CN116273014A - 花状MgFe2O4/ZnO异质结材料的制备方法及其在光催化方面的应用 - Google Patents
花状MgFe2O4/ZnO异质结材料的制备方法及其在光催化方面的应用 Download PDFInfo
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Abstract
本发明的花状MgFe2O4/ZnO异质结材料的制备方法及其在光催化方面的应用属于光催化材料制备的技术领域,首先利用硝酸锌和六次甲基四胺制备ZnO,然后采用共沉积法制备花状MgFe2O4/ZnO异质结材料;所制备的花状MgFe2O4/ZnO异质结材料可以作为催化剂用于光催化降解污染物。本发明操作简单,重复性好,制备出的样品具有形貌优异、比表面积高、产量高、纯度高等特点。
Description
技术领域
本发明属于光催化材料制备的技术领域,特点涉及一种花状MgFe2O4/ZnO异质结复合材料的制备方法及其在光催化降解合成雌激素17α-炔雌醇污染物、有机染料、还原Cr6+方面的应用。
背景技术
17α-炔雌醇(EE2)是一种合成雌激素,具有强烈的雌激素活性,其主要来源是人类排泄。17α-炔雌醇(EE2)因生态毒理学风险较高而引起世界人民越来越多的关注。有机染料(RHB))引起的水污染是最常见的环境污染问题之一,正威胁着地球的生态系统和人类健康。因此,从废水中去除有机染料对保护地球生态系统和人类健康具有重要意义。此外,在重金属离子中,铬(Cr6+)是电镀、钢铁加工、金属加工等多种工业过程中产生的剧毒污染物。在处理这三种污染物过程中,由于其不完全去除,最终进入自然环境,对环境所造成的污染很大。因此,有效降解17α-炔雌醇(EE2)、有机染料(RHB)和还原铬(Cr6+)是缓解自然环境可循环发展的主要途径。
纯ZnO材料易制备,生产成本低,化学稳定性好,多孔性,宽带隙半导体。但由于禁带宽度较宽(约3.2eV),光吸收波长小于400nm,紫外响应有限。因此,对太阳光的利用率低,光催化活性小,其应用领域受到严重限制。尖晶石结构的MgFe2O4窄带隙半导体磁性材料,制备成本较低、光化学稳定性较高。
经研究表明,光催化活性好、稳定性能好和可多次回收利用对于光催化剂是最重要的。影响光催化活性的一个重要的方面就是载流子分离率以及可见光吸收范围。当载流子分离率越高,可见光吸收范围和强度越高,其光催化降解能力以及还原能力好。研究发现成功构建异质结材料可以形成内置电场,有效加快电子和空穴的转移速率,抑制载流子分离率,增加可见光的吸收范围,进而有效的提升光催化降解和还原的能力。
人们致力于降解17α-炔雌醇(EE2)、有机染料(RHB)和还原铬(Cr6+),就目前而言使用花状MgFe2O4/ZnO异质结复合材料作为光催化剂的研究较少。
发明内容
本发明要解决的技术问题是,提供一种新型异质结复合材料的制备方法,并将其用作光催化降解17α-炔雌醇(EE2)、有机染料(RHB)和还原铬(Cr6+)方面,方法简单,易于控制,重复性好,降解效果和还原效果极佳,可二次回收以及稳定性效果极佳。
具体技术方案如下:
一种花状MgFe2O4/ZnO异质结材料的制备方法,有以下步骤:
1)制备ZnO,将硝酸锌水溶液和六次甲基四胺水溶液按摩尔比1:1混合后进行搅拌得到均一的反应溶液,然后将混合溶液密封后置于水浴锅中,90℃,保温24小时,反应结束后,离心干燥,得到ZnO;
2)采用共沉积法制备花状MgFe2O4/ZnO异质结材料,将硝酸铁水溶液和硝酸镁水溶液按摩尔比2:1进行混合,然后加入步骤1)制备的ZnO继续搅拌,按摩尔比硝酸铁:ZnO=3:4,接着将Na2C2O4水溶液缓慢滴入上述混合液中,按摩尔比,硝酸铁:Na2C2O4=1:5,在90℃下继续搅拌2小时,最后对所得沉淀进行离心、清洗、干燥。最后,将所得样品在500℃条件下退火2h,得到花状MgFe2O4/ZnO异质结材料。
作为优选,步骤1)中所述的将硝酸锌水溶液和六次甲基四胺水溶液混合均匀,具体是在磁力搅拌器上搅拌5分钟,搅拌过程中用保鲜膜封口。
作为优选,步骤1)中硝酸锌水溶液和六次甲基四胺水溶液的浓度均为1mol/L,步骤2)中硝酸铁水溶液的浓度为0.005mol/L,硝酸镁水溶液的浓度为0.0025mol/L,Na2C2O4水溶液的浓度为0.025mol/L。
步骤2)中所述的清洗,优选用蒸馏水和无水乙醇各离心清洗3~5次。
步骤2)中所述的干燥,优选在60℃下干燥2小时。
一种花状MgFe2O4/ZnO异质结材料在光催化方面的应用,将污染物原液和MgFe2O4/ZnO异质结材料混合后用超声波处理,光照前,在黑暗条件下搅拌,达到吸附解吸平衡,随后,放置一盏Xe灯进行照射,在光照射期间,相同的时间间隔内测量样品溶液的浓度,降解效率(%)通过以下式计算:
Degradation(%)=(C0-Ct)/C0*100%
式中C0为初始浓度,Ct为t时刻的浓度。
所述污染物原液优选17α-炔雌醇污染物原液、有机染料污染物原液或Cr6+污染物原液。
作为优选,每100ml污染物原液使用50mg所述MgFe2O4/ZnO异质结材料。
有益效果:
1、本发明首次合成出花状MgFe2O4/ZnO异质结材料;制备出的MgFe2O4/ZnO异质结材料形貌优异、比表面积高、产量高、纯度高。本发明使用水浴法以及共沉淀法,操作简单、重复性好、成本低廉;为进一步研究奠定了基础。
2、本发明首次将花状MgFe2O4/ZnO异质结材料应用于光催化方面,在降解17α-炔雌醇(EE2)时,60min内降解率可达到95.6%;在降解有机染料(RHB)时,120min内降解率可达到97.5%;在还原铬(Cr6+)时,18min内还原率可达到94%。经循环降解五次后其降解率依然非常高,未见明显降低。本发明为进一步研究MgFe2O4/ZnO异质结复合材料在降解污染物方面的应用奠定了基础。
附图说明
图1是实施例1制得的MgFe2O4/ZnO异质结材料的SEM谱图。
图2是实施例1制得的MgFe2O4/ZnO异质结材料的TEM谱图。
图3是实施例2利用制得的MgFe2O4/ZnO异质结光催化降解EE2图。
图4是实施例2利用制得的MgFe2O4/ZnO异质结降解EE2循环利用效率。
图5是实施例3利用制得的MgFe2O4/ZnO异质结光催化降解RHB图。
图6是实施例4利用制得的MgFe2O4/ZnO异质结复合材料光催化还原Cr6+图。
具体实施方式
实施例1
花状MgFe2O4/ZnO异质结材料的制备,首先制备ZnO,将100ml硝酸锌水溶液(0.1mol/l)和100ml六次甲基四胺水溶液(0.1mol/l)混合后进行搅拌得到均一的反应溶液。然后将混合溶液密封后置于水浴锅中,90℃,保温24小时。反应结束后,将样品离心干燥得到ZnO。接着采用共沉积法制备花状MgFe2O4/ZnO异质结催化剂。将100ml硝酸铁水溶液(0.005mol/l)和100ml硝酸镁水溶液(0.0025mol/l)进行混合搅拌5min,然后加入0.054g的ZnO(约6.7mmol)继续搅拌40min。接着加入100ml的Na2C2O4水溶液(0.025mol/l)缓慢滴入上述混合液中,在90℃下继续搅拌2小时。最后对所得沉淀进行离心、清洗、干燥以及退火处理。
图1给出本条件所制备的花状MgFe2O4/ZnO异质结材料的SEM图,可看出形貌为花状,其表面粗糙。图2给出本条件所制备的花状MgFe2O4/ZnO异质结材料的TEM图,可以看出ZnO纳米管被MgFe2O4纳米颗粒紧密包裹。
实施例2
花状MgFe2O4/ZnO异质结材料用于光催化降解污染物17α-炔雌醇(EE2),将EE2污染物原液(20ppm,100ml)和MgFe2O4/ZnO异质结材料(50mg)混合后用超声波处理。光照前,在黑暗条件下搅拌2h,达到吸附解吸平衡。随后,放置一盏Xe灯,模拟太阳光辐射,共照射60分钟。在光照射期间,选择每15min取样液10ml置于提前准备好的取样瓶中,待反应结束后用液体紫外分光光度计对样液的光响应情况进行测试,并对数据进行整理,分析,作图,表征样品的催化性能。
图3给出了MgFe2O4/ZnO异质结复合材料的光催化降解EE2图,可以看出其光催化降解率可达到95.6%。图4给出MgFe2O4/ZnO异质结复合材料降解EE2循环利用效率图,可以看出在经过五次循环降解EE2之后,其光催化降解率依然能够达到86%。
实施例3
花状MgFe2O4/ZnO异质结材料用于光催化降解有机染料(RHB)。在本实验中所用的光源为Xe灯,模拟太阳光辐射,测试样品的光催化降解性能。控温温度计检测整个光催化降解实验在25℃的室温条件下完成。将RHB污染物原液(2×10-5mol/L,100ml)和MgFe2O4/ZnO材料(50mg)混合后用超声波处理。光照前,在黑暗条件下搅拌2h,达到吸附解吸平衡。随后,放置模拟太阳光的灯,共照射120分钟。在光照射期间,选择每30min取样液5ml置于提前准备好的取样瓶中,待反应结束后用液体紫外分光光度计对样液的光响应情况进行测试,并对数据进行整理,分析,作图,表征样品的催化性能。
图5给出了MgFe2O4/ZnO异质结复合材料的光催化降解有机染料(RHB)图,可看出经120min后光催化降解率可达到97.5%。
实施例4
花状MgFe2O4/ZnO异质结材料用于光催化还原铬(Cr6+),将富含铬(Cr6+)污染物原液(10mg/L,100ml)和MgFe2O4/ZnO异质结材料(50mg)混合后用超声波处理。光照前,在黑暗条件下搅拌2h,达到吸附解吸平衡。随后,放置一盏Xe灯,模拟太阳光辐射,共照射18分钟。在光照射期间,选择每3min取样液置于提前准备好的取样瓶中,待反应结束后采用1,5-二苯基卡脲比色法测定了上清液中Cr6+(VI)的浓度,并对数据进行整理,分析,作图,表征样品的光催化还原性能。
图6给出了MgFe2O4/ZnO异质结复合材料的光催化还原Cr6+图,可看出经18min后光催化还原率可达到94%。
Claims (8)
1.一种花状MgFe2O4/ZnO异质结材料的制备方法,有以下步骤:
1)制备ZnO,将硝酸锌水溶液和六次甲基四胺水溶液按摩尔比1:1混合后进行搅拌得到均一的反应溶液,然后将混合溶液密封后置于水浴锅中,90℃,保温24小时,反应结束后,离心干燥,得到ZnO;
2)采用共沉积法制备花状MgFe2O4/ZnO异质结材料,将硝酸铁水溶液和硝酸镁水溶液按摩尔比2:1进行混合,然后加入步骤1)制备的ZnO继续搅拌,按摩尔比硝酸铁:ZnO=3:4,接着将Na2C2O4水溶液缓慢滴入上述混合液中,按摩尔比,硝酸铁:Na2C2O4=1:5,在90℃下继续搅拌2小时,最后对所得沉淀进行离心、清洗、干燥。最后,将所得样品在500℃条件下退火2h,得到花状MgFe2O4/ZnO异质结材料。
2.根据权利要求1所述的一种花状MgFe2O4/ZnO异质结材料的制备方法,其特征在于,步骤1)中所述的将硝酸锌水溶液和六次甲基四胺水溶液混合均匀,具体是在磁力搅拌器上搅拌5分钟,搅拌过程中用保鲜膜封口。
3.根据权利要求1所述的一种花状MgFe2O4/ZnO异质结材料的制备方法,其特征在于,步骤1)中硝酸锌水溶液和六次甲基四胺水溶液的浓度均为1mol/L,步骤2)中硝酸铁水溶液的浓度为0.005mol/L,硝酸镁水溶液的浓度为0.0025mol/L,Na2C2O4水溶液的浓度为0.025mol/L。
4.根据权利要求1所述的一种花状MgFe2O4/ZnO异质结材料的制备方法,其特征在于,步骤2)中所述的清洗,是用蒸馏水和无水乙醇各离心清洗3~5次。
5.根据权利要求1所述的一种花状MgFe2O4/ZnO异质结材料的制备方法,其特征在于,步骤2)中所述的干燥,是在60℃下干燥2小时。
6.一种权利要求所述的花状MgFe2O4/ZnO异质结材料在光催化方面的应用,将污染物原液和MgFe2O4/ZnO异质结材料混合后用超声波处理,光照前,在黑暗条件下搅拌,达到吸附解吸平衡,随后,放置一盏Xe灯进行照射,在光照射期间,相同的时间间隔内测量样品溶液的浓度,降解效率(%)通过以下式计算:
Degradation(%)=(C0-Ct)/C0*100%
式中C0为初始浓度,Ct为t时刻的浓度。
7.根据权利要求6所述的一种花状MgFe2O4/ZnO异质结材料在光催化方面的应用,其特征在于,所述污染物原液选自17α-炔雌醇污染物原液、有机染料污染物原液或Cr6+污染物原液。
8.根据权利要求6所述的一种花状MgFe2O4/ZnO异质结材料在光催化方面的应用,其特征在于,每100ml污染物原液使用50mg所述MgFe2O4/ZnO异质结材料。
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