CN105776337B - 一种合成铌酸锰MnNb2O6纳米片的方法 - Google Patents
一种合成铌酸锰MnNb2O6纳米片的方法 Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 17
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 239000002253 acid Substances 0.000 title claims abstract description 10
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 10
- 239000011572 manganese Substances 0.000 title claims abstract description 10
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 10
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 88
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims abstract description 21
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims abstract description 21
- 239000011565 manganese chloride Substances 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 239000004094 surface-active agent Substances 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 150000002894 organic compounds Chemical class 0.000 claims abstract description 3
- HFQQZARZPUDIFP-UHFFFAOYSA-M sodium;2-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HFQQZARZPUDIFP-UHFFFAOYSA-M 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000012545 processing Methods 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 9
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 7
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 239000010955 niobium Substances 0.000 claims description 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 239000002904 solvent Substances 0.000 abstract description 14
- 229940099607 manganese chloride Drugs 0.000 abstract description 9
- 235000002867 manganese chloride Nutrition 0.000 abstract description 9
- 239000010865 sewage Substances 0.000 abstract description 8
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 abstract description 4
- 239000008204 material by function Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 28
- 239000000243 solution Substances 0.000 description 26
- 239000002244 precipitate Substances 0.000 description 14
- 235000011114 ammonium hydroxide Nutrition 0.000 description 7
- 239000011651 chromium Substances 0.000 description 7
- 238000001816 cooling Methods 0.000 description 7
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- 239000013078 crystal Substances 0.000 description 5
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- MZSDGDXXBZSFTG-UHFFFAOYSA-M sodium;benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1 MZSDGDXXBZSFTG-UHFFFAOYSA-M 0.000 description 4
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- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 description 1
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- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
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Abstract
一种合成铌酸锰MnNb2O6纳米片的方法，属于功能材料领域。利用氯化锰(MnCl2·4H2O)和表面活性剂混合物的乙醇溶液，乙醇溶剂热处理无定形相五氧化二铌可制得铌酸锰MnNb2O6纳米片；选用表面活性剂为含有磺酸基基团的有机化合物。所得产在六价铬离子的污水处理领域具有较好的应用前景。
Description
技术领域
本发明涉及一种合成铌酸锰MnNb2O6纳米片的方法,属于功能材料领域。
技术背景
当前，寻找价格低廉、容易合成的纳米结构材料应用于污水处理尤为迫切。锰元素在地球上储量丰富、易于获得，因此锰基氧化物成为污水处理材料的研究热点。另外，铌基化合物是典型的光催化剂，因此二者结合制备MnNb2O6纳米材料可以结合二者自身的优势，开发新型的直接领用太阳能的可见光光催化剂。研究表明，MnNb2O6纳米结构可通过吸收利用太阳光辐射，实现污水中有机、无机污染物的高效光降解移除。通过合成二维片状结构可进一步提高材料的比表面积，尤其是在纳米尺度厚度的片状结构表面构建众多的不饱和化学键以及氧空位，增强界面活性，从而大幅提高MnNb2O6的可见光催化性能，对于提升其光催化能力至关重要。
本发明中，通过控制反应条件，能够可控合成MnNb2O6纳米片。合成过程中发现表面活性剂分子在MnNb2O6纳米片表面的吸附能够实现MnNb2O6的晶面选择性结晶，暴露高活性的(131)晶面，从而大幅提高了MnNb2O6纳米片利用太阳光可见光波段光催化还原六价铬离子的能力，该方法也获得了一种依据有机大分子进行晶面选择性结晶制备铌酸盐纳米片状结构的新机制。
发明内容
本发明的目的是提供一种合成铌酸锰MnNb2O6纳米片的方法，利于批量制备在水处理领域和催化领域具有广泛应用前景的MnNb2O6纳米片状材料，可大大降低成本，提高效率，实际意义重大，利用获得的MnNb2O6纳米片进行可见光光还原重铬酸钾(含有六价的Cr)测试表明，其具有良好的污水处理性能。
本发明需要解决的是通过简便的反应参数控制而选择性可控合成MnNb2O6纳米片，从而提高反应效率，降低成本，以便大批量合成。
本发明涉及一种合成铌酸锰MnNb2O6纳米片的方法，其特征在于，包括以下步骤：
(1)首先用乙醇溶解氯化锰(MnCl2·4H2O)和表面活性剂的混合物；
(2)利用步骤(1)得到的乙醇溶液为反应前驱物，加入无定形相的五氧化二铌粉末，在密闭反应釜中热处理，温度为150-200℃，处理时间为18-48小时，制得MnNb2O6纳米片；
其中表面活性剂为含有磺酸基的有机化合物。表面活性剂为十二烷基苯磺酸钠(SDBS)或十二烷基硫酸钠SDS。
其中MnCl2·4H2O：表面活性剂：乙醇的用量关系为(0.3-0.5)g:(0.08-0.13)g:10ml。
其中进一步无定形相的五氧化二铌的制备，包括以下步骤：
将市售五氧化二铌粉末用氢氟酸配成悬浮液，加热溶解；所得的澄清液冷却后滴加与所用氢氟酸等体积的氨水，得到白色沉淀；此白色沉淀为无定形五氧化二铌。
利用步骤(1)得到的乙醇溶液为反应前驱物，进行热处理无定形相五氧化二铌，无定形相五氧化二铌与乙醇溶液体积的用量关系影响不大，优选步骤(1)中配制的乙醇溶液：无定形相五氧化二铌的用量关系10ml:(0.3-0.5)g。
进一步热处理温度优选180℃，处理时间为48小时。
采用本发明方法得到纳米片，多个纳米片聚合成一花状结构。
表面活性剂可以通过苯磺酸基基团吸附于MnNb2O6的(131)晶面，导致了暴露(131)面的MnNb2O6纳米片结晶。本发明可通过调节表面活性剂浓度实现纳米片厚度的调节，铌酸锰MnNb2O6纳米片可用于太阳可见光还原六价铬(Cr(VI))离子，在污水处理领域具有较大的应用前景。
本发明以氯化锰(MnCl2·4H2O)、表面活性剂十二烷基苯磺酸钠(SDBS)或十二烷基硫酸钠的乙醇溶液，经乙醇溶剂热处理无定形相五氧化二铌，从而可控制备MnNb2O6纳米片的方法，该方法证实了正交晶相的三元复合氧化物MnNb2O6通过结晶过程的化学调控，在溶液获得MnNb2O6纳米片结构的可操作性，所获得的MnNb2O6纳米片展现出了太阳可见光还原六价铬(Cr(VI))离子的优秀能力，在污水处理领域具有较大的应用前景。
本发明的有益效果是：本发明的制备方法所得的产品形貌可控，可重复性好，操作简单，成本低。上述优点使得MnNb2O6纳米片在污水处理领域具有较好的应用前景。
附图说明
图1：合成的MnNb2O6纳米片的X射线衍射图；
图2：MnNb2O6纳米片的扫描电镜图；
图3：MnNb2O6纳米片的透射电镜图；
图4：MnNb2O6纳米片用于可见光还原六价铬(Cr(VI))的性能曲线。
具体实施方式
下面结合实施例对本发明作进一步说明，但本发明并不限于以下实施例。
实施例1
(1)首先配制氯化锰(MnCl2·4H2O)和表面活性剂十二烷基苯磺酸钠(SDBS)的乙醇溶液，MnCl2·4H2O、SDBS与乙醇的用量关系为0.3g:0.08g:10ml；
(2)将市售五氧化二铌粉末用氢氟酸配成悬浮液，加热溶解；所得的澄清液冷却后滴加与所用氢氟酸等体积的氨水，得到白色沉淀；此白色沉淀为无定形五氧化二铌；利用步骤(1)得到的乙醇溶液为反应前驱物，乙醇溶剂热处理所得的上述无定形相五氧化二铌，步骤(1)中配制的乙醇溶液与无定形相五氧化二铌的用量关系0.3g:10ml。
(3)乙醇溶剂热处理温度为160℃，处理时间为18小时。
实施例2
(1)首先配制氯化锰(MnCl2·4H2O)和表面活性剂十二烷基硫酸钠(SDS)的乙醇溶液，MnCl2·4H2O、SDBS与乙醇的用量关系为0.3g:0.08g:10ml；
(2)将市售五氧化二铌粉末用氢氟酸配成悬浮液，加热溶解；所得的澄清液冷却后滴加与所用氢氟酸等体积的氨水，得到白色沉淀；此白色沉淀为无定形五氧化二铌；利用步骤(1)得到的乙醇溶液为反应前驱物，乙醇溶剂热处理所得的上述无定形相五氧化二铌，步骤(1)中配制的乙醇溶液与无定形相五氧化二铌的用量关系0.3g:10ml。
(3)乙醇溶剂热处理温度为160℃，处理时间为18小时。
实施例3
(1)首先配制氯化锰(MnCl2·4H2O)和表面活性剂十二烷基苯磺酸钠(SDBS)的乙醇溶液，MnCl2·4H2O、SDBS与乙醇的用量关系为0.4g:0.1g:10ml；
(2)将市售五氧化二铌粉末用氢氟酸配成悬浮液，加热溶解；所得的澄清液冷却后滴加与所用氢氟酸等体积的氨水，得到白色沉淀；此白色沉淀为无定形五氧化二铌；利用步骤(1)得到的乙醇溶液为反应前驱物，乙醇溶剂热处理所得的上述无定形相五氧化二铌，步骤(1)中配制的乙醇溶液与无定形相五氧化二铌的用量关系0.3g:10ml。
(3)乙醇溶剂热处理温度为180℃，处理时间为48小时。
实施例4
(1)首先配制氯化锰(MnCl2·4H2O)和表面活性剂十二烷基硫酸钠(SDS)的乙醇溶液，MnCl2·4H2O、SDBS与乙醇的用量关系为0.3g:0.1g:10ml；
(2)将市售五氧化二铌粉末用氢氟酸配成悬浮液，加热溶解；所得的澄清液冷却后滴加与所用氢氟酸等体积的氨水，得到白色沉淀；此白色沉淀为无定形五氧化二铌；利用步骤(1)得到的乙醇溶液为反应前驱物，乙醇溶剂热处理所得的上述无定形相五氧化二铌，步骤(1)中配制的乙醇溶液与无定形相五氧化二铌的用量关系0.5g:10ml。
(3)乙醇溶剂热处理温度为180℃，处理时间为36小时。
实施例5
(1)首先配制氯化锰(MnCl2·4H2O)和表面活性剂十二烷基硫酸钠(SDS)的乙醇溶液，MnCl2·4H2O、SDBS与乙醇的用量关系为0.5g:0.13g:10ml；
(2)将市售五氧化二铌粉末用氢氟酸配成悬浮液，加热溶解；所得的澄清液冷却后滴加与所用氢氟酸等体积的氨水，得到白色沉淀；此白色沉淀为无定形五氧化二铌；利用步骤(1)得到的乙醇溶液为反应前驱物，乙醇溶剂热处理所得的上述无定形相五氧化二铌，无定形相五氧化二铌与乙醇溶液体积的用量关系影响不大，优选步骤(1)中配制的乙醇溶液与无定形相五氧化二铌的用量关系0.5g:10ml。
(3)乙醇溶剂热处理温度为200℃，处理时间为48小时。
实施例6
(1)首先配制氯化锰(MnCl2·4H2O)和表面活性剂十二烷基苯磺酸钠(SDBS)的乙醇溶液，MnCl2·4H2O、SDBS与乙醇的用量关系为0.5g:0.13g:10ml；
(2)将市售五氧化二铌粉末用氢氟酸配成悬浮液，加热溶解；所得的澄清液冷却后滴加与所用氢氟酸等体积的氨水，得到白色沉淀；此白色沉淀为无定形五氧化二铌；利用步骤(1)得到的乙醇溶液为反应前驱物，乙醇溶剂热处理所得的上述无定形相五氧化二铌，无定形相五氧化二铌与乙醇溶液体积的用量关系影响不大，优选步骤(1)中配制的乙醇溶液与无定形相五氧化二铌的用量关系0.5g:10ml。
(4)乙醇溶剂热处理温度为200℃，处理时间为48小时。
其中以100mg/L重铬酸钾水溶液为例，MnNb2O6纳米片与重铬酸钾水溶液的用量关系0.02g：60ml，MnNb2O6纳米片用于可见光还原六价铬(Cr(VI))的性能曲线。
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做的任何修改，等同替换和改进等，均应包含在本发明的保护范围之内。
Claims (5)
1.一种合成铌酸锰MnNb2O6纳米片的方法，其特征在于，包括以下步骤：
(1)首先用乙醇溶解MnCl2·4H2O和表面活性剂的混合物；
(2)利用步骤(1)得到的乙醇溶液为反应前驱物，加入无定形相的五氧化二铌粉末，在密闭反应釜中热处理，温度为150-200℃，处理时间为18-48小时，制得MnNb2O6纳米片；
其中表面活性剂为含有磺酸基基团的有机化合物；
其中MnCl2·4H2O：表面活性剂：乙醇的用量关系为(0.3-0.5)g:(0.08-0.13)g:10ml。
2.按照权利要求1的方法，其特征在于，步骤(1)中配制的乙醇溶液：无定形相五氧化二铌的用量关系10ml:(0.3-0.5)g。
3.按照权利要求1的方法，其特征在于，表面活性剂为十二烷基苯磺酸钠SDBS或十二烷基硫酸钠SDS。
4.按照权利要求1的方法，其特征在于，热处理温度优选180℃，处理时间为48小时。
5.按照权利要求1的方法，其特征在于，多个铌酸锰MnNb2O6纳米片聚合成一花状结构。
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