CN115463674A - 一种部分出现氧空位的溴氧化铋的制备方法 - Google Patents
一种部分出现氧空位的溴氧化铋的制备方法 Download PDFInfo
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- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及一种含氧空位溴氧化铋的制备方法。本发明制备方法步骤如下:先利用Bi(NO3)3·5H2O、PVP和KBr,在水热条件下制备BiOBr;将得到的BiOBr和氯铂酸钾溶液混合光照一段时间后获得负载铂的BiOBr粉体;最后把负载铂的BiOBr粉体在有机溶液中光照一段时间,得到由BiOBr、含氧空位的BiOBr和Pt组成的三元结构。本发明具有生产成本低、反应条件温和、易于规模化生产、氧空位能够长时间保存、能够显著提高对可见光的吸收率和光催化性能优异等优点。
Description
技术领域
本发明属于光催化材料领域,涉及一种部分出现氧空位的溴氧化铋的制备方法。
背景技术
由于光催化技术可以直接利用可见光来处理室内空气中含有的有机污染物,通过光催化反应将其矿化后生成无毒无害的小分子物质,因此半导体光催化技术已成为一种有望缓解环境污染的先进技术,在这项技术中光催化剂为核心技术问题。卤氧化铋是近年来发展起来的新型光催化剂,价廉易得且环境友好,但其本身光催化活性较弱,光生电子空穴对的高复合率,太阳光利用率低等,是其实际应用的一个障碍。通过掺杂离子、构建异质结、引入氧空位和用贵金属修饰等被认为是提高其光催化性能的途径。卤氧化铋可以通过工艺调控使其全部出现氧空位,例如在中国专利CN112569969A中,公开了一种含光控氧空位BiOBr光催化剂的制备方法,该方法以五水硝酸铋和溴酸钠为原料,调节反应温度,利用一步水解法制得含光控氧空位的BiOBr材料。在中国专利CN112717958A中,公开了一种富含氧空位BiOBr/HNbO纳米片光催化剂的制备方法与用途。采用自组装法制备具有三维-二维界面的BiOBr-V/HNbO纳米片Z型异质结复合光催化剂。通常来讲,氧空位在富氧条件下,非常容易还原,不易长时间保存。
本发明利用水热法、光沉积和紫外可见光驱动法制备部分出现氧空位的溴氧化铋涂料,涂料具有优异的光催化活性,该制备方法生产成本低、反应条件温和、易于规模化生产、能够显著提高对可见光的吸收率、氧空位能够长时间保存,在国内外文献中尚未有报道。
发明内容
本发明的目的在于提供一种部分出现氧空位的溴氧化铋的制备方法。本发明的另一目的在于提供一种表面氧空位改性的溴氧铋光催化剂,此光催化剂能够有效促进电子-空穴对的有效分离,提高对可见光的利用率,光催化性能优异。本发明解决其技术问题是采用以下技术方案来实现的。
1.一种部分出现氧空位的溴氧化铋的制备方法,其特征在于:所制备的材料由BiOBr、含氧空位的BiOBr和Pt组成的三元结构,其中溴氧化铋晶体结构为四方相,为(110)面择优取向,在暴露面上均匀地覆盖铂颗粒,在铂颗粒的下部的BiOBr不含氧空位,在铂颗粒未覆盖部位的BiOBr含氧空位,并且氧空位能够长时间保存。具体包括以下制备步骤:
步骤1,所述水热法制备的部分出现氧空位的溴氧化铋具体为:将一定量的 Bi(NO)3·5H2O、PVP和KBr溶解在去离子水中,分别分散于24~36mL去离子水中,磁力搅拌30~60min后,分别形成溶液A和B。将溶液B逐滴加入溶液A中,滴加完后继续磁力搅拌1~2h。Bi(NO)3·5H2O、PVP和KBr的质量比为1:0.020:0.245。
步骤2,将搅拌后的溶液投入反应釜中,在140~180℃下水热反应12~18小时,将沉淀过滤、洗涤后获得沿(110)面择优取向BiOBr粉体;
步骤3,将所述步骤2获得的BiOBr粉体,在避光条件下加入到去离子水中,之后滴加氯铂酸钾溶液,滴加完后继续搅拌,开启氙灯后持续搅拌一段时间。将沉淀过滤、洗涤后得到负载铂的BiOBr粉体;
步骤4,将步骤3中获得的负载铂的BiOBr粉体,加入到有机溶液中,在氙灯照射下,持续搅拌一段时间。将沉淀过滤、洗涤后得到BiOBr、BiOBr-OVs、Pt三元构成的 BiOBr。
本发明的基本原理:
酸性条件下制备出晶面(110)择优取向的溴氧化铋,暴露在最外层的为卤素层,而卤素层结构稳定。在本发明中溴氧化铋表面负载上金属铂,在光照过程中金属铂所负载的区域下的溴氧化铋,不受到光照影响,没有获得能量Bi-O键不会发生断裂,因此负载金属铂的区域的溴氧化铋没有获得能量,不发生改变,不产生氧空位,而在铂颗粒未覆盖区域的溴氧化铋得到光照能量,Bi-O键断裂,形成氧空位。从而实现制备出部分出现氧空位的溴氧化铋。
与现有技术相比,本发明具有以下有益效果:
(1)本发明所用的原料易得,降低生产成本。
(2)本发明采用水热法紫外可见光驱动法相结合制备了部分出现氧空位的溴氧化铋光催化剂,由于其具有优秀的光催化性能,且无毒无害,可以作为一种环保涂料使用。
(3)本发明制备的部分出现氧空位的溴氧化铋具有生产成本低,制备周期短等优点,具有较强的市场应用前景。
附图说明
图1是本发明实施例1的XRD衍射图谱。
图2是本发明对比例1-3的XRD衍射图谱。
图3是本发明实施例1和对比例1中制备产品的光催化降解甲基橙性能图。实施例1降解甲基橙的效果比对比例1提高了38.9%。
图4是本发明实施例1和对比例1中制备产品的光催化产氢性能图。实施例1的光催化产氢性能明显提高
图5是本发明实施例中制备产品的高倍透射电镜图。
图6是本发明实施例中制备产品的理论示意图。
具体实施方式
下面结合附图和本发明优选的具体实施例对本发明做进一步描述,原料均为分析纯。
实施例1:
步骤1,将一定量的碱式硝酸铋和聚乙烯吡咯烷酮溶解在去离子水中,加入溴化钾溶液,其中碱式硝酸铋、PVP和溴化钾的质量比为1:0.020:0.245;
步骤2,将所述步骤1获得的溶液搅拌1小时;
步骤3,将搅拌后的溶液投入反应釜中,在160℃下水热反应12小时,将沉淀过滤、洗涤后获得沿(110)面择优取向BiOBr粉体;
步骤4,将所述步骤3获得的BiOBr粉体,在避光条件下加入70mL去离子水中与20mL的0.047M氯铂酸钾溶液混合搅拌1小时,之后在氙灯照射下持续搅拌3小时。将沉淀过滤、洗涤后得到负载铂的BiOBr粉体;
步骤5,将所述步骤4获得的负载铂的BiOBr粉体,加入到100mL的99.6%甲醇溶液中,在氙灯照射下持续搅拌3小时。将沉淀过滤、洗涤后得到部分出现氧空位的BiOBr。
对比例1
步骤1,将一定量的碱式硝酸铋和聚乙烯吡咯烷酮溶解在去离子水中,加入溴化钾溶液,其中碱式硝酸铋、PVP和溴化钾的质量比为1:0.020:0.245;
步骤2,将所述步骤1获得的溶液搅拌1小时;
步骤3,将搅拌后的溶液投入反应釜中,在160℃下水热反应12小时,将沉淀过滤、洗涤后获得沿(110)面择优取向BiOBr粉体。
对比例2
步骤1,将一定量的碱式硝酸铋和聚乙烯吡咯烷酮溶解在去离子水中,加入溴化钾溶液,其中碱式硝酸铋、PVP和溴化钾的质量比为1:0.020:0.245;
步骤2,将所述步骤1获得的溶液搅拌1小时;
步骤3,将搅拌后的溶液投入反应釜中,在160℃下水热反应12小时,将沉淀过滤、洗涤后获得沿(110)面择优取向BiOBr粉体。
步骤4,将所述步骤3获得的BiOBr粉体,在避光条件下加入70mL去离子水中与20mL的 0.047M的氯铂酸钾溶液混合搅拌1小时,之后在氙灯照射下持续搅拌3小时。将沉淀过滤、洗涤后得到负载铂的BiOBr粉体;
对比例3
步骤1,将一定量的碱式硝酸铋和聚乙烯吡咯烷酮溶解在去离子水中,加入溴化钾溶液,其中碱式硝酸铋、PVP和溴化钾的质量比为1:0.020:0.245;
步骤2,将所述步骤1获得的溶液搅拌1小时;
步骤3,将搅拌后的溶液投入反应釜中,在160℃下水热反应12小时,将沉淀过滤、洗涤后获得沿(110)面择优取向BiOBr粉体。
步骤4,将所述步骤3获得的BiOBr,加入到100mL的99.6%甲醇溶液中,在氙灯照射下持续搅拌3小时。将沉淀过滤、洗涤后得到完全出现氧空位的BiOBr。
应用例1:
对实施列1、对比例1-3中所制得的部分出现氧空位的BiOBr、BiOBr、负载Pt的BiOBr 和完全出现氧空位的BiOBr进行降解甲基橙和产氢光催化活性评价,具体操作步骤为:
对实施例1和对比例1-3中所制得的部分出现氧空位的BiOBr、BiOBr、BiOBr-Pt和BiOBr-OVs分别称量光催化剂10mg,分别与甲基橙溶液(100mL,10mg·L-1)混合后,在黑暗条件下搅拌30分钟,开启500W氙灯照,每隔30分钟取一次反应液,通过离心、过滤,测试溶液的吸光度,利用吸光度的变化测试光催化剂对甲基橙的脱色率情况。
对实施例1和对比例1-3中所制得的部分出现氧空位的BiOBr、BiOBr、BiOBr-Pt和BiOBr-OVs分别称量光催化剂10mg,分别加入到48mL去离子水和2mL甲醇中,通过 labsolar6A系统检测实施列1和对比例1-3氢气产生量。
以上所述内容仅为本发明构思下的基本说明,通过阅读本发明说明书而对本发明技术方案采取的任何等效的变换,只要不脱离本发明技术方案的精神和范围,均应属本发明的保护范围。
Claims (7)
1.一种含氧空位溴氧化铋的制备方法,其特征在于:所制备的材料由BiOBr、含氧空位的BiOBr和Pt组成的三元结构,其中溴氧化铋晶体结构为四方相,为(110)面择优取向,在暴露面上均匀地覆盖铂颗粒,在铂颗粒的下部的BiOBr不含氧空位,在铂颗粒未覆盖部位的BiOBr含氧空位。具体包括以下制备步骤:
步骤1,所述水热法制备的部分出现氧空位的溴氧化铋具体为:将一定量的Bi(NO)3·5H2O、PVP和KBr溶解在去离子水中,分别分散于24~36mL去离子水中,磁力搅拌30~60min后,分别形成溶液A和B。将溶液B逐滴加入溶液A中,滴加完后继续磁力搅拌一段时间。
步骤2,将混合好的溶液转移至聚四氟乙烯反应釜中,水热反应一定时间,将沉淀洗涤、干燥、研磨后获得(110)面取向的BiOBr粉体。
步骤3,将步骤3中获得的BiOBr粉体,在避光条件下加入去离子水中搅拌30min后,滴加氯铂酸钾溶液,滴加完后继续搅拌30min,开启氙灯后继续搅拌3~4h后,获得负载Pt的BiOBr粉体。
步骤4,将步骤4中获得的负载铂的BiOBr粉体,加入到含有有机溶剂的溶液中,在氙灯照射下持续搅拌3~4h。将沉淀过滤、洗涤后得到由BiOBr、含氧空位的BiOBr和Pt组成的三元结构。
2.根据权利要求1所述的制备方法,步骤1其特征在于:所述的Bi(NO)3·5H2O、PVP和KBr的质量比为1:0.020:0.245,搅拌至溶解均匀。溶液A和B的体积分别为24mL和36mL。磁力搅拌为1~2h。
3.根据权利要求1所述的制备方法,步骤2其特征在于:所述加热温度为140~180℃,所述加热时间为12~18h,所述烘干温度为60~80℃,所述烘干时间为12~24h。
4.根据权利要求1所述的制备方法,步骤3其特征在于:氯铂酸钾溶液浓度为0.047M,滴加量为20mL,滴加速度为0.097mL·s-1。
5.根据权利要求1所述的制备方法,步骤5其特征在于:使用有机溶剂为甲醇,浓度为99.6%,使用量为100mL。
6.如权利要求1-5任一制备方法得到的部分出现氧空位的溴氧化铋光催化剂。
7.如权利要求1-5任一制备方法得到的部分出现氧空位的溴氧化铋光催化剂在光催化降解和产氢的应用。
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