CN108636457A - 一种可用于光催化剂的APTES-Sb2WO6-GQDs复合材料的制备方法 - Google Patents
一种可用于光催化剂的APTES-Sb2WO6-GQDs复合材料的制备方法 Download PDFInfo
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Abstract
本发明涉及一种可用于光催化剂的3‑氨丙基三乙氧基硅烷(APTES)‑Sb2WO6‑石墨烯量子点(GQDs)复合材料的制备方法。包括以下步骤:制备Sb2WO6、用APTES修饰Sb2WO6、制备GQDs、制备APTES‑Sb2WO6‑GQDs复合材料光催化剂、将APTES‑Sb2WO6‑GQDs复合材料光催化剂应用于水体污染物甲基橙的光催化降解。本发明的有益效果是:APTES‑Sb2WO6‑GQDs复合材料光催化剂对甲基橙的降解速率较快且易于重复利用。
Description
技术领域
本发明涉及一种可用于光催化剂的3-氨丙基三乙氧基硅烷(APTES)-Sb2WO6-石墨烯量子点(GQDs)复合材料的制备方法,属于水处理和材料合成领域。
技术背景
由于环境污染日益严重,化石燃料储备逐渐枯竭,可再生能源的研究及环境修复技术的发展变得更加重要和紧迫。当前世界的快速工业化,使得有机污染物成为了主要水体污染物之一。为了高效降解这些污染物,科研工作者们开始尝试将光催化技术应用到水处理领域,从而缓解环境和能源问题。光催化使用清洁的光能作为能量来源,可以将水体有机污染物无选择性矿化为二氧化碳和水,在水处理领域展现出巨大的优势。
甲基橙是一种偶氮染料,水溶液呈橙色,工业生产中若不加处理便排放到水体中,一方面会使有色水体阻碍水中植物吸收利用阳光,另一方面甲基橙本身有毒,这对被污染水体周边动植物的生存造成了严重的威胁。由于甲基橙是一种典型的持久性有机污染物,因此本发明以甲基橙作为目标降解物,具有一定的代表性。
为了寻求一种自身可以吸收绝大部分可见光波段的光催化剂,科研工作者们对大量的半导体进行了光催化方面的研究。但是,由于半导体材料种类繁多,很多半导体材料还尚未得到充分的研究。Sb2WO6就是其中一种研究较少的半导体材料。与Bi2WO6相似,Sb2WO6同样具有独特的奥里维里斯结构,并且由于[WO4]n层嵌入两个[Sb2O2]n层导致结构的扭曲。到目前为止,只发现了三种合成Sb2WO6的方法:水热法、固态反应以及溶剂热法。其中,固态反应的过程相当复杂,并且无法获得纯的Sb2WO6产品。水热法可以通过控制反应液的pH值来控制Sb2WO6的形貌,但是得到的粒子粒径分布范围宽(微米及以上级别)。最近,溶剂热法制备Sb2WO6取得了进展。在制备过程中,通过控制乙二醇和水的体积比来得到不同层次结构的Sb2WO6。并且通过溶剂热法制备的Sb2WO6产品也有纯度较高、粒径分布范围较窄等优点。Sb2WO6具有较强的可见光吸收能力,但目前对它的研究还较少。
石墨烯量子点(GQDs)作为一种新型碳材料,属于零维纳米材料。GQDs与石墨烯相同之处在于厚度约在0.4nm到2.0nm之间,通常为一至三层堆叠而成,差异在于平面大小的不同,前者小于100nm,而后者则在微米级以上,这种差异使得GQDs具有一些特殊的性能。由于内部电子在各方向上的运动均受到限制,所以GQDs的量子局域效应尤为明显,具有许多独特的物理和化学性质。这些性质使得GQDs在光催化领域具备了一定的应用前景。
发明内容
本发明的目的在于提供一种可用于光催化剂的APTES-Sb2WO6-GQDs复合材料的制备方法。
本发明所述一种可用于光催化剂的APTES-Sb2WO6-GQDs复合材料的制备方法,包括以下步骤:
a、制备Sb2WO6:在乙二醇和水的混合溶液中加入Na2WO4,搅拌均匀后继续添加SbCl3;将混合液转移至100mL水热反应釜中,180℃反应12h;将析出的黄色固体沉淀离心分离并用无水乙醇和超纯水交替洗涤各3次,放入烘箱烘干,得到Sb2WO6;
b、用APTES修饰Sb2WO6:将Sb2WO6溶于无水乙醇中,超声分散并逐滴加入APTES,在70℃条件下水浴保温4h;抽滤、烘干,得到APTES-Sb2WO6;
c、制备GQDs溶液:取适量一水合柠檬酸,研磨后加入坩埚中,在200℃条件下保温0.5h,反应结束后,加入一定量超纯水,超声使产物溶解。待产物充分溶解后,抽滤得黄色透明的GQDs溶液;
d、制备APTES-Sb2WO6-GQDs复合材料光催化剂:称取步骤b制得的APTES-Sb2WO6和步骤c制得的GQDs溶液,将其分散在适量无水乙醇中,超声0.5h,于60℃条件下烘干,得到APTES-Sb2WO6-GQDs复合材料光催化剂;
e、APTES-Sb2WO6-GQDs复合材料光催化剂应用于降解水中的甲基橙:配制一定浓度的甲基橙溶液,用步骤d制得的APTES-Sb2WO6-GQDs复合材料光催化剂降解水中的甲基橙,同时使用紫外可见分光光度计检测甲基橙溶液的特征吸收峰强度,当特征吸收峰消失时,即说明溶液中的甲基橙降解完全,记录下降解所用时间。
进一步地,步骤a中乙二醇在混合溶液中所占比例为0.1~0.9,混合溶液总量为50~80mL,SbCl3用量为0.1~10g,Na2WO4用量为0.05~5g。
进一步地,步骤b中Sb2WO6用量为0.1~1g,无水乙醇用量为100~500mL,APTES用量为0.1~5mL。
进一步地,步骤c中一水合柠檬酸用量为0.1~5g,超纯水用量为1~100mL。
进一步地,步骤d中APTES-Sb2WO6用量为0.01~1g,GQDs溶液用量为0.1~100mL,无水乙醇用量为0.1~100mL。
进一步地,步骤e中甲基橙溶液的浓度为1~100mg/L,APTES-Sb2WO6-GQDs复合材料光催化剂的浓度为0.01~1g/L,甲基橙的特征吸收峰在465nm处。
本发明的有益效果是:APTES-Sb2WO6-GQDs复合材料光催化剂的制备方法简单且对甲基橙的降解速率较快。
附图说明
下面结合附图对本实验进一步说明。
图1为实施例一中APTES-Sb2WO6-GQDs复合材料光催化剂的X射线衍射图;
图2为实施例一中APTES-Sb2WO6-GQDs复合材料光催化剂的紫外漫反射图;
图3为实施例一中APTES-Sb2WO6-GQDs复合材料光催化剂的透射电子显微镜图;
图4为实施例二中APTES-Sb2WO6-GQDs复合材料光催化剂应用于甲基橙降解的效果图;
图5为实施例三中不同的组分配比对复合材料光催化剂光催化效果的影响。
具体实施方式
现在结合具体实施例对本发明做进一步说明,以下实施例旨在说明本发明而不是对本发明的进一步限定。
在本发明的实施例中甲基橙溶液的脱色率是按下述方法计算的:配制一定浓度的甲基橙溶液,使用紫外-可见光分光光度计测量465nm处的吸光度,记为a0。在紫外降解过程中取样,使用紫外-可见光分光光度计测量465nm处的吸光度,记为an(n为取样次数)。脱色率bn由以下公式算出:
bn=1-an/a0(n=0,1,2······)
实施例一:
在乙二醇和水比例为3:1的80mL混合溶液中加入0.91g Na2WO4,搅拌均匀后继续添加0.66g SbCl3。将混合液转移至100mL水热反应釜中,180℃反应12h。将析出的黄色固体沉淀离心分离并用无水乙醇和超纯水交替洗涤各3次,放入烘箱烘干,得到Sb2WO6。将0.6gSb2WO6溶于300mL无水乙醇中,超声分散并逐滴加入2mL APTES。在70℃条件下水浴保温4h。抽滤、烘干,得到APTES-Sb2WO6。取2g一水合柠檬酸,研磨后加入坩埚中,在200℃条件下保温0.5h。反应结束后,加入10mL超纯水,超声使产物溶解。待产物充分溶解后,抽滤得黄色透明的GQDs溶液。称取0.2g APTES-Sb2WO6并将其分散在10mL无水乙醇中,加入5mL GQDs溶液,超声0.5h。于60℃条件下烘干,得到APTES-Sb2WO6-GQDs复合材料光催化剂。X射线衍射图谱如附图1所示,表明得到的反应产物为APTES-Sb2WO6-GQDs。固体紫外漫反射图谱如附图2所示,表明APTES-Sb2WO6-GQDs复合材料光催化剂对可见光具有良好的吸收能力。透射电子显微镜图如附图3所示,表明Sb2WO6与GQDs成功复合在一起。
实施例二:
配制浓度为6mg/L的甲基橙溶液500mL,称取实施例一制备的APTES-Sb2WO6-GQDs复合材料光催化剂0.05g,在功率为11W的紫外灯照射下降解水中的甲基橙,每一小时取样一次,使用紫外可见分光光度计检测甲基橙溶液的特征吸收峰强度,计算溶液脱色率。结果如附图4所示,紫外照射3h后脱色率为100%。
实施例三:
考察不同的组分配比对APTES-Sb2WO6-GQDs复合材料光催化剂光催化效果的影响。分别称取0.15g、0.2g、0.25g APTES-Sb2WO6,将其分散在10mL无水乙醇中,并加入5mL GQDs溶液,超声0.5h。于60℃条件下烘干,得到不同组分配比的APTES-Sb2WO6-GQDs复合材料光催化剂,分别标记为APTES-Sb2WO6-GQDs1、APTES-Sb2WO6-GQDs2和APTES-Sb2WO6-GQDs3。配制浓度为6mg/L甲基橙溶液500mL,分别称取0.05g上述APTES-Sb2WO6-GQDs样品,在功率为11W的紫外灯照射下降解水中的甲基橙,每一小时取样一次,使用紫外可见分光光度计检测甲基橙溶液的特征吸收峰强度,计算溶液脱色率。结果如附图5所示,APTES-Sb2WO6-GQDs2复合材料光催化剂的光催化效果最佳。
Claims (6)
1.一种可用于光催化剂的APTES-Sb2WO6-GQDs复合材料的制备方法,步骤如下:
a、制备Sb2WO6:在乙二醇和水的混合溶液中加入Na2WO4,搅拌均匀后继续添加SbCl3,将混合液转移至100mL水热反应釜中,180℃反应12h,将析出的黄色固体沉淀离心分离并用无水乙醇和超纯水交替洗涤各3次,放入烘箱烘干,得到Sb2WO6;
b、用3-氨丙基三乙氧基硅烷(APTES)修饰Sb2WO6:将Sb2WO6溶于无水乙醇中,超声分散并逐滴加入APTES,在70℃条件下水浴保温4h,抽滤、烘干,得到APTES-Sb2WO6;
c、制备石墨烯量子点(GQDs)溶液:取适量一水合柠檬酸,研磨后加入坩埚中,在200℃条件下保温0.5h,反应结束后,加入一定量超纯水,超声使产物溶解,待产物充分溶解后,抽滤得黄色透明的GQDs溶液;
d、制备APTES-Sb2WO6-GQDs复合材料光催化剂:称取步骤b制得的APTES-Sb2WO6和步骤c制得的GQDs溶液,将其分散在适量无水乙醇中,超声0.5h,于60℃条件下烘干,得到APTES-Sb2WO6-GQDs复合材料光催化剂;
e、APTES-Sb2WO6-GQDs复合材料光催化剂应用于降解水中的甲基橙:配制一定浓度的甲基橙溶液,用步骤d制得的APTES-Sb2WO6-GQDs复合材料光催化剂降解水中的甲基橙,同时使用紫外可见分光光度计检测甲基橙溶液的特征吸收峰强度,当特征吸收峰消失时,即说明溶液中的甲基橙降解完全,记录下降解所用时间。
2.根据权利要求1所述一种可用于光催化剂的APTES-Sb2WO6-GQDs复合材料的制备方法,其特征是:所述步骤a中乙二醇在混合溶液中所占体积比为0.1~0.9,混合溶液总量为50~80mL,SbCl3用量为0.1~10g,Na2WO4用量为0.05~5g。
3.根据权利要求1所述一种可用于光催化剂的APTES-Sb2WO6-GQDs复合材料的制备方法,其特征是:所述步骤b中Sb2WO6用量为0.1~1g,无水乙醇用量为100~500mL,APTES用量为0.1~5mL。
4.根据权利要求1所述一种可用于光催化剂的APTES-Sb2WO6-GQDs复合材料的制备方法,其特征是:所述步骤c中一水合柠檬酸用量为0.1~5g,超纯水用量为1~100mL。
5.根据权利要求1所述一种可用于光催化剂的APTES-Sb2WO6-GQDs复合材料的制备方法,其特征是:所述步骤d中APTES-Sb2WO6用量为0.01~1g,GQDs溶液用量为0.1~100mL,无水乙醇用量为0.1~100mL。
6.根据权利要求1所述一种可用于光催化剂的APTES-Sb2WO6-GQDs复合材料的制备方法,其特征是:所述步骤e中甲基橙溶液的浓度为1~100mg/L,APTES-Sb2WO6-GQDs复合材料光催化剂的浓度为0.01~1g/L,甲基橙的特征吸收峰在465nm处。
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