CN106179230A - 一种磁性四氧化三铁纳米粒子‑石墨烯复合材料及其制备方法与应用 - Google Patents
一种磁性四氧化三铁纳米粒子‑石墨烯复合材料及其制备方法与应用 Download PDFInfo
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- CN106179230A CN106179230A CN201610878020.8A CN201610878020A CN106179230A CN 106179230 A CN106179230 A CN 106179230A CN 201610878020 A CN201610878020 A CN 201610878020A CN 106179230 A CN106179230 A CN 106179230A
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 239000002131 composite material Substances 0.000 title claims abstract description 67
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 45
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims description 16
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229940056319 ferrosoferric oxide Drugs 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 15
- 239000010865 sewage Substances 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 25
- 239000002202 Polyethylene glycol Substances 0.000 claims description 13
- 229920001223 polyethylene glycol Polymers 0.000 claims description 13
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 7
- 239000003344 environmental pollutant Substances 0.000 claims description 6
- 231100000719 pollutant Toxicity 0.000 claims description 6
- 229910001385 heavy metal Inorganic materials 0.000 claims description 5
- 229910001430 chromium ion Inorganic materials 0.000 claims description 4
- 231100000614 poison Toxicity 0.000 claims description 4
- 230000007096 poisonous effect Effects 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 239000011651 chromium Substances 0.000 abstract description 25
- 238000000034 method Methods 0.000 abstract description 24
- 239000002351 wastewater Substances 0.000 abstract description 13
- 230000008569 process Effects 0.000 abstract description 11
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052804 chromium Inorganic materials 0.000 abstract description 7
- 239000003054 catalyst Substances 0.000 abstract description 6
- 238000004064 recycling Methods 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 22
- 239000000243 solution Substances 0.000 description 16
- 238000001179 sorption measurement Methods 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
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- 230000000694 effects Effects 0.000 description 8
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- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 6
- 238000002835 absorbance Methods 0.000 description 6
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 238000007639 printing Methods 0.000 description 4
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- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
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- BTKKSDUIJSJYGN-UHFFFAOYSA-N C(C)O.C1(=CC=CC=C1)N(C(N(N)C1=CC=CC=C1)=O)N Chemical compound C(C)O.C1(=CC=CC=C1)N(C(N(N)C1=CC=CC=C1)=O)N BTKKSDUIJSJYGN-UHFFFAOYSA-N 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- ZRALSGWEFCBTJO-UHFFFAOYSA-N Guanidine Chemical compound NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
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- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
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- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 244000137852 Petrea volubilis Species 0.000 description 1
- DYAHQFWOVKZOOW-UHFFFAOYSA-N Sarin Chemical compound CC(C)OP(C)(F)=O DYAHQFWOVKZOOW-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
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- 239000003513 alkali Substances 0.000 description 1
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- 230000008033 biological extinction Effects 0.000 description 1
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- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- VQWFNAGFNGABOH-UHFFFAOYSA-K chromium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Cr+3] VQWFNAGFNGABOH-UHFFFAOYSA-K 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
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- 230000005494 condensation Effects 0.000 description 1
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 description 1
- 239000011267 electrode slurry Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 229960002089 ferrous chloride Drugs 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
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- 239000002184 metal Substances 0.000 description 1
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- 229910000510 noble metal Inorganic materials 0.000 description 1
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- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- RDRCCJPEJDWSRJ-UHFFFAOYSA-N pyridine;1h-pyrrole Chemical compound C=1C=CNC=1.C1=CC=NC=C1 RDRCCJPEJDWSRJ-UHFFFAOYSA-N 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
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- 238000005507 spraying Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- -1 sulfur nitrile Chemical class 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
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- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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Abstract
本发明公开了一种磁性四氧化三铁纳米粒子‑石墨烯复合材料,所述复合材料的比表面积为60‑65m2/g,复合材料中,四氧化三铁的粒子大小为10‑35nm,四氧化三铁支撑石墨烯片状材料,使石墨烯片状材料堆积形成缝隙,缝隙大小为20‑100nm。利用本发明复合材料进行废水处理,复合材料中的Fe3O4既可以有效的去除废水中的铬,又不会产生污泥,也不会造成二次污染。同时石墨烯极强的吸附性,又可以除去纳米粒子和悬浮物,更好的净化废水。为治理污水提供了一种既廉价又可靠并且能循环使用的方法。并且还可以将吸附过六价铬离子的复合材料作为电催化剂应用于染料敏化太阳能电池的对电极,从而实现对废物的再利用,减少了浪费,节约了资源。
Description
技术领域
本发明涉及污水处理技术领域和电催化剂技术领域,具体涉及一种磁性四氧化三铁纳米粒子-石墨烯复合材料及其制备方法与应用。
背景技术
金属铬是一种有害的重金属,尤其是六价铬具有很强的毒性。含铬废水是一种对环境具有巨大危害的工业废水,含铬废水主要来源于冶炼,电镀,机械加工和皮革加工业。长期以来,治理铬污染一直为全世界所瞩目,各国为此投入人力物力进行广泛的研究,并取得一定的研究成果和发明专利。到目前为止,用于治理六价铬废水的方法主要以化学法为主,其过程包括:用还原剂如氯化亚铁,硫酸亚铁等将其还原为三价铬,然后用碱与三价铬反应,使其生成氢氧化铬沉淀,从而将其从废水中除去。近来广泛应用的铁氧体共沉淀法也属于这一范畴。这种方法虽然能够有效的去除六价铬,但是过程耗时长,设施占地大,同时产生大量的污泥,容易造成二次污染。除了化学法以外,还有其它一些技术相继应用于含铬废液的处理,这些包括:电解法,吸附法,离子交换法,膜分离法。虽然这些技术对处理含铬废水各自具有一定的优点,但是仍然存在成本过高或可靠性不够等缺点。
染料敏化太阳能电池的是新型的薄膜太阳能电池,优点是工艺简易、成本较低、原材料来源广泛、可大面积印刷、理论能量转化效率高等,因此受到世界各国科研工作者的广泛关注。染料敏化太阳能电池主要由三部分组成:一是光阳极,主要由吸附有染料的纳米晶半导体多孔薄膜组成;二是电解质,由氧化还原电对和添加剂组成;三是具有催化作用的对电极,传统的方法是将贵金属Pt通过溅射或者热解的方法制备于导电玻璃上。由于贵金属Pt储量有限,价格昂贵,大大增加了对电极成本,影响了DSCs未来大规模生产。此外,从目前一些研究结果发现Pt对电极对S2-/Sn 2-,T-/T2等电对催化活性不高,影响了整个DSCs能量转化效率。因此降低对电极成本,开发高效稳定非铂对电极是急需解决的关键问题之一。
发明内容
针对上述现有技术,本发明的目的是一种磁性四氧化三铁纳米粒子-石墨烯复合材料及其制备方法。
本发明的另一目的是提供该磁性四氧化三铁纳米粒子-石墨烯复合材料在快速污水处理中的用途。
本发明的再一目的是提供处理废水后的该磁性四氧化三铁纳米粒子-石墨烯复合材料在制备染料敏化太阳能电池对电极中的用途。
为实现上述目的,本发明采用下述技术方案:
本发明的第一方面,提供一种磁性四氧化三铁纳米粒子-石墨烯复合材料(Fe3O4@RGO),所述复合材料的比表面积为60-65m2/g,复合材料中,四氧化三铁的粒子大小为10-35nm,四氧化三铁支撑石墨烯片状材料,使石墨烯片状材料堆积形成缝隙,缝隙大小为20-100nm。
上述磁性四氧化三铁纳米粒子-石墨烯复合材料的制备方法,步骤如下:
分别将六水氯化铁、聚乙二醇(PEG)、氢氧化钠和氧化石墨烯用乙二醇溶解,然后混合,搅拌均匀,在180-220℃加热,保持20-28h,即得到磁性四氧化三铁纳米粒子-石墨烯复合材料。
所述六水氯化铁、聚乙二醇(PEG)、氢氧化钠、氧化石墨烯和乙二醇加入的比为(30-35)g:(20-28)g:(12-16)g:(100-120)g:(200-250)ml;
优选的,所述六水氯化铁、聚乙二醇(PEG)、氢氧化钠、氧化石墨烯和乙二醇加入的比为32.4g:24g:14.4g:110.688g:240ml。
上述制备方法中,优选的,在200℃烘箱中加热,保持24h。
本发明的Fe3O4@RGO复合材料的制备原料中,通过选择加入聚乙二醇,利用其作为一种高分子表面活性剂,可以有效防止Fe3O4纳米粒子的聚集;而氢氧化钠的作用主要是为了调节整个溶液的pH,使乙二醇的还原性增加。通过聚乙二醇和氢氧化钠的共同作用可以使形成Fe3O4纳米粒子较均匀的分散在石墨烯表面。
本发明的第二方面,提供上述磁性四氧化三铁纳米粒子-石墨烯复合材料在快速污水处理中的用途。
上述用途中,污水中的污染物包括:重金属铬离子,有毒的CdS纳米粒子和河水中的悬浮物。
本发明的磁性四氧化三铁纳米粒子-石墨烯复合材料,只需1分钟就可以有效吸附水中的重金属铬离子,有毒的CdS纳米粒子、河水中的悬浮物,实现了对水中各类污染物的快速吸附。
本发明的第三方面,提供吸附过六价铬离子的磁性四氧化三铁纳米粒子-石墨烯复合材料(CrxFe3-xO4@RGO)在制备染料敏化太阳能电池对电极中的用途。
本发明利用复合材料中四氧化三铁的磁性,可以进行吸附后的快速回收,将吸附过六价铬离子的磁性四氧化三铁纳米粒子-石墨烯复合材料回收后,作为电催化剂应用于染料敏化太阳能电池对电极中,能量转化效率达到了5.26%,实现了废物的再利用。
本发明的有益效果:
(1)本发明利用具有磁性的四氧化三铁和微米级氧化石墨烯为原料制备形成Fe3O4@RGO复合材料,利用四氧化三铁纳米粒子表面的二价铁与污水中的Cr6+粒子发生氧化还原反应,从而吸附废水中的Cr6+;利用还原氧化石墨烯的吸附性,可以有效吸附水中的纳米粒子和悬浮物,达到净水的目的。
其中,微米级的氧化石墨烯材料可以大大增加Fe3O4@RGO复合材料的比表面积,增加复合材料的吸附性能。复合材料中,四氧化三铁的支撑作用造成的石墨烯片状材料堆积形成的缝隙。这种平板狭缝结构非常有利于进行污水处理时与污水的充分接触和吸附,增加吸附效果。
(2)本发明的Fe3O4@RGO复合材料能够快速吸附水中的各类污染物,加入Fe3O4@RGO复合材料之后只需1分钟就可以有效吸附水中的重金属铬离子,有毒的CdS纳米粒子、河水中的悬浮物。而且,在酸性和中性条件下均能有效的吸附水中的污染物,特别是在中性条件下进行吸附,不仅可以节约大量的酸,而且经过处理后的污水还可以保持中性条件,可以直接被排放。
(3)利用本发明的Fe3O4@RGO复合材料中四氧化三铁的磁性,可以进行吸附后的快速回收。
(4)吸附过六价铬离子的Fe3O4@RGO复合材料还可以作为电催化剂应用于染料敏化太阳能电池的对电极,能量转化效率达到了5.26%,实现了废物的再利用。
(5)利用本发明Fe3O4@RGO复合材料进行废水处理,复合材料中的Fe3O4既可以有效的去除废水中的铬,又不会产生污泥,也不会造成二次污染。同时石墨烯极强的吸附性,又可以除去纳米粒子和悬浮物,更好的净化废水。为治理污水提供了一种既廉价又可靠并且能循环使用的方法。并且还可以将吸附过六价铬离子的Fe3O4@RGO吸附剂作为电催化剂应用于染料敏化太阳能电池的对电极,从而实现对吸附过六价铬离子的Fe3O4@RGO复合材料的再利用,减少了浪费,节约了资源。
附图说明
图1:制备Fe3O4@RGO复合材料所用的微米级尺寸的氧化还原石墨烯;
图2:Fe3O4@RGO复合材料的吸附脱附曲线;
图3:Fe3O4@RGO复合材料的孔分布曲线;
图4:按照相同方法制备的聚集较严重的纯Fe3O4;
图5:Fe3O4@RGO复合材料的TEM图;
图6:六价铬离子标准溶液的紫外可见吸收光谱和标准曲线;
图7:Fe3O4@RGO复合材料对水溶液中六价铬吸附的紫外可见吸收光谱;
图8:Fe3O4@RGO复合材料对水溶液中CdS纳米粒子的吸附;
图9:Fe3O4@RGO复合材料对徒骇河水中悬浮物的吸附;
图10:CrxFe3-xO4@RGO复合材料喷涂形成的染料敏化太阳能电池对电极;
图11:基于CrxFe3-xO4@RGO对电极的染料敏化太阳能电池光电转化效率。
具体实施方式
下面结合实施例对本发明作进一步的说明,应该说明的是,下述说明仅是为了解释本发明,并不对其内容进行限定。
实施例1:磁性四氧化三铁纳米粒子-石墨烯复合材料(Fe3O4@RGO)的制备
分别向32.4g的六水氯化铁、24g的聚乙二醇(PEG)、14.4g的氢氧化钠和110.688g的氧化石墨烯中加入240毫升的乙二醇(EG),然后分别用磁力搅拌器进行搅拌,使其充分溶解。然后将这四份溶液混合,搅拌均匀。放入反应釜中,在200摄氏度烘箱中加热,保持24小时,即得磁性四氧化三铁纳米粒子-石墨烯复合材料。
本实施例采用的是微米级的氧化石墨烯材料(如图1),这种微米级的氧化石墨烯可以大大增大复合材料的比表面积,BET测试表明其比表面积为64.3m2/g。吸附脱附曲线可以看出(图2),滞后环的形状属于H3形,形状像新月,比较狭长,这是四氧化三铁的支撑作用造成的石墨烯片状材料堆积形成的缝隙。这种平板狭缝结构非常有利于进行污水处理时与污水的充分接触和吸附,增加吸附效果。复合材料料堆积形成的缝隙的孔主要在20~100nm之间分布(图3)。与纯的四氧化三铁相比(图4),复合之后四氧化三铁的聚集效应明显减弱。通过TEM照片可以看出(图5),复合材料中四氧化三铁的粒子大小分布在10~35nm之间。
将制备的磁性四氧化三铁纳米粒子-石墨烯复合材料用去离子水洗涤三次后,分散在水中,制备成固含量为10.75mg/ml的Fe3O4@RGO复合材料分散液,备用。
实施例2:Fe3O4@RGO复合材料对于六价铬离子的吸附试验
1.六价铬标准溶液的配制:
由于六价铬的颜色不是很明显,我们加入了显色剂二苯碳酰二肼乙醇溶液(DPCI)作为Cr6+离子浓度的探针。具体标准溶液和标准曲线做法如下:取五支50ml比色管,编号为1-5。分别取0.10、0.18、0.35、0.75、1.50ml的100mg/L的重铬酸钾溶液于上述50ml比色管中,再分别向其中依次加入两滴混酸,然后加入1.5ml的显色剂二苯碳酰二肼乙醇溶液(DPCI)。将上述溶液摇匀,加水稀释至50ml,定容,即为标准色阶。
从图6中可以看出,加入DPCI之后,标准溶液呈现出依次加深的红色(图6中上方的图,自左向右,颜色依次加深)。然后进行紫外可见吸收光谱的测量,从图6中可以看出,DPCI被Cr6+氧化之后,在544nm处出现一个特征吸收峰(图6中中间的图)。通过绘制541nm处吸光度和浓度之间的A--C关系图(图6中下方的图),可以看出两者存在明显的线性关系。线性拟合之后,线性方程为y=0.55113x+0.0337,相关系数为99.7%,说明拟合度较好。
2.吸附试验:
首先,分别取1.5ml 100mg/L的六价铬的标准溶液(0.15mg Cr6+)于干净的试剂瓶中,为了增加Cr6+与Fe3O4@RGO表面Fe2+的反应,再向其中依次加入适量混酸调pH为1-2,增加Cr6+的氧化性,增加吸附效果。然后,加入1mL Fe3O4@RGO复合材料的分散液(10.75mg),将其震荡5分钟,使其充分吸附。然后,利用四氧化三铁的磁性,用磁铁吸引,使其固液分离,将液体吸出。加入1.5ml DPCI显色剂,然后转移至比色管中定容到50mL。与没有加入Fe3O4@RGO复合材料的相同浓度的六价铬溶液相比,添加Fe3O4@RGO吸附剂的样品颜色明显较浅,说明Fe3O4@RGO可以有效的吸附Cr6+从而降低了溶液中Cr6+的浓度。经过紫外可见吸收光谱测试结果表明(图7),544nm处的吸光度从1.664下降到0.771,吸光度下降了0.893.按照相同的方法,当加入2ml Fe3O4@RGO复合材料的分散液(21.5mg)后,在经过磁性分离和显色之后可以看出,红色进一步降低,经过紫外可见吸收光谱测试结果表明,544nm处的吸光度从1.664下降到0.082,吸光度下降了1.582.按照相同的方法,当加入3ml Fe3O4@RGO复合材料的分散液(32.25mg)后,在经过磁性分离和显色之后可以看出,溶液基本无色,经过紫外可见吸收光谱测试结果表明,544nm处的已经没有特征吸收峰,吸光度从1.664下降到0.02.说明此时溶液中的Cr6+已经被完全吸附。综合上述结果,Fe3O4@RGO复合材料对Cr6+的吸附量为6.7mg/g。即使用Fe3O4@RGO对pH=7的Cr6+溶液进行吸附,从紫外可见吸收光谱可以看出,544nm处的吸光度从1.664也明显降低到1.028。Fe3O4@RGO复合材料对Cr6+的吸附量为5mg/g。
实施例3:Fe3O4@RGO复合材料对于CdS纳米粒子的吸附试验
由于CdS纳米粒子紫外-可见吸收光谱没有峰,所以只有观察宏观分离现象。从图8中可以看出,经吸附后溶液由橙黄色(图8中左图)变得澄清透明(图8中右图),说明分散液中的纳米粒子也可以被吸附,说明Fe3O4@RGO复合材料对CdS纳米粒子有明显的吸附效果。最后我们计算出1克Fe3O4@RGO复合材料可以吸附1.37g的CdS纳米粒子。由此看来,该物质可用于对污水中的悬浮纳米固体污染物进行有效的吸附,从而达到净化污水的目的。
实施例4:Fe3O4@RGO复合材料处理徒骇河河水的应用试验
首先,向烧杯中加入50ml徒骇河水,然后向徒骇河水中加5ml实施例1制备的Fe3O4@RGO分散液,振荡1min之后,将磁铁放在烧杯的一侧,实现固液分离。从初步的实验结果可以看出,与没有经过吸附的河水的相比,经过Fe3O4/RGO吸附后的河水明显变澄清。通过透光率测试可以看出(图9),最初河水的透光率在90%左右,而经过Fe3O4/RGO吸附后的河水的透光率在300~800nm范围内均达到95%的透光率。可见,将这种处理方法应用于实践是完全可行的,有效的。
实施例5:吸附过六价铬离子的Fe3O4@RGO吸附剂的再利用
将吸附过六价铬离子的Fe3O4@RGO吸附剂作为电催化剂应用于染料敏化太阳能电池的对电极。具体过程如下:
FTO导电玻璃的清洗:
将10×10cm2的FTO导电玻璃四周在砂纸上打磨,防止其在印刷过程中破坏印刷板。然后将打磨好的FTO导电玻璃依次经过清洗剂,去离子水和无水乙醇的超声清洗,每次清洗时间为15min。
对电极制备:将0.5g吸附过六价铬离子的Fe3O4@RGO(CrxFe3-xO4@RGO)复合材料置于10mL玻璃瓶中,然后置于台式分散机(日本三菱电机株式会社,NV-2F)进行球磨分散,频率为34Hz,分散时间为2h。用喷笔将分散好的对电极浆料均匀的喷涂在洗净的10cm×0.8cmFTO导电玻璃上,膜厚控制为2μm。喷好的对电极如图10所示。
光阳极制备:通过丝网印刷法将二氧化钛浆料印刷到洗净的FTO导电玻璃上,光阳极厚度可以通过调节刮刀与印刷版之间的压力及印刷不同的层数来控制。光阳极的厚度控制在12μm左右,每块光阳极膜的面积为0.16cm2。将印刷好的光阳极膜在空气中进行500℃烧结用于除去光阳极中的造孔剂(乙基纤维素)。待上述光阳极膜温度降至室温,将其浸泡在0.05M的TiCl4水溶液中,70℃处理30min。然后用去离子水冲洗TiCl4溶液处理的光阳极膜,随即将其吹干,并再次进行500℃的烧结。等经过烧结的光阳极膜自然冷却至90℃时,将其浸泡在浓度为5×10-4M N719溶液中(溶剂:乙腈与叔丁醇体积比为1:1),敏化时间为20h。敏化完毕后,取出光阳极膜,然后用无水乙醇冲掉其表面物理吸附的N719敏化剂。然后烘干光阳极膜表面的乙醇,光阳极膜制备完毕。
电池组装:将敏化好的光阳极膜与制备好的对电极用30μm沙林膜隔开,从而形成三明治结构光伏器件,然后将配制好的电解质注入其中。碘电对电解质组成为:0.03M I2,0.1M LiI,0.6M 1-丁基-3-甲基咪唑碘(BMII),0.1M异硫腈酸胍(GuSCN),0.5M 4-叔丁基吡啶(TBP),溶剂为乙腈。
组装好电池之后,再进行光电转化效率的测试。测试结果如图11所示。测试的数据显示,其光电转化效率为5.26%,说明将吸附过六价铬离子的Fe3O4@RGO吸附剂作为电催化剂应用于染料敏化太阳能电池的对电极是可行的。这样就可以实现对其再利用,变废为宝。
Claims (8)
1.一种磁性四氧化三铁纳米粒子-石墨烯复合材料,其特征在于,所述复合材料的比表面积为60-65m2/g,复合材料中,四氧化三铁的粒子大小为10-35nm,四氧化三铁支撑石墨烯片状材料,使石墨烯片状材料堆积形成缝隙,缝隙大小为20-100nm。
2.权利要求1所述的磁性四氧化三铁纳米粒子-石墨烯复合材料的制备方法,其特征在于,步骤如下:
分别将六水氯化铁、聚乙二醇、氢氧化钠和氧化石墨烯用乙二醇溶解,然后混合,搅拌均匀,在180-220℃加热,保持20-28h,即得到磁性四氧化三铁纳米粒子-石墨烯复合材料。
3.如权利要求2所述的制备方法,其特征在于,所述六水氯化铁、聚乙二醇、氢氧化钠、氧化石墨烯和乙二醇加入的比为(30-35)g:(20-28)g:(12-16)g:(100-120)g:(200-250)ml。
4.如权利要求3所述的制备方法,其特征在于,所述六水氯化铁、聚乙二醇、氢氧化钠、氧化石墨烯和乙二醇加入的比为32.4g:24g:14.4g:110.688g:240ml。
5.如权利要求2所述的制备方法,其特征在于,在200℃烘箱中加热,保持24h。
6.权利要求1所述的磁性四氧化三铁纳米粒子-石墨烯复合材料在快速污水处理中的用途。
7.如权利要求6所述的用途,其特征在于,污水中的污染物包括:重金属铬离子,有毒的CdS纳米粒子和河水中的悬浮物中的任一种或多种。
8.吸附过六价铬离子的权利要求1所述的磁性四氧化三铁纳米粒子-石墨烯复合材料在制备染料敏化太阳能电池对电极中的用途。
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