CN105688898A - 光辐射下利用荧光碳点制备纳米银光催化剂的方法及应用 - Google Patents
光辐射下利用荧光碳点制备纳米银光催化剂的方法及应用 Download PDFInfo
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Abstract
光辐射下利用荧光碳点制备纳米银光催化剂的方法及应用,涉及一种制备催化剂的方法及应用,本发明通过热分解技术,先以抗坏血酸和尿素为反应物制备了荧光碳点。将制备的荧光碳点超声分散于水中,其在水中的质量浓度为0.0005 0.005wt%。向该荧光碳点水溶液中加入一定浓度的硝酸银溶液,其中,硝酸银溶液的摩尔浓度为0.0002 0.001摩尔每升。在可见光辐射下反应15 60分钟,可以制备出高催化效率的纳米银光催化剂。该纳米银光催化剂粒径小,单分散性良好,可见光辐射下,对水体中模拟污染物亚甲基蓝具有很高的光催化降解效率。催化剂在光催化降解有机染料中应用。本发明合成时间短、效率高,有很大的工业化生产前景。
Description
技术领域
本发明涉及一种制备催化剂的方法及应用,特别是涉及一种光辐射下利用荧光碳点制备纳米银光催化剂的方法及应用。
背景技术
荧光碳点是一种新型的小尺寸碳纳米材料,具有良好的水溶性,高稳定性,低毒性和良好的生物相容性。碳点具有优异的上下转换发光性质,而且可以作为光诱导的电子受体或电子供体,具有光生电子转移的特性。它们不仅可以作为一种高效光催化剂用于有机合成高选择性氧化,也可在光催化剂设计中作为一个多功能组分来促进更宽光谱响应的电子−空穴的产生和分离。
目前世界上各个国家都在积极推进节能减排,来应对日益突出的能源和环境问题。工业污染物的排放严重威胁着人类的进一步发展,特别是一些有机污染物毒性大、可生化性差,很难被微生物降解,活性炭吸附、膜分离、混凝等物化法处理工艺仅仅是将污染物分离转移,不能实现真正降解。光催化氧化技术可以将有机污染物高效、彻底降解,被誉为最有希望解决能源危机和环境污染的技术之一。光催化氧化技术的关键是光催化剂,常见的光催化剂如TiO2、ZnO、CdS等难以实现可见光响应的高效催化。解决光催化剂的可见光响应活性是实现可见光催化降解有机污染物的根本前提。
本发明利用水热合成技术制备了发光性能优异的荧光碳点,利用荧光碳点的光生电子转移特性,通过光化学反应合成策略,诱导荧光碳点的光生电子还原硝酸银成功制备出了可见光响应的纳米银光催化剂。以亚甲基蓝为模拟处理对象,以制备的纳米银为光催化剂,在过氧化氢协同作用下,可以实现亚甲基蓝可见光响应的高效降解。
发明内容
本发明的目的在于提供一种光辐射下利用荧光碳点制备纳米银光催化剂的方法及应用,本发明利用荧光碳点光化学反应特性还原硝酸银制备纳米银光催化剂的方法,利用该方法制备的纳米银光催化剂在可见光辐射下可以高效降解模拟污染物亚甲基蓝;制备的纳米银光催化剂在光催化降解有机染料中应用。
本发明的目的是通过以下技术方案实现的:
光辐射下利用荧光碳点制备纳米银光催化剂的方法,所述方法包括以下制备过程:
步骤1:荧光碳点的制备
采用热分解法制备荧光碳点,称取2.0克抗坏血酸和1.0克尿素溶解在20毫升蒸馏水中,然后将此溶液放进烘箱中于150℃反应2小时得到棕黄色泡沫状固体反应物,自然冷却后,研磨得到荧光碳点粉末;
步骤2 :利用荧光碳点光诱导反应制备纳米银光催化剂
称取步骤1 制备的荧光碳点粉末,加入100毫升去离子水并超声分散30分钟得到荧光碳点水溶液;室温磁力搅拌下向该荧光碳点水溶液中加入0.10摩尔每升的硝酸银溶液,继续搅拌20分钟后,以300瓦卤钨灯可见光照射下反应15−60分钟,将所得产物离心,并用蒸馏水和无水乙醇洗涤,室温下自然干燥后得到纳米银光催化剂。
所述的光辐射下利用荧光碳点制备纳米银光催化剂的方法,所述步骤2中,纳米银光催化剂的制备是以荧光碳点光诱导电子转移还原硝酸银生成纳米银为特征。
所述的光辐射下利用荧光碳点制备纳米银光催化剂的方法,所述步骤2中,荧光碳点的质量浓度为0.0005−0.005 wt%。
所述的光辐射下利用荧光碳点制备纳米银光催化剂的方法,所述步骤2中,硝酸银的摩尔浓度为0.0002−0.001摩尔每升。
所述的光辐射下利用荧光碳点制备纳米银光催化剂的方法,所述的步骤2中,光照反应时间为15−60分钟。
光辐射下利用荧光碳点制备纳米银光催化剂的应用,其特征在于,利用荧光碳点光诱导反应制备的纳米银光催化剂在光催化降解有机染料中应用。
本发明的优点与效果是:
1.本发明所述利用荧光碳点的光诱导电子转移特性制备纳米银光催化剂的方法简单有效,反应条件温和且环境友好。
2.制备的纳米银光催化剂在有效抑制光生电子−空穴的复合率的同时宽化了其对可见光谱的利用范围,与传统方法制备的纳米银光催化材料相比可见光催化活性明显提高。
附图说明
图1:碳点水溶液在不同波长光激发下的下转换荧光光谱图;
图2:碳点水溶液在不同波长光激发下的上转换荧光光谱图;
图3:制备的纳米银光催化剂的透射电镜照片(对应实施例1产物);
图4:制备的纳米银光催化剂去除水体中染料亚甲基蓝的降解曲线(对应实施例1产物)。
具体实施方式
下面结合实施例对本发明进行详细说明。
实施例1
称取制备的荧光碳点粉末100毫克,加入100毫升去离子水并超声分散30分钟,室温磁力搅拌下加入500微升0.10摩尔每升的硝酸银溶液,继续搅拌20分钟后,以300瓦卤钨灯可见光照射下反应30分钟,将所得产物离心,并用蒸馏水和无水乙醇洗涤,室温下自然干燥后得到纳米银光催化剂。
光催化降解亚甲基蓝溶液实验:
将实施例1制备得到的纳米银光催化剂的催化效果进行了测试。以亚甲基蓝为模拟污染物,室温下,30毫克纳米银光催化剂加入到100毫升 10毫克每升的亚甲基蓝溶液中,搅拌30分钟。然后加入500微升30% 的H2O2,以300瓦的卤钨灯为光源光照,定时取样通过紫外−可见分光光度计测量亚甲基蓝溶液的吸光度值变化。
降解率通过公式:降解率=×100%计算,式中:A0为亚甲基蓝溶液起始吸光度,A为t时刻亚甲基蓝溶液吸光度。
图1为制备的荧光碳点水溶液在不同激发波长下的下转换荧光光谱图。碳点溶液具有荧光激发依赖性,激发波长在320−420纳米范围内,随着激发光波长增加,荧光发射强度先增强后降低,并且最大发射波长峰位红移。
图2是制备的荧光碳点水溶液在不同激发波长下的上转换荧光光谱图。由图可见,在700−850纳米的激发波长范围,荧光碳点具有优异的上转换发光性能,使其可以应用于高性能光催化剂的设计。
图3 为实施例1制备的纳米银光催化剂的透射电镜照片。从图中可以看出,制备的纳米银光催化剂单分散性好,粒径大约在20−40纳米。
图4 为所制备的纳米银光催化剂在过氧化氢存在下去除水体中亚甲基蓝的降解曲线。从降解曲线可以明显看出制备的纳米银光催化剂对水体中亚甲基蓝 具有较高的降解效率,60分钟内降解率可以达到99%。
实施例2
称取制备的荧光碳点粉末100毫克,加入100毫升去离子水并超声分散30分钟,室温磁力搅拌下加入500微升0.10摩尔每升的硝酸银溶液,继续搅拌20分钟后,以300瓦卤钨灯可见光照射下反应15分钟,将所得产物离心,并用蒸馏水和无水乙醇洗涤,室温下自然干燥后得到纳米银光催化剂。
实施例3
称取制备的荧光碳点粉末50毫克,加入100毫升去离子水并超声分散30分钟,室温磁力搅拌下加入200微升的0.10摩尔每升的硝酸银溶液,继续搅拌20分钟后,以300瓦卤钨灯可见光照射下反应60分钟,将所得产物离心,并用蒸馏水和无水乙醇洗涤,室温下自然干燥后得到纳米银光催化剂。
实施例4
称取制备的荧光碳点粉末500毫克,加入100毫升去离子水并超声分散30分钟,室温磁力搅拌下加入1000微升0.10摩尔每升的硝酸银溶液,继续搅拌20分钟后,以300瓦卤钨灯可见光照射下反应30分钟,将所得产物离心,并用蒸馏水和无水乙醇洗涤,室温下自然干燥后得到纳米银光催化剂。
Claims (6)
1.光辐射下利用荧光碳点制备纳米银光催化剂的方法,其特征在于,所述方法包括以下制备过程:
步骤1:荧光碳点的制备
采用热分解法制备荧光碳点,称取2.0克抗坏血酸和1.0克尿素溶解在20毫升蒸馏水中,然后将此溶液放进烘箱中于150℃反应2小时得到棕黄色泡沫状固体反应物,自然冷却后,研磨得到荧光碳点粉末;
步骤2 :利用荧光碳点光诱导反应制备纳米银光催化剂
称取步骤1 制备的荧光碳点粉末,加入100毫升去离子水并超声分散30分钟得到荧光碳点水溶液;室温磁力搅拌下向该荧光碳点水溶液中加入0.10摩尔每升的硝酸银溶液,继续搅拌20分钟后,以300瓦卤钨灯可见光照射下反应15−60分钟,将所得产物离心,并用蒸馏水和无水乙醇洗涤,室温下自然干燥后得到纳米银光催化剂。
2.根据权利要求1所述的光辐射下利用荧光碳点制备纳米银光催化剂的方法,其特征在于,所述步骤2中,纳米银光催化剂的制备是以荧光碳点光诱导电子转移还原硝酸银生成纳米银为特征。
3.根据权利要求1所述的光辐射下利用荧光碳点制备纳米银光催化剂的方法,其特征在于,所述步骤2中,荧光碳点的质量浓度为0.0005−0.005 wt%。
4.根据权利要求1所述的光辐射下利用荧光碳点制备纳米银光催化剂的方法,其特征在于,所述步骤2中,硝酸银的摩尔浓度为0.0002−0.001摩尔每升。
5.根据权利要求1所述的光辐射下利用荧光碳点制备纳米银光催化剂的方法,其特征在于,所述的步骤2中,光照反应时间为15−60分钟。
6.光辐射下利用荧光碳点制备纳米银光催化剂的应用,其特征在于,利用荧光碳点光诱导反应制备的纳米银光催化剂在光催化降解有机染料中应用。
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