CN114918422B - 一种机械化学制备纳米材料及纳米复合材料的方法 - Google Patents
一种机械化学制备纳米材料及纳米复合材料的方法 Download PDFInfo
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- CN114918422B CN114918422B CN202210452795.4A CN202210452795A CN114918422B CN 114918422 B CN114918422 B CN 114918422B CN 202210452795 A CN202210452795 A CN 202210452795A CN 114918422 B CN114918422 B CN 114918422B
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- 239000000463 material Substances 0.000 title claims abstract description 43
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- 238000000498 ball milling Methods 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 31
- 238000000227 grinding Methods 0.000 claims abstract description 21
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 19
- 241001464837 Viridiplantae Species 0.000 claims abstract description 18
- 238000011049 filling Methods 0.000 claims abstract description 17
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- 150000001875 compounds Chemical class 0.000 claims description 34
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 23
- 229910052742 iron Inorganic materials 0.000 claims description 15
- 239000000126 substance Substances 0.000 claims description 10
- 235000002639 sodium chloride Nutrition 0.000 claims description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- 229920000642 polymer Polymers 0.000 claims description 6
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 239000012876 carrier material Substances 0.000 claims description 4
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- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims description 4
- 150000004676 glycans Chemical class 0.000 claims description 4
- NPFOYSMITVOQOS-UHFFFAOYSA-K iron(III) citrate Chemical compound [Fe+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NPFOYSMITVOQOS-UHFFFAOYSA-K 0.000 claims description 4
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- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- CDVAIHNNWWJFJW-UHFFFAOYSA-N 3,5-diethoxycarbonyl-1,4-dihydrocollidine Chemical compound CCOC(=O)C1=C(C)NC(C)=C(C(=O)OCC)C1C CDVAIHNNWWJFJW-UHFFFAOYSA-N 0.000 claims description 2
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- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
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- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical group C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 claims description 2
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- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 claims description 2
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- OWZIYWAUNZMLRT-UHFFFAOYSA-L iron(2+);oxalate Chemical compound [Fe+2].[O-]C(=O)C([O-])=O OWZIYWAUNZMLRT-UHFFFAOYSA-L 0.000 claims description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 2
- KAEAMHPPLLJBKF-UHFFFAOYSA-N iron(3+) sulfide Chemical compound [S-2].[S-2].[S-2].[Fe+3].[Fe+3] KAEAMHPPLLJBKF-UHFFFAOYSA-N 0.000 claims description 2
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 claims description 2
- YPJCVYYCWSFGRM-UHFFFAOYSA-H iron(3+);tricarbonate Chemical compound [Fe+3].[Fe+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O YPJCVYYCWSFGRM-UHFFFAOYSA-H 0.000 claims description 2
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- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 2
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- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical compound [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 description 1
- CHACQUSVOVNARW-LNKPDPKZSA-M silver;(z)-4-oxopent-2-en-2-olate Chemical compound [Ag+].C\C([O-])=C\C(C)=O CHACQUSVOVNARW-LNKPDPKZSA-M 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- CADICXFYUNYKGD-UHFFFAOYSA-N sulfanylidenemanganese Chemical compound [Mn]=S CADICXFYUNYKGD-UHFFFAOYSA-N 0.000 description 1
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 description 1
- NRUVOKMCGYWODZ-UHFFFAOYSA-N sulfanylidenepalladium Chemical compound [Pd]=S NRUVOKMCGYWODZ-UHFFFAOYSA-N 0.000 description 1
- JOKPITBUODAHEN-UHFFFAOYSA-N sulfanylideneplatinum Chemical compound [Pt]=S JOKPITBUODAHEN-UHFFFAOYSA-N 0.000 description 1
- BVJAAVMKGRODCT-UHFFFAOYSA-N sulfanylidenerhodium Chemical compound [Rh]=S BVJAAVMKGRODCT-UHFFFAOYSA-N 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- RYSQYJQRXZRRPH-UHFFFAOYSA-J tin(4+);dicarbonate Chemical compound [Sn+4].[O-]C([O-])=O.[O-]C([O-])=O RYSQYJQRXZRRPH-UHFFFAOYSA-J 0.000 description 1
- CVNKFOIOZXAFBO-UHFFFAOYSA-J tin(4+);tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Sn+4] CVNKFOIOZXAFBO-UHFFFAOYSA-J 0.000 description 1
- AFNRRBXCCXDRPS-UHFFFAOYSA-N tin(ii) sulfide Chemical compound [Sn]=S AFNRRBXCCXDRPS-UHFFFAOYSA-N 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- YJGJRYWNNHUESM-UHFFFAOYSA-J triacetyloxystannyl acetate Chemical compound [Sn+4].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O YJGJRYWNNHUESM-UHFFFAOYSA-J 0.000 description 1
- DANYXEHCMQHDNX-UHFFFAOYSA-K trichloroiridium Chemical compound Cl[Ir](Cl)Cl DANYXEHCMQHDNX-UHFFFAOYSA-K 0.000 description 1
- YQMWDQQWGKVOSQ-UHFFFAOYSA-N trinitrooxystannyl nitrate Chemical compound [Sn+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YQMWDQQWGKVOSQ-UHFFFAOYSA-N 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
- 239000011667 zinc carbonate Substances 0.000 description 1
- 235000004416 zinc carbonate Nutrition 0.000 description 1
- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 1
- 229910021511 zinc hydroxide Inorganic materials 0.000 description 1
- 229940007718 zinc hydroxide Drugs 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
- ZPEJZWGMHAKWNL-UHFFFAOYSA-L zinc;oxalate Chemical compound [Zn+2].[O-]C(=O)C([O-])=O ZPEJZWGMHAKWNL-UHFFFAOYSA-L 0.000 description 1
- NHXVNEDMKGDNPR-UHFFFAOYSA-N zinc;pentane-2,4-dione Chemical compound [Zn+2].CC(=O)[CH-]C(C)=O.CC(=O)[CH-]C(C)=O NHXVNEDMKGDNPR-UHFFFAOYSA-N 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种机械化学制备纳米材料及纳米复合材料的方法。所述机械化学制备纳米材料的方法包括以下步骤：将金属化合物和含有还原性物质的绿色植物材料或其提取物按照一定质量比例混合后，放入研磨罐中并加入玛瑙或氧化锆小球；研磨罐充填惰性气体密封后，置于球磨机械上以50~800 rpm研磨0.5~96 h；采用非氧化性溶剂对获得的产物进行清洗，得到纳米材料。本发明结合球磨技术和绿色植物还原两种技术的优势，工艺简单、生产成本较低、产量大、操作性强、易于实现工业化生产，而且对环境友好，是一种绿色环保合成工艺。
Description
技术领域
本发明涉及纳米材料制备技术领域，特别涉及一种机械化学制备纳米材料及纳米复合材料的方法。
背景技术
纳米材料比表面大、反应活性高，具有较强的还原和催化作用，广泛用于环境保护领域。纳米材料的合成方法主要有化学气相沉积法、高能球磨法和液相化学还原法。高能球磨法是通过机械力作用，将大尺寸的金属或者其氧化物破碎成纳米材料。高能球磨法不需要添加溶剂，合成效率高，成本较低。但是由于球磨法是一种自上而下制备材料的方法，所制备的纳米材料的极限尺寸很难达到纳米级别，一般为亚微米、微米级别。
绿色植物中含有还原性物质，如多酚类、多糖类、生物碱类和多肽类等还原性物质。采用绿色植物作为还原剂，制备纳米材料具有生产低成本、过程绿色等特点。而且多酚类、多糖类等物质还可以吸附在纳米材料表面的活性位点，起到稳定剂的作用，增强其在空气中的稳定性，而且能够有效防止纳米材料团聚。但是目前采用绿色植物还原制备纳米材料均是通过萃取技术提取绿色植物中的还原性物质，然后采用液相合成法合成纳米材料，不但步骤繁琐，而且效率不高，产量比较低。
发明内容
本发明为了解决上述技术问题，提供了一种机械化学制备纳米材料及纳米复合材料的方法。
第一方面，本发明提供一种机械化学制备纳米材料的方法，是采用以下技术方案得以实现的。
一种机械化学制备纳米材料的方法，包括以下步骤：
S1.将金属化合物和含有还原性物质的绿色植物材料或其提取物按照质量比为1:1~100的比例混合后，放入研磨罐中并加入玛瑙或氧化锆小球；
S2.研磨罐充填惰性气体密封后，置于球磨机械上以50~800 rpm研磨0.5~96 h；
S3.采用非氧化性溶剂对步骤S2获得的产物进行清洗，得到纳米材料。
进一步的，所述金属化合物选自含锰化合物、含铁化合物、含钴化合物、含镍化合物、含铜化合物、含锌化合物、含钌化合物、含铑化合物、含钯化合物、含银化合物、含锡化合物、含铱化合物、含金化合物、含铂化合物、含铈化合物、含镧化合物中的一种或几种。
进一步的，所述含锰化合物选自氯化锰、硝酸锰、硫酸锰、碳酸锰、醋酸锰、氧化锰、四氧化三锰、硫化锰中的一种或几种。
进一步的，所述含铁化合物选自氯化铁、氯化亚铁、硫酸铁、醋酸铁、碳酸铁、硫酸亚铁、草酸亚铁、柠檬酸铁、氢氧化铁、氧化铁、硫化铁、二茂铁、乙酰丙酮铁中的一种或几种。
进一步的，所述含钴化合物选自氯化钴、硝酸钴、硫酸钴、醋酸钴、碳酸钴、氧化钴、四氧化三钴、氢氧化钴、硫化钴、乙酰丙酮钴中的一种或几种。
进一步的，所述含镍化合物选自氯化镍、硫酸镍、草酸镍、柠檬酸镍、氢氧化镍、氧化镍、硫化镍、乙酰丙酮镍中的一种或几种。
进一步的，所述含铜化合物选自氯化铜、硝酸铜、碳酸铜、磷酸铜、碱式碳酸铜、醋酸铜、草酸铜、氧化铜、氢氧化铜、硫化铜中的一种或几种。
进一步的，所述含锌化合物选自氯化锌、硝酸锌、碳酸锌、磷酸锌、碱式碳酸锌、醋酸锌、草酸锌、氧化锌、氢氧化锌、硫化锌、乙酰丙酮锌中的一种或几种。
进一步的，所述含钌化合物选自氯化钌、硝酸钌、碳酸钌、醋酸钌、草酸钌、氧化钌、氢氧化钌、硫化钌、乙酰丙酮钌中的一种或几种。
进一步的，所述含铑化合物选自氯化铑、硝酸铑、碳酸铑、醋酸铑、草酸铑、氧化铑、氢氧化铑、硫化铑、乙酰丙酮铑中的一种或几种。
进一步的，所述含钯化合物选自氯化钯、硝酸钯、碳酸钯、醋酸钯、草酸钯、氧化钯、氢氧化钯、硫化钯、乙酰丙酮钯中的一种或几种。
进一步的，所述含银化合物选自氯化银、硝酸银、碳酸银、醋酸银、草酸银、氧化银、硫化银、乙酰丙酮银中的一种或几种。
进一步的，所述含锡化合物选自氯化锡、硝酸锡、碳酸锡、醋酸锡、草酸锡、氧化锡、氢氧化锡、硫化锡、乙酰丙酮锡中的一种或几种。
进一步的，所述含铱化合物选自氯化铱、硝酸铱、碳酸铱、醋酸铱、草酸铱、氧化铱、氢氧化铱、硫化铱、乙酰丙酮铱中的一种或几种。
进一步的，所述含金化合物选自氯化金、氯金酸、氧化金、氢氧化金、氰化金钾、硫化金中的一种或几种。
进一步的，所述含铂化合物选自氯化铂、氯铂酸、醋酸铂、氧化铂、硫化铂、氰化铂中的一种或几种。
进一步的，所述含铈化合物选自氯化铈、硝酸铈、醋酸铈、硫酸铈、草酸铈、乙酰丙酮铈、硝酸铈铵、氧化铈、硫化铈中的一种或几种。
进一步的，所述含镧化合物选自氯化镧、硝酸镧、醋酸镧、硫酸镧、草酸镧、乙酰丙酮镧、硝酸镧铵、氧化镧、硫化镧中的一种或几种。
进一步的，所述含有还原性物质的绿色植物材料为含有还原性物质的绿色植物的根、茎、叶、花、果实以及种子；所述还原性物质为叶绿素、多糖、还原性糖(蔗糖、壳聚糖等)、多酚、黄酮类、萜类、没食子酸、维生素C、蛋白质。含有还原性物质的绿色植物材料优选为柑橘属植物的果实及果皮、山茶属植物的叶子和果实、仙人掌属植物、油料作物的种子及榨油后的残渣、藻类、桉树叶、冬青叶、浒苔、咖啡渣、甘蔗渣、香蕉皮、柿子、甜菜渣、苹果核、橙子渣、地瓜渣、五倍子和蘑菇。
进一步的，所述非氧化性溶剂选用乙醇、异丙醇、丙醇、丙酮、乙酸乙酯中的一种或几种。
第二方面，本申请提供一种机械化学制备纳米复合材料的方法，是采用以下技术方案得以实现的。
一种机械化学制备纳米复合材料的方法，向上述金属化合物和含有还原性物质的绿色植物材料或其提取物中加入一定质量的高分子聚合物、惰性盐类、掺杂物质前躯体或载体材料，再放入研磨罐中；Fe、高分子聚合物、惰性盐类、掺杂物质前躯体和载体材料的质量比为1:1~100:1~50:0~2:0~50。
进一步的，所述高分子聚合物选自聚乙烯吡咯烷酮、聚乙烯醇、聚丙烯酰胺、聚丙烯酸、羧甲基纤维素、淀粉、十二烷基磺酸钠中的一种或几种。
进一步的，所述惰性盐类选自氯化钠、氯化钾、硫酸钠、硫酸钾、碳酸钠、碳酸钾中的一种或几种。
进一步的，所述掺杂物质前躯体选自硼化合物、硫化合物、磷化合物、钙化合物、镁化合物、镍化合物、钴化合物、锰化合物、铜化合物、锌化合物、硒化合物、锡化合物、锆化合物、钼化合物、钌化合物、铑化合物、钯化合物、镧化合物、铈化合物中的一种或几种。
进一步的，所述载体材料选自碳材料、金属氧化物、金属氢氧化物、层状双金属氢氧化物、石墨化氮化碳、天然矿物材料、天然纤维材料中的一种或几种。
进一步的，所述球磨机械选自行星式球磨机、振动式球磨机、卧式滚筒球磨机、搅拌式球磨机中的一种。
本申请具有以下有益效果。
本发明结合球磨技术和绿色植物还原两种技术的优势，直接采用绿色植物作为还原剂，和金属化合物混合在一起，再在惰性气氛下球磨，一步即可制备纳米材料。本申请方法是自下而上制备纳米材料的方法，不同于传统球磨技术的从上而下制备材料的方法，本申请的非溶剂固相合成过程，操作过程简单、绿色，绿色植物中还原性物质的利用率高，生产成本低，产量大。而且本申请方法拓展性强，通过加入高分聚合物或惰性盐类等材料，可制备得到纳米复合材料。
附图说明
图1是本发明实施例1合成的纳米铁材料的TEM照片；
图2是本发明实施例1合成的纳米铁材料的XRD图；
图3是本发明实施例2合成的碳纳米管负载纳米铁复合材料的TEM照片；
图4是本发明实施例3合成的硫化纳米铁材料的TEM照片；
图5是本发明实施例4合成的纳米银颗粒的TEM照片；
图6为本发明实施例5合成的纳米金材料的TEM照片；
图7为本发明实施例6合成的碳纳米管负载纳米钯复合纳米材料的TEM照片；
图8为本发明实施例7合成的LDH负载纳米铜复合纳米材料的TEM照片。
具体实施方式
以下结合附图和实施例对本专利申请进行进一步的说明。
实施例1
采用柿饼为还原剂制备纳米铁材料，具体制备步骤如下：
1）将总质量为500 g的干燥柿饼、醋酸铁、羧甲基纤维素钠按照质量比3:1:1.5混合均匀，装填到体积为2 L的球磨罐中，加入氧化锆研磨小球，球磨罐密封后，抽真空然后充入氩气，反复几次以保证罐体内的空气被完全置换；
2）将球磨罐固定到行星式球磨机上，以300 rpm球磨24 h；
3）将球磨罐置于手套箱中打开，材料用乙醇反复清洗几次后（乙醇收集后回收利用），氮气气氛下干燥即可得到纳米铁材料。
从图1可以看出，材料粒径比较均匀，分布在50~200 nm之间，XRD显示材料主要成分为零价铁。
实施例2
采用绿茶为还原剂制备纳米铁复合材料，具体制备步骤如下：
1）将总质量为500 g的干燥绿茶、柠檬酸铁、羧甲基纤维素钠和碳纳米管按照质量比3:1:1.5:2混合均匀，装填到体积为2 L的球磨罐中，加入氧化锆研磨小球，球磨罐密封后，抽真空然后充入氩气，反复几次以保证罐体内的空气被完全置换；
2）将球磨罐固定到行星式球磨机上，以200 rpm球磨24 h；
3）将球磨罐置于手套箱中打开，材料用乙醇反复清洗几次后（乙醇收集后回收利用），氮气气氛下干燥即可得到碳纳米管负载的纳米铁材料。
图3为本实施例合成的碳纳米管负载纳米铁复合纳米材料的TEM结果。
实施例3
采用绿茶为还原剂制备硫化纳米铁材料，具体制备步骤如下：
1）将总质量为500 g的干燥绿茶、柠檬酸铁、羧甲基纤维素钠和升华硫粉按照质量比3:1:1.5:0.1混合均匀，装填到体积为2 L的球磨罐中，加入氧化锆研磨小球，球磨罐密封后，抽真空然后充入氩气，反复几次以保证罐体内的空气被完全置换；
2）将球磨罐固定到行星式球磨机上，以200 rpm球磨24 h；
3）将球磨罐置于手套箱中打开，材料用乙醇反复清洗几次后（乙醇收集后回收利用），氮气气氛下干燥即可得到硫化纳米铁材料。
图4为本实施例合成的硫化纳米铁材料的TEM结果。
实施例4
采用绿茶为还原剂制备纳米银材料，具体制备步骤如下：
1）将总质量为500 g的干燥绿茶、醋酸银、聚乙烯吡咯烷酮按照质量比5:1:5混合均匀，装填到体积为2 L的球磨罐中，加入氧化锆研磨小球，球磨罐密封后，抽真空然后充入氩气，反复几次以保证罐体内的空气被完全置换；
2）将球磨罐固定到行星式球磨机上，以200 rpm球磨24 h；
3）将球磨罐置于手套箱中打开，材料用乙醇反复清洗几次后（乙醇收集后回收利用），氮气气氛下干燥即可得到纳米银材料。
图5为本实施例合成的纳米银材料的TEM结果。
实施例5
采用葡萄籽为还原剂制备纳米金材料，具体制备步骤如下：
1）将总质量为2 g的干燥葡萄籽、氯金酸、聚乙烯吡咯烷酮按照质量比5:1:5混合均匀，装填到体积为50 mL的球磨罐中，加入氧化锆研磨小球，球磨罐密封后，抽真空然后充入氩气，反复几次以保证罐体内的空气被完全置换；
2）将球磨罐固定到行星式球磨机上，以200 rpm球磨4 h；
3）将球磨罐置于手套箱中打开，材料用乙醇反复清洗几次后（乙醇收集后回收利用），氮气气氛下干燥即可得到纳米金材料。
图6为本实施例合成的纳米金材料的TEM结果。
实施例6
采用绿茶为还原剂制备碳纳米管负载纳米钯复合材料，具体制备步骤如下：
1）将总质量为50 g的干燥绿茶、醋酸钯、聚乙烯吡咯烷酮和碳纳米管按照质量比3:1:1.5:2混合均匀，装填到体积为250 mL的球磨罐中，加入氧化锆研磨小球，球磨罐密封后，抽真空然后充入氩气，反复几次以保证罐体内的空气被完全置换；
2）将球磨罐固定到行星式球磨机上，以200 rpm球磨6 h；
3）将球磨罐置于手套箱中打开，材料用乙醇反复清洗几次后（乙醇收集后回收利用），氮气气氛下干燥即可得到碳纳米管负载的纳米钯材料。
图7为本实施例合成的碳纳米管负载纳米钯复合纳米材料的TEM照片。
实施例7
采用绿茶为还原剂制备镁铝双金属氢氧化物（LDH）负载纳米铜复合材料，具体制备步骤如下：
1）将总质量为100 g的干燥绿茶、醋酸铜、聚乙烯吡咯烷酮、LDH和NaCl按照质量比3:1:1.5:10：5混合均匀，装填到体积为500 mL的球磨罐中，加入氧化锆研磨小球，球磨罐密封后，抽真空然后充入氩气，反复几次以保证罐体内的空气被完全置换；
2）将球磨罐固定到行星式球磨机上，以200 rpm球磨8 h；
3）将球磨罐置于手套箱中打开，材料用乙醇反复清洗几次后（乙醇收集后回收利用），氮气气氛下干燥即可得到LDH的纳米铜材料。
图8为本实施例合成的LDH负载纳米铜复合纳米材料的TEM照片。
本具体实施方式的实施例均为本发明的较佳实施例，并非依此限制本发明的保护范围，故：凡依本发明的结构、形状、原理所做的等效变化，均应涵盖于本发明的保护范围之内。
Claims (6)
1.一种机械化学制备纳米材料的方法，其特征在于：包括以下步骤：
S1.将含铁化合物和含有还原性物质的绿色植物材料按照质量比为1:1~100的比例混合后，放入研磨罐中并加入玛瑙或氧化锆小球；
所述含有还原性物质的绿色植物材料为含有还原性物质的绿色植物的根、茎、叶、花、果实以及种子；所述还原性物质为叶绿素、多糖、黄酮类、萜类或没食子酸；
S2.研磨罐充填惰性气体密封后，置于球磨机械上以50~800rpm研磨0.5~96h；所述球磨机械采用振动式球磨机；
S3.采用非氧化性溶剂对步骤S2获得的产物进行清洗，得到纳米铁材料。
2.根据权利要求1所述的一种机械化学制备纳米材料的方法，其特征在于：所述含铁化合物选自氯化铁、氯化亚铁、硫酸铁、醋酸铁、碳酸铁、硫酸亚铁、草酸亚铁、柠檬酸铁、氢氧化铁、氧化铁、硫化铁、二茂铁、乙酰丙酮铁中的一种或几种。
3.根据权利要求1所述的一种机械化学制备纳米材料的方法，其特征在于：步骤S1中还加入一定质量的高分子聚合物、惰性盐类、掺杂物质前躯体或载体材料，混合后再放入研磨罐中。
4.根据权利要求3所述的一种机械化学制备纳米材料的方法，其特征在于：所述高分子聚合物选自聚乙烯吡咯烷酮、聚乙烯醇、聚丙烯酰胺、聚丙烯酸、羧甲基纤维素、淀粉、十二烷基磺酸钠中的一种或几种。
5.根据权利要求3所述的一种机械化学制备纳米材料的方法，其特征在于：所述惰性盐类选自氯化钠、氯化钾、硫酸钠、硫酸钾、碳酸钠、碳酸钾中的一种或几种。
6.根据权利要求3所述的一种机械化学制备纳米材料的方法，其特征在于：所述掺杂物质前躯体选自硼化合物、硫化合物、磷化合物、钙化合物、镁化合物、镍化合物、钴化合物、锰化合物、铜化合物、锌化合物、硒化合物、锡化合物、锆化合物、钼化合物、钌化合物、铑化合物、钯化合物、镧化合物、铈化合物中的一种或几种。
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