CN112517030A - 一种层层替换BSO-BiOXmYn复合光催化剂的制备方法 - Google Patents
一种层层替换BSO-BiOXmYn复合光催化剂的制备方法 Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052794 bromium Inorganic materials 0.000 claims abstract description 10
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 10
- 229910052740 iodine Inorganic materials 0.000 claims abstract description 10
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 claims description 60
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 52
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 52
- 238000003756 stirring Methods 0.000 claims description 29
- 239000011780 sodium chloride Substances 0.000 claims description 26
- 235000009518 sodium iodide Nutrition 0.000 claims description 18
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 5
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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 abstract description 3
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Abstract
一种层层替换BSO‑BiOXmYn(X,Y∈Cl,Br,I)复合光催化剂及其制备方法，通过共享[Bi2O2]2+层，引入卤素，调整材料的结构。卤素离子取代偏硅酸根离子后，与[Bi2O2]2+层交替，该结构可提供内部静电场，为光生载流子的分离提供驱动力，大大提高其光催化性能。同时通过不同离子的调节，可有效调节材料的电子带隙位置，形成双异质结构，更好地调节所需要的异质结构。制备出的BSO‑BiOXmYn复合光催化剂，在具备较高吸附效果的同时又兼具可降解有机阳离子型染料罗丹明B、阴离子型甲基橙以及抗生素盐酸四环素的效果，能够大大提升水体污染处理效率。该制备过程较传统水热法更安全，生产工艺更简单、周期更短。
Description
技术领域
本发明属于材料技术领域，特别涉及一种层层替换BSO-BiOXmYn(X,Y∈Cl,Br,I)复合光催化剂的制备方法。
背景技术
铋系半导体光催化剂由于其合适的禁带宽度，特殊的层状结构等特征，能够响应可见光，具有光催化性能。但由于大多单一的铋系氧化物半导体均存在禁带宽度过宽或过窄的情况，使其响应波长范围不足。卤氧化铋BiOXmYn(X＝Cl，Br，I)属于Aurivillius族材料，其具有的层状结构可以提供内部静电场，为光生载流子的分离提供驱动力。在BiOXmYn中，由于排列原因，卤素原子容易相互替换。这使得BiOXmYn中Cl，Br，I几乎可以以任意比例存在。现有技术所制备材料存在制备周期长、团聚严重等问题，同时所制备材料无法通过调控兼顾不同类型有机物的降解。
发明内容
为了克服上述现有技术的缺点，本发明的目的在于提供一种层层替换BSO-BiOXmYn(X,Y∈Cl,Br,I)复合光催化剂的制备方法，较传统水热法更安全，生产工艺更简单、周期更短，所得光催化剂在具备较高吸附效果的同时又兼具可降解有机染料罗丹明B、甲基橙以及抗生素盐酸四环素的效果。
为了实现上述目的，本发明采用的技术方案是：
一种层层替换BSO-BiOXmYn复合光催化剂的制备方法，X、Y均为Cl,Br,I中的任一种，且X、Y不为同一种，0＜m＜1，0＜n＜1，且m+n＝1；
其特征在于，包括如下步骤：
步骤1)，分别称取氯化钠、溴化钠、碘化钠加入水中搅拌至溶解，超声5min～10min，分散均匀，分别获得氯化钠溶液、溴化钠溶液和碘化钠溶液，氯化钠溶液、溴化钠溶液和碘化钠溶液的物质的量浓度均控制在1mol/L～1.5mol/L；
步骤2)，将无水乙醇与去离子水以体积比为(1.5～2):1混合，加入1.3g～1.6g柠檬酸，溶解充分后，按铋:硅为(5～7):1加入硝酸铋和正硅酸乙酯总计2.8-3g，待充分溶解后，加入1.8g～2.5g聚乙二醇，搅拌1h后在80℃～90℃下水浴蒸发3h～4h，并于150℃～160℃下干燥7h～10h，最后在600℃～650℃煅烧2h～5h，得到BSO粉体；
步骤3)，配制质量浓度7mg/mL～10mg/mL的BSO溶液，搅拌2h～3h，用硝酸将pH调节为1～3后继续搅拌20min～30min获得B液；
步骤4)，按氯化钠溶液和溴化钠溶液体积比为4:1～12：1量取溶液共4mL～8mL加入B液中，搅拌30min后得到C1溶液；或按溴化钠溶液和碘化钠溶液体积比为4:1～12：1量取溶液共4mL～8mL加入B液，搅拌30min后得到C2溶液；或按氯化钠溶液和碘化钠溶液体积比4:1～12：1量取溶液共4mL～8mL加入B液，搅拌30min后得到C3溶液；
步骤5)，将C1溶液、C2溶液或C3溶液经过离心，水洗，醇洗，随后在70℃～90℃下热处理10h～20h，获得BSO-BiOXmYn复合光催化剂。
与现有技术相比，本发明的有益效果是：
本发明提供的一种层层替换BSO-BiOXmYn(X,Y∈Cl,Br,I)复合光催化剂及其制备方法，通过共享[Bi2O2]2+层，引入卤素，调整材料的结构。卤素离子取代偏硅酸根离子后，与[Bi2O2]2+层交替，该结构可提供内部静电场，为光生载流子的分离提供驱动力，大大提高其光催化性能。同时通过不同离子的调节，可有效调节材料的电子带隙位置，形成双异质结构，更好地调节所需要的异质结构。制备出的BSO-BiOXmYn复合光催化剂，在具备较高吸附效果的同时又兼具可降解有机阳离子型染料罗丹明B、阴离子型甲基橙以及抗生素盐酸四环素的效果，能够大大提升水体污染处理效率。该制备过程较传统水热法更安全，生产工艺更简单、周期更短。
附图说明
图1是实施例1所得C1对20mg/L RhB吸附/催化性能图。
图2是实施例2所得C2对10mg/L MO吸附/催化性能图。
图3是实施例3所得C3对10mg/L TCH吸附/催化性能图。
具体实施方式
下面结合附图和实施例详细说明本发明的实施方式。
本发明以卤化盐为卤源，加入到BSO体系中，调节溶液pH，反应充分后，经过离心，水洗，醇洗，热处理后制备出一种层层替换BSO-BiOXmYn(X,Y∈Cl,Br,I)光催化剂。该复合催化剂较传统水热法更安全，生产工艺更简单、周期更短，所得光催化材料粉体表现出高的光催化性能。本发明提供如下具体实施例：
实施例1
一种层层替换BSO-BiOCl0.8Br0.2复合光催化剂的制备方法，步骤如下：
(1)称取一定量的氯化钠、溴化钠(其物质的量浓度控制在1.1mol/L)搅拌至溶解，超声5min，分散均匀，分别获得氯化钠溶液、溴化钠溶液；
(2)将无水乙醇与去离子水以体积比为1.5:1混合，加入1.3g柠檬酸，溶解充分后，按铋:硅为4:1加入硝酸铋和正硅酸乙酯，待充分溶解后，加入1.8g聚乙二醇，搅拌1h后在82℃下水浴蒸发2h，并于150℃下干燥7h，最后将其在600℃煅烧2h，得到BSO粉体；
(3)称取一定量BSO粉体，加入去离子水中(其质量浓度控制在7mg/mL)，搅拌2h，用硝酸将pH调节为2后继续搅拌20min为B液；
(4)按一定体积比量取氯化钠溶液、溴化钠溶液(V氯化钠：V溴化钠＝4：1)共4mL加入B液中，搅拌30min后得到C1溶液；
(5)将C1溶液经过离心，水洗，醇洗等步骤，随后在70℃下热处理10h，获得C1复合光催化剂。
图1是由实例1制得的光催化剂C1对20mg/L RhB吸附/催化性能图，可看出其具有较好的吸附催化性能，30mgC1对于30mL 20mg/L RhB溶液能够做到60min内吸附超过40％，30min催化超过90％的吸附/催化效果。
实施例2
一种层层替换BSO-BiOCl0.5I0.5复合光催化剂的制备方法，步骤如下：
(1)称取一定量的氯化钠、碘化钠(其物质的量浓度控制在1.2mol/L)搅拌至溶解，超声5min，分散均匀，分别获得氯化钠溶液、溴化钠溶液；
(2)将无水乙醇与去离子水以体积比为1.6:1混合，加入1.4g柠檬酸，溶解充分后，按铋:硅为6:1加入硝酸铋和正硅酸乙酯，待充分溶解后，加入1.9g聚乙二醇，搅拌1h后在84℃下水浴蒸发2h，并于155℃下干燥8h，最后将其在620℃煅烧3h，得到BSO粉体；
(3)称取一定量BSO粉体，加入去离子水中(其质量浓度控制在8mg/mL)，搅拌2h，用硝酸将pH调节为3后继续搅拌20min为B液；
(4)按一定体积比量取氯化钠溶液、溴化钠溶液(V氯化钠：V碘化钠＝1：1)共6mL加入B液中，搅拌30min后得到C2溶液；
(5)将C1，C2，C3溶液经过离心，水洗，醇洗，随后在80℃下热处理10h，C2复合光催化剂。
图2是由实例2制得的光催化剂C2对10mg/L MO吸附/催化性能图，可看出其具有较好的吸附催化性能，30mgC2对于30mL 10mg/L MO溶液能够做到60min内吸附超过10％，60min催化超过90％的吸附/催化效果。
实施例3
一种层层替换BSO-BiOBr0.923I0.077复合光催化剂的制备方法，步骤如下：
(1)称取一定量的溴化钠、碘化钠(其物质的量浓度控制在1.4mol/L)搅拌至溶解，超声5min，分散均匀，分别获得氯化钠溶液、溴化钠溶液；
(2)将无水乙醇与去离子水以体积比为2:1混合，加入1.6g柠檬酸，溶解充分后，按铋:硅为7:1加入硝酸铋和正硅酸乙酯，待充分溶解后，加入2.5g聚乙二醇，搅拌1h后在88℃下水浴蒸发2h，并于160℃下干燥8h，最后将其在650℃煅烧3h，得到BSO粉体；
(3)称取一定量BSO粉体，加入去离子水中(其质量浓度控制在10mg/mL)，搅拌2h，用硝酸将pH调节为3后继续搅拌20min为B液；
(4)按一定体积比量取氯化钠溶液、溴化钠溶液(V溴化钠：V碘化钠＝12：1)共8mL加入B液中，搅拌30min后得到C3溶液；
(5)将C1，C2，C3溶液经过离心，水洗，醇洗，随后在90℃下热处理10h，获得C3复合光催化剂。
图3是由实例3制得的光催化剂C3对10mg/L TCH吸附/催化性能图，可看出其具有较好的吸附催化性能，30mgC3对于30mL 10mg/L TCH溶液能够做到60min内吸附超过30％，60min催化超过75％的吸附/催化效果。
Claims (2)
1.一种层层替换BSO-BiOXmYn复合光催化剂的制备方法，X、Y均为Cl,Br,I中的任一种，且X、Y不为同一种，0＜m＜1，0＜n＜1，且m+n＝1；
其特征在于，包括如下步骤：
步骤1)，分别称取氯化钠、溴化钠、碘化钠加入水中搅拌至溶解，超声5min～10min，分散均匀，分别获得氯化钠溶液、溴化钠溶液和碘化钠溶液；
步骤2)，将无水乙醇与去离子水以体积比为(1.5～2):1混合，加入1.3g～1.6g柠檬酸，溶解充分后，按铋:硅为(5～7):1加入硝酸铋和正硅酸乙酯总计2.8-3g，待充分溶解后，加入1.8g～2.5g聚乙二醇，搅拌1h后在80℃～90℃下水浴蒸发3h～4h，并于150℃～160℃下干燥7h～10h，最后在600℃～650℃煅烧2h～5h，得到BSO粉体；
步骤3)，配制质量浓度7mg/mL～10mg/mL的BSO溶液，搅拌2h～3h，用硝酸将pH调节为1～3后继续搅拌20min～30min获得B液；
步骤4)，按氯化钠溶液和溴化钠溶液体积比为4:1～12：1量取溶液共4mL～8mL加入B液中，搅拌30min后得到C1溶液；或按溴化钠溶液和碘化钠溶液体积比为4:1～12：1量取溶液共4mL～8mL加入B液，搅拌30min后得到C2溶液；或按氯化钠溶液和碘化钠溶液体积比4:1～12：1量取溶液共4mL～8mL加入B液，搅拌30min后得到C3溶液；
步骤5)，将C1溶液、C2溶液或C3溶液经过离心，水洗，醇洗，随后在70℃～90℃下热处理10h～20h，获得BSO-BiOXmYn复合光催化剂。
2.根据权利要求1所述层层替换BSO-BiOXmYn(X,Y∈Cl,Br,I)复合光催化剂的制备方法，其特征在于，所述步骤1)中，氯化钠溶液、溴化钠溶液和碘化钠溶液的物质的量浓度均控制在1mol/L～1.5mol/L。
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