CN108755103B - 一种光催化自清洁防紫外织物的制备方法 - Google Patents
一种光催化自清洁防紫外织物的制备方法 Download PDFInfo
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Abstract
本发明公开了一种光催化自清洁防紫外织物的制备方法,其特征在于,将含氮化合物溶液、碱剂、蒸馏水超声混合,依次经烘干、研磨、煅烧后,得到改性介孔氮化碳;将金属盐溶液逐滴滴入改性介孔氮化碳分散液中,搅拌至溶剂挥发,将固体干燥,煅烧后,得到金属离子掺杂改性介孔氮化碳;将其与TiO2溶胶、硅溶胶混合分散,将织物浸渍于该混合分散液中,预烘,再汽蒸,之后干燥,得到光催化自清洁防紫外织物。本发明利用碱剂中氢氧根离子与铁离子掺杂降低光生电子‑空穴对的复合,提高催化剂对可见光的利用率,光催化性能得到较大提升,制备的复合纳米材料催化波长范围宽、催化效率高。
Description
技术领域
本发明属于功能织物的制备技术领域,具体涉及一种光催化自清洁防紫外织物的制备方法。
背景技术
随着经济发展和人们生活水平的提高,人们对于室内纺织品的要求除了其基本的服用和装饰作用外,对于其自清洁、抗紫外线等功能性的需求也越来越高。而纺织品自清洁功能的赋予不仅可以省去洗涤的人力,还可以减轻污水处理等带来的环境和能源的负担。同时,由于科学技术的迅速发展、先进表征手段和制备方法的不断更新,人们对于光催化剂的研究也日益成熟,对基于光催化技术的功能性织物已有初步研究成果。目前比较多的在纺织品上应用主要涉及商业化光催化剂二氧化钛(P25),而P25只能在占太阳能量3-5%的紫外光下发挥作用,需要再开发可见光下响应的光催化剂。氮化碳具有可见光响应、操作简单等优点,具有较好的应用前景。但也存在着比表面积小、光生电子-空穴对易分离时间短、带隙相对较大等方面的问题,我们选取含氮化合物为前驱体,通过碱剂改性及金属离子掺杂,改善其结构和光学性能,克服石墨相氮化碳的缺点与不足,提升其光催化性能。
目前国内外将光催化材料应用在纺织品上主要有共混纺丝法和后整理。前者将催化剂加入到纺丝液中制备功能性纤维时,大多数的催化剂被包覆在纤维内部,在纤维表面裸露的很少,不能充分的接受光照,所以其自清洁、抗紫外线等功能得不到充分的发挥而影响其性能。后整理法主要有通过丙烯酸酯、树脂等粘合剂将氮化碳涂覆在织物表面,粘合剂也会将催化剂包裹在内,影响其光催化性能,其中聚丙烯酸酯等粘合剂在处理过程中还会有烯烃气体析出,加重光催化降解的负担。制备的氮化碳基光催化材料是纳米颗粒的,纳米材料的粒径相对较小、表面能较高,极易发生团聚,分散性不好。尤其对于涤纶织物结构紧密,极性较小,氮化碳为无机材料与涤纶织物的亲和力很低,耐水洗性能差。同时,光催化材料处理的纺织品在实际使用过程中,由于催化剂较强的氧化还原性能会使织物纤维发生脆损等问题。
近来,无机氧化物涂膜整理到织物上是改善织物性能的一种新途径。溶胶-凝胶法是最常用的制备无机氧化膜的方法。利用溶胶与催化剂之间的静电作用形成稳定分散液后,再在织物表面形成一层具有紫外-可见光响应的透明薄膜,其与织物纤维通过库仑力结合而具有较好的结合牢度,赋予织物功能性,而且在获得功能性的同时还要保持对织物原有的服用性能的影响最小,使得制备的光催化纺织品能兼具功能性和服用性。
发明内容
本发明所要解决的技术问题是:提供一种光催化自清洁防紫外织物的制备方法。
为了解决上述问题,本发明提供了一种光催化自清洁防紫外织物的制备方法,其特征在于,包括以下步骤:
步骤1):室温条件下,将含氮化合物溶液、碱剂、蒸馏水超声混合,依次经烘干、研磨、煅烧后,得到改性介孔氮化碳;
步骤2):将金属盐溶液逐滴滴入事先用水分散好的改性介孔氮化碳分散液中,持续搅拌直至溶剂完全挥发,将固体置于真空烘箱中60~80℃下干燥16~20h,经研磨、煅烧后,得到金属离子掺杂改性介孔氮化碳;
步骤3):将金属掺杂改性介孔氮化碳与TiO2溶胶、硅溶胶进行超声混合分散,将织物浸渍于该混合分散液中,然后60~80℃预烘3min,再100℃汽蒸,之后置于50~60℃的真空干燥箱中干燥36-48h,得到光催化自清洁防紫外织物。
优选地,所述步骤1)中含氮化合物为尿素、单氰胺或两者的混合物,采用的溶剂为水,含氮化合物溶液的质量浓度为20~30%;碱剂为氢氧化钾、氢氧化钠或两者混合物的水溶液水,浓度为0.5~10g/L。
优选地,所述步骤1)中含氮化合物、碱剂的溶质、蒸馏水的摩尔比为1∶0.0001~0.01∶3;煅烧设备采用马弗炉,工艺参数为:以10~15℃/min的升温速度升温到450~550℃后保温2~4h。
优选地,所述步骤2)中的搅拌温度为50~70℃。
优选地,所述步骤2)中金属盐溶液中的阳离子为Fe3+、Co2+或Ni2+,阴离子为醋酸根、硝酸根或草酸根,溶剂采用水、乙醇或乙二醇。
优选地,所述步骤2)中金属盐溶液的浓度为0.018~0.3mol/L,改性介孔氮化碳分散液的固体含量为0.2~0.5%,金属硝酸盐溶液与改性介孔氮化碳分散液的体积比为2∶1~1∶2。
优选地,所述步骤3)中TiO2溶胶的质量浓度为1~3%,硅溶胶的质量浓度为10~20%。
优选地,所述步骤3)中金属掺杂改性介孔氮化碳、TiO2溶胶、硅溶胶的质量比为1∶10∶15~1∶4∶5。
优选地,所述步骤3)中织物与混合分散液的浴比为1∶20~1∶40,织物浸入时混合分散液的温度为20~30℃,浸渍时长为1~2h;汽蒸时长为1~3h。
本发明利用碱剂改性与金属离子掺杂共同作用获得了在可见光范围内具有较高催化活性的氮化碳基光催化剂,并利用与紫外光响应型半导体催化剂在织物表面原位复合,获得了对织物基底损伤小且催化波长范围宽、催化效率高的可见光催化复合膜。该织物具有在可见光下光催化自清洁、抗紫外、杀菌的效果,其制备方法简单,制备的织物可应用于医院、室内装饰、汽车内部装饰等领域。
与现有技术相比,本发明具有以下有益效果:
(1)本发明的光催化自清洁防紫外织物具有高催化活性和良好稳定性、无二次污染、在可见光照的条件下具有良好的自清洁效果以及防紫外性能;
(2)本发明的制备方法简单,便于实验室操作,反应液组成简单且成本低,对设备要求性能低,可用于工业化生产。
附图说明
图1为实施例1中光催化剂B与P25的UV-Vis图;
图2为实施例1中光催化剂B处理到织物上的电镜图;
图3为实施例1中原布、P25、处理后的织物降解红酒和咖啡渍的对比图;
图4为实施例1中原布、P25、处理后的织物的紫外线透射率;
图5为实施例1中原布、P25、处理后的织物的紫外线防护系数。
具体实施方式
为使本发明更明显易懂,兹以优选实施例,并配合附图作详细说明如下。
实施例1
一种光催化自清洁防紫外织物的制备方法:
1、室温下将尿素溶液、KOH溶液和去离子水混合均匀后,在60℃下烘干12h,研磨成粉末状,放置马弗炉中以10℃/min升温速率升至550℃保温4h,自然降温,形成粉体A;其中,尿素溶液的质量浓度为30%,KOH溶液的浓度为1g/L,尿素、KOH、蒸馏水的物质的量之比为1∶0.01∶3;
2、将用水分散好的A分散液与硝酸铁溶液持续搅拌然后在60℃真空烘箱中烘16h,得到粉体B;其中,粉体A分散液的固含量为0.5%,硝酸铁溶液的浓度为0.094mol/L,硝酸铁溶液与粉体A分散液的体积比为1∶1;
3、室温下,将粉体B与TiO2溶胶、硅溶胶混合分散后,将聚酯纤维面料浸渍于混合分散液中2h,取出后在80℃下预烘3min、100℃汽蒸2h,之后置于60℃的真空干燥箱中干燥36h,得到所述光催化自清洁防紫外织物;其中,TiO2溶胶的质量浓度为2%,硅溶胶的质量浓度为20%,粉体B与TiO2溶胶、硅溶胶的质量比为1∶4∶5,浴比为1∶30。
将红酒和咖啡污渍作为降解目标产物;抗紫外性能参照澳大利亚-新西兰AS/NZS4399:1996标准来测定织物的紫外线防护效果,并用紫外线防护系数(UPF)和紫外线透射率(UVA、UVB)来表示。实验结果表明本技术处理的涤纶织物具有良好的自清洁和防紫外线性能。
实施例2
一种光催化自清洁防紫外织物的制备方法:
1、室温下将尿素溶液、KOH溶液和去离子水混合均匀后,在60℃下烘干12h,研磨成粉末状,放置马弗炉中以10℃/min升温速率升至550℃保温4h,自然降温,形成粉体A;其中,尿素溶液的质量浓度为30%,KOH溶液的浓度为1g/L;尿素、KOH、蒸馏水的物质的量之比为1∶0.01∶3;
2、将用水分散好的A分散液与硝酸铁溶液持续搅拌然后在60℃真空烘箱中烘16h,得到粉体B;其中,粉体A分散液的固含量为0.5%,硝酸铁溶液的浓度0.094mol/L,硝酸铁溶液与粉体A分散液的体积比为2∶1;
3、室温下,将粉体B与二氧化钛溶胶、硅溶胶混合分散后,将聚酯纤维面浸渍于混合分散液中2h,取出后在80℃下预烘3min、100℃汽蒸2h,之后置于60℃的真空干燥箱中干燥36h,得到所述光催化自清洁防紫外织物;其中,TiO2溶胶的质量浓度为2%;硅溶胶的质量浓度为20%,粉体B与TiO2溶胶、硅溶胶的质量比为1∶4∶5,浴比为1∶30。
将红酒和咖啡污渍作为降解目标产物;抗紫外性能参照澳大利亚-新西兰AS/NZS4399:1996标准来测定织物的紫外线防护效果,并用紫外线防护系数(UPF)和紫外线透射率(UVA、UVB)来表示。实验结果表明本技术处理的涤纶织物具有良好的自清洁和防紫外线性能。
实施例3
一种光催化自清洁防紫外织物的制备方法:
1、室温下将尿素溶液、NaOH溶液和去离子水混合均匀后,在60℃下烘干12h,研磨成粉末状,放置马弗炉中以10℃/min升温速率升至550℃保温2h,自然降温,形成粉体A;其中,尿素溶液的质量浓度为30%,KOH溶液的浓度为1g/L,尿素、KOH、蒸馏水的物质的量之比为:1∶0.01∶3;
2、将用水分散好的A分散液与一定量的硝酸铁溶液持续搅拌然后在60℃真空烘箱中烘16h,得到粉体B;其中,粉体A分散液的固含量为0.5%,醋酸镍溶液的浓度为0.094mol/L,醋酸镍溶液与粉体A分散液的体积比为1∶1;
3、室温下,将B与TiO2溶胶、硅溶胶混合分散后,将聚酯纤维面料浸渍于混合分散液中2h,取出后在80℃下预烘3min、100℃汽蒸2h,之后置于60℃的真空干燥箱中干燥48h,得到所述光催化自清洁防紫外织物;其中,TiO2溶胶的质量浓度为2%,硅溶胶的质量浓度为20%,粉体B与TiO2溶胶、硅溶胶的质量比为1∶4∶5,浴比为1∶30。
将红酒和咖啡污渍作为降解目标产物;抗紫外性能参照澳大利亚-新西兰AS/NZS4399:1996标准来测定织物的紫外线防护效果,并用紫外线防护系数(UPF)和紫外线透射率(UVA、UVB)来表示。实验结果表明本技术处理的涤纶织物具有良好的自清洁和防紫外线性能。
实施例4
一种光催化自清洁防紫外织物的制备方法:
1、室温下将单氰胺溶液、KOH溶液和去离子水混合均匀后,在60℃下烘干12h,研磨成粉末状,放置马弗炉中以10℃/min升温速率升至550℃保温2h,自然降温,形成粉体A;其中,单氰胺溶液的质量浓度为30%,KOH溶液的浓度为1g/L,单氰胺、KOH、蒸馏水的物质的量之比为:1∶0.01∶3;
2、将用水分散好的A分散液与草酸钴溶液持续搅拌然后在60℃真空烘箱中烘16h,得到粉体B;其中,粉体A分散液的固含量为0.5%,草酸钴溶液的浓度为0.094mol/L,草酸钴溶液与粉体A分散液的体积比为1∶1;
3、室温下,将粉体B与TiO2溶胶、硅溶胶混合分散后,将聚酯纤维面料浸渍于混合分散液中2h,取出后在80℃下预烘3min、100℃汽蒸2h,之后置于60℃的真空干燥箱中干燥36h,得到所述光催化自清洁防紫外织物;其中,TiO2溶胶的质量浓度为2%,硅溶胶的质量浓度为20%,粉体B与TiO2溶胶、硅溶胶的质量比为1∶4∶5,浴比为1∶30。
将红酒和咖啡污渍作为降解目标产物;抗紫外性能参照澳大利亚-新西兰AS/NZS4399:1996标准来测定织物的紫外线防护效果,并用紫外线防护系数(UPF)和紫外线透射率(UVA、UVB)来表示。实验结果表明本技术处理的涤纶织物具有良好的自清洁和防紫外线性能。
Claims (5)
1.一种光催化自清洁防紫外织物的制备方法,其特征在于,包括以下步骤:
步骤1):室温条件下,将含氮化合物溶液、碱剂、蒸馏水超声混合,依次经烘干、研磨、煅烧后,得到改性介孔氮化碳;所述含氮化合物、碱剂的溶质、蒸馏水的摩尔比为1:0.0001~0.01:3;煅烧设备采用马弗炉,工艺参数为:以10~15℃/min的升温速度升温到450~550℃后保温2~4h;
步骤2):将金属盐溶液逐滴滴入事先用水分散好的改性介孔氮化碳分散液中,持续搅拌直至溶剂完全挥发,将固体置于真空烘箱中60~80℃下干燥16~20h,经研磨、煅烧后,得到金属离子掺杂改性介孔氮化碳;所述金属盐溶液中的阳离子为Fe3+、Co2+或Ni2+,阴离子为醋酸根、硝酸根或草酸根,溶剂采用水、乙醇或乙二醇;所述金属盐溶液的浓度为0.018~0.3mol/L,改性介孔氮化碳分散液的固体含量为0.2~0.5%,金属硝酸盐溶液与改性介孔氮化碳分散液的体积比为2:1~1:2;
步骤3):将金属掺杂改性介孔氮化碳与TiO2溶胶、硅溶胶进行超声混合分散,将织物浸渍于该混合分散液中,然后60~80℃预烘3min,再100℃汽蒸,之后置于50~60℃的真空干燥箱中干燥36-48h,得到光催化自清洁防紫外织物;所述金属掺杂改性介孔氮化碳、TiO2溶胶、硅溶胶的质量比为1:10:15~1:4:5。
2.如权利要求1所述的光催化自清洁防紫外织物的制备方法,其特征在于,所述步骤1)中含氮化合物为尿素、单氰胺或两者的混合物,采用的溶剂为水,含氮化合物溶液的质量浓度为20~30%;碱剂为氢氧化钾、氢氧化钠或两者混合物的水溶液水,浓度为0.5~10g/L。
3.如权利要求1所述的光催化自清洁防紫外织物的制备方法,其特征在于,所述步骤2)中的搅拌温度为50~70℃。
4.如权利要求1所述的光催化自清洁防紫外织物的制备方法,其特征在于,所述步骤3)中TiO2溶胶的质量浓度为1~3%,硅溶胶的质量浓度为10~20%。
5.如权利要求1所述的光催化自清洁防紫外织物的制备方法,其特征在于,所述步骤3)中织物与混合分散液的浴比为1:20~1:40,织物浸入时混合分散液的温度为20~30℃,浸渍时长为1~2h;汽蒸时长为1~3h。
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