CN113181965B - 一种纳米纤维素负载氯氧铋复合光催化剂的制备方法及其应用 - Google Patents
一种纳米纤维素负载氯氧铋复合光催化剂的制备方法及其应用 Download PDFInfo
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Abstract
本发明申请属于无机合成技术领域,具体公开了一种纳米纤维素负载氯氧铋复合光催化剂的制备方法及其应用,包括以下步骤:(1)向H2SO4溶液中加入微晶纤维素搅拌,待微晶纤维素完全溶解后为黄色溶液,然后加入相比H2SO4溶液6‑8倍体积的超纯水淬灭上述反应,得到分层悬液;将悬液进行离心、透析、超声,得到纳米纤维素悬液;(2)将步骤(1)中的纳米纤维素悬液分散在超纯水中,加入KCl;将Bi(NO3)3·5H2O溶于乙二醇超声分散至透明溶液加至KCl溶液中得到固相产物,将所得产物经离心、洗涤、真空干燥得到纳米纤维素负载氯氧铋复合光催化剂。本发明是为了解决现有光催剂应用于有机染料降解的可见光光催化效率低、催化剂难回收等问题。
Description
技术领域
本发明属于无机合成技术领域,具体公开了一种纳米纤维素负载氯氧铋复合光催化剂的制备方法及其应用。
背景技术
随着全球工业化和现代化进程的加速,水污染已经严重危及人类健康,其中印染工业产生的废水已经成为当前最重要的水体污染源之一,急需开发高效的污水净化技术来缓解人类面临的日益严峻的环境问题。半导体光催化技术是近年来最有效和发展最快的催化技术之一,能够高效解决能源和环境问题,如空气净化,产氢,抗菌活性和有机染料的降解。
传统半导体光催化技术已经取得丰硕的理论成果,但将半导体催化技术全面推广至有机染料降解上,还是存在很多问题。多数光催化剂没有合适的禁带宽度,对太阳光的利用率较低,且有些半导体催化剂的光生电子和空穴的复合率很高,极大地限制了其实际应用。复合半导体材料虽然在一定程度抑制电子和空穴的复合,但也会降低其氧化还原能力,不利于染料降解。因此现有技术中光催剂应用于有机染料降解的可见光光催化效率低,催化剂不易回收等问题使得处理染料废水的成本提高。
发明内容
本发明的目的在于提供一种纳米纤维素负载氯氧铋复合光催化剂的制备方法及其应用,以解决现有光催剂应用于有机染料降解的可见光光催化效率低,催化剂难回收等问题。
为了达到上述目的,本发明的技术方案为:
(1)向质量分数为56%~65%的H2SO4溶液中加入微晶纤维素,置于40~50℃水浴搅拌,待微晶纤维素完全溶解后为黄色溶液,然后加入相比H2SO4溶液6-8倍体积的超纯水淬灭上述反应,得到分层悬液;将悬液进行离心、透析至中性,再经过超声得到均一的纳米纤维素悬液;
(2)将步骤(1)中的纳米纤维素悬液分散在超纯水中,然后加入KCl超声溶解;将Bi(NO3)3·5H2O溶于乙二醇超声分散至透明溶液,将该溶液滴加至KCl溶液中,搅拌10~15h得固相产物,将所得固相产物经离心、洗涤、真空干燥后得到纳米纤维素负载氯氧铋复合光催化剂
进一步,步骤(1)中硫酸溶液的质量分数为64%。
进一步,步骤(1)中水浴温度为45℃。
进一步,步骤(1)中加入相比H2SO4溶液7倍体积的超纯水淬灭反应。
进一步,步骤(1)中用超纯水离心洗至不再分层。
进一步,步骤(2)中纳米纤维素悬液与超纯水的体积比为1∶1。
进一步,步骤(2)中所用KCl与Bi(NO3)3·5H2O的摩尔比为1∶1;步骤(2)中固相产物分别采用超纯水和无水乙醇各洗涤3次。
进一步,步骤(2)中固相产物的干燥温度为60℃,时间为8h。
进一步,制备的纳米纤维素负载氯氧铋复合光催化剂应用于降解有机染料。将本方案制备得到的纳米纤维素负载氯氧铋复合光催化剂应用于降解有机染料:量取50mL已经配好的20mg/L的罗丹明B溶液于石英烧杯中,用电子天平准确称取5mg催化剂,加入到罗丹明B溶液中,暗处搅拌30min使之吸附-脱附平衡;将混合液移到300W氙灯下进行光催化降解实验,每间隔10min取4mL罗丹明B溶液,离心分离取上层清液测紫外。
本技术方案的有益效果在于:
(1)本发明通过简单的原位合成的方法制备出纳米纤维素负载氯氧铋复合材料,该方法具有简单、节能、高效等多种优点;
(2)本发明是将氯氧铋和纳米纤维素进行有机结合,[Bi2O2]2+层与双卤层交替形成的层状结构具有足够的空间来极化相应的原子和原子轨道,有效分离光生电子和空穴,纳米纤维素具有比表面积大、高结晶度和生物相容性优点,融合二者的优点使得复合材料具有高吸附性、高催化活性及稳定的重复使用性等优点;
(3)制备出的纳米纤维素负载氯氧铋复合光催化剂材料的微观形貌为立体交叉的薄层片状,比表面积增大,在降解过程中与污染物的接触面积增大,利于提高催化活性。
附图说明
图1是不同光催化剂的XRD图;
图2是氯氧铋光催化剂的扫描电镜图;
图3是本实施例得到的纳米纤维素负载氯氧铋复合光催化剂的扫描电镜图;
图4是本实施例得到的纳米纤维素负载氯氧铋复合光催化剂的透射电镜图;
图5是不同光催化体系中罗丹明B的降解效率图;
图6是本实施例得到的纳米纤维素负载氯氧铋复合光催化剂降解罗丹明B的循环稳定性图;
图7是本实施例得到的复合光催化剂对罗丹明B降解的自由基捕获实验图;
图8是本实施例得到的复合光催化剂在自然光下对罗丹明B的降解效率图。
具体实施方式
下面通过具体实施方式进一步详细说明:
实施例如下所示,纳米纤维素负载氯氧铋复合光催化剂的制备方法按下列步骤实施:
(1)向质量分数为56%~65%的H2SO4溶液中加入微晶纤维素,置于40~50℃水浴搅拌,待完全溶为黄色溶液,然后加入相比H2SO4溶液6-8倍体积的超纯水淬灭上述反应,得到分层悬液;将悬液进行离心、透析至中性,再经过超声得到均一的纳米纤维素悬液;
(2)将纳米纤维素悬液分散在超纯水中,然后加入KCl超声溶解;将Bi(NO3)3·5H2O溶于乙二醇超声分散至透明溶液,将该溶液滴加至KCl溶液中,搅拌10~15h,所得固相产物经离心、洗涤、真空干燥后得到纳米纤维素负载氯氧铋复合光催化剂;
本实施例的步骤(1)中硫酸浓度优选为64%;
本实施例的步骤(1)中水浴温度优选为45℃;
本实施例的步骤(1)中加入相比H2SO4溶液7倍体积的超纯水淬灭反应;
本实施例的步骤(1)中用超纯水离心洗至不再分层为止;
本实施例的步骤(2)中所用将纳米纤维素悬液和超纯水的体积比优选为1∶1;
本实施例的步骤(2)中固相产物分别采用超纯水和无水乙醇各洗涤3次;
本实施例的步骤(2)中固相产物的干燥温度优选为60℃,时间优选为8h;
本实施例中所得到的纳米纤维素负载氯氧铋复合光催化剂作为光催化剂应用于降解罗丹明B。将本发明制备得到的纳米纤维素负载氯氧铋复合光催化剂应用于降解有机染料:量取50mL已经配好的20mg/L的罗丹明B溶液于石英烧杯中,用电子天平准确称取5mg催化剂,加入到罗丹明B溶液中,暗处搅拌30min使之吸附-脱附平衡;将混合液移到300W氙灯下进行光催化降解实验,每间隔10min取4mL罗丹明B溶液,离心分离取上层清液测紫外。
图1是不同光催化剂的XRD图,本发明得到的纳米纤维素负载氯氧铋光催化剂晶型良好,将其与氯氧铋及纳米纤维素标准卡对比,可以看出氯氧铋成功负载到纳米纤维素上,表明氯氧铋与纳米纤维素有良好的兼容性;
图2是区别于实施例步骤(2)中将KCl加入到超纯水中溶解,其它步骤及参数与步骤(1)、(2)相同,得到的氯氧铋光催化剂的扫描电镜图,可以看出氯氧铋形貌为表面较为平整的片状结构;
图3是本实施例得到的纳米纤维素负载氯氧铋复合光催化剂的扫描电镜图,与氯氧铋相比,其形貌变为立体交叉的薄层片状,这样的结构使其比表面增大,在降解过程中可以吸收更多的活性物质,有利于催化污染物的降解;
图4是本实施例得到的纳米纤维素负载氯氧铋复合光催化剂的透射电镜图,从图中可以看出纳米尺寸的氯氧铋负载于纳米纤维素上,没有出现聚集现象;
图5是不同光催化体系中罗丹明B的降解效率图,在黑暗条件下,本发明得到的纳米纤维素负载氯氧铋对罗丹明B的吸附最强,在可见光下,该复合光催化剂在30min内对罗丹明B的降解率约为99%;
图6是本实施例得到的纳米纤维素负载氯氧铋复合光催化剂降解罗丹明B的循环稳定性图,催化剂在循环催化4次之后降解率约70%;
图7是本实施例得到的复合光催化剂对罗丹明B降解的自由基捕获实验图,加入异丙醇捕获对反应没有影响,说明·OH不是该降解反应的活性物种;然而加入对苯醌、EDTA、AgNO3,降解效果明显下降,因此本发明中的光催化降解主要的活性物种为·O2 -、h+和e-;
图8本实施例得到的复合光催化剂在自然光下对罗丹明B的降解效率图,光照40min降解率达到98%以上,因此本发明制得的催化剂在自然光下也具有优异的催化性能。
以上所述的仅是本发明的实施例,方案中公知的具体结构及特性等常识在此未作过多描述。应当指出,对于本领域的技术人员来说,在不脱离本发明结构的前提下,还可以作出若干变形和改进,这些也应该视为本发明的保护范围,这些都不会影响本发明实施的效果和专利的实用性。
Claims (8)
1.纳米纤维素负载氯氧铋复合光催化剂的制备方法,其特征在于,包括以下步骤:
(1)向质量分数为56%~65%的H2SO4溶液中加入微晶纤维素,置于40~50℃水浴搅拌,待微晶纤维素完全溶解后为黄色溶液,然后加入相比H2SO4溶液6-8倍体积的超纯水淬灭上述反应,得到分层悬液;将悬液进行离心、透析至中性,再经过超声得到均一的纳米纤维素悬液;
(2)将步骤(1)中的纳米纤维素悬液分散在超纯水中,然后加入KCl超声溶解;将Bi(NO3)3·5H2O溶于乙二醇超声分散至透明溶液,所用Bi(NO3)3·5H2O与KCl的摩尔比为1:1,然后将该溶液滴加至KCl溶液中,搅拌10~15h得固相产物;将该固相产物分别经过离心、超纯水和无水乙醇各洗涤3次、真空干燥后得到纳米纤维素负载氯氧铋复合光催化剂。
2.根据权利要求1所述的纳米纤维素负载氯氧铋复合光催化剂的制备方法,其特征在于,步骤(1)中硫酸溶液的质量分数为64%。
3.根据权利要求1所述的纳米纤维素负载氯氧铋复合光催化剂的制备方法,其特征在于,步骤(1)中水浴温度为45℃。
4.根据权利要求1所述的纳米纤维素负载氯氧铋复合光催化剂的制备方法,其特征在于,步骤(1)中加入相比H2SO4溶液7倍体积的超纯水淬灭反应。
5.根据权利要求1所述的纳米纤维素负载氯氧铋复合光催化剂的制备方法,其特征在于,步骤(1)中用超纯水离心洗至不再分层。
6.根据权利要求1所述的纳米纤维素负载氯氧铋复合光催化剂的制备方法,其特征在于,步骤(2)中纳米纤维素悬液与超纯水的体积比为1:1。
7.根据权利要求1所述的纳米纤维素负载氯氧铋复合光催化剂的制备方法,其特征在于,步骤(2)中固相产物的干燥温度为60℃,时间为8h。
8.根据权利要求1所述制备方法制备的纳米纤维素负载氯氧铋复合光催化剂应用于降解有机染料。
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