979-2002《一次性使用卫生标准》附录C所述方法进行抗菌性能测试,以金黄色葡萄球菌作为测试菌种计算抗菌率。
实施例1纳米黑色二氧化钛的制备
将铝粉与商品化的P25二氧化钛粉末在500摄氏度真空炉中烧结2h,用盐酸、去离子水反复洗涤,干燥后得到黑色二氧化钛。
实施例2负载寡量金属原子的纳米黑色二氧化钛的制备
将0.1M氨水溶液加入10mM硝酸银溶液中,超声5分钟后加入实施例1中的纳米黑色二氧化钛粉末,再加入10mL葡萄糖溶液,超声,过滤后用去离子水清洗,真空干燥后得到负载寡量银的纳米黑色二氧化钛。
实施例3负载纳米半导体的纳米黑色二氧化钛的制备
将氧化石墨烯石墨烯,硼酸氢钠和纳米黑色二氧化钛一起进行在120℃下进行水热反应8h,将所得产物氩气保护500℃下处理2h,得复载硼掺杂石墨烯的纳米黑色二氧化钛材料。
实施例4负载金属离子的纳米黑色二氧化钛的制备
在0.5M氯化铜,磷酸银,氯化锌水溶液中加入实施例1中的纳米黑色二氧化钛,过滤,干燥后获得负载金属离子的纳米黑色二氧化钛的制备。
实施例5负载寡量金属原子和金属离子的纳米黑色二氧化钛的制备
在0.5M氯化铜,磷酸银,氯化锌水溶液中加入实施例2中的负载寡量银的纳米黑色二氧化钛,过滤,干燥后获得负载寡量金属原子和金属离子的纳米黑色二氧化钛。
实施例6负载纳米半导体、寡量金属原子和金属离子的半导体广谱杀菌抗病毒复合材料和分散液制备
将1mL 10mM硝酸银溶液、1g实施例1中的纳米黑色二氧化钛,1g氧化石墨烯,0.1g硼酸氢钠放入反应釜进行水热反应120℃,2小时。过滤,洗涤真空干燥后再加入到100mL0.5M氯化铜,磷酸银,氯化锌水溶液中,得到半导体广谱杀菌抗病毒复合材料分散液。过滤,干燥后得到半导体广谱杀菌抗病毒复合材料。
实施例7无纺布负载的半导体广谱杀菌抗病毒复合材料的制备
将实施例6中半导体广谱杀菌抗病毒复合材料分散液通过连续喷涂到亲水无纺布上,烘干,裁剪后装入已消毒塑料袋密封,得到无纺布负载的半导体广谱杀菌抗病毒复合材料。测试无纺布负载的半导体广谱杀菌抗病毒复合材料的抗病毒性能和抗菌性能。所得抗病毒活性值为3.2,抗菌率99.7%。
实施例8石墨烯布负载的半导体广谱杀菌抗病毒复合材料的制备
将石墨烯分散液通过连续喷涂到亲水无纺布上,烘干,得到石墨烯无纺布。再将实施例6中半导体广谱杀菌抗病毒复合材料分散液连续喷涂到石墨烯无纺布上,烘干,裁剪后装入已消毒塑料袋密封,得到石墨烯无纺布负载的半导体广谱杀菌抗病毒复合材料。测试石墨烯无纺布负载的半导体广谱杀菌抗病毒复合材料的抗病毒性能和抗菌性能。所得抗病毒活性值为3.4,抗菌率99.8%。
实施例9植物纤维负载的半导体广谱杀菌抗病毒复合材料的制备
将实施例6中半导体广谱杀菌抗病毒复合材料分散液通过连续喷涂到棉纺布上,烘干,裁剪后装入已消毒塑料袋密封,得到棉纺布负载的半导体广谱杀菌抗病毒复合材料。测试棉纺布负载的半导体广谱杀菌抗病毒复合材料的抗病毒性能和抗菌性能。所得抗病毒活性值为2.8,抗菌率95.5%。
实施例10半导体广谱杀菌抗病毒复合材料防护层的制备
将实施例6中的半导体广谱杀菌抗病毒复合材料分散液喷涂到聚乙烯透气膜上,烘干后即可以得到半导体广谱杀菌抗病毒复合材料防护层,并可用于医用防护服的外层杀菌抗病毒防护层。
实施例11半导体广谱杀菌抗病毒复合材料口罩的制备
将实施例7中的无纺布负载的半导体广谱杀菌抗病毒复合材料作为口罩夹层,再结合无纺布、静电滤棉和熔喷布,即可以制备半导体广谱杀菌抗病毒复合材料口罩。
Claims (12)
1.一种半导体杀菌抗病毒复合材料,其特征在于,具有纳米黑色二氧化钛半导体以及所锚定的多种增效活性物质,具体增效活性物质包括:
a. 基于低温等离子体的常温催化氧化反应能杀灭病原体的寡量金属,包括锰、银、铜、铂、钯、金、铑和钌中的一种或组合;
b. 与含铌、钽、钨、锆、钼中一种或几种过渡金属的氧化物或其含氧酸、黑色二氧化钛能级匹配并能协同常温催化杀灭病原体的纳米p型半导体,包括纳米氧化镍、纳米氧化钌和硼掺杂石墨烯中的一种或组合;
c. 能抑制杀灭细菌病毒的金属离子,包括钾、钠、锰、铁、铜、铋、铝、锌、银、镁、钙和稀土离子的一种或组合。
2.根据权利要求1所述的半导体杀菌抗病毒复合材料,其特征在于,所述纳米黑色二氧化钛半导体材料具有壳核结构,以二氧化钛为核,缺陷态为壳;二氧化钛内核粒径为10-30nm,二氧化钛外壳厚度为1-10 nm。
3.根据权利要求1所述的半导体杀菌抗病毒复合材料,其特征在于,所述寡量金属的原子聚集数为1-1000,尺寸为0.1 nm-100 nm。
4.根据权利要求1所述的半导体杀菌抗病毒复合材料,其特征在于,所述半导体杀菌抗病毒复合材料适合负载在滤层材料上,具有抑制或灭杀细菌和病毒的效果,所述滤层材料包含由高分子、碳、或无机氧化物组成的多孔层状材料。
5.根据权利要求4所述的半导体杀菌抗病毒复合材料,其特征在于,所述滤层材料为无纺布或熔喷布、聚合物织物、植物纤维织物、石墨烯或者碳管布、氧化物纤维布。
6.根据权利要求1-5的任一项所述的半导体杀菌抗病毒复合材料的制备方法,其特征在于,将各种前驱体溶液加入到黑色二氧化钛溶液中,通过物理、化学方法一次处理后获得负载有多种增效活性物质的黑色二氧化钛材料。
7.根据权利要求6所述的制备方法,其特征在于,所述物理、化学方法处理包括超声、洗涤、过滤、干燥、水热反应、还原性气体中焙烧、真空焙烧、化学还原。
8.根据权利要求7所述的制备方法,其特征在于,通过一次水热反应和干燥后完成制备材料。
9.根据权利要求6所述的制备方法,其特征在于,所述黑色二氧化钛溶液的溶剂选自乙醇、水、异丙醇中的一种或组合。
10.根据权利要求6所述的制备方法,其特征在于,所述前驱体溶液包括寡量金属原子的前驱体溶液以及所需的还原剂、稳定剂,纳米半导体的前驱体溶液和金属离子溶液。
11.根据权利要求1-5的任一项所述的半导体杀菌抗病毒复合材料的制备方法,其特征在于,将不同类型的增效活性物质依次按照权利要求6或7所述的制备方法,按照一定次序重复多次进行负载,获得负载有多种增效活性物质的广谱杀菌抗病毒材料。
12.一种权利要求1-5中任一项所述的半导体杀菌抗病毒复合材料的用途,其特征在于,包括制作口罩滤层、防护服、空气净化滤层、喷雾剂、消毒剂、表面防护涂层。
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