CN106978715A - 一种具有光催化和抗菌性能的纺织布复合材料及其制备方法 - Google Patents
一种具有光催化和抗菌性能的纺织布复合材料及其制备方法 Download PDFInfo
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- CN106978715A CN106978715A CN201710261028.4A CN201710261028A CN106978715A CN 106978715 A CN106978715 A CN 106978715A CN 201710261028 A CN201710261028 A CN 201710261028A CN 106978715 A CN106978715 A CN 106978715A
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- 229910052797 bismuth Inorganic materials 0.000 claims description 16
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- XKKVXDJVQGBBFQ-UHFFFAOYSA-L zinc ethanol diacetate Chemical compound C(C)O.C(C)(=O)[O-].[Zn+2].C(C)(=O)[O-] XKKVXDJVQGBBFQ-UHFFFAOYSA-L 0.000 claims description 14
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Abstract
本发明公开了一种具有光催化和抗菌性能的纺织布复合材料,它为纺织布上负载着片状AgBr/ZnO/BiOBr的复合材料,它由BiOBr纳米片附着在纺织布纤维表面而成,其中BiOBr纳米片上负载着ZnO和AgBr纳米颗粒。该复合材料涉及的制备方法简单,反应耗时短、效率高、能耗低,所纺织布复合材料对常见皮肤致病菌金黄色葡萄球菌和绿脓杆菌均具有优异的抑菌活性,可在光照下反复降解吸附在其表面上的有机染料,并具有稳定的光催化自清洁的效果,适用于医疗、环保、日用生活品等领域,适合推广应用。
Description
技术领域
本发明属于功能复合材料制备技术领域,具体涉及一种具有光催化和抗菌性能的纺织布复合材料及其制备方法。
背景技术
我国是纺织品生产和加工大国,随着科技和社会的不断发展与进步,人民生活水平逐渐提高,人们对纺织品的要求也正在逐步变化,从较为单一的保暖舒适型逐渐向安全、健康、自洁、美观等功能型转变。为了适应社会市场需求,提升产品档次,增加产品附加值,新型的多功能纺织品得到了广泛关注。
日常生活中常见的纺织物往往容易遭受有机污染物和细菌的污染。纺织物上滋生的细菌容易导致皮肤病及其他传染病的发生,严重危害人们的身体健康;而纺织物一旦沾上有机污染物,往往不易清洗,使纺织品的使用寿命大为缩短。因此,开发具有光催化降解有机污染物和抗菌性能的纺织布有着广阔的应用前景。
目前已有一些关于同时具有光催化和抗菌性能的纺织布复合材料的报道。例如Joydeb Manna等[ACS Applied Materials&Interfaces,2015,7:8076-8082]制备了Ag/ZnO/棉布复合材料,以棉布为底材,先将棉布投入聚丙烯酸和硝酸锌的混合溶液中,在60℃下加热1h,室温晾干后得到ZnO/棉布复合材料,再将制得的ZnO/棉布复合材料投入硝酸银溶液过夜搅拌,晾干后得到Ag/ZnO/棉布复合材料。该方法涉及的制备过程耗时长,步骤繁琐,制得的样品稳定性不好,Ag和ZnO纳米粒子易从材料表面脱落,且通过该方法制得的样品光催化和抗菌活性不高,需要4h以上才能对金黄色葡萄球菌和绿脓杆菌达到100%的抑菌率,而在可见光照射下需要2.5h才能完全降解罗丹明B染料。Amir Behzadnia等[Ultrasonics Sonochemistry,2015,27:10-21]以呢绒为底材,采用超声波法制备了ZnO/TiO2/呢绒复合材料。该方法将呢绒加入醋酸锌溶液中,通过滴加氨水控制pH为9-10,然后控制升温速度为1℃/min,超声15min,待温度升至40-50℃后逐滴加入异丙醇钛,等温度升至75-80℃后保持该温度和pH值继续超声45min,最后将该样品在60℃下干燥15min,120℃下处理3min得到呢绒复合材料。该方法步骤繁琐,合成周期长,对反应温度的控制要求苛刻,且通过该方法制得的材料同样存在光催化和抗菌活性不足等缺点,在日光照射下7天也不能完全降解亚甲基蓝染料,对金黄色葡萄球菌的抑菌率24h才达到97%。因此,进一步探索具有光催化降解有机污染物和抗菌性能的纺织布复合材料及其制备方法具有重要的实际应用意义。
发明内容
本发明的主要目的在于解决现有纺织布复合材料光催化和抗菌活性不高的问题,提供一种具有优异抗菌活性和光催化自清洁能力的复合材料。
本发明的另一目的在于解决目前纺织布复合材料制备技术上存在的不足,提供一种简单快捷制备AgBr/ZnO/BiOBr/纺织布复合材料的方法,解决当前复合材料制备过程中,制备工艺繁琐、周期长等问题。
为实现上述目的,本发明采用的技术方案为:一种具有光催化和抗菌性能的纺织布复合材料,该复合材料为AgBr/ZnO/BiOBr/纺织布,它由BiOBr纳米片附着在纺织布纤维表面而成,其中BiOBr纳米片上负载着ZnO和AgBr纳米颗粒。
上述方案中,所述BiOBr纳米片的尺寸大小为200-500nm,ZnO纳米颗粒的尺寸大小为50-100nm,AgBr纳米颗粒的尺寸大小为20-30nm。
上述方案中,所述纺织布可选用棉布、羊毛织物、丝绸织物或聚酯布。
上述一种具有光催化和抗菌性能的纺织布复合材料的制备方法,其特征在于,包括如下步骤:
1)纺织布预处理:将纺织布浸泡在有机溶剂中进行超声清洗,再经水洗、烘干、备用;
2)将硝酸铋和溴化钾、醋酸锌、硝酸银分别加入乙醇水溶液中,分别配制硝酸铋-溴化钾乙醇水溶液、醋酸锌乙醇水溶液和硝酸银乙醇水溶液,然后分别调节三种乙醇水溶液的pH值;
3)将经步骤1)预处理的纺织布置于微波-超声波反应器中,加入硝酸铋-溴化钾乙醇水溶液,在微波和超声波共同作用进行保温反应,然后依次间隔加入配制的醋酸锌乙醇水溶液和硝酸银乙醇水溶液,再在相同的微波、超声波和温度条件下进行二次保温反应,反应结束后将所得复合材料取出,依次进行水洗、干燥,即得所述具有光催化和抗菌性能的纺织布复合材料。
上述方案中,步骤1)中所述有机溶剂为甲醇、乙醇、异丙醇、乙酸乙酯、丙酮、己烷、石油醚或二氯甲烷。
上述方案中,步骤2)中所述乙醇水溶液中,无水乙醇和水的体积比均为1-10:1。
上述方案中,所述硝酸铋-溴化钾乙醇水溶液、醋酸锌乙醇水溶液和硝酸银乙醇水溶液中分别引入的K+、Zn2+、Bi3+、Ag+的摩尔比为1:1:(0.7-0.95):(0.05-0.3)。
优选的,所述硝酸铋-溴化钾乙醇水溶液中Bi3+的浓度为15-30mmol/L。
上述方案中,步骤2)中分别调节三种乙醇水溶液的pH值至8-9。
上述方案中,采用氨水调节步骤2)中所述溶液的pH值。
上述方案中,步骤3)中采用的微波功率为300-800W,超声波功率为600-1200W。
上述方案中,所述保温反应温度为60-90℃,时间为15~30min。
上述方案中,所述醋酸锌乙醇水溶液和硝酸银乙醇水溶液的添加时间间隔为15~30min。
本发明的原理为:
1)光催化降解有机污染物:在光催化降解过程中,限制光催化效果的主要原因包括光响应能力不足以及光生电子和空穴容易自相复合等,从而导致产生的氧化剂的含量下降、催化活性不高的问题;以ZnO光催化剂为例,由于其禁带宽度较大(Eg=3.37eV),导致其吸收光范围较窄,主要在紫外光区域响应,产生的电子和空穴数量有限;当ZnO与BiOBr复合时,由于BiOBr的禁带宽度较小(Eg=2.90eV),可提高其在可见光下的响应,产生较多的电子和空穴,但其电子和空穴的自相复合仍然是限制其光催化活性的主要因素之一;本发明在此基础上进一步加入AgBr,由于AgBr有着更小的禁带宽度(Eg=2.69eV),使得光响应范围进一步增大,在可见光照射下,可产生更多的光生电子和空穴;另一方面,AgBr和ZnO以及BiOBr和ZnO之间可形成两个串联的异质结,在串联异质结形成的静电场下,光生电子从AgBr和BiOBr的导带转移到ZnO的导带上,由于AgBr和BiOBr的价带能级小于ZnO,空穴仍留在AgBr和BiOBr的价带上,最终使电子和空穴有效地分离开来,并提高了电子-空穴对的存在时间,从而提高了所得复合材料的光催化性能。
2)抗菌性能和稳定性:ZnO属于一种具有广谱抗菌活性的抗菌剂,但其抗菌活性不高,而BiOBr同样对大肠杆菌和金黄色葡萄球菌有抑制活性,BiOBr是片层结构,其可作为ZnO与AgBr纳米颗粒的载体,引入AgBr纳米粒子能不断提供Ag+,而Ag+具有更强的杀菌性能,有利于显著提高抗菌活性;本发明在超声-微波的共同作用下,由于超声作用溶液中形成了声空穴作用气泡,当气泡与纳米颗粒或纳米片接触时,会发生变形甚至是破裂,形成了高速的喷气和振动波;这些喷气和振动波以高能快速地将推向纺织布的表面,使ZnO纳米颗粒、AgBr纳米颗粒以及BiOBr纳米片和纺织布发生强烈冲撞作用;同时微波的热效应也促进了BiOBr纳米片与纺织布纤维两者间的相互作用,最终使BiOBr纳米片均匀且稳定地附着在纺织布表面,而ZnO和AgBr纳米颗粒均匀地附着在BiOBr纳米片上,提高了纺织布上功能材料的负载量,从而提高了复合材料的抗菌活性和稳定性;另一方面,由于复合材料在可见光下产生的活性氧和羟基自由基可破坏细胞膜,杀灭微生物,可进一步提高了材料的抗菌活性;上述效果协同作用,使所得AgBr/ZnO/BiOBr/纺织布复合材料表现出更加优异的抗菌活性和稳定性。
本发明与现有技术相比,具有如下优点:
1)采用微波与超声波结合工艺,涉及的制备工艺简单,反应耗时短,效率高,能耗低,且制得复合材料中BiOBr纳米片与纤维表面结合紧密,其生长方向与纤维方向一致,同时BiOBr纳米片上负载着ZnO和AgBr纳米颗粒,该结构具有很好的稳定性,可多次循环使用。
2)通过本方法制备的AgBr/ZnO/BiOBr/纺织布复合材料,相比于现有的光催化和抗菌复合材料,具有更加优良的抗菌活性及光催化自清洁性能。
附图说明
图1为实施例1所得AgBr/ZnO/BiOBr复合材料的X射线衍射图。
图2为实施例2所得AgBr/ZnO/BiOBr/棉布复合材料的扫描电子显微镜图。
图3为实施例2所得AgBr/ZnO/BiOBr/棉布复合材料的透射电子显微镜图。
图4为实施例3所得AgBr/ZnO/BiOBr/聚酯布复合材料的扫描电子显微镜图。
图5为实施例2所得AgBr/ZnO/BiOBr/棉布复合材料对金黄色葡萄球菌和绿脓杆菌的抑菌率图。
图6为实施例2所得AgBr/ZnO/BiOBr/棉布复合材料在可见光下降解RhB的光催化活性图。
图7为实施例2所得AgBr/ZnO/BiOBr/棉布复合材料RhB的光催化循环图。
具体实施方式
为了便于理解本发明,列举实施例如下。但本发明并不局限于这些实施例,本技术领域相关人员应了解,所举实施例仅用于帮助理解本发明,不应该视其为对本发明的具体限制,而本发明要求保护的范围也并不局限于实施例列举的范围。
以下实施例中,所述ZnO/BiOBr/棉布复合材料、BiOBr/棉布复合材料、ZnO/棉布复合材料的制备方法与实施例2的制备方法大致相同,不同之处在于如下:ZnO/BiOBr/棉布复合材料不添加硝酸银乙醇水溶液进行二次保温反应;BiOBr/棉布复合材料不添加醋酸锌乙醇水溶液和硝酸银乙醇水溶液进行二次保温反应;ZnO/棉布复合材料不添加硝酸铋-溴化钾乙醇水溶液和硝酸银乙醇水溶液进行保温反应。
实施例1
一种具有光催化和抗菌性能的纺织布复合材料,该材料为AgBr/ZnO/BiOBr/丝绸复合材料,其制备方法包括以下步骤:
1)底材的预处理
纺织布预处理:将纺织布浸泡在有机溶剂中进行超声清洗,再经水洗、烘干、备用;
2)称取1.4mmol五水合硝酸铋和2mmol溴化钾溶于60mL乙醇水溶液中配制硝酸铋-溴化钾乙醇水溶液,称取2mmol二水合醋酸锌溶于10mL乙醇水溶液中配制醋酸锌乙醇水溶液,称取0.1mmol硝酸银溶于10mL乙醇水溶液中配制硝酸银乙醇水溶液,其中乙醇和水的体积比为10:1,然后滴加氨水分别调节上述所配置的溶液的pH值在8-9;
3)将预处理过的丝绸置于微波-超声波反应器中,加入硝酸铋-溴化钾乙醇水溶液,调节微波功率为600W,超声波功率为900W,反应温度为70℃,在微波和超声波共同作用下反应30min,然后依次加入醋酸锌乙醇水溶液和硝酸银乙醇水溶液,两次加入的时间间隔为20min,并分别在相同的超声波、微波和温度条件继续反应15min,反应结束后将所得丝绸复合材料取出,用蒸馏水清洗、干燥,即得所述AgBr/ZnO/BiOBr/丝绸复合材料。
图1为本实施例所得AgBr/ZnO/BiOBr/丝绸复合材料表面收集所得固体粉末的X射线衍射图。从图中可见,该特征吸收峰可分别与BiOBr,ZnO和AgBr标准图谱中的特征吸收峰一一对应,表明丝绸表面附着的复合材料组成为AgBr/ZnO/BiOBr。
实施例2
一种具有光催化和抗菌性能的纺织布复合材料,该材料为AgBr/ZnO/BiOBr/棉布复合材料,其制备方法包括以下步骤:
1)底材的预处理
纺织布预处理:将纺织布浸泡在有机溶剂中进行超声清洗,再经水洗、烘干、备用;
2)称取0.95mmol五水合硝酸铋和1mmol溴化钾溶于40mL乙醇水溶液中配制硝酸铋-溴化钾乙醇水溶液,称取1mmol二水合醋酸锌溶于20mL乙醇水溶液中配制醋酸锌乙醇水溶液,称取0.3mmol硝酸银溶于20mL乙醇水溶液中配制硝酸银乙醇水溶液,其中乙醇和水的体积比为1:1,然后滴加氨水分别调节上述所配置的溶液的pH值在8-9;
3)将预处理过的丝绸置于微波-超声波反应器中,加入硝酸铋-溴化钾乙醇水溶液,调节微波功率为300W,超声波功率为600W,反应温度为90℃,在微波和超声波共同作用下反应30min,然后依次加入醋酸锌乙醇水溶液和硝酸银乙醇水溶液,两次加入的时间间隔为30min,并分别在相同的超声波、微波和温度条件继续反应30min,反应结束后将所得丝绸复合材料取出,用蒸馏水清洗、干燥,即得所述AgBr/ZnO/BiOBr/棉布复合材料。
图2为本实施例所制备的AgBr/ZnO/BiOBr/棉布复合材料的扫描电子显微镜图,从图中可见,在棉纤维表面上分布着大量的纳米片,这些纳米片为BiOBr纳米材料。
图3为本实施例所制备的AgBr/ZnO/BiOBr/棉布复合材料表面收集的固体粉末的透射电子显微镜图,从图中可见,纳米片上附着大小不同的纳米颗粒,尺寸大小为200-500nm,其中大颗粒为ZnO纳米材料,粒径为50-100nm,小颗粒为AgBr纳米材料,粒径为20-30nm。
实施例3
一种具有光催化和抗菌性能的纺织布复合材料,该材料为AgBr/ZnO/BiOBr/棉布复合材料,其制备方法包括以下步骤:
1)纺织布预处理:将普通聚酯布浸泡在乙酸乙酯中进行超声清洗,再经水洗、烘干、备用;
2)称取1.5mmol五水合硝酸铋和2mmol溴化钾溶于80mL乙醇水溶液中配制硝酸铋-溴化钾乙醇水溶液,称取2mmol二水合醋酸锌溶于40mL乙醇水溶液中配制醋酸锌乙醇水溶液,称取0.4mmol硝酸银溶于20mL乙醇水溶液中配制硝酸银乙醇水溶液,其中乙醇和水的体积比为5:1,然后滴加氨水分别调节上述所配置的溶液的pH值在8-9;
3)将预处理过的丝绸置于微波-超声波反应器中,加入硝酸铋-溴化钾乙醇水溶液,调节微波功率为800W,超声波功率为1000W,反应温度为60℃,在微波和超声波共同作用下反应15min,然后依次加入醋酸锌乙醇水溶液和硝酸银乙醇水溶液,两次加入的时间间隔为15min,并分别在相同的超声波、微波和温度条件继续反应20min,反应结束后将所得丝绸复合材料取出,用蒸馏水清洗、干燥,即得所述AgBr/ZnO/BiOBr/聚酯布复合材料。
图4为本实施例所制备的AgBr/ZnO/BiOBr/聚酯布复合材料的扫描电子显微镜图,从图中可见,在聚酯布表面上聚集着纳米片状AgBr/ZnO/BiOBr复合材料。
实施例4
一种具有光催化和抗菌性能的纺织布复合材料,该材料为AgBr/ZnO/BiOBr/棉布复合材料,其制备方法包括以下步骤:
1)纺织布预处理:将普通羊毛织布浸泡在丙酮中进行超声清洗,再用去离子水冲洗,取出后烘干、备用;
2)称取4mmol五水合硝酸铋和5mmol溴化钾溶于160mL乙醇水溶液中配制硝酸铋-溴化钾乙醇水溶液,称取5mmol二水合醋酸锌溶于60mL乙醇水溶液中配制醋酸锌乙醇水溶液,称取1.5mmol硝酸银溶于30mL乙醇水溶液中配制硝酸银乙醇水溶液,其中乙醇和水的体积比为8:1,然后滴加氨水分别调节上述所配置的溶液的pH值在8-9;
3)将预处理过的丝绸置于微波-超声波反应器中,加入硝酸铋-溴化钾乙醇水溶液,调节微波功率为600W,超声波功率为1200W,反应温度为80℃,在微波和超声波共同作用下反应20min,然后依次加入醋酸锌乙醇水溶液和硝酸银乙醇水溶液,两次加入的时间间隔为15min,并分别在相同的超声波、微波和温度条件继续反应15min,反应结束后将所得羊毛织物复合材料取出,用蒸馏水清洗、干燥,即得所述AgBr/ZnO/BiOBr/羊毛织物复合材料。
应用例1
将实施例2所得AgBr/ZnO/BiOBr/棉布复合材料应用于进行抗菌性能测试,具体步骤如下:
1)预处理:ZnO/BiOBr/棉布复合材料、BiOBr/棉布复合材料、ZnO/棉布复合材料和AgBr/ZnO/BiOBr/棉布复合材料分别置于超净工作台中,正反面分别照射30min紫外线进行杀菌处理;
2)AgBr/ZnO/BiOBr/棉布复合材料的细菌实验:
将过夜培养的细菌悬浊液(金黄色葡萄球菌和绿脓杆菌)分散在无菌的生理盐水中,调节OD值使细菌初始浓度为1.0×108CFU/mL,稀释1000倍置于无菌的液体培养基中,将ZnO/BiOBr/棉布复合材料、BiOBr/棉布复合材料、ZnO/棉布复合材料和AgBr/ZnO/BiOBr/棉布复合材料分别置于相同的菌液浓度的液体培养基中振荡培养,分别培养0.5h,1h取点涂板,将固体培养基放入37℃恒温培养箱中培养24h,数菌落个数并计算其抑菌率。
图5为实施例2所得AgBr/ZnO/BiOBr/棉布复合材料对金黄色葡萄球菌和绿脓杆菌的抑菌率图,从图中可以看出,AgBr/ZnO/BiOBr/棉布复合材料(AgBr/ZnO/BiOBr)对金黄色葡萄球菌和绿脓杆菌的抗菌活性均明显地高于BiOBr/棉布(BiOBr)、ZnO/棉布(ZnO)和ZnO/BiOBr/棉布复合材料(ZnO/BiOBr),且其对两种细菌作用1h后的抑菌率均能达到90%以上。
应用例2
将实施例2所得AgBr/ZnO/BiOBr/棉布复合材料应用于进行光催化性能测试,具体步骤如下:
ZnO/BiOBr/棉布复合材料、BiOBr/棉布复合材料、ZnO/棉布复合材料和AgBr/ZnO/BiOBr/棉布复合材料分别浸入浓度为1×10-4M的RhB溶液中暗处吸附12h,取出后置于30℃烘箱中烘干,通过紫外可见漫反射光谱仪(DRS)测得其吸附染料后的吸光值,记为C0;然后置于500W氙灯下用400nm滤光片滤去紫外光后照射,每隔一段时间取出,用DRS测得其吸光值,记为C;最后通过C/C0计算得出不同样品对RhB染料的降解率。
图6为实施例2所得AgBr/ZnO/BiOBr/棉布复合材料在可见光下降解RhB的光催化活性图,从图中可看出,AgBr/ZnO/BiOBr/棉布复合材料在可见光下对RhB染料的光催化活性明显高于BiOBr/棉布复合材料、ZnO/棉布复合材料和ZnO/BiOBr/棉布复合材料,其在可见光下光照5min后,表面所吸附的RhB染料降解率接近80%,继续光照至30min后,表面所吸附的RhB染料完全降解。
应用例3
将实施例2所得AgBr/ZnO/BiOBr/棉布复合材料应用于进行光催化循环性能测试,具体步骤如下:
将经500W氙灯可见光照射0.5h后的AgBr/ZnO/BiOBr/棉布复合材料重新浸入浓度为1×10-4M的RhB溶液中暗处吸附12h,取出后放入30℃烘箱中干燥,再置于可见光下照射0.5h;将该过程重复10次分别得到光催化循环1至10次的样品;其吸光值均由紫外可见漫反射光谱仪(DRS)测得,通过计算评估AgBr/ZnO/BiOBr/棉布复合材料的光催化自清洁循环使用性能。
图7为实施例2中所制备的AgBr/ZnO/BiOBr/棉布复合材料对RhB的光催化循环图,从图中可看出,AgBr/ZnO/BiOBr/棉布复合材料循环使用六次后对RhB的光催化降解率仍然接近100%,而循环使用十次后对RhB的光催化降解率保持90%以上,说明其具有稳定的光催化自清洁效果。
以上所述仅为本发明的优选实施方式,应当指出,对于本领域的普通技术人员来说,在不脱离本发明创造构思的前提下,做出若干改进和变换,这些都属于本发明的保护范围。
Claims (9)
1.一种具有光催化和抗菌性能的纺织布复合材料,该复合材料为AgBr/ZnO/BiOBr/纺织布,它由BiOBr纳米片附着在纺织布纤维表面而成,其中BiOBr纳米片上负载着ZnO和AgBr纳米颗粒。
2.根据权利要求1所述的纺织布复合材料,其特征在于,所述BiOBr纳米片的尺寸大小为200-500nm,ZnO纳米颗粒的尺寸为50-100nm,AgBr纳米颗粒的尺寸为20-30nm。
3.根据权利要求1所述的纺织布复合材料,其特征在于,所述纺织布可选用棉布、羊毛织物、丝绸织物或聚酯布。
4.权利要求1~3任一项所述具有光催化和抗菌性能的纺织布复合材料的制备方法,其特征在于,包括如下步骤:
1)纺织布预处理:将纺织布浸泡在有机溶剂中进行超声清洗,再经水洗、烘干、备用;
2)分别配制硝酸铋-溴化钾乙醇水溶液、醋酸锌乙醇水溶液和硝酸银乙醇水溶液,然后分别调节所得三种乙醇水溶液的pH值;
3)将经预处理的纺织布置于微波-超声波反应器中,加入硝酸铋-溴化钾乙醇水溶液,在微波和超声波共同作用进行保温反应,然后依次间隔加入配制的醋酸锌乙醇水溶液和硝酸银乙醇水溶液,再在相同的微波、超声波和温度条件下进行二次保温反应,反应结束后将所得复合材料取出,依次进行水洗、干燥,即得所述具有光催化和抗菌性能的纺织布复合材料。
5.根据权利要求4所述的制备方法,其特征在于,所述硝酸铋-溴化钾乙醇水溶液、醋酸锌乙醇水溶液和硝酸银乙醇水溶液中分别引入的K+、Zn2+、Bi3+、Ag+的摩尔比为1:1:(0.7-0.95):(0.05-0.3)。
6.根据权利要求4所述的制备方法,其特征在于,所述硝酸铋-溴化钾乙醇水溶液中Bi3+的浓度为15-30mmol/L。
7.根据权利要求4所述的制备方法,其特征在于,步骤2)中分别调节三种乙醇水溶液的pH值至8-9。
8.根据权利要求4所述的制备方法,其特征在于,步骤3)中采用的微波功率为300-800W,超声波功率为600-1200W。
9.根据权利要求4所述的制备方法,其特征在于,所述保温反应温度为60-90℃,时间为15~30min。
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