CN110152609A - 一种高效石墨烯基铋系纳米复合材料及其制备方法 - Google Patents
一种高效石墨烯基铋系纳米复合材料及其制备方法 Download PDFInfo
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- CN110152609A CN110152609A CN201910505260.7A CN201910505260A CN110152609A CN 110152609 A CN110152609 A CN 110152609A CN 201910505260 A CN201910505260 A CN 201910505260A CN 110152609 A CN110152609 A CN 110152609A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 50
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 38
- 239000010439 graphite Substances 0.000 title claims abstract description 38
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 30
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 125000003342 alkenyl group Chemical group 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 43
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 26
- 150000001661 cadmium Chemical class 0.000 claims abstract description 17
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 16
- 150000001621 bismuth Chemical class 0.000 claims abstract description 15
- 239000006185 dispersion Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- MYSWGUAQZAJSOK-UHFFFAOYSA-N ciprofloxacin Chemical compound C12=CC(N3CCNCC3)=C(F)C=C2C(=O)C(C(=O)O)=CN1C1CC1 MYSWGUAQZAJSOK-UHFFFAOYSA-N 0.000 claims description 60
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 42
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 229910002900 Bi2MoO6 Inorganic materials 0.000 claims description 32
- 229960003405 ciprofloxacin Drugs 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 239000002904 solvent Substances 0.000 claims description 22
- 230000015556 catabolic process Effects 0.000 claims description 18
- 238000006731 degradation reaction Methods 0.000 claims description 18
- 239000003638 chemical reducing agent Substances 0.000 claims description 16
- 150000002751 molybdenum Chemical class 0.000 claims description 14
- 239000011684 sodium molybdate Substances 0.000 claims description 11
- 235000015393 sodium molybdate Nutrition 0.000 claims description 11
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- 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 claims description 8
- 238000004090 dissolution Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 229910000380 bismuth sulfate Inorganic materials 0.000 claims description 5
- BEQZMQXCOWIHRY-UHFFFAOYSA-H dibismuth;trisulfate Chemical compound [Bi+3].[Bi+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BEQZMQXCOWIHRY-UHFFFAOYSA-H 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 4
- 239000005864 Sulphur Substances 0.000 claims description 4
- KPWJBEFBFLRCLH-UHFFFAOYSA-L cadmium bromide Chemical compound Br[Cd]Br KPWJBEFBFLRCLH-UHFFFAOYSA-L 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- QDAYJHVWIRGGJM-UHFFFAOYSA-B [Mo+4].[Mo+4].[Mo+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O Chemical compound [Mo+4].[Mo+4].[Mo+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QDAYJHVWIRGGJM-UHFFFAOYSA-B 0.000 claims description 3
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims description 3
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 claims description 3
- 235000018417 cysteine Nutrition 0.000 claims description 3
- 229910000014 Bismuth subcarbonate Inorganic materials 0.000 claims description 2
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 2
- 239000011609 ammonium molybdate Substances 0.000 claims description 2
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 2
- 229940010552 ammonium molybdate Drugs 0.000 claims description 2
- MGLUJXPJRXTKJM-UHFFFAOYSA-L bismuth subcarbonate Chemical compound O=[Bi]OC(=O)O[Bi]=O MGLUJXPJRXTKJM-UHFFFAOYSA-L 0.000 claims description 2
- 229940036358 bismuth subcarbonate Drugs 0.000 claims description 2
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims description 2
- QCUOBSQYDGUHHT-UHFFFAOYSA-L cadmium sulfate Chemical compound [Cd+2].[O-]S([O-])(=O)=O QCUOBSQYDGUHHT-UHFFFAOYSA-L 0.000 claims description 2
- 229910000331 cadmium sulfate Inorganic materials 0.000 claims description 2
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims description 2
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 2
- 235000011151 potassium sulphates Nutrition 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- PNYYBUOBTVHFDN-UHFFFAOYSA-N sodium bismuthate Chemical compound [Na+].[O-][Bi](=O)=O PNYYBUOBTVHFDN-UHFFFAOYSA-N 0.000 claims description 2
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 2
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 17
- 239000002131 composite material Substances 0.000 abstract description 12
- 238000007146 photocatalysis Methods 0.000 abstract description 8
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- -1 graphite alkene Chemical class 0.000 abstract 1
- 159000000000 sodium salts Chemical class 0.000 abstract 1
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 12
- 239000000463 material Substances 0.000 description 11
- 238000006555 catalytic reaction Methods 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 10
- 230000009102 absorption Effects 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 8
- 229940106691 bisphenol a Drugs 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000002604 ultrasonography Methods 0.000 description 4
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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- 238000000227 grinding Methods 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000011259 mixed solution Substances 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
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
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- 238000000634 powder X-ray diffraction Methods 0.000 description 1
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- 230000006798 recombination Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 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 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
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- 238000000967 suction filtration Methods 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0262—Compounds of O, S, Se, Te
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
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Abstract
本发明公开了一种高效石墨烯基铋系纳米复合材料及其制备方法,其包括,溶解氧化石墨,分散,得到化石墨烯溶液;溶解铋盐、钠盐,搅拌均匀,加入所述氧化石墨烯溶液中;加入硫脲和镉盐,搅拌;调节pH,搅拌,反应;抽滤、洗涤和干燥后研磨,即得石墨烯基铋系纳米复合材料。本发明所制备的CdS‑Bi2MoO6/RGO复合材料尺寸小,各组分分布均匀,该复合材料中石墨烯与Bi2MoO6和CdS三组分之间具有良好的协同效应,从而增加了复合物材料的光催化性能。
Description
技术领域
本发明属于光催化降解技术领域,具体涉及一种高效石墨烯基铋系纳米复合材料及其制备方法。
背景技术
如今,工业化和城市化的快速发展导致全球能源短缺,大量有毒有害的化学污染物被排放到我们周围的环境。因此迫切需要我们找到解决上述能源和环境危机的新型绿色技术。半导体光催化技术被认为是解决全球能源短缺和环境污染的安全有效方法之一。半导体光催化材料可以有效地利用太阳能将有机物彻底分解为CO2和水等无机小分子,无二次污染;同时利用光催化技术还可以直接将水分解来制备清洁能源氢气,从而在根本上解决能源短缺和环境污染这两大难题。
铋系氧化物作为一种新型半导体光催化材料因其独特的层状结构、合适的带隙宽度、较高的光催化活性、良好的稳定性等一系列优点受到极大关注。最近的研究结果表明Bi2MoO6是可见光照射下降解有机污染物的优良光催化材料。然而,在可见光照射下,由于纯Bi2MoO6的光生电子-空穴对具有较高的复合率,进而阻碍了其在光催化方面的广泛应用。通过改进制备方法、掺杂负载、构建异质结等技术,可以有效提高铋系半导体材料的可见光吸收性能或抑制光生电子和空穴的复合,从而进一步提高其光催化性能。这些方法都起到了一定的提高光催化效果的作用,但对可见光的反应活性以及稳定性仍然不能满足实际需要。
发明内容
本部分的目的在于概述本发明的实施例的一些方面以及简要介绍一些较佳实施例。在本部分以及本申请的说明书摘要和发明名称中可能会做些简化或省略以避免使本部分、说明书摘要和发明名称的目的模糊,而这种简化或省略不能用于限制本发明的范围。
鉴于上述的技术缺陷,提出了本发明。
因此,作为本发明其中一个方面,本发明克服现有技术中存在的不足,提供一种高效石墨烯基铋系纳米复合材料的制备方法。
为解决上述技术问题,本发明提供了如下技术方案:一种高效石墨烯基铋系纳米复合材料的制备方法,其包括,溶解氧化石墨,分散,得氧化石墨烯溶液;溶解铋盐、钼盐,搅拌均匀,加入所述氧化石墨烯溶液中;加入还原剂和镉盐,搅拌;调节pH,搅拌,反应;抽滤、洗涤和干燥后研磨,即得石墨烯基铋系纳米复合材料。
作为本发明所述的高效石墨烯基铋系纳米复合材料的制备方法的优选方案,其中:所述溶解氧化石墨,分散,其溶剂为水、乙醇、乙二醇或甘油中的一种或多种;所述溶解铋盐、钼盐,其溶剂为乙二醇;所述铋盐包括硝酸铋、铋酸钠、硫酸铋、次碳酸铋中的一种或几种;所述钼盐包括钼酸钠、钼酸铵、磷酸钼、钼酸钾的一种或几种;所述镉盐包括乙酸镉、硫酸镉、硝酸镉和溴化镉中的一种或几种;所述还原剂包括硫脲、硫代乙酰胺、半胱氨酸、硫化钠、硫磺和硫酸钾中的一种或几种;所述调节pH,其调节剂为NaOH。
作为本发明所述的高效石墨烯基铋系纳米复合材料的制备方法的优选方案,其中:所述氧化石墨烯与所述溶剂的质量比为1:1090~1:4360;所述铋盐和所述钼盐与所述溶剂的质量比为1:10~1:20;所述还原剂和所述镉盐的摩尔比为1:2~1:8;所述氧化石墨烯与所述还原剂和所述镉盐质量之和的质量比为1:30~1:120。
作为本发明所述的高效石墨烯基铋系纳米复合材料的制备方法的优选方案,其中:所述氧化石墨烯与所述溶剂的质量比为1:2180;所述铋盐和所述钼盐与所述溶剂的质量比为1:16;所述还原剂和所述镉盐的摩尔比为1:4;所述氧化石墨烯与所述还原剂和所述镉盐质量之和的质量比为1:80。
作为本发明所述的高效石墨烯基铋系纳米复合材料的制备方法的优选方案,其中:所述分散,其为超声分散,超声频率为20~60KHz,超声时间为20~60min;所述溶解铋盐、钼盐,搅拌均匀,加入所述氧化石墨烯溶液中,其中所述搅拌均匀为剧烈搅拌,所述加入其方式为滴加;所述加入还原剂和镉盐,搅拌,其中所述搅拌为搅拌1~2h;所述调节pH,搅拌,反应,其为调节pH至碱性,调节后继续搅拌2h,所述反应其反应温度为120℃~200℃,反应时间为12h~24h。
作为本发明所述的高效石墨烯基铋系纳米复合材料的制备方法的优选方案,其中:所述分散,其为超声分散,超声频率为40KHz,超声时间为30min;所述溶解铋盐、钼盐,搅拌均匀,加入所述氧化石墨烯溶液中,其中所述搅拌均匀为剧烈搅拌,所述加入其方式为滴加;所述加入还原剂和镉盐,搅拌,其中所述搅拌为搅拌1h;所述调节pH,搅拌,反应,其为调节pH至碱性,调节后继续搅拌2h,所述反应其反应温度为160℃,反应时间为16h。
作为本发明的另一方面,提供一种高效石墨烯基铋系纳米复合材料,其包括:包括CdS、Bi2MoO6和石墨烯。
作为本发明所述的高效石墨烯基铋系纳米复合材料的优选方案,其中:对环丙沙星的最大吸附量为52%。
作为本发明所述的高效石墨烯基铋系纳米复合材料的优选方案,其中:1h内对环丙沙星降解率大于等于91%。
作为本发明的另一方面,提供一种高效石墨烯基铋系纳米复合材料的应用,其包括:用于环丙沙星和/或罗丹明B的降解。
本发明的有益效果:
本发明所制备的CdS-Bi2MoO6/RGO复合材料尺寸小,各组分分布均匀,该复合材料中石墨烯与Bi2MoO6和CdS三组分之间具有良好的协同效应,从而增加了复合物材料的光催化性能。
附图说明
为了更清楚地说明本发明实施例的技术方案,下面将对实施例描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动性的前提下,还可以根据这些附图获得其它的附图。其中:
图1为实施例1所制得的CdS-Bi2MoO6/RGO复合材料的工艺流程图。
图2为实施例1所制得的CdS-Bi2MoO6/RGO复合材料的XRD图。
图3为实施例1所制得的CdS-Bi2MoO6/RGO复合材料的SEM图。
图4为实施例1所制得的CdS-Bi2MoO6/RGO复合材料的循环使用效果图。
图5为制得的Bi2MoO6、CdS、CdS-Bi2MoO6、Bi2MoO6/RGO和CdS-Bi2MoO6/RGO复合材料在可见光照射下对环丙沙星的光催化降解图。
具体实施方式
为使本发明的上述目的、特征和优点能够更加明显易懂,下面结合具体实施例对本发明的具体实施方式做详细的说明。
在下面的描述中阐述了很多具体细节以便于充分理解本发明,但是本发明还可以采用其他不同于在此描述的其它方式来实施,本领域技术人员可以在不违背本发明内涵的情况下做类似推广,因此本发明不受下面公开的具体实施例的限制。
其次,此处所称的“一个实施例”或“实施例”是指可包含于本发明至少一个实现方式中的特定特征、结构或特性。在本说明书中不同地方出现的“在一个实施例中”并非均指同一个实施例,也不是单独的或选择性的与其他实施例互相排斥的实施例。
实施例1:
(1)将0.0164g氧化石墨溶解于40mL乙醇中并超声,超声频率为40KHz,超声时间为30min,使其分散均匀;
(2)称取2.44g硝酸铋和0.605g钼酸钠于20mL乙二醇中,剧烈搅拌,并滴加进(1)中;
(3)再将0.761g硫脲、2.28g氯化镉加入(2)中,搅拌2h;
(4)对步骤(3)的混合液用5M的NaOH调节pH至碱性,搅拌2h,最后进行溶剂热反应,反应条件为160℃,16h;
(5)将水热釜取出,进行抽滤、洗涤和干燥后得到CdS-Bi2MoO6/RGO纳米复合材料。
黑暗状态下,用所制备的CdS-Bi2MoO6/RGO纳米复合材料进行环丙沙星吸附,其最大吸附量为35%;将所制备的CdS-Bi2MoO6/RGO纳米复合材料在可见光下降解水中污染物以测其光催化活性,发现1h内环丙沙星降解率为91%;降解RhB可达80%;双酚A只有30%(各污染物初始浓度均为20mg/L)。抽滤之后在真空烘箱中过夜,再次使用,循环吸附5次后,CdS-Bi2MoO6/RGO纳米复合材料1h内环丙沙星降解率仍接近90%,说明抑制了CdS的光腐蚀。
图2为所制备的CdS-Bi2MoO6/RGO光催化材料的XRD图,经X射线粉末衍射表征,所制得的产物为CdS-Bi2MoO6/RGO。
图3为CdS-Bi2MoO6/RGO光催化材料的SEM图,该表征表明,所制备的CdS-Bi2MoO6/RGO上各组分均匀,且尺寸较小和Bi2MoO6相比,材料尺寸缩小了100nm左右,尺寸小有利于提供更多的光吸收以及分子反应位点,有利于提高材料的光催化性能,且在室温条件下放置一年仍可以使用。
在可见光照射下,Bi2MoO6和CdS光催化剂分别被激发,分别在其导带(CB)和价带(VB)产生电子和空穴。电子可从传递到石墨烯上,Bi2MoO6的CB电位经计算为0.22eV,比标准氧化还原电位O2/OH-(0.40eV)更负。由于OH-/OH(1.99eV)和H2O/OH(2.27eV)的电位较低,所以CdS的VB电位(2.58eV)足以与吸附的氧反应以产生OH-自由基。另外,CdS的CB上的电子可以快速转移到石墨烯片层上。同时,Bi2MoO6中VB的光生h可以直接氧化CIP分子,这些空穴可以转移到CdS的VB上,并与表面水或羟基反应生成OH自由基。最后,这些高活性的自由基物质作用于CIP分子并导致增强的光催化反应。
实施例2:
(1)将0.0328g氧化石墨溶解于40mL去离子水中超声,超声频率为60KHz,超声时间为20min,使其分散均匀;
(2)称取2.44g硝酸铋和0.605g磷酸钼于20mL乙二醇中,剧烈搅拌,并滴加进(1)中;
(3)再将0.761g硫脲、2.28g氯化镉加入(2)中,搅拌2h;
(4)对步骤(3)的混合液用5M的NaOH调节pH至碱性,搅拌2h,最后进行溶剂热反应,反应条件为160℃,20h;
(5)将水热釜取出,进行抽滤、洗涤和干燥后得到CdS-Bi2MoO6/RGO纳米复合材料。
黑暗状态下,用所制备的CdS-Bi2MoO6/RGO纳米复合材料进行环丙沙星吸附,其最大吸附量为38%。将所制备的CdS-Bi2MoO6/RGO纳米复合材料在可见光下降解水中环丙沙星以测其光催化活性,发现2h内环丙沙星降解率超过85%,1h内降解RhB可达74%;双酚A只有28%。
实施例3:
(1)将0.0492g氧化石墨溶解于10mL的甘油和30mL的去离子水混合溶液中超声,超声频率为40KHz,超声时间为30min,使其分散均匀;
(2)称取2.44g硫酸铋和0.605g钼酸钠于20mL乙二醇中,剧烈搅拌,并滴加进(1)中;
(3)再将0.761g硫脲、2.28g乙酸镉加入(2)中,搅拌2h;
(4)对步骤(3)的混合液用5M的NaOH调节pH至碱性,搅拌2h,最后进行溶剂热反应,反应条件为150℃,22h;
(5)将水热釜取出,进行抽滤、洗涤和干燥后得到CdS-Bi2MoO6/RGO纳米复合材料。
黑暗状态下,用所制备的CdS-Bi2MoO6/RGO纳米复合材料进行环丙沙星吸附,其最大吸附量为52%;将所制备的CdS-Bi2MoO6/RGO纳米复合材料在可见光下降解水中环丙沙星以测其光催化活性,发现2h内环丙沙星降解率超过80%,1h内降解RhB可达70%;双酚A只有23%。
实施例4:
(1)将0.0246g氧化石墨溶解于40mL乙二醇中超声,超声频率为40KHz,超声时间为30min,使其分散均匀;
(2)称取2.44g硝酸铋和0.605g钼酸钠于20mL乙二醇中,剧烈搅拌,并滴加进(1)中;
(3)再将0.761g半胱氨酸、2.28g氯化镉加入(2)中,搅拌2h;
(4)对步骤(3)的混合液用5M的NaOH调节pH至碱性,搅拌2h,最后进行溶剂热反应,反应条件为160℃,20h;
(5)将水热釜取出,进行抽滤、洗涤和干燥后得到CdS-Bi2MoO6/RGO纳米复合材料。
黑暗状态下,用所制备的CdS-Bi2MoO6/RGO纳米复合材料进行环丙沙星吸附,其最大吸附量为35%。将所制备的CdS-Bi2MoO6/RGO纳米复合材料在可见光下降解水中环丙沙星以测其光催化活性,发现2h内环丙沙星降解率超过75%,1h降解RhB可达66%;双酚A只有19%。
实施例5:
(1)将0.0328g氧化石墨溶解于40mL乙醇中超声,超声频率为40KHz,超声时间为30min,使其分散均匀;
(2)称取2.44g硫酸铋和0.605g钼酸钠于20mL乙二醇中,剧烈搅拌,并滴加进(1)中;
(3)再将0.761g硫化钠、2.28g氯化镉加入(2)中,搅拌2h;
(4)对步骤(3)的混合液用5M的NaOH调节pH至碱性,搅拌2h,最后进行溶剂热反应,反应条件为160℃,20h;
(5)将水热釜取出,进行抽滤、洗涤和干燥后得到CdS-Bi2MoO6/RGO纳米复合材料。
黑暗状态下,用所制备的CdS-Bi2MoO6/RGO纳米复合材料进行环丙沙星吸附,其最大吸附量为36%。将所制备的CdS-Bi2MoO6/RGO纳米复合材料在可见光下降解水中环丙沙星以测其光催化活性,发现2h内环丙沙星降解率只有45%,1h降解RhB可达55%;双酚A只有14%。
实施例6:
(1)将0.0328g氧化石墨溶解于40mL乙醇中超声,超声频率为20KHz,超声时间为60min,使其分散均匀;
(2)称取2.44g硫酸铋和0.605g钼酸钠于20mL乙二醇中,剧烈搅拌,并滴加进(1)中;
(3)再将0.761g硫化钠、2.28g氯化镉加入(2)中,搅拌2h;
(4)对步骤(3)的混合液用5M的NaOH调节pH至碱性,搅拌2h,最后进行溶剂热反应,反应条件为100℃,36h;
(5)将水热釜取出,进行抽滤、洗涤和干燥后得到CdS-Bi2MoO6/RGO纳米复合材料。
黑暗状态下,用所制备的CdS-Bi2MoO6/RGO纳米复合材料进行环丙沙星吸附,其最大吸附量为12%。将所制备的CdS-Bi2MoO6/RGO纳米复合材料在可见光下降解水中环丙沙星以测其光催化活性,发现2h内环丙沙星降解率只有13%。
对照例1:
(1)称取0.49g硝酸铋和0.24g钼酸钠于20mL的乙二醇中,超声频率为40KHz,超声时间为20min,剧烈搅拌,使其完全溶解;
(2)再将和0.24g钼酸钠加入(1)中,搅拌2h,使体系充分混合均匀;
(3)对步骤(2)的混合液用5M的NaOH调节pH至弱酸性,搅拌2h,最后进行溶剂热反应,反应条件为160℃,20h;
(4)将水热釜取出,进行抽滤、洗涤和干燥后得到Bi2MoO6纳米复合材料。
将所制备的Bi2MoO6光催化材料在可见光下降解水中环丙沙星以测其光催化活性,发现1h内环丙沙星降解率超过21%,降解RhB只有38%;双酚A只有12%。
对照例2:
(1)称取0.456g氯化镉于10mL的去离子水中,剧烈搅拌,使其完全溶解;
(2)再将0.152g硫脲加入(1)中,搅拌2h,使体系充分混合均匀;
(3)对步骤(2)的混合液用5M的NaOH调节pH至中性,搅拌2h,最后进行溶剂热反应,反应条件为160℃,20h;
(4)将水热釜取出,进行抽滤、洗涤和干燥后得到CdS纳米复合材料。
将所制备的CdS光催化材料在可见光下降解水中环丙沙星以测其光催化活性,发现1h内环丙沙星降解率超过31%。
对照例3:
(1)将0.0164g氧化石墨于40mL去离子水中超声,超声频率为70KHz,超声时间为15min,使其分散均匀;
(2)称取0.49g硝酸铋于20mL乙二醇中,剧烈搅拌,并滴加进(1)中;
(3)再将0.24g钼酸钠加入(2)中,搅拌2h,使体系充分混合均匀;
(4)对步骤(3)的混合液用5M的NaOH调节pH至碱性,搅拌2h,最后进行溶剂热反应,反应条件为160℃,20h;
(5)将水热釜取出,进行抽滤、洗涤和干燥后得到Bi2MoO6/RGO纳米复合材料。
将所制备的Bi2MoO6/RGO光催化材料在可见光下降解水中环丙沙星以测其光催化活性,发现2h内环丙沙星降解率超过39%。
对照例4:
(1)称取2.44g硝酸铋和0.605g钼酸钠于20mL乙二醇中,剧烈搅拌,使其完全溶解;
(2)再将0.761g硫脲、2.28g氯化镉加入(1)中,搅拌2h;
(3)对步骤(2)的混合液用5M的NaOH调节pH至碱性,搅拌2h,最后进行溶剂热反应,反应条件为160℃,20h;
(4)将水热釜取出,进行抽滤、洗涤和干燥后得到CdS-Bi2MoO6纳米复合材料。
将所制备的CdS-Bi2MoO6光催化材料在可见光下降解水中环丙沙星以测其光催化活性,发现1h内环丙沙星降解率超过34%。
应说明的是,以上实施例仅用以说明本发明的技术方案而非限制,尽管参照较佳实施例对本发明进行了详细说明,本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本发明技术方案的精神和范围,其均应涵盖在本发明的权利要求范围当中。
Claims (10)
1.一种高效石墨烯基铋系纳米复合材料的制备方法,其特征在于:包括,
溶解氧化石墨,分散,得氧化石墨烯溶液;
溶解铋盐、钼盐,搅拌均匀,加入所述氧化石墨烯溶液中;
加入还原剂和镉盐,搅拌;
调节pH,搅拌,反应;
抽滤、洗涤和干燥后研磨,即得石墨烯基铋系纳米复合材料。
2.如权利要求1所述的高效石墨烯基铋系纳米复合材料的制备方法,其特征在于:所述溶解氧化石墨,分散,其溶剂为水、乙醇、乙二醇或甘油中的一种或多种;所述溶解铋盐、钼盐,其溶剂为乙二醇;所述铋盐包括硝酸铋、铋酸钠、硫酸铋、次碳酸铋中的一种或几种;所述钼盐包括钼酸钠、钼酸铵、磷酸钼、钼酸钾的一种或几种;所述镉盐包括乙酸镉、硫酸镉、硝酸镉和溴化镉中的一种或几种;所述还原剂包括硫脲、硫代乙酰胺、半胱氨酸、硫化钠、硫磺和硫酸钾中的一种或几种;所述调节pH,其调节剂为NaOH。
3.如权利要求1或2所述的高效石墨烯基铋系纳米复合材料的制备方法,其特征在于:所述氧化石墨烯与所述溶剂的质量比为1:1090~1:4360;所述铋盐和所述钼盐与所述溶剂的质量比为1:10~1:20;所述还原剂和所述镉盐的摩尔比为1:2~1:8;所述氧化石墨烯与所述还原剂和所述镉盐质量之和的质量比为1:30~1:120。
4.如权利要求1或2所述的高效石墨烯基铋系纳米复合材料的制备方法,其特征在于:所述氧化石墨烯与所述溶剂的质量比为1:2180;所述铋盐和所述钼盐与所述溶剂的质量比为1:16;所述还原剂和所述镉盐的摩尔比为1:4;所述氧化石墨烯与所述还原剂和所述镉盐质量之和的质量比为1:80。
5.如权利要求1~4任一所述的高效石墨烯基铋系纳米复合材料的制备方法,其特征在于:所述分散,其为超声分散,超声频率为20~60KHz,超声时间为20~60min;所述溶解铋盐、钼盐,搅拌均匀,加入所述氧化石墨烯溶液中,其中所述搅拌均匀为剧烈搅拌,所述加入其方式为滴加;所述加入还原剂和镉盐,搅拌,其中所述搅拌为搅拌1~2h;所述调节pH,搅拌,反应,其为调节pH至碱性,调节后继续搅拌2h,所述反应其反应温度为120℃~200℃,反应时间为12h~24h。
6.如权利要求1~4任一所述的高效石墨烯基铋系纳米复合材料的制备方法,其特征在于:所述分散,其为超声分散,超声频率为40KHz,超声时间为30min;所述溶解铋盐、钼盐,搅拌均匀,加入所述氧化石墨烯溶液中,其中所述搅拌均匀为剧烈搅拌,所述加入其方式为滴加;所述加入还原剂和镉盐,搅拌,其中所述搅拌为搅拌1h;所述调节pH,搅拌,反应,其为调节pH至碱性,调节后继续搅拌2h,所述反应其反应温度为160℃,反应时间为16h。
7.利用权利要求1~6任一所述方法制备的高效石墨烯基铋系纳米复合材料,其特征在于:包括CdS、Bi2MoO6和石墨烯。
8.如权利要求7所述的高效石墨烯基铋系纳米复合材料,其特征在于:对环丙沙星的最大吸附量为52%。
9.如权利要求7所述的高效石墨烯基铋系纳米复合材料,其特征在于:1h内对环丙沙星降解率大于等于91%。
10.一种高效石墨烯基铋系纳米复合材料的应用,其特征在于:用于环丙沙星和/或罗丹明B的降解。
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