CN110586181A - 室温固相研磨法制备的HCOOBiO光催化剂及其方法 - Google Patents
室温固相研磨法制备的HCOOBiO光催化剂及其方法 Download PDFInfo
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- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 claims abstract description 25
- 235000019254 sodium formate Nutrition 0.000 claims abstract description 25
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- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 14
- 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 claims abstract description 12
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 12
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- 230000000694 effects Effects 0.000 abstract description 13
- 229910052797 bismuth Inorganic materials 0.000 abstract description 11
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 abstract description 11
- 239000002159 nanocrystal Substances 0.000 abstract description 4
- 239000004280 Sodium formate Substances 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 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 abstract description 2
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 abstract 3
- 150000001621 bismuth Chemical class 0.000 abstract 1
- 239000003344 environmental pollutant Substances 0.000 abstract 1
- 231100000719 pollutant Toxicity 0.000 abstract 1
- 239000000843 powder Substances 0.000 abstract 1
- 239000007787 solid Substances 0.000 abstract 1
- 230000015556 catabolic process Effects 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- 238000006731 degradation reaction Methods 0.000 description 10
- 230000005540 biological transmission Effects 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
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- 238000002441 X-ray diffraction Methods 0.000 description 3
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- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 2
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- HWSISDHAHRVNMT-UHFFFAOYSA-N Bismuth subnitrate Chemical compound O[NH+]([O-])O[Bi](O[N+]([O-])=O)O[N+]([O-])=O HWSISDHAHRVNMT-UHFFFAOYSA-N 0.000 description 1
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 description 1
- 229930195725 Mannitol Natural products 0.000 description 1
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
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- 239000010457 zeolite Substances 0.000 description 1
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Abstract
本发明涉及一种室温研磨制备的HCOOBiO光催化剂及其方法，其步骤为：将五水硝酸铋与甲酸钠固体粉末置于研钵中，常温下研磨，反应结束洗涤后即得圆片状在可见光下具有光催化性能的甲酸氧铋纳米晶；将所述甲酸氧铋纳米晶直接加入碘化钾继续研磨，反应结束后洗涤即得改性的甲酸氧铋。未掺杂的甲酸氧铋具有很好的结晶度，掺杂后的甲酸氧铋在降解模拟污染物罗丹明B时具有很好效果，表明其在环境污染治理方面具有良好的应用前景。
Description
技术领域
本发明涉及一种室温研磨制备的HCOOBiO光催化剂及其方法，属于无机纳米材料制备领域。
背景技术
随着环境污染问题的日益严重，研究光催化剂降解治理环境污染成为愈来愈火热的课题。近年来，Bi基半导体光催化剂受到更多的关注，如BiVO4，Bi2WO6等，Bi的氧化物具有[Bi2O2]2+层状结构，使其可自组装成不同形貌。其中BiOX(X＝Cl，Br，I)，Bi2O3，Bi2O2CO3等被较多报道，然而，关于甲酸氧铋(HCOOBiO)的合成研究相对不足。由于[Bi2O2]2+是由双层的羧基离子组成的沸石层状结构，因此类似于由[Bi2O2]2+组成的HCOOBiO结构也为层状结构，类似于Sillen系材料，并且已发现其在光催化降解染料方面具有较好的性能。
甲酸氧铋具有良好的紫外光催化性能，Zhang等人采用以硝酸铋为原料，DMF作为反应物，水作为溶剂，在120℃下水热制得细棒状HCOOBiO；Xiong等人以甲酸钠及硝酸铋为原料，分别以甘露醇、EG、DEG、TEG为溶剂在150℃下水热制得HCOOBiO，所制得HCOOBiO均为纳米片组装形成的花状结构。
而花状及其他形貌的甲酸氧铋只在紫外光下有光催化效果，为了提高其光催化响应范围，我们采用研磨法合成了花状甲酸氧铋，使其在可见光范围内(390-780nm)也有响应。
发明内容
本发明的目的在于提供一种独特形貌的HCOOBiO光催化剂及其制备方法。
本发明的另一目的是提供一种基于HCOOBiO的可见光催化组合物及其制备方法。
实现本发明目的的技术解决方案为：一种独特形貌的HCOOBiO光催化剂，所述HCOOBiO为圆片状。
优选的，所述的HCOOBiO在可见光下具有光催化性能。
优选的，所述的HCOOBiO通过研磨法制备。
利用固相研磨法制备上述具有独特形貌的HCOOBiO光催化剂的方法，包括以下步骤：
步骤一：将Bi(NO3)3·5H2O与HCOONa置于研钵中研磨；
步骤二：反应结束后洗涤、干燥即得圆片状HCOOBiO。
优选的，Bi(NO3)3·5H2O与HCOONa的摩尔比为1：2至1：10，更优选为1：5
优选的，研磨时间为不少于30min。
一种可见光催化组合物，将圆片状的HCOOBiO与KI通过研磨法制得。
上述可见光催化组合物的制备方法，包括如下步骤：
步骤一：将Bi(NO3)3·5H2O与HCOONa置于研钵中研磨；
步骤二：加入KI继续研磨；
步骤三：反应结束后洗涤、干燥即得光催化组合物。
优选的，步骤一和步骤二中的研磨时间均不少于30min。
优选的，Bi(NO3)3·5H2O与HCOONa与KI三者的摩尔比为1：5：0.2。
上述HCOOBiO光催化剂或可见光催化组合物在降解废水中的有机污染物中的应用，优选的，有机污染物为罗丹明B。
与现有技术相比，本发明有以下显著优点：
1、方法简单，实验周期短，节约时间。无需加入任何模板剂，仅使用五水硝酸铋及甲酸钠两种原料得到了HCOOBiO纳米晶。
2、所制得的HCOOBiO纳米晶为圆片状。
3、该纳米晶经KI掺杂改性后对罗丹明B(Rh B)表现出优异的可见光催化降解性能，有望在工业废水治理领域具有良好的应用。
附图说明
图1为本发明制备圆片状HCOOBiO的流程示意图。
图2为本发明所得HCOOBiO的透射电镜图片。
图3为现有技术所述的细棒状HCOOBiO透射电镜图片。
图4为本发明所得HCOOBiO掺杂0.2mmol KI的样品透射电镜图片。
图5为本发明所得HCOOBiO及其掺杂不同含量KI后的样品对10mg/L罗丹明B的降解率图。
图6为实施例1(Bi(NO3)3·5H2O与HCOONa摩尔比为1:5，研磨时间为1小时)所得样品XRD谱图。
图7为实施例2(Bi(NO3)3·5H2O与HCOONa摩尔比为1:5，研磨0.5小时后加入0.2mmolKI继续研磨0.5小时)所得样品XRD谱图。
图8为对比例1(Bi(NO3)3·5H2O与HCOONa摩尔比为1:5，研磨时间为0.5小时)所得样品XRD谱图。
图9为对比例2(Bi(NO3)3·5H2O与HCOONa摩尔比为1:10，研磨时间为1小时)所得样品XRD谱图。
图10为对比例6(Bi(NO3)3·5H2O与HCOONa摩尔比为1:5，研磨0.5小时后加入1mmolKI继续研磨0.5小时)所得样品XRD谱图。
具体实施方式
下面结合附图和具体实施方式对本发明作进一步详细说明。
结合图1，本发明利用研磨法制备具有独特形貌的改性HCOOBiO催化剂的方法，
其特征包括以下步骤：
步骤一：将Bi(NO3)3·5H2O与HCOONa置于研钵中研磨；
步骤二：研磨一定时间后直接加入KI继续研磨；
步骤三：反应结束后洗涤即得改性HCOOBiO。
下面结合实施例、对比例和附图对本发明做进一步详细的说明：
实施例1：
步骤一：将1mmol Bi(NO3)3·5H2O与5mmol HCOONa置于研钵中研磨1h；
步骤二：反应结束后洗涤即得圆片状HCOOBiO。
所得产物透射电镜图片如图2所示，为圆片状，有团聚现象。图4显示其对罗丹明B的降解效果，可以看出有效果但不理想。图8为其XRD谱图，谱图显示产物结晶度较好，但存在少量杂质，经对比杂质为碱式硝酸铋。做为对比，图3为文献中报道的细棒状HCOOBiO透射电镜图片，其只在紫外光下有响应。
实施例2：
步骤一：将1mmol Bi(NO3)3·5H2O与5mmol HCOONa置于研钵中研磨；
步骤二：研磨0.5h后直接加入0.2mmol KI继续研磨0.5h；
步骤三：反应结束后洗涤即得改性HCOOBiO。
所得产物透射电镜如图4所示，还是圆片状，但颗粒体积变小，团聚加重。图5显示其对罗丹明B的降解效果，可看出效果较未掺杂的样品明显增强，两个小时内对罗丹明B的降解率达98％。图9为其XRD谱图，谱图显示掺杂后结晶度下降，但杂质消失。
对比例1：
步骤一：将1mmol Bi(NO3)3·5H2O与5mmol HCOONa置于研钵中研磨0.5h；
步骤二：反应结束后洗涤即得圆片状HCOOBiO。
所得产物XRD谱图如图6所示，可以看出结晶度下降，而杂质依旧存在。
对比例2：
步骤一：将1mmol Bi(NO3)3·5H2O与10mmol HCOONa置于研钵中研磨1h；
步骤二：反应结束后洗涤即得圆片状HCOOBiO。
所得产物XRD谱图如图7所示，谱图显示结晶度更差，杂质也消除。
对比例3：
步骤一：将1mmol Bi(NO3)3·5H2O与5mmol HCOONa置于研钵中研磨；
步骤二：研磨0.5h后直接加入0.1mmol KI继续研磨0.5h；
步骤三：反应结束后洗涤即得改性HCOOBiO。
所得产物对罗丹明B的降解效果如图5所示，效果比实施例1明显要好，但差于实施例2。
对比例4：
步骤一：将1mmol Bi(NO3)3·5H2O与5mmol HCOONa置于研钵中研磨；
步骤二：研磨0.5h后直接加入0.3mmol KI继续研磨0.5h；
步骤三：反应结束后洗涤即得改性HCOOBiO。
所得产物对罗丹明B的降解效果如图5所示，效果与实施例2接近。
对比例5：
步骤一：将1mmol Bi(NO3)3·5H2O与5mmol HCOONa置于研钵中研磨；
步骤二：研磨0.5h后直接加入0.5mmol KI继续研磨0.5h；
步骤三：反应结束后洗涤即得改性HCOOBiO。
所得产物对罗丹明B的降解效果如图5所示，效果与实施例2接近。
对比例6：
步骤一：将1mmol Bi(NO3)3·5H2O与5mmol HCOONa置于研钵中研磨；
步骤二：研磨0.5h后直接加入1.0mmol KI继续研磨0.5h；
步骤三：反应结束后洗涤即得改性HCOOBiO。
所得产物对罗丹明B的降解效果如图5所示，效果与实施例2差不多，不过前期效果好于实施例2。其XRD谱图如图10所示，经对比，所得产物完全变成BiOI。
Claims (10)
1.一种独特形貌的HCOOBiO光催化剂，其特征在于，所述HCOOBiO为圆片状。
2.如权利要求1所述的HCOOBiO光催化剂，其特征在于，所述的HCOOBiO在可见光下具有光催化性能。
3.如权利要求1所述的HCOOBiO光催化剂，其特征在于，所述的HCOOBiO通过研磨法制备。
4.利用固相研磨法制备如权利要求1所述的独特形貌的HCOOBiO光催化剂的方法，包括以下步骤：
步骤一：将Bi(NO3)3·5H2O与HCOONa置于研钵中研磨；
步骤二：反应结束后洗涤、干燥即得圆片状HCOOBiO。
5.如权利要求4所述的方法，其特征在于，Bi(NO3)3·5H2O与HCOONa的摩尔比为1：2至1：10，更优选为1：5。
6.如权利要求4所述的方法，其特征在于，研磨时间为不少于30min。
7.一种可见光催化组合物，其特征在于，将如权利要求1-3任一所述的HCOOBiO与KI按摩尔比1:0.2混合后通过研磨法制得所述组合物。
8.如权利要求7所述的可见光催化组合物的制备方法，包括如下步骤：
步骤一：将Bi(NO3)3·5H2O与HCOONa置于研钵中研磨；
步骤二：加入KI继续研磨；
步骤三：反应结束后洗涤、干燥即得光催化组合物。
9.如权利要求8所述的方法，其特征在于，步骤一和步骤二中的研磨时间均不少于30min；Bi(NO3)3·5H2O与HCOONa与KI三者的摩尔比为1：5：0.2。
10.如权利要求1-3任一所述的HCOOBiO光催化剂或如权利要求7所述的可见光催化组合物在降解废水中的有机污染物中的应用，优选的，有机污染物为罗丹明B。
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