CN112588284A - 制备光催化空气净化棒状二氧化钛颗粒复合纤维毡的方法 - Google Patents
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Abstract
本发明公开了制备光催化空气净化棒状二氧化钛颗粒复合纤维毡的方法,包括如下步骤:配置二氧化钛前驱体溶液;将光催化纳米颗粒用去离子水分散,超声震荡得到分散液,将纤维毡浸渍于分散液中超声,然后烘干;将纤维毡放入二氧化钛前驱体溶液中,随后放入微波快速反应合成器中进行退火,即得纤维表面被均匀的棒状光催化复合纳米颗粒包覆的复合纤维毡。本发明将二氧化钛颗粒以前驱体混合液的形式分散附着在纤维表面,复合纤维毡特殊三维网状结构均匀负载紧密包覆光催化颗粒,增大了原有单一超细纤维的比表面积,增加了催化剂与细菌微生物的接触面积和参与氧化还原反应的活性位点数量,更高效捕获空气中的微生物颗粒实现快速光催化响应,实现光催化抗菌灭活。
Description
技术领域
本发明属于空气过滤纤维毡技术领域,具体涉及制备光催化空气净化棒状二氧化钛颗粒复合纤维毡的方法。
背景技术
随着社会的发展,各行各业对空气质量的要求也越来越高,尤其是当前像新冠病毒这种空气传播疾病对全球影响程度越来越深,迫使我们对空气净化用过滤材料提出了更高的要求。未来高性能空气净化滤材的发展趋势不仅需要具有非常强的细颗粒污染物捕获能力,同时还需要具备有抗菌杀菌的复合功能,对于应用在人口密集的场所显得十分重要,如交通工具、超市、医院等。纤维过滤毡可以利用其纤维搭建的三维网络结构来通过物理拦截和静电吸附捕获细小颗粒污染物,但纤维过滤毡对空气中存在病毒微生物无能为力,并且当条件合适时一些微生物可以在纤维过滤毡上生存繁殖。利用光催化机理的二二氧化钛、石墨烯和还原氧化石墨烯等光触媒具有良好的空气杀菌能力,并且非常经济适用,但缺少可有效负载的空气过滤介质和光触煤颗粒自身独特的结构,使得光触媒可以在可见光条件下和空气净化滤材介质有效融合短时间内起到杀菌净化空气的作用。因此,开发出高性能光触煤和纤维毡复合空气净化滤材是一个亟待解决的问题。
发明内容
综上所述,本发明的目的在于提供制备空气净化用棒状二氧化钛光催化颗粒复合纤维毡的方法,以达到优异的空气过滤和可见光条件下的快速光催化抗菌响应。
为达到上述目的,本发明提供如下技术方案:制备光催化空气净化棒状二氧化钛颗粒复合纤维毡的方法,包括如下步骤:
步骤1,配置二氧化钛前驱体溶液;
步骤2,将6mg/mL的光催化纳米颗粒用去离子水分散为50mL,超声震荡30min,得到分散液,将纤维毡浸渍于分散液中超声5min,然后烘干,烘干条件为135℃保持20min,浸渍烘干重复三次;
步骤3,将步骤2中的纤维毡放入步骤1中的二氧化钛前驱体溶液中,随后放入微波快速反应合成器中进行退火,即得棒状二氧化钛光催化颗粒复合纤维毡。
进一步的,步骤1配置二氧化钛前驱体溶液的方法为:将二氧化钛钛源溶解在去离子水里面,通过加入氨水控制沉淀析出,将沉淀抽滤并烘干,沉淀为钛氨络合物,再取沉淀抽滤的钛氨络合物加氨水和水配置成摩尔浓度为0.5-3.0mol/L的二氧化钛前驱体溶液。
进一步的,步骤2中二氧化钛钛源为四氯化钛、钛酸四丁酯、硫酸氧钛、异丙醇钛、硫酸钛和二氟氧钛其中的一种或几种。
进一步的,步骤2中光催化纳米颗粒为石墨烯、氧化石墨烯、还原氧化石墨烯或石墨烯量子点中的一种或几种,颗粒直径为20-200nm。
进一步的,步骤2中超细玻璃纤维为玻璃纤维或玄武岩纤维,平均纤维直径为0.5-4μm。
进一步的,步骤3的二氧化钛前驱体溶液中加入偶联剂,偶联剂选用KH560、三甲基氯硅烷、六甲基二硅烷中的一种或几种。
进一步的,步骤3的微波快速反应加热温度为125-185℃,反应时间为6-8min。
进一步的,步骤3中的退火工艺为H2氛围250℃-350℃退火2-3h。
本发明的有益效果在于:
1、本发明将二氧化钛纳米颗粒以前驱体混合液的形式分散附着在纤维表面,同时将光催化纳米颗粒和纤维一同置于二氧化钛前驱体溶液微波超声分散,在不破坏复合纤维毡特殊三维网状结构的前提下,保留其优异的空气过滤性能的同时去均匀负载和紧密包覆的光催化纳米颗粒。
2、均匀负载和紧密包覆在纤维表面的纳米二氧化钛光催化颗粒成棒状,使得其在可见光照射下自身能产生强氧化性的羟基自由基;同时,也可以提高复合纤维毡的比表面积,提供更多的活性位点数量,都可以有效提高制得复合纤维毡的抗菌杀菌效果。
3、通过负载光催化纳米颗粒后的纤维毡,光催化剂二氧化钛在石墨烯基体上的均匀分散并附着在复合纤维毡表面,增加了催化剂与细菌微生物的接触面积,一定程度上增加了参与氧化还原反应的活性位点数量,以便更高效率捕获空气中的微生物颗粒实现快速光催化响应。
4、通过石墨烯量子点的引入,石墨烯量子点作为一种零维石墨烯材料,相较于氧化石墨烯和还原氧化石墨烯有更小的粒径,其晶格结构与石墨烯无异,但比表面积比石墨烯更大,活性也更高。除此以外,石墨烯量子点还具有良好的水溶性、无毒性及稳定的光致发光特性等,且属于碳材料,一定条件下可大量获得。同时石墨烯量子点外观极小因此内部电子在各个方向上的运动都会受到限制,从而表现出量子限域效应和边界效应,使其表现出更出色的电子传输能力,从而延长载流子寿命,所以能有效的较低二氧化钛的光生载流子对的复合,使得于复合纤维毡能在可见光的条件下在短时间内对大肠杆菌和金黄色葡萄球菌实现光催化抗菌灭活。
附图说明
图1为对比实施例制得的超细玻璃纤维复合毡放大10000显微组织图;
图2为实施例2制得的超细玻璃纤维复合毡放大10000倍显微组织图。
具体实施方式
以下实施例制备空气净化用棒状二氧化钛光催化颗粒复合纤维毡的方法,但本实施例不能用于限制本发明,凡是采用本发明的相似方法及其相似变化,均应列入本发明的保护范围。
纤维准备:对比实施例和实施例1-2的超细玻璃纤维选取的原料为按质量比称取63份石英砂、6.5份纯碱、3份钾长石、5钠长石、7份方解石、5硼砂、4白云石、1.5份碳酸钡、1份氧化锌和4份平板废玻璃,然后将选取制备超细玻璃纤维的原料混合均匀后投入到1460℃的窑炉中高温熔融成透明均匀的玻璃液,其中熔融均匀的玻璃液温度为1160℃,然后将透明均匀的玻璃液通过2条料道分别流过温度为1000℃、材质为PtRh10的铂铑合金漏板1和温度为990℃、材质为GH4169钴镍合金漏板2分别形成一次玻璃纤维丝,合金漏板1形成的一次玻璃纤维丝再经过温度为1020℃火焰喷吹炉头1形成叩解度为39±1的超细玻璃纤维;合金漏板2形成的一次玻璃纤维丝再经过温度为1005℃火焰喷吹炉头2形成叩解度为32±1的超细玻璃纤维。
实施例3的玄武岩纤维选取质量百分比组分为SiO2:53.5%,Al2O3:15%,Fe2O3:4%,FeO:7%,CaO:8%,Na2O:5.5%,K2O:2%,MgO:3.5%和TiO2:1.5%的纯天然玄武岩作为原料,经在1475℃的窑炉中高温熔融成均匀的熔浆,然后通过料道1250℃的玄武岩熔浆流入材质为PtRh10的400孔铂铑合金漏板,最后经过快速拉丝形成玄武岩纤维。
对比实施例:参见公开号CN111905452A实施例2制备出的一种光催化空气净化用超细玻璃纤维棉毡可以达到在可见光的条件下1h降解85%的10mg/L的罗丹明B溶液,定量80g/m2,过滤阻力125Pa,过滤效率80%,透气量190L/m2·min。
实施例1-3按照如下步骤实施:
制备光催化空气净化棒状二氧化钛颗粒复合纤维毡的方法,包括如下步骤:
步骤1,配置二氧化钛前驱体溶液:将异丙醇钛和四氯化钛的混合物溶解在去离子水里面,通过加入氨水控制沉淀析出,将沉淀抽滤并烘干,沉淀为钛氨络合物,再取沉淀抽滤的钛氨络合物加氨水和水配置成最佳摩尔浓度为2.5mol/L的二氧化钛前驱体溶液;
步骤2,将6mg/mL的光催化纳米颗粒用去离子水分散为50mL,超声震荡30min,得到分散液,将超细纤维放入分散液中超声5min,然后烘干,烘干条件为135℃保持20min,浸渍烘干重复三次;
步骤3,将步骤2中的超细纤维放入步骤1中二氧化钛前驱体溶液中,随后放入微波快速反应合成器进行退火,即得纳米棒状光催化颗粒复合纤维毡。
实施例1
步骤2中二氧化钛钛源为异丙醇钛和四氯化钛。步骤2中光催化纳米颗粒为纳米氧化石墨烯,颗粒直径为55nm。步骤2中超细纤维为平均直径为2.5μm的超细玻璃纤维。步骤3的二氧化钛前驱体溶液中加入粘接剂。步骤3的微波快速反应加热温度为175℃,反应时间为7min。步骤3中的退火工艺为H2氛围280℃退火2.5h。最终制备出的光催化空气净化棒状二氧化钛颗粒复合纤维毡的光催化降解性能达到在可见光的条件下55min降解95%的10mg/L的罗丹明B溶液;空气过滤性能达到定量90g/m2,过滤阻力107Pa,过滤效率93.5%和透气量240L/m2·min;力学性能达到沿纤维长度方向为21N/25mm,沿纤维宽度方向为11N/25mm;结构特点为纤维表面被的棒状包覆,比表面积由原有单一超细玻璃纤维的2.3641m2/g增大到均匀包覆棒状光催化复合纳米颗粒的7.8795m2/g。
实施例2
步骤2中,二氧化钛钛源为硫酸氧钛和二氟氧钛。步骤2中光催化纳米颗粒为石墨烯量子点,颗粒直径为30nm。步骤2中超细纤维为平均直径为2μm的超细玻璃纤维。步骤3的微波快速反应加热温度为185℃,反应时间为6min。步骤3中的退火工艺为H2氛围350℃退火2h。最终制备出的光催化空气净化纳米棒状颗粒复合纤维毡的光催化降解性能达到在可见光的条件下40min降解97%的10mg/L的罗丹明B溶液;空气过滤性能达到定量92g/m2,过滤阻力98Pa,过滤效率97%和透气量225L/m2·min;力学性能达到沿纤维长度方向为23N/25mm,沿纤维宽度方向为12.5N/25mm;比表面积由原有单一超细玻璃纤维的2.3641m2/g增大到均匀包覆棒状光催化复合纳米颗粒的9.7256m2/g。
实施例3
步骤2中,二氧化钛钛源为为异丙醇钛和和二氟氧钛。步骤2中光催化纳米颗粒为还原氧化石墨烯,颗粒直径为30nm。步骤2中超细纤维为平均直径为2.5μm的超细玄武岩纤维。步骤3的微波快速反应加热温度为185℃,反应时间为6min。步骤3中的退火工艺为H2氛围350℃退火2h。最终制备出的光催化空气净化纳米棒状颗粒复合纤维毡的光催化降解性能达到在可见光的条件下40min降解95%的10mg/L的罗丹明B溶液;空气过滤性能达到定量81g/m2,过滤阻力101Pa,过滤效率95%和透气量228L/m2·min;力学性能达到沿纤维长度方向为21N/25mm,沿纤维宽度方向为10.5N/25mm;结构特点为纤维表面被均匀的棒状光催化复合纳米颗粒包覆,比表面积由原有单一超细玻璃纤维的2.3641m2/g增大到均匀包覆棒状光催化复合纳米颗粒的8.8265m2/g。
最后说明的是,以上优选实施例仅用以说明本发明的技术方案而非限制,尽管通过上述优选实施例已经对本发明进行了详细的描述,但本领域技术人员应当理解,可以在形式上和细节上对其作出各种各样的改变,而不偏离本发明权利要求书所限。
Claims (8)
1.制备光催化空气净化棒状二氧化钛颗粒复合纤维毡的方法,其特征在于,包括如下步骤:
步骤1,配置二氧化钛前驱体溶液;
步骤2,将6mg/mL的光催化纳米颗粒用去离子水分散为50mL,超声震荡30min,得到分散液,将纤维毡浸渍于分散液中超声5min,然后烘干,烘干条件为135℃保持20min,浸渍烘干重复三次;
步骤3,将步骤2中的纤维毡放入步骤1中的二氧化钛前驱体溶液中,随后放入微波快速反应合成器中进行退火,即得棒状二氧化钛光催化颗粒复合纤维毡。
2.根据权利要求1所述的制备棒状二氧化钛光催化颗粒复合纤维毡的方法,其特征在于,步骤1配置二氧化钛前驱体溶液的方法为:将二氧化钛钛源溶解在去离子水里面,通过加入氨水控制沉淀析出,将沉淀抽滤并烘干,沉淀为钛氨络合物,再取沉淀抽滤的钛氨络合物加氨水和水配置成摩尔浓度为0.5 -3.0 mol/L的二氧化钛前驱体溶液。
3.根据权利要求2所述的制备棒状二氧化钛光催化颗粒复合纤维毡的方法,其特征在于,步骤2中二氧化钛钛源为四氯化钛、钛酸四丁酯、硫酸氧钛、异丙醇钛、硫酸钛和二氟氧钛其中的一种或几种。
4.根据权利要求1所述的制备棒状二氧化钛光催化颗粒复合纤维毡的方法,其特征在于,步骤2中光催化纳米颗粒为石墨烯、氧化石墨烯、还原氧化石墨烯或石墨烯量子点中的一种或几种,颗粒直径为20-200nm。
5.根据权利要求1所述的制备棒状二氧化钛光催化颗粒复合纤维毡的方法,其特征在于,步骤2中超细玻璃纤维为玻璃纤维或玄武岩纤维,平均纤维直径为0.5-4μm。
6.根据权利要求1所述的制备棒状二氧化钛光催化颗粒复合纤维毡的方法,其特征在于,步骤3的二氧化钛前驱体溶液中加入偶联剂,偶联剂选用KH560、三甲基氯硅烷、六甲基二硅烷中的一种或几种。
7.根据权利要求1所述的制备棒状二氧化钛光催化颗粒复合纤维毡的方法,其特征在于,步骤3的微波快速反应加热温度为125-185℃,反应时间为6-8min。
8.根据权利要求1所述的制备棒状二氧化钛光催化颗粒复合纤维毡的方法,其特征在于,步骤3中的退火工艺为H2氛围250℃-350℃退火2-3h。
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