CN113856757A - 一种聚多巴胺修饰氮化碳/二氧化钛负载泡沫镍复合光催化剂及其制备方法和应用 - Google Patents
一种聚多巴胺修饰氮化碳/二氧化钛负载泡沫镍复合光催化剂及其制备方法和应用 Download PDFInfo
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Abstract
本发明属于过滤光催化材料技术领域,公开了一种聚多巴胺修饰氮化碳/二氧化钛负载泡沫镍复合光催化剂及其制备方法和应用。该复合光催化剂通过两步法制得,先将商业泡沫镍置于有机溶剂中浸泡、超声,洗净干燥后,在80~120℃真空干燥,制得泡沫镍载体;然后将洁净的泡沫镍载体浸泡在多巴胺盐酸盐溶液中反应制得聚多巴胺修饰泡沫镍;另将洁净的泡沫镍置于g‑C3N4/TiO2分散液中通过电泳法将g‑C3N4/TiO2负载在泡沫镍表面得到g‑C3N4/TiO2负载泡沫镍;最后通过粘附剂将聚多巴胺修饰的泡沫镍与g‑C3N4/TiO2负载的泡沫镍进行有机复合。本发明以大孔径泡沫镍为基底,结合修饰的聚多巴胺和g‑C3N4/TiO2对生物气溶胶有粘附亲和力和光催化杀灭效果,不仅能高气流量和长时间捕获高浓度的生物气溶胶,同时能在光照情况下将捕获的生物气溶胶原位杀灭,避免其二次污染。
Description
技术领域
本发明属于过滤光催化材料技术领域,特别涉及一种聚多巴胺修饰氮化碳/二氧化钛(g-C3N4/TiO2)负载泡沫镍复合光催化剂及其制备方法和应用。
背景技术
生物气溶胶(含有生物性粒子的气溶胶)携带病原微生物可以在空气中长期持留并进行远距离传播,给空气造成了严重污染并可能引发呼吸道传染病的大规模传播。大多数报道的生物气溶胶捕获方法依赖于多孔材料的小尺寸孔径将微生物过滤在材料表面,而过滤材料上累积的微生物可能会在气流扰动下二次悬浮,造成污染;此外,多孔材料孔径小、堆积密集,因此压降大,易堵塞,使用寿命短。因此,研制一种不依赖于小孔径阻留生物气溶胶中的微生物并能原位将其杀灭,避免二次污染的材料成为亟待解决的问题。目前,由于光催化氧化技术环境友好、高效、无污染、无需外加设备、相容性好并且有优异的氧化性等优点,在光照条件下能产生自由基杀灭微生物,因而在生物气溶胶的捕获与原位杀灭方面存在潜在应用。
贻贝类分泌的多巴胺分子具有强粘附作用,因而他们可以粘附在船舶、礁石等的表面不被水流冲走。通过分子间和分子内的自聚合,多巴胺几乎可在任何材料表面形成聚多巴胺膜(PDA)。PDA膜表面有多种活性基团,对生物分子具有亲和性,如儿茶酚基、酚羟基、氨基、醛基等可以与生物分子形成氢键、化学键及静电吸引等,对生物气溶胶具有较强的粘附力。然而仅通过化学粘附捕获生物气溶胶中的微生物仍不能完全避免污染,因此还需结合光催化原位杀灭,从根本上解决微生物的二次污染问题。
发明内容
为了解决上述现有技术中存在的缺点和不足之处,本发明的首要目的在于提供一种聚多巴胺修饰氮化碳/二氧化钛(g-C3N4/TiO2)负载泡沫镍复合光催化剂的制备方法;该方法以商业的泡沫镍为多孔基底,将聚多巴胺和g-C3N4/TiO2分别修饰与负载于泡沫镍表面,并将二者通过黏合剂复合制备生物气溶胶捕获杀灭材料。
本发明的另一目的在于提供上述制备方法制备得到的聚多巴胺修饰氮化碳/二氧化钛(g-C3N4/TiO2)负载泡沫镍复合光催化剂。
本发明的再一目的在于提供上述聚多巴胺修饰氮化碳/二氧化钛(g-C3N4/TiO2)负载泡沫镍复合光催化剂在生物气溶胶捕获与杀灭领域中的应用。
本发明的目的通过下述技术方案实现:
一种聚多巴胺修饰氮化碳/二氧化钛负载泡沫镍复合光催化剂的制备方法,包括如下步骤:
(1)首先将1~5mm厚的商业泡沫镍置于有机溶剂中浸泡超声,然后用去离子水清洗干净,经真空干燥获得表面洁净的泡沫镍;
(2)将0.01~10g多巴胺盐酸盐加入到5~500mL去离子水中,在10~50℃下搅拌5~60min,得到澄清溶液a;
(3)将0.05~1g pH缓冲剂加入步骤(2)所得澄清溶液a,在10~50℃下搅拌5~60min,得到棕色透亮溶液b;
(4)将步骤(1)所得表面洁净的泡沫镍浸泡于50~500mL步骤(3)所得的棕色透亮溶液b中,在转速为100~5000转/min及10~50℃下反应2~72h,待反应完毕后,用去离子水清洗泡沫镍表面,在50~180℃下真空干燥1~36h,得到聚多巴胺修饰的泡沫镍;
(5)将0.05~5g的三聚氰胺与1g商业纳米TiO2超声分散于50~500mL的乙醇中,处理时间为0.5~2h,再在搅拌中以20~80℃蒸发除去乙醇,所得干燥混合物研磨成粉,干燥2h获得干燥粉末;
(6)将步骤(5)所得干燥粉末放置于陶瓷坩埚中,用锡箔纸包裹好后放入马弗炉中以2~20℃/min的升温速度升温至400~600℃,煅烧0.5~4h;
(7)称取步骤(6)煅烧后的粉末0.1~5g,超声分散于200mL去离子水中,采用酸调节pH值到2~9,得到分散液;
(8)另将步骤(1)所得表面洁净的泡沫镍和Ti片电极浸入步骤(7)所得分散液中,在泡沫镍与Ti片电极间施加50~300V的电压,泡沫镍与Ti片电极距离2~10cm,在100~5000转/min搅拌速度下,电泳1~10min,并用去离子水冲洗泡沫镍表面未附着的颗粒物,在50~180℃下真空干燥1~36h,即获得g-C3N4/TiO2负载的泡沫镍;
(9)将步骤(4)与步骤(8)分别获得的聚多巴胺修饰的泡沫镍和g-C3N4/TiO2负载的泡沫镍通过黏合剂粘接复合,或者采用物理压合,得到聚多巴胺修饰氮化碳/二氧化钛负载泡沫镍复合光催化剂。
优选地,步骤(1)所述有机溶剂为乙醇、丙酮、甲醇、N,N-二甲基甲酰胺、二氯甲烷和甲苯中的一种或两种。
优选地,步骤(3)所述pH缓冲剂为磷酸氢二钠、三羟甲基氨基甲烷、氢氧化钠、碳酸氢钠或四硼酸钠缓冲液。
优选地,步骤(7)所述酸为稀盐酸、稀硫酸、醋酸、磷酸或硅酸。
优选地,步骤(9)所述黏合剂为羧甲基纤维素或聚乙烯醇。
一种聚多巴胺修饰氮化碳/二氧化钛负载泡沫镍复合光催化剂,是由权利要求1~5中任一项所述的制备方法制备得到的。
上述的基于聚多巴胺修饰氮化碳/二氧化钛负载泡沫镍复合光催化剂在捕获与杀灭生物气溶胶领域的应用,所述应用按照以下步骤:采用抽气泵将生物气溶胶通过聚多巴胺修饰氮化碳/二氧化钛负载泡沫镍复合光催化剂,光照强度为10~1000mW/cm2,过滤时间为5~120min。
本发明的功能化修饰的泡沫镍复合材料以具有大孔径、高比表面积的泡沫镍为基底,通过分别表面修饰聚多巴胺和电泳沉积法快速负载g-C3N4/TiO2,制备出一种新型低压降、高流量原位杀灭生物气溶胶的过滤催化材料。该材料可以粘附捕获高流速、高浓度的生物气溶胶并在太阳光驱动下可高效杀灭生物气溶胶,并具有优异的稳定性。这是由于PDA修饰的泡沫镍表面具有丰富的官能团,对生物分子具有较好的粘附性;另外,g-C3N4/TiO2催化剂均匀负载在具有大孔的泡沫镍表面,既增强了对光的吸收和利用,又可以降低压降,提高生物气溶胶的传质;而且由于泡沫镍的导电性有利于光生电子的传输,减少电子-空穴的体相复合,可有效提高光生载流子的分离效率,进而提高复合光催化剂的光催化活性和稳定性。本发明可以在空气净化领域作为生物气溶胶的捕获与原位杀灭的过滤材料,具有广阔的环境保护应用潜力。
本发明和现有技术相比,具有如下优点和有益效果:
1.本发明克服传统滤材高压降、易堵塞且单一功能的不足,将聚多巴胺对生物气溶胶的粘附捕获作用与g-C3N4/TiO2催化剂的光催化杀灭作用相结合,制备出一种新型高效、低压降、高流量的捕获-光催化杀灭复合材料——功能化修饰泡沫镍。通过实验发现本发明制备出的复合材料对生物气溶胶具有良好的捕获与原位杀灭性能,以0.7m/s的面风速,在60分钟内对107CFU/m3大肠杆菌生物气溶胶过滤效率保持90%以上。
2.本发明克服传统滤材过滤生物气溶胶后无法杀灭生物气溶胶的不足,利用光催化剂在连续光照下,原位杀灭生物气溶胶。通过实验发现该复合材料在连续过滤时,杀灭效率高达50%,实现了生物气溶胶的捕获与原位光催化杀灭一体化,使得负载g-C3N4/TiO2催化剂表面在光照下产生的自由基在原位可以有效地杀灭PDA修饰泡沫镍捕获的微生物,避免了滤材堵塞及二次污染问题。
3.本发明以大孔径的泡沫镍作为基材,不依赖小尺寸的截留作用;制备的聚多巴胺修饰g-C3N4/TiO2负载泡沫镍复合光催化剂方法简单、快速。经过实验发现,本发明制备的复合材料在0.7m/s的面风速下压降仅为600Pa,因此具有流量大,不堵塞,节约能源,且可以高效去除高浓度的生物气溶胶的优点。
附图说明
图1是聚多巴胺修饰g-C3N4/TiO2负载泡沫镍复合光催化剂对生物气溶胶的过滤效率图。
图2是聚多巴胺修饰g-C3N4/TiO2负载泡沫镍复合光催化剂对生物气溶胶光催化杀灭效率图。
图3是聚多巴胺修饰泡沫镍SEM图。
图4是g-C3N4/TiO2负载泡沫镍SEM图。
具体实施方式
下面结合实施例及附图对本发明作进一步详细的描述,但本发明的实施方式不限于此。
实施例1
(1)首先将1.5mm厚的商业泡沫镍置于乙醇中浸泡超声,然后用去离子水清洗干净,经真空干燥获得表面洁净的泡沫镍(Ni);
(2)将0.1g多巴胺盐酸盐加入到100mL去离子水中,在25℃下搅拌5min,得到澄清溶液a;
(3)将0.5g三羟甲基氨基甲烷加入步骤(2)所得澄清溶液a,在25℃下搅拌5min,得到棕色透亮溶液b;
(4)将步骤(1)所得表面洁净的泡沫镍浸泡于100mL步骤(3)所得棕色透亮溶液b中,在转速为100转/min及25℃下反应24h,待反应完毕后,用去离子水清洗泡沫镍表面,在60℃下真空干燥12h,得到聚多巴胺修饰的泡沫镍(PDA-Ni);
(5)将0.3g的三聚氰胺与1g商业纳米TiO2超声分散于100mL的乙醇中,处理时间为1h,再在搅拌中以60℃蒸发除去乙醇,所得干燥混合物研磨成粉,干燥2h获得干燥粉末;
(6)将步骤(5)所得干燥粉末放置于陶瓷坩埚中,用锡箔纸包裹好后放入马弗炉中以10℃/min的升温速度,以550℃煅烧2h;
(7)称取步骤(6)煅烧后的粉末1g,超声分散于200mL去离子水中,采用醋酸调节pH值到5,得到分散液;
(8)另将(1)所得表面洁净的泡沫镍和Ti片电极浸入(7)所得的分散液中,在泡沫镍与Ti片电极间施加150V的电压,泡沫镍与Ti片电极距离3cm,在1000转/min搅拌速度下,电泳2min,并用去离子水冲洗泡沫镍表面未附着的颗粒物,在80℃下真空干燥12h,即获得g-C3N4/TiO2负载的泡沫镍(CT-Ni);
(9)将步骤(4)与步骤(8)分别所获得的聚多巴胺修饰的泡沫镍和g-C3N4/TiO2负载的泡沫镍通过物理机械压合边缘粘接复合,得到聚多巴胺修饰g-C3N4/TiO2负载泡沫镍复合光催化剂(PDA-CT-Ni)。
图1为聚多巴胺修饰g-C3N4/TiO2负载泡沫镍复合光催化剂(PDA-CT-Ni)、表面洁净的泡沫镍(Ni)、聚多巴胺修饰的泡沫镍(PDA-Ni)和g-C3N4/TiO2负载的泡沫镍(CT-Ni)对生物气溶胶的去除效率。由图可以看出,单层Ni和CT-Ni对生物气溶胶的去除效率较低,而经过PDA修饰后的PDA-Ni去除效率提高到70%,而通过将PDA-Ni与CT-Ni复合后,其生物气溶胶去除率高达93%。
图2为PDA-CT-Ni、Ni、PDA-Ni和CT-Ni表面的微生物存活率。从图2可以看出,经过光照后,CT-Ni表面的微生物几乎已经完全杀灭,而PDA-Ni表面的微生物也杀灭50%。
通过以上结果可以看出本发明制备的聚多巴胺修饰g-C3N4/TiO2负载泡沫镍复合光催化剂是一种结合大孔径粘附捕获与光催化原位杀灭的新型生物气溶胶过滤材料。
实施例2
(1)首先将1.5mm厚的商业泡沫镍置于乙醇中浸泡超声,然后用去离子水清洗干净,经真空干燥获得表面洁净的泡沫镍;
(2)将0.1g多巴胺盐酸盐加入到100mL去离子水中,在25℃下搅拌5min,得到澄清溶液a;
(3)将0.5g三羟甲基氨基甲烷加入步骤(2)所得澄清溶液a,在25℃下搅拌5min,得到棕色透亮溶液b;
(4)将步骤(1)所得表面洁净的泡沫镍浸泡于100mL步骤(3)所得的溶液b中,在转速为100转/min及25℃下反应24h,待反应完毕后,用去离子水清洗泡沫镍表面,在60℃下真空干燥12h,得到聚多巴胺修饰的泡沫镍;
(5)将0.5g的三聚氰胺与1g商业纳米TiO2超声分散于200mL的乙醇中,处理时间为2h,再在搅拌中以80℃蒸发除去乙醇,所得干燥混合物研磨成粉,干燥2h获得干燥粉末;
(6)将步骤(5)所得干燥粉末放置于陶瓷坩埚中,用锡箔纸包裹好后放入马弗炉中以20℃/min的升温速度,以500℃煅烧4h;
(7)称取步骤(6)煅烧所得粉末2g,超声分散于200mL去离子水中,采用醋酸调节pH值到4,得到分散液;
(8)另将(1)所得的表面洁净的泡沫镍和Ti片电极浸入(7)所得的分散液中,在泡沫镍与Ti片电极间施加100V的电压,泡沫镍与Ti片电极距离6cm,在3000转/min搅拌速度下,电泳4min,并用去离子水冲洗泡沫镍表面未附着的颗粒物,在80℃下真空干燥12h,即获得g-C3N4/TiO2负载的泡沫镍;
(9)将步骤(4)与步骤(8)分别所获得的聚多巴胺修饰的泡沫镍和g-C3N4/TiO2负载的泡沫镍通过聚乙烯醇黏合剂粘接复合,得到聚多巴胺修饰g-C3N4/TiO2负载泡沫镍复合光催化剂。
图3为步骤(4)所得聚多巴胺修饰的泡沫镍的扫描电镜图,可以看出泡沫镍表面形成了一层较为均匀的聚多巴胺颗粒物层。
图4为步骤(8)所得g-C3N4/TiO2负载的泡沫镍扫描电镜图,由于表面负载了致密的g-C3N4/TiO2颗粒层,因而泡沫镍表面的沟槽纹路被覆盖。从图中可以看出g-C3N4/TiO2颗粒均匀,完全覆盖泡沫镍表面,形成致密的镀层。
实施例3
(1)首先将3mm厚的商业泡沫镍置于丙酮中浸泡超声,然后用去离子水清洗干净,经真空干燥获得表面洁净的泡沫镍;
(2)将0.5g多巴胺盐酸盐加入到100mL去离子水中,在45℃下搅拌10min,得到澄清溶液a;
(3)将0.1g氢氧化钠加入步骤(2)所得澄清溶液a,在45℃下搅拌10min,得到棕色溶液b;
(4)将步骤(1)所得表面洁净的泡沫镍浸泡于100mL步骤(3)所得的溶液b中,在转速为50转/min及25℃下反应18h,待反应完毕后,用去离子水清洗泡沫镍表面,在60℃下真空干燥12h,得到聚多巴胺修饰的泡沫镍;
(5)将0.4g的三聚氰胺与1g商业纳米TiO2超声分散于200mL的乙醇中,处理时间为0.5h,再在搅拌中以80℃蒸发除去乙醇,所得干燥混合物研磨成粉,干燥2h获得干燥粉末;
(6)将步骤(5)所得干燥粉末放置于陶瓷坩埚中,用锡箔纸包裹好后放入马弗炉中以5℃/min的升温速度,以500℃煅烧2h;
(7)称取步骤(6)煅烧后的粉末1g,超声分散于200mL去离子水中,采用稀盐酸调节pH值到4;
(8)另将(1)所得表面洁净的泡沫镍和Ti片电极浸入(7)所得的分散液中,在泡沫镍与Ti片电极间施加200V的电压,泡沫镍与Ti片电极距离5cm,在2000转/min搅拌速度下,电泳3min,并用去离子水冲洗泡沫镍表面未附着的颗粒物,在80℃下真空干燥12h,即获得g-C3N4/TiO2负载的泡沫镍;
(9)将步骤(4)与步骤(8)分别所获得的聚多巴胺修饰泡沫镍和g-C3N4/TiO2负载泡沫镍通过物理压合粘接复合,得到聚多巴胺修饰g-C3N4/TiO2负载泡沫镍复合光催化剂。
实施例4
(1)首先将3mm厚的商业泡沫镍置于乙醇中浸泡超声,然后用去离子水清洗干净,经真空干燥获得表面洁净的泡沫镍;
(2)将1g多巴胺盐酸盐加入到500mL去离子水中,在40℃下搅拌5min,得到澄清溶液a;
(3)将1g三羟甲基氨基甲烷加入步骤(2)所得澄清溶液a,在40℃下搅拌5min,得到棕色透亮溶液b;
(4)将步骤(1)所得表面洁净的泡沫镍浸泡于200mL步骤(3)所得的溶液b中,在转速为1000转/min及25℃下反应12h,待反应完毕后,用去离子水清洗泡沫镍表面,在60℃下真空干燥12h,得到聚多巴胺修饰的泡沫镍;
(5)将0.3g的三聚氰胺与1g商业纳米TiO2超声分散于200mL的乙醇中,处理时间为2h,再在搅拌中以80℃蒸发除去乙醇,所得干燥混合物研磨成粉,干燥2h获得干燥粉末;
(6)将步骤(5)所得干燥粉末放置于陶瓷坩埚中,用锡箔纸包裹好后放入马弗炉中以20℃/min的升温速度,以550℃煅烧2h;
(7)称取步骤(6)煅烧后的粉末1g,超声分散于200mL去离子水中,采用醋酸调节pH值到5,得到分散液;
(8)另将(1)所得表面洁净的泡沫镍和Ti片电极浸入(7)所得的分散液中,在泡沫镍与Ti片电极间施加150V的电压,泡沫镍与Ti片电极距离10cm,在1000转/min搅拌速度下,电泳3min,并用去离子水冲洗泡沫镍表面未附着的颗粒物,在80℃下真空干燥12h,即获得g-C3N4/TiO2负载的泡沫镍;
(9)将步骤(4)与步骤(8)分别所获得的聚多巴胺修饰泡沫镍和g-C3N4/TiO2负载泡沫镍通过聚乙烯醇黏合剂粘接复合,得到聚多巴胺修饰g-C3N4/TiO2负载泡沫镍复合光催化剂。
上述实施例为本发明较佳的实施方式,但本发明的实施方式并不受上述实施例的限制,其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。
Claims (7)
1.一种聚多巴胺修饰氮化碳/二氧化钛负载泡沫镍复合光催化剂的制备方法,其特征在于包括如下步骤:
(1)首先将1~5mm厚的商业泡沫镍置于有机溶剂中浸泡超声,然后用去离子水清洗干净,经真空干燥获得表面洁净的泡沫镍;
(2)将0.01~10g多巴胺盐酸盐加入到5~500mL去离子水中,在10~50℃下搅拌5~60min,得到澄清溶液a;
(3)将0.05~1g pH缓冲剂加入步骤(2)所得澄清溶液a,在10~50℃下搅拌5~60min,得到棕色透亮溶液b;
(4)将步骤(1)所得表面洁净的泡沫镍浸泡于50~500mL步骤(3)所得的棕色透亮溶液b中,在转速为100~5000转/min及10~50℃下反应2~72h,待反应完毕后,用去离子水清洗泡沫镍表面,在50~180℃下真空干燥1~36h,得到聚多巴胺修饰的泡沫镍;
(5)将0.05~5g的三聚氰胺与1g商业纳米TiO2超声分散于50~500mL的乙醇中,处理时间为0.5~2h,再在搅拌中以20~80℃蒸发除去乙醇,所得干燥混合物研磨成粉,干燥2h获得干燥粉末;
(6)将步骤(5)所得干燥粉末放置于陶瓷坩埚中,用锡箔纸包裹好后放入马弗炉中以2~20℃/min的升温速度升温至400~600℃,煅烧0.5~4h;
(7)称取步骤(6)煅烧后的粉末0.1~5g,超声分散于200mL去离子水中,采用酸调节pH值到2~9,得到分散液;
(8)另将步骤(1)所得表面洁净的泡沫镍和Ti片电极浸入步骤(7)所得分散液中,在泡沫镍与Ti片电极间施加50~300V的电压,泡沫镍与Ti片电极距离2~10cm,在100~5000转/min搅拌速度下,电泳1~10min,并用去离子水冲洗泡沫镍表面未附着的颗粒物,在50~180℃下真空干燥1~36h,即获得g-C3N4/TiO2负载的泡沫镍;
(9)将步骤(4)与步骤(8)分别获得的聚多巴胺修饰的泡沫镍和g-C3N4/TiO2负载的泡沫镍通过黏合剂粘接复合,或者采用物理压合,得到聚多巴胺修饰氮化碳/二氧化钛负载泡沫镍复合光催化剂。
2.根据权利要求1所述的制备方法,其特征在于:步骤(1)所述有机溶剂为乙醇、丙酮、甲醇、N,N-二甲基甲酰胺、二氯甲烷和甲苯中的一种或两种。
3.根据权利要求1所述的制备方法,其特征在于:步骤(3)所述pH缓冲剂为磷酸氢二钠、三羟甲基氨基甲烷、氢氧化钠、碳酸氢钠或四硼酸钠缓冲液。
4.根据权利要求1所述的制备方法,其特征在于:步骤(7)所述酸为稀盐酸、稀硫酸、醋酸、磷酸或硅酸。
5.根据权利要求1所述的制备方法,其特征在于:步骤(9)所述黏合剂为羧甲基纤维素或聚乙烯醇。
6.一种聚多巴胺修饰氮化碳/二氧化钛负载泡沫镍复合光催化剂,是由权利要求1~5中任一项所述的制备方法制备得到的。
7.权利要求6所述的基于聚多巴胺修饰氮化碳/二氧化钛负载泡沫镍复合光催化剂在捕获与杀灭生物气溶胶领域的应用,其特征在于:所述应用按照以下步骤:采用抽气泵将生物气溶胶通过聚多巴胺修饰氮化碳/二氧化钛负载泡沫镍复合光催化剂,光照强度为10~1000mW/cm2,过滤时间为5~120min。
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