CN108940261A - 一种整合同质结与异质结复合光催化剂的制备方法及用途 - Google Patents
一种整合同质结与异质结复合光催化剂的制备方法及用途 Download PDFInfo
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Abstract
本发明属于环境材料制备技术领域,具体提供了一种整合同质结与异质结复合光催化剂的制备方法及用途。步骤如下:步骤1、Bi3Ti4O12纳米片的制备;步骤2、量子点自掺杂Bi2MoO6/Bi3Ti4O12异质结复合光催化剂的制备。本发明所述的方法制备的量子点自掺杂Bi2MoO6/Bi3Ti4O12复合光催化剂具有较好的光催化活性和稳定性。
Description
技术领域
本发明属于环境材料制备技术领域,涉及一种整合同质结与异质结复合光催化剂的制备方法及用途,具体涉及一种利用钼酸铋(Bi2MoO6)量子点自掺杂Bi2MoO6修饰的钛酸铋(Bi3Ti4O12)异质结复合光催化剂的制备方法及用途。
背景技术
今年来,国际上对环境质量的恶化于生态平衡的失调十分关切,人类正面临着有史以来最严重的环境危机。在环境污染中,大部分直接与工业和工业产品的污染有关。染料废水是主要的有害工业废水之一,主要来源于染料及染料中间体生产行业。染料种类繁多,给人们的生活带来绚丽多彩的颜色并产生巨大经济效益,但也产生大量的染料废水排放到环境水体中,导致对自然水体的污染。其主要危害如下:
(1)染料的色度废水中的染料能吸收光线,降低水体的透明度,大量消耗水中的氧,造成水体缺氧,影响水生生物和微生物生长,破坏水体自净,同时易造成视觉上的污染。(2)染料是有机芳香族化合物苯环上的氢被卤素、硝基、胺基取代以后生成的芳香族卤化物、芳香族硝基化合物、芳香族胺类化学物、联苯等多苯环取代化合物,生物毒性都较大,有的还是“三致”物质。(3)染料中存在的重金属废水中的铬、铅、汞、砷、锌等重金属盐类无法生物降解,他们在自然环境中能长期存在,并且会通过食物链不断传递,在人体内积累。(4)废水中有机物含量高,成分复杂,有害物质含量高。一般的酸、碱、盐等物质和肥皂等洗涤剂虽然相对无害,但他们对环境仍有一定影响。近年来,许多含氮、磷的化合物大量用于洗净剂,尿素也常用于印染各道工序,使废水中总磷、总氮含量增高,排放后使水体富营养化。如果染料废水不加处理直接排放,将会对日益紧张的饮用水源造成极大的威胁。染料中较为常见的染料为罗丹明B(Rhodamine B)。罗丹明B是一种具有鲜桃红色的人工合成染料,经老鼠试验发现,罗丹明B会引致皮下组织生肉瘤,被怀疑是致癌物质,并在溶液中具有强烈的荧光,用作实验中细胞荧光染色剂、有色玻璃、特色烟花爆竹等行业。虽然染料给人类带来了色彩斑斓的生活,但其危害也不容小觑。因此,彻底根除环境中染料已经成为科研工作者迫切需要解决的重大问题。当前,染料的处理技术已经取得较大进展,并发展了诸多方法,如:物理法、化学法和生物法等,它们各具优点和特色。然而,利用这些传统方法处理染料废水,通常仍会有一定量的染料残留物排放到环境中,很难将其彻底根除,具有明显的局限性。
近年新兴的半导体光催化技术具有绿色、节能等优势,能够彻底降解染料污染物,可以补充传统处理方法的不足甚至取代传统方法。因此,利用光催化技术把难降解的染料污染物矿化分解为H2O、CO2和其他小分子物质,有望成为新的高效节能的环境污染治理技术,也是当今环境科学与技术领域研究热点。
Bi2MoO6作为一种新型光催化材料,化学性质稳定,无毒且具有合适的带隙(2.5-2.8eV)已经被广泛应用于光催化领域中,如Wang等报道通过两步沉积法制备了Z-型异质结光催化剂BiOBr-Bi2MoO6并用于降解罗丹明B(A plate-on-plate sandwiched Z-schemeheterojunction photocatalyst:BiOBr-Bi2MoO6with enhanced photocatalyticperformance.Applied Surface Science,2017,391,194-210.),以及Meng等(Integratingboth homojunction and heterojunction in QDs self-decorated Bi2MoO6/BCNcomposites to achieve an efficient photocatalyst for Cr(VI)reduction.ChemicalEngineering Journal,2018,334,334-343.)报道了量子点(Quantum Dot,QDs)自修饰Bi2MoO6形成单质结的同时与BCN结合形成异质结,整合同质结与异质结有利于电子-空穴对的分离,提高量子产率。所以,合成异质结是一种有效的提高光催化活性的方法。Bi3Ti4O12具有多种形貌,例如:纳米粒子、纳米点、介孔网装等,其中二维纳米薄片具有大的比表面积和较短的载流子传输距离,因而具有良好的光催化性能。利用Bi3Ti4O12修饰Bi2MoO6形成异质结可以进一步抑制载流子复合。目前,Bi3Ti4O12量子点自掺杂Bi2MoO6并且修饰Bi3Ti4O12形成异质结的还没有相关报道。
发明内容
本发明的目的是结合熔盐法与水热法的技术手段制备出Bi2MoO6量子点自掺杂Bi2MoO6/Bi3Ti4O12异质结复合光催化剂。
本发明是通过如下技术方案实现的:
利用熔盐法与水热法合成Bi2MoO6量子点自掺杂Bi2MoO6/Bi3Ti4O12异质结复合光催化剂,按照如下步骤进行:
步骤1、制备Bi3Ti4O12纳米薄片:
将Bi2O3与TiO2混合均匀后,得到混合物A;向混合物A中同时加入NaCl和KCl,然后用研钵将其研碎且混合均匀,得到混合物B;随后,将混合物B转移至管式炉中进行煅烧反应;待反应结束后降到室温,用去离子水、乙醇洗涤固体产物,干燥,得到Bi3Ti4O12纳米薄片。
步骤2、制备Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12异质结复合光催化剂:
将Bi(NO3)3·5H2O与Na2MoO4分别加入到含有乙二醇的烧杯中超声分散,分别得到混合液C和D;然后将混合溶液C和D混合在一起,搅拌均匀后加入乙醇,继续搅拌得到混合溶液E;随后,将步骤1中得到的Bi3Ti4O12纳米薄片加入到混合液E中搅拌均匀得到混合液F;最后,将混合溶液F转移至反应釜中进行恒温热反应;待反应结束后降到室温,洗涤,干燥,得到Bi2MoO6量子点自掺杂Bi2MoO6/Bi3Ti4O12异质结复合光催化剂,即一种整合同质结与异质结复合光催化剂。
步骤1中,所使用的Bi2O3:TiO2:NaCl:KCl=0.795g:0.102g:2.5g:3.18g。
步骤1中,所述的煅烧温度为800℃,煅烧反应的时间为2h,管式炉的升温速率为5℃/min。
步骤2中,所使用的Bi(NO3)3·5H2O:Na2MoO4:Bi3Ti4O12:乙二醇:乙醇=0.024g~0.10g:0.006g~0.0240g:0.2g:5mL:20mL。
步骤2中,所述的恒温热反应的温度为180℃,时间为24h。
步骤2中,所述洗涤为:先用去离子水、乙醇洗涤固体产物,干燥,再用乙醇洗涤沉淀物。
所制备的Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12异质结复合光催化剂,用于降解废水中的罗丹明B或MBT。
光催化活性评价:在DW-01型光化学反应仪(购自扬州大学教学仪器厂)中进行,可见光灯照射,将100ml罗丹明B或MBT模拟废水加入反应器中并测定其初始值,然后加入复合光催化剂,磁力搅拌并开启曝气装置通入空气保持催化剂处于悬浮或飘浮状态,光照过程中间隔10min取样分析,离心分离后取上层清液在分光光度计λmax=553nm或者320nm处测定吸光度,并通过公式:DR=[(A0-Ai)/A0]×100%算出降解率,其中A0为达到吸附平衡时罗丹明B或MBT溶液的吸光度,Ai为定时取样测定的罗丹明B或MBT溶液的吸光度。
本发明中所用的五水合硝酸铋,钼酸钠、乙二醇、乙醇等均为分析纯,购于国药化学试剂有限公司;罗丹明B或MBT为标品,购于上海顺勃生物工程有限公司。
本发明的有益效果为:
本发明实现了以Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12异质结作为光催化剂降解染料废水的目的。半导体材料作为光催化剂,可见光作为激发,通过与有机污染物分子的界面相互作用实现特殊的催化或转化效应,使周围的氧气及水分子激发成极具氧化力的自由负离子,从而达到降解环境中有害有机物质的目的,该方法不会造成资源浪费与附加污染的形成,且操作简便,是一种绿色环保的高效处理技术。
附图说明
图1为所制备样品的XRD图,分别为Bi3Ti4O12(A),5-Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12(B),10-Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12(C),15-Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12(D)和20-Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12(E);
图2为Bi3Ti4O12的TEM图(a)-(b),选取电子衍射(c)与Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12复合光催化剂的HRTEM图;
图3为Bi3Ti4O12(A),5-Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12(B),10-Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12(C),15-Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12(D)和20-Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12(E)复合光催化剂的固体紫外图。
具体实施方式
下面结合具体实施实例对本发明做进一步说明。
实施例1:
(1)Bi3Ti4O12纳米薄片的制备:
将0.795g Bi2O3与0.102g TiO2混合均匀;向混合物中同时加入2.5g NaCl和3.18gKCl,然后用研钵将其研碎且混合均匀;随后,将上述混合物转移至800℃管式炉中进行恒温热反应2h,升温速率为5℃/min;待反应结束后降到室温,用去离子水、乙醇洗涤固体产物,干燥,得到Bi3Ti4O12纳米薄片。
(2)Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12异质结复合光催化剂的制备:
将0.0716g Bi(NO3)3·5H2O与0.0178g Na2MoO4分别加入到含有5ml乙二醇的烧杯中超声分散;然后将以上两种溶液混合在一起搅拌2h,随后,将混合溶液中加入20ml乙醇,继续搅拌;将步骤1中得到的0.2g Bi3Ti4O12纳米薄片加入到上述混合液中搅拌均匀;最后,将得到的混合溶液转移至180℃反应釜中进行恒温热反应24h;待反应结束后降到室温,用去离子水、乙醇洗涤固体产物,干燥,用乙醇洗涤沉淀物,干燥,得到Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12异质结复合光催化剂。
(3)取(2)中样品在光化学反应仪中进行光催化降解试验,测得该光催化剂对罗丹明B的降解率在120min内达到88.78%。
(4)取(2)中样品在光化学反应仪中进行光催化降解试验,测得该光催化剂对MBT的降解率在120min内达到98.85%。
实施例2:
(1)Bi3Ti4O12纳米薄片的制备:
将0.795g Bi2O3与0.102g TiO2混合均匀;向混合物中同时加入2.5g NaCl和3.18gKCl,然后用研钵将其研碎且混合均匀;随后,将上述混合物转移至800℃管式炉中进行恒温热反应2h,升温速率为5℃/min;待反应结束后降到室温,用去离子水、乙醇洗涤固体产物,干燥,得到Bi3Ti4O12纳米薄片。
(2)Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12异质结复合光催化剂的制备:
将0.0239g Bi(NO3)3·5H2O与0.00595g Na2MoO4分别加入到含有5ml乙二醇的烧杯中超声分散;然后将以上两种溶液混合在一起搅拌2h,随后,将混合溶液中加入20ml乙醇,继续搅拌;将步骤1中得到的0.2g Bi3Ti4O12纳米薄片加入到上述混合液中搅拌均匀;最后,将得到的混合溶液转移至180℃反应釜中进行恒温热反应24h;待反应结束后降到室温,用去离子水、乙醇洗涤固体产物,干燥,用乙醇洗涤沉淀物,干燥,得到Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12异质结复合光催化剂。
(3)取(2)中样品在光化学反应仪中进行光催化降解试验,测得该光催化剂对罗丹明B的降解率在120min内达到57.31%。
(4)取(2)中样品在光化学反应仪中进行光催化降解试验,测得该光催化剂对MBT的降解率在120min内达到90.80%。
实施例3:
(1)Bi3Ti4O12纳米薄片的制备:
将0.795g Bi2O3与0.102g TiO2混合均匀;向混合物中同时加入2.5g NaCl和3.18gKCl,然后用研钵将其研碎且混合均匀;随后,将上述混合物转移至800℃管式炉中进行恒温热反应2h,升温速率为5℃/min;待反应结束后降到室温,用去离子水、乙醇洗涤固体产物,干燥,得到Bi3Ti4O12纳米薄片。
(2)Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12异质结复合光催化剂的制备:
将0.0477g Bi(NO3)3·5H2O与0.012g Na2MoO4分别加入到含有5ml乙二醇的烧杯中超声分散;然后将以上两种溶液混合在一起搅拌2h,随后,将混合溶液中加入20ml乙醇,继续搅拌;将步骤1中得到的0.2g Bi3Ti4O12纳米薄片加入到上述混合液中搅拌均匀;最后,将得到的混合溶液转移至180℃反应釜中进行恒温热反应24h;待反应结束后降到室温,用去离子水、乙醇洗涤固体产物,干燥,用乙醇洗涤沉淀物,干燥,得到Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12异质结复合光催化剂。
(3)取(2)中样品在光化学反应仪中进行光催化降解试验,测得该光催化剂对罗丹明B的降解率在120min内达到73.12%。
(4)取(2)中样品在光化学反应仪中进行光催化降解试验,测得该光催化剂对MBT的降解率在120min内达到95.85%。
实施例4:
(1)Bi3Ti4O12纳米薄片的制备:
将0.795g Bi2O3与0.102g TiO2混合均匀;向混合物中同时加入2.5g NaCl和3.18gKCl,然后用研钵将其研碎且混合均匀;随后,将上述混合物转移至800℃管式炉中进行恒温热反应2h,升温速率为5℃/min;待反应结束后降到室温,用去离子水、乙醇洗涤固体产物,干燥,得到Bi3Ti4O12纳米薄片。
(2)Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12异质结复合光催化剂的制备:
将0.0954g Bi(NO3)3·5H2O与0.0238g Na2MoO4分别加入到含有5ml乙二醇的烧杯中超声分散;然后将以上两种溶液混合在一起搅拌2h,随后,将混合溶液中加入20ml乙醇,继续搅拌;将步骤1中得到的0.2g Bi3Ti4O12纳米薄片加入到上述混合液中搅拌均匀;最后,将得到的混合溶液转移至180℃反应釜中进行恒温热反应24h;待反应结束后降到室温,用去离子水、乙醇洗涤固体产物,干燥,用乙醇洗涤沉淀物,干燥,得到Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12异质结复合光催化剂。
(3)取(2)中样品在光化学反应仪中进行光催化降解试验,测得该光催化剂对罗丹明B
B的降解率在120min内达到80.35%。
(4)取(2)中样品在光化学反应仪中进行光催化降解试验,测得该光催化剂对MBT的降解率在120min内达到96.20%。
图1为所制备样品的XRD图,分别为Bi3Ti4O12(A),5-Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12(B),10-Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12(C),15-Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12(D)和20-Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12(E),证明了本申请所制备的样品中确实为Bi3Ti4O12与Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12异质结复合光催化剂。
图2为Bi3Ti4O12与Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12复合光催化剂的TEM和HRTEM图,通过从TEM图观察到的物质形貌与HETEM的晶格间距可以进一步证实Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12复合光催化剂的成功制备。
图3分别为Bi3Ti4O12(A),5-Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12(B),10-Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12(C),15-Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12(D)和20-Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12(E)复合光催化剂的固体紫外图。从图中可以看出纯的Bi3Ti4O12具有狭窄的带隙并在可见光区域有良好的吸收,随着Bi2MoO6量子点掺杂Bi2MoO6的负载量逐渐增多,复合催化剂在可见光范围内的吸收逐渐增强。
Claims (7)
1.一种整合同质结与异质结复合光催化剂的制备方法,其特征在于,
步骤1、制备Bi3Ti4O12纳米薄片:
将Bi2O3与TiO2混合均匀后,得到混合物A;向混合物A中同时加入NaCl和KCl,然后用研钵将其研碎且混合均匀,得到混合物B;随后,将混合物B转移至管式炉中进行煅烧反应;待反应结束后降到室温,用去离子水、乙醇洗涤固体产物,干燥,得到Bi3Ti4O12纳米薄片;
步骤2、制备Bi2MoO6量子点掺杂Bi2MoO6/Bi3Ti4O12异质结复合光催化剂:
将Bi(NO3)3·5H2O与Na2MoO4分别加入到含有乙二醇的烧杯中超声分散,分别得到混合液C和D;然后将混合溶液C和D混合在一起,搅拌均匀后加入乙醇,继续搅拌得到混合溶液E;随后,将步骤1中得到的Bi3Ti4O12纳米薄片加入到混合液E中搅拌均匀得到混合液F;最后,将混合溶液F转移至反应釜中进行恒温热反应;待反应结束后降到室温,洗涤,干燥,得到Bi2MoO6量子点自掺杂Bi2MoO6/Bi3Ti4O12异质结复合光催化剂,即一种整合同质结与异质结复合光催化剂。
2.如权利要求1所述的一种整合同质结与异质结复合光催化剂的制备方法,其特征在于,步骤1中,所使用的Bi2O3:TiO2:NaCl:KCl=0.795g:0.102g:2.5g:3.18g。
3.如权利要求1所述的一种整合同质结与异质结复合光催化剂的制备方法,其特征在于,步骤1中,所述的煅烧温度为800℃,煅烧反应的时间为2h,管式炉的升温速率为5℃/min。
4.如权利要求1所述的一种整合同质结与异质结复合光催化剂的制备方法,其特征在于,步骤2中,所使用的Bi(NO3)3·5H2O:Na2MoO4:Bi3Ti4O12:乙二醇:乙醇=0.024g~0.10g:0.006g~0.0240g:0.2g:5mL:20mL。
5.如权利要求1所述的一种整合同质结与异质结复合光催化剂的制备方法,其特征在于,步骤2中,所述的恒温热反应的温度为180℃,时间为24h。
6.如权利要求1所述的一种整合同质结与异质结复合光催化剂的制备方法,其特征在于,步骤2中,所述洗涤为:先用去离子水、乙醇洗涤固体产物,干燥,再用乙醇洗涤沉淀物。
7.将权利要求1~6任意一项所述的方法制备的一种整合同质结与异质结复合光催化剂用于光催化降解罗丹明B或MBT。
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