CN107777732A - 一种纳米晶体Fe3O4微粒的制备方法 - Google Patents
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- 239000002159 nanocrystal Substances 0.000 title claims abstract description 30
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 30
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract description 17
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910001447 ferric ion Inorganic materials 0.000 claims abstract description 17
- 239000011259 mixed solution Substances 0.000 claims abstract description 16
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 15
- 238000001556 precipitation Methods 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 11
- 238000001291 vacuum drying Methods 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- 239000007790 solid phase Substances 0.000 claims abstract description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 13
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 239000006210 lotion Substances 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 4
- -1 iron ion Chemical class 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims 1
- 230000005415 magnetization Effects 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 7
- 150000002500 ions Chemical class 0.000 abstract description 6
- 239000002351 wastewater Substances 0.000 abstract description 6
- 238000005119 centrifugation Methods 0.000 abstract description 4
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 231100000331 toxic Toxicity 0.000 abstract description 3
- 230000002588 toxic effect Effects 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 2
- 230000005291 magnetic effect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 238000005272 metallurgy Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000002122 magnetic nanoparticle Substances 0.000 description 1
- 238000002595 magnetic resonance imaging Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- 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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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Abstract
一种纳米晶体Fe3O4微粒的制备方法，按以下步骤进行：（1）在容器中配制含Fe3＋和Fe2+混合溶液；（2）加入氨水溶液，然后在氮气和搅拌条件下超声分散，再加热到68±1℃搅拌40~60min，静置后过滤；（3）将固体沉淀水洗至中性，离心分离后的固相真空干燥去除水分。本发明的方法制备的纳米晶体Fe3O4微粒尺寸分布范围较窄；对废水中的有毒重金属离子具有非常高的吸附容量。
Description
技术领域
本发明属于材料科学领域，特别涉及一种纳米晶体Fe3O4微粒的制备方法。
背景技术
在冶金、制革、化工、矿冶、电池制造等行业的工业废水中均含有一种或几种上述的有毒金属，而且其浓度高于允许排放标准。废水中的有害金属通常经过沉淀、蒸发、溶剂萃取、离子交换 、反渗透、膜分离等方法脱除。其中，沉淀法需要消耗大量化学物品且产生废渣，对这些废渣的后续处理成本较高。
磁性纳米材料具有许多不同于常规材料的独特效应, 如量子尺寸效应、表面效应、小尺寸效应及宏观量子隧道效应等, 这些效应使磁性纳米粒子具有不同于常规材料的光、电、声、热、磁、敏感特性。因此使它们在诸如生物传感器、药物输送、润滑、太阳能电池等诸多领域得到应用，而这些用途与纳米粒子的微观结构密切相关。磁性纳米Fe3O4粒子由于其极小的颗粒尺寸、生物兼容性及铁磁特性在磁纪录、颜料、光催化、磁感应医学治疗（细胞分离、磁共振成像、视网膜切除、放射性治疗、药物定向输送）等领域得到广泛应用或引起关注。
发明内容
本发明的目的是提供一种纳米晶体Fe3O4微粒的制备方法，该微粒具有良好的吸附能力，能够用于废水。
本发明的方法按以下步骤进行：
1、在容器中配制含Fe3＋和Fe2+混合溶液，Fe2+与Fe3＋的摩尔比为Fe2+∶Fe3＋=1∶1.8，全部铁离子的浓度为0.6~0.8mol/L；
2、向混合溶液中加入氨水溶液，加入量按加入氨水溶液后混合溶液的pH ≥9；然后在氮气和搅拌条件下超声分散至少1h，再加热到68±1℃，在氮气条件下搅拌40~60min，静置至少3h后过滤分离出固体沉淀；
3、将固体沉淀水洗至洗液为中性，在转数为7000~15000 rpm的条件下离心分离，将离心分离后的固相真空干燥去除水分，获得纳米晶体Fe3O4微粒。
上述的氨水浓度为0.5~2mol/ L。
上述的超声分散时的超声频率为20kHz。
上述的真空干燥条件为：温度60±5℃，真空度小于60 Pa，时间不少于24h。
上述的纳米晶体Fe3O4微粒的微观结构由等轴的纳米晶粒组成，纳米晶粒的粒径为40~90 nm；饱和磁化强度M S= 7~7.1×10-3 A/m。
上述方法的主要反应方程式为：
Fe2 + + 2Fe3 + + 8NH3 ·H2O = Fe3O4 ↓+ 8NH+ 4 + 4H2O。
采用本发明的纳米晶体Fe3O4微粒对废水中的重金属离子的饱和吸附容量最高为36 mg/g。
本发明利用化学反应共沉淀技术在超声波的搅拌作用下，制备的纳米晶体Fe3O4微粒尺寸分布范围较窄；对废水中的有毒重金属离子具有非常高的吸附容量，对高密度磁带、集成电路的电磁波吸收、动态轴承密封、靶向药物、废水净化等领域的技术革新具有良好的应用前景。
具体实施方式
本发明实施例中采用的设备包括85-2数显恒温搅拌器，600-B型电热恒温水浴箱，CPS-3型超声搅拌装置，GL-16A型高速冷冻离心分离设备。
本发明实施例中采用氯化亚铁( FeCl2 ·4H2O)、三价铁盐( FeCl3 ·6H2O)与去离子水或蒸馏水配制含三价铁离子和二价铁离子的溶液。
实施例1
在容器中配制含Fe3＋和Fe2+混合溶液，Fe2+与Fe3＋的摩尔比为Fe2+∶Fe3＋=1∶1.8，全部铁离子的浓度为0.6mol/L；
向混合溶液中加入氨水溶液，加入量按加入氨水溶液后混合溶液的pH ≥9；然后在氮气和搅拌条件下超声分散1h，再加热到68±1℃，在氮气条件下搅拌40min，静置至少3h后过滤分离出固体沉淀；氨水浓度为0.5mol/ L，超声分散时的超声频率为20kHz；
将固体沉淀水洗至洗液为中性，在转数为15000 rpm的条件下离心分离，将离心分离后的固相真空干燥去除水分，获得纳米晶体Fe3O4微粒；真空干燥条件为：温度60±5℃，真空度小于60 Pa，时间不少于24h；
纳米晶体Fe3O4微粒的微观结构由等轴的纳米晶粒组成，纳米晶粒的粒径为40~90 nm；饱和磁化强度M S= 7×10-3 A/m。
实施例2
在容器中配制含Fe3＋和Fe2+混合溶液，Fe2+与Fe3＋的摩尔比为Fe2+∶Fe3＋=1∶1.8，全部铁离子的浓度为0.7mol/L；
向混合溶液中加入氨水溶液，加入量按加入氨水溶液后混合溶液的pH ≥9；然后在氮气和搅拌条件下超声分散1h，再加热到68±1℃，在氮气条件下搅拌50min，静置至少3h后过滤分离出固体沉淀；氨水浓度为1mol/ L，超声分散时的超声频率为20kHz；
将固体沉淀水洗至洗液为中性，在转数为10000 rpm的条件下离心分离，将离心分离后的固相真空干燥去除水分，获得纳米晶体Fe3O4微粒；真空干燥条件为：温度60±5℃，真空度小于60 Pa，时间不少于24h；
纳米晶体Fe3O4微粒的微观结构由等轴的纳米晶粒组成，纳米晶粒的粒径为40~90 nm；饱和磁化强度M S= 7.1×10-3 A/m。
实施例3
在容器中配制含Fe3＋和Fe2+混合溶液，Fe2+与Fe3＋的摩尔比为Fe2+∶Fe3＋=1∶1.8，全部铁离子的浓度为0.8mol/L；
向混合溶液中加入氨水溶液，加入量按加入氨水溶液后混合溶液的pH ≥9；然后在氮气和搅拌条件下超声分散1h，再加热到68±1℃，在氮气条件下搅拌60min，静置至少3h后过滤分离出固体沉淀；氨水浓度为2mol/ L，超声分散时的超声频率为20kHz；
将固体沉淀水洗至洗液为中性，在转数为7000rpm的条件下离心分离，将离心分离后的固相真空干燥去除水分，获得纳米晶体Fe3O4微粒；真空干燥条件为：温度60±5℃，真空度小于60 Pa，时间不少于24h；
纳米晶体Fe3O4微粒的微观结构由等轴的纳米晶粒组成，纳米晶粒的粒径为40~90 nm；饱和磁化强度M S= 7.1×10-3 A/m。
Claims (3)
1.一种纳米晶体Fe3O4微粒的制备方法，其特征在于按以下步骤进行：
（1）在容器中配制含Fe3＋和Fe2+混合溶液，Fe2+与Fe3＋的摩尔比为Fe2+∶Fe3＋=1∶1.8，全部铁离子的浓度为0.6~0.8mol/L；
（2）向混合溶液中加入氨水溶液，加入量按加入氨水溶液后混合溶液的pH ≥9；然后在氮气和搅拌条件下超声分散至少1h，再加热到68±1℃，在氮气条件下搅拌40~60min，静置至少3h后过滤分离出固体沉淀；
（3）将固体沉淀水洗至洗液为中性，在转数为7000~15000 rpm的条件下离心分离，将离心分离后的固相真空干燥去除水分，获得纳米晶体Fe3O4微粒。
2.根据权利要求1所述的一种纳米晶体Fe3O4微粒的制备方法，其特征在于所述的氨水的浓度为0.5~2mol/ L。
3.根据权利要求1所述的一种纳米晶体Fe3O4微粒的制备方法，其特征在于所述的纳米晶体Fe3O4微粒的微观结构由等轴的纳米晶粒组成，纳米晶粒的粒径为40~90 nm；饱和磁化强度M S= 7~7.1×10-3 A/m。
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| CN110655118A (zh) * | 2019-10-31 | 2020-01-07 | 吉林大学 | 一种四氧化三铁纳米晶的制备方法 |
| CN113117698A (zh) * | 2021-04-21 | 2021-07-16 | 宁夏大学 | 一种磁性纳米铁钼复合催化剂的制备方法及该催化剂的应用 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110655118A (zh) * | 2019-10-31 | 2020-01-07 | 吉林大学 | 一种四氧化三铁纳米晶的制备方法 |
| CN113117698A (zh) * | 2021-04-21 | 2021-07-16 | 宁夏大学 | 一种磁性纳米铁钼复合催化剂的制备方法及该催化剂的应用 |
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