CN107790165B - 一种具有吸附特性的Zn2SnO4@mpg-C3N4光催化剂及其制备方法 - Google Patents
一种具有吸附特性的Zn2SnO4@mpg-C3N4光催化剂及其制备方法 Download PDFInfo
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000011941 photocatalyst Substances 0.000 claims abstract description 22
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
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- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 abstract description 3
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- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 4
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Abstract
一种具有吸附特性的Zn2SnO4@mpg‑C3N4光催化剂及其制备方法,将mpg‑C3N4加入到去离子水中超声分散,再加入SnCl4·5H2O搅拌均匀后得A溶液;向Zn(NO3)2·6H2O中加入乙二醇搅拌均匀得B液;将A液缓慢加入B液中搅拌均匀后加入NaN3,得C溶液;最后向C溶液中加入水合肼溶液调节pH得前驱液,将前驱液采用微波溶剂热法制备出具有良好吸附性能的Zn2SnO4@mpg‑C3N4光催化剂。本发明一步合成Zn2SnO4@mpg‑C3N4光催化剂,其流程简易,操作简单,反应时间短,反应条件温和,合成的Zn2SnO4@mpg‑C3N4光催化剂具有良好的吸附性能,可用于处理环境污染。
Description
技术领域
本发明属于功能材料领域,具体涉及一种具有吸附特性的Zn2SnO4@ mpg-C3N4光催化剂及其制备方法。
背景技术
目前,水体污染越来越严重,已经到了威胁人类社会生存的地步。常规水处理方法,比如生化法、物理吸附法以及混凝沉降法等,虽然可以部分去除有机污染物,但是某些的有机物,效果却非常差,而且常常会造成二次污染。相比这些方法,化学吸附法可以在吸附材料与被吸附的污染物分子之间形成牢固的化学键,从而抑制污染物分子的脱附,可以广泛应用于环境污水处理。
大量研究表明,吸附材料的吸附性能与材料自身比表面积、孔结构和孔径分布有关。mpg-C3N4具有多孔结构、比表面积大等优点,将mpg-C3N4与Zn2SnO4复合可以提高mpg-C3N4的吸附性能并改善其脱附现象,采用微波溶剂热法合成的Zn2SnO4@mpg-C3N4光催化剂拥有良好的吸附性能,可应用于环境污水处理。
发明内容
本发明的目的在于提供一种具有吸附特性的Zn2SnO4@mpg-C3N4光催化剂及其制备方法,该方法操作简单,反应时间短,反应条件温和,制备的Zn2SnO4@ mpg-C3N4光催化剂具有良好的吸附性能。
为达到上述目的,本发明的制备方法如下:
步骤1:将60mL浓度为2.64mol/L的三聚氰胺溶液与40mL浓度为0.83mol/L 的纳米SiO2溶液混合,超声分散、搅拌均匀后放入80℃的烘箱烘干得白色固体,将其研磨细后装入坩埚,在N2气氛炉中以2.5℃/min的升温速度升至550℃保温 4h煅烧得到淡黄色粉末,再用4mol/L的NH4HF2水溶液进行腐蚀,最后进行洗涤干燥得到mpg-C3N4粉体;
步骤2:取0.15g-1.2g的mpg-C3N4粉体加到20mL去离子水中,高速搅拌、超声分散后再向mpg-C3N4的悬浊液中加入0.351g的SnCl4·5H2O,磁力搅拌得A 溶液;
步骤3:取0.595g的Zn(NO3)2·6H2O加入到20mL乙二醇中,磁力搅拌得B 溶液;
步骤4:将A液缓慢加入B液中,磁力搅拌并加入NaN3,搅拌均匀后得C 溶液;
步骤5:向C溶液中加入水合肼溶液调节C溶液的pH值至7-9,磁力搅拌得反应前驱液;
步骤6:将反应前驱液加入微波水热反应釜中,将微波水热反应釜置于微波辅助水热合成仪中,在300W的微波功率下,10min从室温升温至160-200℃反应;
步骤7:待反应结束后,自然冷却至70℃,取出微波水热反应釜中的沉淀物,用去离子水和无水乙醇洗涤,最后在80℃下恒温干燥得到mpg-C3N4/Zn2SnO4复合材料。
所述步骤1)中mpg-C3N4粉体为介孔mpg-C3N4粉体,孔径分布在3-65nm。
所述的步骤4)中C溶液中NaN3的浓度为0.025-0.08mol/L。
所述的步骤5中水合肼溶液的浓度为0.6mol/L。
所述的步骤6)微波水热反应釜的填充比为40-70%。
所述的步骤7)制备的mpg-C3N4/Zn2SnO4复合材料中,mpg-C3N4质量百分数为30%-80%。
按以上方法制备的Zn2SnO4@mpg-C3N4光催化剂中Zn2SnO4被mpg-C3N4包裹,形成Zn2SnO4@mpg-C3N4光催化剂。
相对于现有技术,本发明的有益效果为:
本发明以SnCl4·5H2O为锡源,Zn(NO3)2·6H2O为锌源,NaN3为添加剂, mpg-C3N4为载体,通过微波溶剂热法一步成功制备Zn2SnO4@mpg-C3N4光催化剂。本发明采用微波溶剂热法一步合成Zn2SnO4@mpg-C3N4光催化剂,结合了微波加热与溶剂热法的优点,其流程简易,操作简单,反应时间短,反应条件温和,合成的mpg-C3N4/Zn2SnO4复合材料具有良好的吸附性能,可用于污水处理。
附图说明
图1是本发明制备的粉体的FT-IR图,其中a-c分别为实施例1-实施例3制备的粉体的FT-IR图。
图2是本发明实施例1制备的粉体的XRD图,其中a-c分别为实施例1-实施例3制备的粉体的XRD图。
图3是本发明制备的粉体的降解罗丹明B的降解率-时间曲线,其中a-c分别为实施例1-实施例3制备的粉体的降解曲线。
具体实施方式
下面结合具体实施例和附图对本发明作进一步详细说明。
实施例1:
步骤1:将60mL浓度为2.64mol/L的三聚氰胺溶液与40mL浓度为0.83mol/L 的纳米SiO2溶液混合,超声分散、搅拌均匀后放入80℃的烘箱烘干得白色固体,将其研磨细后装入坩埚,在N2气氛炉中以2.5℃/min的升温速度升至550℃保温 4h煅烧得到淡黄色粉末,再用4mol/L的NH4HF2水溶液进行腐蚀,最后进行洗涤干燥得mpg-C3N4粉体;
步骤2:取0.3g的mpg-C3N4粉体加到20mL去离子水中,高速搅拌、超声分散后再向mpg-C3N4的悬浊液中加入0.351g的SnCl4·5H2O,磁力搅拌得A溶液;
步骤3:取0.595g的Zn(NO3)2·6H2O加入到20mL乙二醇中,磁力搅拌得B 溶液;
步骤4:将A液缓慢加入B液中,磁力搅拌并加入NaN3,搅拌均匀后得 NaN3的浓度为0.08mol/L的C溶液;
步骤5:向C溶液中加入浓度为0.6mol/L的水合肼溶液调节C溶液的pH 值至7,磁力搅拌得反应前驱液;
步骤6:按60%的填充比将反应前驱液加入微波水热反应釜中,将微波水热反应釜置于微波辅助水热合成仪中,在300W的微波功率下,10min从室温升温至200℃反应;
步骤7:待反应结束后,自然冷却至70℃,取出微波水热反应釜中的沉淀物,用去离子水和无水乙醇洗涤,最后在80℃下恒温干燥得到mpg-C3N4/Zn2SnO4复合材料。
实施例2:
步骤1:将60mL浓度为2.64mol/L的三聚氰胺溶液与40mL浓度为0.83mol/L 的纳米SiO2溶液混合,超声分散、搅拌均匀后放入80℃的烘箱烘干得白色固体,将其研磨细后装入坩埚,在N2气氛炉中以2.5℃/min的升温速度升至550℃保温 4h煅烧得到淡黄色粉末,再用4mol/L的NH4HF2水溶液进行腐蚀,最后进行洗涤干燥得mpg-C3N4粉体;
步骤2:取0.557g的mpg-C3N4粉体加到20mL去离子水中,高速搅拌、超声分散后再向mpg-C3N4的悬浊液中加入0.351g的SnCl4·5H2O,磁力搅拌得A 溶液;
步骤3:取0.595g的Zn(NO3)2·6H2O加入到20mL乙二醇中,磁力搅拌得B 溶液;
步骤4:将A液缓慢加入B液中,磁力搅拌并加入NaN3,搅拌均匀后得 NaN3的浓度为0.025mol/L的C溶液;
步骤5:向C溶液中加入浓度为0.6mol/L的水合肼溶液调节C溶液的pH 值至9,磁力搅拌得反应前驱液;
步骤6:按40%的填充比将反应前驱液加入微波水热反应釜中,将微波水热反应釜置于微波辅助水热合成仪中,在300W的微波功率下,10min从室温升温至180℃反应;
步骤7:待反应结束后,自然冷却至70℃,取出微波水热反应釜中的沉淀物,用去离子水和无水乙醇洗涤,最后在80℃下恒温干燥得到mpg-C3N4/Zn2SnO4复合材料。
实施例3:
步骤1:将60mL浓度为2.64mol/L的三聚氰胺溶液与40mL浓度为0.83mol/L 的纳米SiO2溶液混合,超声分散、搅拌均匀后放入80℃的烘箱烘干得白色固体,将其研磨细后装入坩埚,在N2气氛炉中以2.5℃/min的升温速度升至550℃保温 4h煅烧得到淡黄色粉末,再用4mol/L的NH4HF2水溶液进行腐蚀,最后进行洗涤干燥得mpg-C3N4粉体;
步骤2:取1.2g的mpg-C3N4粉体加到20mL去离子水中,高速搅拌、超声分散后再向mpg-C3N4的悬浊液中加入0.351g的SnCl4·5H2O,磁力搅拌得A溶液;
步骤3:取0.595g的Zn(NO3)2·6H2O加入到20mL乙二醇中,磁力搅拌得B 溶液;
步骤4:将A液缓慢加入B液中,磁力搅拌并加入NaN3,搅拌均匀后得 NaN3的浓度为0.05mol/L的C溶液;
步骤5:向C溶液中加入浓度为0.6mol/L的水合肼溶液调节C溶液的pH 值至8,磁力搅拌得反应前驱液;
步骤6:按70%的填充比将反应前驱液加入微波水热反应釜中,将微波水热反应釜置于微波辅助水热合成仪中,在300W的微波功率下,10min从室温升温至160℃反应;
步骤7:待反应结束后,自然冷却至70℃,取出微波水热反应釜中的沉淀物,用去离子水和无水乙醇洗涤,最后在80℃下恒温干燥得到mpg-C3N4/Zn2SnO4复合材料。
图1是本发明制备的复合材料的FT-IR图,其中a-c分别为实施例1-实施例 3制备的粉体的FT-IR图。570cm-1左右的吸收峰为Zn2SnO4晶胞中[ZnO4]四面体中Zn-O键的特征吸收峰,800cm-1和890cm-1左右的特征吸收峰为三嗪环的振动峰和C-H键的伸缩振动峰,1200cm-1-1700cm-1范围内的大部分特征峰为C=N 双键和C-N单键的伸缩振动峰,表明样品中存在mpg-C3N4和Zn2SnO4两相。
图2是本发明制备的复合材料的XRD图。2θ=27.4°左右的衍射峰为 mpg-C3N4中的共轭芳香体系组成的芳香段经过层间堆积形成的(002)晶面所对应的衍射峰;衍射角2θ=34.20°、55.09°衍射峰为Zn2SnO4(JCPDF No.24-1470)的衍射峰,宽化的馒头峰表明该复合材料中的Zn2SnO4被mpg-C3N4包裹,形成了 Zn2SnO4@mpg-C3N4光催化剂,Zn2SnO4在mpg-C3N4介孔中生成,mpg-C3N4阻止了Zn2SnO4生长,Zn2SnO4衍射峰出现了宽化。
图3是本发明制备的复合催化剂粉体的降解罗丹明B的降解率-时间曲线,其中a-c分别为实施例1-实施例3制备的粉体的降解曲线。图3中纵坐标的C/C0为某时刻罗丹明B降解后的浓度与其初始浓度的比值。从图中可以看出,实施例1所制备出的粉体具有良好的吸附性能,暗反应30min后,对RhB染料分子的吸附率可达80%以上,并且在之后的光照和搅拌过程中并不存在脱附现象。
Claims (7)
1.一种具有吸附特性的Zn2SnO4@mpg-C3N4光催化剂的制备方法,其特征在于,包括以下步骤:
步骤1:将60mL浓度为2.64mol/L的三聚氰胺溶液与40mL浓度为0.83mol/L的纳米SiO2溶液混合,超声分散、搅拌均匀后放入80℃的烘箱烘干得白色固体,将其研磨细后装入坩埚,在N2气氛炉中以2.5℃/min的升温速度升至550℃保温4h煅烧得到淡黄色粉末,再用4mol/L的NH4HF2水溶液进行腐蚀,最后进行洗涤干燥得到mpg-C3N4粉体;
步骤2:取0.15g-1.2g的mpg-C3N4粉体加到20mL去离子水中,高速搅拌、超声分散后再向mpg-C3N4的悬浊液中加入0.351g的SnCl4·5H2O,磁力搅拌得A溶液;
步骤3:取0.595g的Zn(NO3)2·6H2O加入到20mL乙二醇中,磁力搅拌得B溶液;
步骤4:将A液缓慢加入B液中,磁力搅拌并加入NaN3,搅拌均匀后得C溶液;
步骤5:向C溶液中加入水合肼溶液调节C溶液的pH值至7-9,磁力搅拌得反应前驱液;
步骤6:将反应前驱液加入微波水热反应釜中,将微波水热反应釜置于微波辅助水热合成仪中,在300W的微波功率下,10min从室温升温至160-200℃反应;
步骤7:待反应结束后,自然冷却至70℃,取出微波水热反应釜中的沉淀物,用去离子水和无水乙醇洗涤,最后在80℃下恒温干燥得到Zn2SnO4@mpg-C3N4复合材料。
2.根据权利要求1所述的具有吸附特性的Zn2SnO4@mpg-C3N4光催化剂的制备方法,其特征在于:所述步骤1)中mpg-C3N4粉体为介孔mpg-C3N4粉体,孔径分布在3-65nm。
3.根据权利要求1所述的具有吸附特性的Zn2SnO4@mpg-C3N4光催化剂的制备方法,其特征在于:所述的步骤4)中C溶液中NaN3的浓度为0.025-0.08mol/L。
4.根据权利要求1所述的具有吸附特性的Zn2SnO4@mpg-C3N4光催化剂的制备方法,其特征在于:所述的步骤5中水合肼溶液的浓度为0.6mol/L。
5.根据权利要求1所述的具有吸附特性的Zn2SnO4@mpg-C3N4光催化剂的制备方法,其特征在于:所述的步骤6)微波水热反应釜的填充比为40-70%。
6.根据权利要求1所述的具有吸附特性的Zn2SnO4@mpg-C3N4光催化剂的制备方法,其特征在于:所述的步骤7)制备的mpg-C3N4/Zn2SnO4复合材料中,mpg-C3N4质量百分数为30%-80%。
7.一种如权利要求1所述的制备方法制得的Zn2SnO4@mpg-C3N4光催化剂,其特征在于:Zn2SnO4@mpg-C3N4光催化剂中Zn2SnO4被mpg-C3N4包裹,形成Zn2SnO4@mpg-C3N4光催化剂。
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