CN113209995A - 一种提高CdS微米管光催化性能的处理方法 - Google Patents
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Abstract
本发明公开了一种提高CdS微米管光催化性能的处理方法,包括以下步骤:1)在烧杯中加入硫氰酸钾和四水合硝酸镉,搅拌均匀后转移到马弗炉中煅烧,之后自然冷却至室温,离心、洗涤、干燥,产物即为CdS;2)在烧杯中加入无水乙醇,搅拌条件下,加入步骤1)所得的CdS,以及NH4F,搅拌;3)将步骤2)所得混合液转移至聚四氟乙烯内衬高压釜中,恒温水热反应,之后自然冷却至室温,离心、洗涤、干燥,产物即为F‑CdS。本发明的处理方法简单易行、成本低廉、重现性好,相较于未处理的CdS,经过氟化处理的F‑CdS在可见光下能够实现光催化性能的提高。
Description
技术领域
本发明属于半导体光催化技术领域,具体涉及一种提高CdS微米管光催化性能的处理方法。
背景技术
进入21世纪,人类面临着能源和环境两个非常严峻的问题,特别是有毒且难降解有机污染物(如多环芳烃、多氯联苯、农药、染料等)引起的环境问题,已成为影响人类生存与健康的重大问题。利用半导体材料在太阳光照射下表面能受激活化的特性,可有效地氧化分解有机污染物。与传统的净化环境处理方法相比,半导体光催化技术拥有反应条件温和、无二次污染、操作简单和降解效果显著等优势。硫化镉由于其具有合适的禁带宽度(2.4eV)和较负的导带位置,吸引了研究者的关注。在已有的报道中,潘军等人报道了一种纳米花状硫化镉作为光催化剂(申请公告号:CN 1070743124 B),但是硫化镉相较于广泛商用的二氧化钛,性能仍有差距。
发明内容
针对现有技术的不足,本发明的目的是提供一种提高CdS微米管光催化性能的处理方法,本发明采用简单氟化处理大幅提高硫化镉的光催化性能,该处理方法简单易行、成本低廉,同时适用于其他催化剂,具有良好的应用前景。
本发明解决其技术问题采用的技术方案是:
一种提高CdS微米管光催化性能的处理方法,包括以下步骤:
1)在烧杯中加入硫氰酸钾和四水合硝酸镉,搅拌均匀后转移到马弗炉中煅烧,之后自然冷却至室温,离心、洗涤、干燥,产物即为CdS;
2)在烧杯中加入无水乙醇,搅拌条件下,加入步骤1)所得的CdS,以及NH4F,搅拌;
3)将步骤2)所得混合液转移至聚四氟乙烯内衬高压釜中,恒温水热反应,之后自然冷却至室温,离心、洗涤、干燥,产物即为F-CdS。
作为本申请的优选技术方案,所述步骤2)中,CdS和NH4F的摩尔比为1:0.5~5。
作为本申请的优选技术方案,所述步骤2)中,CdS与无水乙醇的比例为1:20mol/L。
作为本申请的优选技术方案,所述步骤1)中,硫氰酸钾和四水合硝酸镉的质量比为10:1。
作为本申请的优选技术方案,所述步骤1)中,煅烧温度为300℃,煅烧时间为2小时。
作为本申请的优选技术方案,所述步骤2)中,搅拌时间为30分钟。
作为本申请的优选技术方案,所述步骤3)中,恒温水热反应温度为170℃,反应时间为6小时。
有益效果:
本发明的处理方法简单易行、成本低廉、重现性好,相较于未处理的CdS,经过氟化处理的F-CdS在可见光下能够实现光催化性能的提高。
附图说明
图1是实施例1的CdS和实施例2的F-CdS光催化剂的X射线衍射图;
图2是实施例1的CdS光催化剂的扫描电子显微镜图(图中的标尺是10μm);
图3是实施例2的F-CdS光催化剂的扫描电子显微镜图(图中的标尺是5μm);
图4是实施例1的CdS和实施例2的F-CdS光催化剂在可见光(λ>420nm)下降解RhB的性能对比图。
具体实施方式
以下结合实施例对本发明做进一步详细说明。所用试剂或者仪器设备未注明生产厂商的,均视为可以通过市场购买的常规产品。
实施例1
室温下,将40g硫氰酸钾和4g四水合硝酸镉加入烧杯中,搅拌均匀后转移至马弗炉中,300℃煅烧反应2小时后,自然冷却至室温,离心、洗涤、干燥,产物即为CdS。
实施例2
同实施例1,与实施例1不同的是,得到CdS后继续进行以下操作:在烧杯中加入20mL无水乙醇,搅拌条件下,加入1mmolCdS和1mmolNH4F;将所得混合液转移至聚四氟乙烯内衬高压釜中,170℃恒温水热反应6小时后,自然冷却至室温,离心、洗涤、干燥,产物即为F-CdS。
实施例3
同实施例2,与实施例2不同的是,加入的是1mmolCdS和5mmolNH4F。
实施例4
同实施例2,与实施例2不同的是,加入的是1mmolCdS和0.5mmolNH4F。
对实施例1和实施例2的产品进行XRD和SEM表征。
由图1可见,实施例1的CdS和实施例2的F-CdS与CdS标准卡(JCPDS:77-2306)一致,因此实施例1制备的产品为纯相的CdS,并且氟化处理之后,实施例2的产品仍然为纯相的CdS。
图2为实施例1的CdS光催化剂的扫描电子显微镜(SEM)图,由图2可见,实施例1的CdS光催化剂形貌为中空纳米管,纳米管直径为1000-1200nm左右,长度为5-6μm左右。
图3为实施例2的F-CdS光催化剂的扫描电子显微镜(SEM)图,由图3可见,实施例2氟处理CdS后,F-CdS仍然保持中空纳米管形貌,纳米管直径为1000-1200nm左右,长度为5-6μm左右。
测试实施例1~2:
分别将实施例1的CdS光催化剂、实施例2的F-CdS光催化剂,降解含有RhB的废水溶液(RhB中文名称:罗丹明B,分子式:C28H31ClN2O3,分子量:479.01)。
过程如下:
称取实施例1和实施例2的样品各0.05g,分别加入200mL RhB水溶液,其中RhB浓度都为7.5mg/L,先避光搅拌30min,使染料在催化剂表面达到吸附/脱附平衡。然后开启装有420nm滤光片的氙灯光源在可见光光照射下进行光催化反应,上清液用分光光度计检测。
根据Lambert–Beer定律,有机物特征吸收峰强度的变化,可以定量计算其浓度变化。当吸光物质相同、厚度相同时,可以用吸光度的变化直接表示溶液浓度的变化。因为RhB在554nm处有一个特征吸收峰,所以可以利用吸光度的变化来衡量溶液中RhB的浓度变化。
从图4(横坐标:紫外光照射时间;纵坐标:经过可见光照射一段时间后测量的RhB浓度值与RhB的初始浓度的比值)可以看出,经过紫外光照射90分钟后,通过氟处理CdS得到的F-CdS光催化剂,相较于未处理过的CdS,催化活性提高了1.8倍,性能提高原因可能是通过F处理实现了表面改性和F离子掺杂。
以上所述仅针对本发明的优选实施例进行举例说明,并非对本发明做任何形式上的限制。本发明的保护内容不局限于以上实施例。在不背离发明构思的精神和范围下,本领域技术人员能够想到的变化和优点都被包括在本发明中,并且以所附的权利要求为保护范围。
Claims (7)
1.一种提高CdS微米管光催化性能的处理方法,其特征在于:包括以下步骤:
1)在烧杯中加入硫氰酸钾和四水合硝酸镉,搅拌均匀后转移到马弗炉中煅烧,之后自然冷却至室温,离心、洗涤、干燥,产物即为CdS;
2)在烧杯中加入无水乙醇,搅拌条件下,加入步骤1)所得的CdS,以及NH4F,搅拌;
3)将步骤2)所得混合液转移至聚四氟乙烯内衬高压釜中,恒温水热反应,之后自然冷却至室温,离心、洗涤、干燥,产物即为F-CdS。
2.根据权利要求1所述的一种提高CdS微米管光催化性能的处理方法,其特征在于:所述步骤2)中,CdS和NH4F的摩尔比为1:0.5~5。
3.根据权利要求1所述的一种提高CdS微米管光催化性能的处理方法,其特征在于:所述步骤2)中,CdS与无水乙醇的比例为1:20mol/L。
4.根据权利要求1所述的一种提高CdS微米管光催化性能的处理方法,其特征在于:所述步骤1)中,硫氰酸钾和四水合硝酸镉的质量比为10:1。
5.根据权利要求1所述的一种提高CdS微米管光催化性能的处理方法,其特征在于:所述步骤1)中,煅烧温度为300℃,煅烧时间为2小时。
6.根据权利要求1所述的一种提高CdS微米管光催化性能的处理方法,其特征在于:所述步骤2)中,搅拌时间为30分钟。
7.根据权利要求1所述的一种提高CdS微米管光催化性能的处理方法,其特征在于:所述步骤3)中,恒温水热反应温度为170℃,反应时间为6小时。
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CN106311288A (zh) * | 2016-07-26 | 2017-01-11 | 南京信息工程大学 | 一种新型Bi7F11O5/BiOCl复合光催化剂的简易制备方法及其光催化性能 |
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