CN113318759B - 一种多巴胺介导的氯氧化铋光催化剂及其制备方法与应用 - Google Patents
一种多巴胺介导的氯氧化铋光催化剂及其制备方法与应用 Download PDFInfo
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- 229940073609 bismuth oxychloride Drugs 0.000 title claims abstract description 60
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- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims abstract description 12
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Abstract
本发明提供了一种多巴胺介导的氯氧化铋光催化剂及其制备方法与应用。首先,将铋源Bi(NO3)3·5H2O溶解在去离子水中,通过加入冰醋酸控制溶液体系的pH值为1.5~4,将上述所得溶液缓慢加入到浓度为1~8mg/mL的盐酸多巴胺水溶液中,控制卤源和铋源的摩尔比为(0.2~2.4):1,室温下,搅拌至反应完全。通过离心分离,用乙醇和去离子水洗涤所得沉淀,后干燥,即得到多巴胺介导的氯氧化铋。本发明得到的多巴胺介导的氯氧化铋光催化剂相比于片状的氯氧化铋光催化剂具有更高的光催化活性。
Description
技术领域
本发明涉及光催化材料技术领域,具体涉及一种多巴胺介导的氯氧化铋光催化剂及其制备方法与应用。
背景技术
近年来,铋基半导体因其优异的光催化性能被广泛应用于有机污染物的降解、光解水产氢,以及二氧化碳的还原反应中。其中,氯氧化铋是一种p型半导体,禁带宽度约为3.3eV,对紫外光具有良好的响应,在光催化反应中表现出优异的反应活性。然而,紫外光仅占太阳光的4%,为了充分利用太阳能,开发高效的可见光光催化剂引起了广泛关注。
目前,氯氧化铋材料最常用的制备方法是水热或溶剂热法。然而,该制备方法非常耗时,既要求比较高的反应温度,又要求在强酸或有毒的有机溶剂体系下反应。因此,通过模板剂介导的合成方法,在相对温和的反应条件下制备氯氧化铋光催化材料具有重要的意义。
发明内容
本发明为解决氯氧化铋催化剂太阳光利用效率低、制备条件较苛刻、可见光下污染物催化降解能力差等问题,提供了一种多巴胺介导的氯氧化铋光催化剂的制备方法,适用于可见光光催化领域,为降解罗丹明B等有机染料提供了一种新的技术方案。
本发明的主要技术方案是:一种多巴胺介导的氯氧化铋光催化剂,其特征在于,包括以下步骤:
步骤一:将铋源Bi(NO3)3·5H2O溶解在去离子水中,通过加入冰醋酸控制溶液体系为酸性,超声处理10min;
步骤二:将步骤一所得溶液缓慢加入到卤源盐酸多巴胺水溶液中,持续搅拌进行反应,反应结束后通过离心分离所得沉淀,将沉淀物洗涤后干燥,即得到多巴胺介导的氯氧化铋。
优选地,步骤一中Bi(NO3)3·5H2O溶液的浓度为2~4mmol/L,且pH值为1.5~4。
优选地,步骤二中卤源和铋源之间的摩尔比为(0.2~2.4):1,且盐酸多巴胺的溶液体系为水,浓度为1~8mg/mL。
优选地,步骤二中反应温度为20~40℃,反应时间为0.5~12h。
优选地,步骤二中将沉淀物用去离子水和无水乙醇分别洗涤两次。
优选地,步骤二中干燥温度为85℃,干燥时间为10h。
一种多巴胺介导的氯氧化铋光催化剂,采用上述的一种多巴胺介导的氯氧化铋光催化剂的制备方法制得。
优选地,所述多巴胺介导的氯氧化铋光催化剂形貌为花球状。
优选地,所述多巴胺介导的氯氧化铋光催化剂对有机染料罗丹明B的去除率在20min内达到99%以上。
与现有技术相比,本发明具有以下优异的技术效果:
1)在室温以及水溶液等温和的反应条件下,通过简单的一步反应法,制备出了一种多巴胺介导的氯氧化铋光催化剂,且合成反应时间很短,重复性强,极具市场商品化潜力。
2)制备过程中加入的盐酸多巴胺不仅仅是反应物,还充当了模板剂和结构导向剂的作用,促进了纳米片的成核和定向聚集,通过自组装,形成了花球状氯氧化铋。
3)本发明原材料采用绿色、无毒、无害组分,减少了对人体健康和生态环境的危害。
4)本发明所述的光催化剂,具有孔隙率高,比表面积大,吸附能力强的特点。
5)本发明所述的光催化剂,由于多巴胺在材料表面上的相互作用,使得禁带宽度变窄,扩大了光的吸收范围,容易受到光的激发产生光生电子和空穴。且由于价带的位置发生了正移,光生空穴具有了更强的氧化能力,可见光下,多巴胺介导的氯氧化铋光催化剂对有机染料罗丹明B的去除率在20min内达到99%以上。
附图说明
图1为实施例1-4制得的多巴胺介导的氯氧化铋的XRD图;
图2为实施例1制得的多巴胺介导的氯氧化铋的SEM图;
图3为实施例2制得的多巴胺介导的氯氧化铋的SEM图;
图4为实施例3制得的多巴胺介导的氯氧化铋的SEM图;
图5为实施例4制得的多巴胺介导的氯氧化铋的SEM图;
图6为实施例1制得的多巴胺介导的氯氧化铋的TEM图;
图7为实施例2制得的多巴胺介导的氯氧化铋的TEM图;
图8为实施例3制得的多巴胺介导的氯氧化铋的TEM图;
图9为实施例4制得的多巴胺介导的氯氧化铋的TEM图;
图10为实施例1-2制得的多巴胺介导的氯氧化铋的氮气吸附解析等温线;
图11为实施例3-4制得的多巴胺介导的氯氧化铋的氮气吸附解析等温线;
图12为实施例1-4制得的多巴胺介导的氯氧化铋的BET孔径分布图;
图13为实施例1-4制得的多巴胺介导的氯氧化铋的UV-Vis DRS谱图;
图14为实施例1-4制得的多巴胺介导的氯氧化铋的Tauc Plots曲线;
图15为对比例1和实施例1-4制得的多巴胺介导的氯氧化铋的RhB光催化降解活性图;
图16为对比例1和实施例1-4制得的多巴胺介导的氯氧化铋的反应速率常数图。
具体实施方式
为使本发明的目的、技术方案和优点更加清晰,以下结合附图及实施例对本发明作进一步地详细描述。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。
对比例1
在室温、磁力搅拌下(500~600r/s),将0.244g的Bi(NO3)3·5H2O和0.0292g的NaCl溶于50mL去离子水中,持续搅拌30min。将上述溶液转入100mL高压反应釜中,加入30mL去离子水使装填量达到80%,在160℃下烘箱中保持16h。自然冷却,过滤,依次用乙醇、去离子水分别洗涤两次,所得固体样品于85℃干燥12h,制得片状氯氧化铋光催化剂。
实施例1
步骤一:将Bi(NO3)3·5H2O溶解在去离子水中,制得浓度为3.18mmol/L的Bi(NO3)3·5H2O水溶液。通过加入冰醋酸控制溶液体系的pH值为2.15,超声处理10min。
步骤二:将70.8mL步骤一所得溶液缓慢加入到12mL浓度为1mg/mL的盐酸多巴胺水溶液中,在室温下持续搅拌30min。反应结束后通过离心分离所得沉淀,将沉淀物用蒸馏水和无水乙醇洗涤两次,在85℃下干燥10h,即得到多巴胺介导的花球状的氯氧化铋光催化剂。
实施例2
步骤一:将Bi(NO3)3·5H2O溶解在去离子水中,制得浓度为3.18mmol/L的Bi(NO3)3·5H2O水溶液。通过加入冰醋酸控制溶液体系的pH值为2.15,超声处理10min。
步骤二:将70.8mL步骤一所得溶液缓慢加入到12mL浓度为2mg/mL的盐酸多巴胺水溶液中,在室温下持续搅拌30min。反应结束后通过离心分离所得沉淀,将沉淀物用蒸馏水和无水乙醇洗涤两次,在85℃下干燥10h,即得到多巴胺介导的花球状的氯氧化铋光催化剂。
实施例3
步骤一:将Bi(NO3)3·5H2O溶解在去离子水中,制得浓度为3.18mmol/L的Bi(NO3)3·5H2O水溶液。通过加入冰醋酸控制溶液体系的pH值为2.15,超声处理10min。
步骤二:将70.8mL步骤一所得溶液缓慢加入到12mL浓度为4mg/mL的盐酸多巴胺水溶液中,在室温下持续搅拌30min。反应结束后通过离心分离所得沉淀,将沉淀物用蒸馏水和无水乙醇洗涤两次,在85℃下干燥10h,即得到多巴胺介导的花球状的氯氧化铋光催化剂。
实施例4
步骤一:将Bi(NO3)3·5H2O溶解在去离子水中,制得浓度为3.18mmol/L的Bi(NO3)3·5H2O水溶液。通过加入冰醋酸控制溶液体系的pH值为2.15,超声处理10min。
步骤二:将70.8mL步骤一所得溶液缓慢加入到12mL浓度为8mg/mL的盐酸多巴胺水溶液中,在室温下持续搅拌30min。反应结束后通过离心分离所得沉淀,将沉淀物用蒸馏水和无水乙醇洗涤两次,在85℃下干燥10h,即得到多巴胺介导的花球状的氯氧化铋光催化剂。
从图1可以看出,实施例1-4制备出的多巴胺介导的氯氧化铋的衍射峰,并且没有产生杂质峰,表明成功制备出来纯的氯氧化铋晶体。
图2-5为不同盐酸多巴胺浓度下花球状的氯氧化铋的SEM图。
图6-9为不同盐酸多巴胺浓度下花球状的氯氧化铋的TEM图。
从图10、图11和图12可以看出,实施例1-4制备出的多巴胺介导的氯氧化铋的孔的结构很不规整,以平板狭缝结构为主,其中,实施例4拥有最大的的比表面积(25.95m2/g)。
从图13和图14可以看出实施例1-4制备出的多巴胺介导的氯氧化铋的吸收边发生了一定程度上的红移,扩大了光的吸收范围,提升了该材料的可见光光催化能力。
从图15和图16可以看出,实施例4制备出的多巴胺介导的氯氧化铋,可见光下对有机染料罗丹明B的去除率在15min内达到99%以上。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (6)
1.一种多巴胺介导的氯氧化铋光催化剂的制备方法,其特征在于,包括以下步骤:
步骤一:将铋源Bi(NO3)3•5H2O溶解在去离子水中,通过加入冰醋酸控制溶液体系为酸性,超声处理10 min;
步骤二:将步骤一所得溶液缓慢加入到卤源盐酸多巴胺水溶液中,持续搅拌进行反应,反应结束后通过离心分离所得沉淀,将沉淀物洗涤后干燥,即得到多巴胺介导的氯氧化铋,
其中,步骤二中卤源和铋源之间的摩尔比为(0.2~2.4) : 1,且盐酸多巴胺的溶液体系为水,浓度为1~8 mg/mL,
步骤二中反应温度为20~40 ℃,反应时间为0.5~12h。
2.如权利要求1所述的一种多巴胺介导的氯氧化铋光催化剂的制备方法,其特征在于,步骤一中Bi(NO3)3•5H2O溶液的浓度为2~4 mmol/L,且pH值为1.5~4。
3.如权利要求1所述的一种多巴胺介导的氯氧化铋光催化剂的制备方法,其特征在于,步骤二中将沉淀物用去离子水和无水乙醇分别洗涤两次。
4.如权利要求1所述的一种多巴胺介导的氯氧化铋光催化剂的制备方法,其特征在于,步骤二中干燥温度为85 ℃,干燥时间为10 h。
5.一种多巴胺介导的氯氧化铋光催化剂,其特征在于,采用权利要求1-4任一项所述的一种多巴胺介导的氯氧化铋光催化剂的制备方法制得多巴胺介导的氯氧化铋光催化剂,所述多巴胺介导的氯氧化铋光催化剂形貌为花球状。
6.如权利要求5所述的一种多巴胺介导的氯氧化铋光催化剂的应用,其特征在于,所述多巴胺介导的氯氧化铋光催化剂对有机染料罗丹明B的去除率在20 min内达到99%以上。
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