CN110202132A - 一种埃洛石-铁镍合金复合材料及其制备方法 - Google Patents
一种埃洛石-铁镍合金复合材料及其制备方法 Download PDFInfo
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- 229910001030 Iron–nickel alloy Inorganic materials 0.000 title claims abstract description 37
- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- MTNDZQHUAFNZQY-UHFFFAOYSA-N imidazoline Chemical compound C1CN=CN1 MTNDZQHUAFNZQY-UHFFFAOYSA-N 0.000 claims abstract description 17
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 15
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 15
- -1 iron ions Chemical class 0.000 claims abstract description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- 229910052742 iron Inorganic materials 0.000 claims abstract description 8
- 238000009830 intercalation Methods 0.000 claims abstract description 7
- 230000002687 intercalation Effects 0.000 claims abstract description 7
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 6
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- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract 2
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- 238000006243 chemical reaction Methods 0.000 claims description 26
- 238000001291 vacuum drying Methods 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 13
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N dimethyl sulfoxide Natural products CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 238000004064 recycling Methods 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 229960001760 dimethyl sulfoxide Drugs 0.000 claims description 7
- NZJXADCEESMBPW-UHFFFAOYSA-N 1-methylsulfinyldecane Chemical compound CCCCCCCCCCS(C)=O NZJXADCEESMBPW-UHFFFAOYSA-N 0.000 claims description 6
- 150000003462 sulfoxides Chemical class 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 5
- 239000011229 interlayer Substances 0.000 claims description 4
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 claims description 4
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 4
- IAZDPXIOMUYVGZ-WFGJKAKNSA-N Dimethyl sulfoxide Chemical group [2H]C([2H])([2H])S(=O)C([2H])([2H])[2H] IAZDPXIOMUYVGZ-WFGJKAKNSA-N 0.000 claims description 3
- 241000446313 Lamella Species 0.000 claims description 3
- 229910000323 aluminium silicate Inorganic materials 0.000 claims description 3
- 239000002734 clay mineral Substances 0.000 claims description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000006460 hydrolysis reaction Methods 0.000 claims description 3
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 claims description 3
- 230000008595 infiltration Effects 0.000 claims description 3
- 238000001764 infiltration Methods 0.000 claims description 3
- 229910052622 kaolinite Inorganic materials 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
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- 230000000536 complexating effect Effects 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims 1
- 229910052782 aluminium Inorganic materials 0.000 claims 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 1
- 229910045601 alloy Inorganic materials 0.000 abstract description 8
- 239000000956 alloy Substances 0.000 abstract description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 6
- HPTYUNKZVDYXLP-UHFFFAOYSA-N aluminum;trihydroxy(trihydroxysilyloxy)silane;hydrate Chemical compound O.[Al].[Al].O[Si](O)(O)O[Si](O)(O)O HPTYUNKZVDYXLP-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052621 halloysite Inorganic materials 0.000 abstract description 6
- 239000011358 absorbing material Substances 0.000 abstract description 3
- 230000005389 magnetism Effects 0.000 abstract description 3
- 230000005415 magnetization Effects 0.000 abstract description 3
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 abstract description 2
- 239000006249 magnetic particle Substances 0.000 abstract description 2
- 229910052759 nickel Inorganic materials 0.000 abstract description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 abstract description 2
- 150000004696 coordination complex Chemical class 0.000 abstract 2
- 238000005054 agglomeration Methods 0.000 abstract 1
- 230000002776 aggregation Effects 0.000 abstract 1
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- 229910052739 hydrogen Inorganic materials 0.000 abstract 1
- 239000001257 hydrogen Substances 0.000 abstract 1
- 150000002500 ions Chemical group 0.000 abstract 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 abstract 1
- 239000002105 nanoparticle Substances 0.000 abstract 1
- 230000003647 oxidation Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 abstract 1
- 238000009736 wetting Methods 0.000 abstract 1
- 238000002604 ultrasonography Methods 0.000 description 7
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 229910018512 Al—OH Inorganic materials 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical compound [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- LVIYYTJTOKJJOC-UHFFFAOYSA-N nickel phthalocyanine Chemical compound [Ni+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 LVIYYTJTOKJJOC-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 229910002656 O–Si–O Inorganic materials 0.000 description 1
- 229910008051 Si-OH Inorganic materials 0.000 description 1
- 229910006358 Si—OH Inorganic materials 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 229960004887 ferric hydroxide Drugs 0.000 description 1
- 150000004687 hexahydrates Chemical class 0.000 description 1
- 125000002636 imidazolinyl group Chemical group 0.000 description 1
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
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- 238000001179 sorption measurement Methods 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/48—Coating with alloys
- C23C18/50—Coating with alloys with alloys based on iron, cobalt or nickel
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
本发明公开了一种埃洛石‑铁镍合金复合材料及其制备方法。首先将埃洛石分散于氯化铁、氯化镍混合溶液中，铁离子水解生成氢离子对埃洛石内壁进行酸蚀，扩大其内径；利用羧乙基两性咪唑啉对金属离子络合形成可溶性有机金属络合物，有机金属络合物具有羧乙基两性咪唑啉低表面能、润湿等特性，迅速在埃洛石内壁铺展开来，真空环境经水合肼还原处理，可得到铁镍合金插层的复合材料。本发明制备的埃洛石‑铁镍合金复合材料利用了埃洛石管状结构特点，将其作为纳米反应器，降低了铁、镍纳米颗粒被氧化的程度且限制了磁性颗粒之间的团聚，制备出磁能积更高、剩磁对温度依赖小、磁化特性优良的铁镍合金，可广泛应用于吸波材料、硬质合金、合金镀层等行业。
Description
技术领域
本发明涉及化合物的制备方法，尤其涉及一种埃洛石-铁镍合金复合材料及其制备方法。
背景技术
埃洛石是一种1:1二八面体高岭土系矿物，Al：Si为1:1，该矿物最普遍的形貌是中空管状结构，铝氧八面体层与硅氧四面体层间空间的不相匹配错位促使片状晶体卷曲成管。管内侧为Al-OH基团，管边缘为Al-OH和Si-OH基团，管外表面基团主要以O-Si-O存在，铝氧化物与硅氧化物等电点相异导致内层表征为带正电，外层表征为带负电。内外基团特征及带电性质为其选择性改性提供了多种途径，使其具有优良的材料加强性能，其在物质吸附、存储、运输以及电化学、储能等方面都具有优良的性能。
铁镍纳米合金粉体由于具有不同于单质铁、镍金属粉末的特殊性能以及特殊的表面磁性，在吸波材料、硬质合金、合金镀层等行业具有广泛的应用前景，例如由于晶粒细化，在记忆磁鼓、磁卡等电子产品方面也得到了广泛应用。铁镍合金粉体处纳米粒径将表现出磁能积更高、剩磁对温度依赖小、磁化特性优良等特点。
发明内容
为了克服现有技术的不足，本发明的目的是提供一种埃洛石-铁镍合金复合材料及其制备方法，通过创新的技术手段将铁镍合金插层进入埃洛石内管，控制粒径与分散性。本发明充分利用了我国丰富的埃洛石矿，为制备铁镍纳米合金粉体提供了优良的纳米反应材料，同时丰富了其制备途径与应用前景。
一种埃洛石-铁镍合金复合材料，由铁镍合金插层埃洛石得到；所述的埃洛石(HNTs)是一种天然铝硅酸盐管状粘土矿物，由高岭石片层在天然条件下卷曲而成；铁镍合金颗粒均匀分布于埃洛石层间。
一种所述的埃洛石-单质铁复合材料的制备方法，将埃洛石分散于氯化铁、氯化镍六水合物混合溶液中，加热促进金属离子水解，产生酸性环境，氢离子进入埃洛石内管，与铝氧八面体层反应，酸化生成无定型铝氧化物以及铝离子，酸蚀扩大埃洛石管内径；利用羧乙基两性咪唑啉对金属离子络合形成可溶性有机金属络合物，可溶性有机金属络合物在埃洛石内壁铺展开来，真空环境经水合肼还原处理，得到铁镍合金插层的复合材料。
所述的制备方法，步骤如下：
1）取10g粒径分布为0.1～200μm的埃洛石，加入50～100mL FeCl3浓度为3～5.67mol/L、NiCl2.6H2O浓度为0.33～0.81 mol/L混合溶液，80～120℃回流反应10～30h，反应完成后将混合体系过滤，取液相，记为液相①，取过滤后固体水洗三次，60℃真空干燥，记为固体①；
2）取1～3g羧乙基两性咪唑啉溶于50～100mL亚砜溶剂，加入固体①，超声20min，室温磁力搅拌20～40h，过滤回收固体，水洗三次，40～60℃烘干，磨细备用，记为固体②；
3）取固体②与液相①均匀混合，室温抽真空磁力搅拌20～30min，重复两次，过滤回收固体，水洗三次，记为固体③；
4）取固体③分散于浓度为2～4mol/L的水合肼水溶液中，室温磁力搅拌10～30min，过滤回收固体，水洗三次，40～60℃真空干燥即得到埃洛石-铁镍合金复合材料。
所述的亚砜溶剂为二甲基亚砜或癸基甲基亚砜，作为溶解和促渗体系。
本发明的有益效果：
提出的埃洛石-铁镍合金复合材料的制备方法，矿石来源丰富，价格低廉，涉及的表面活性剂绿色环保易降解，反应原理与工艺流程可通过简易反应器实现，操作条件节能环保。制备的埃洛石-铁镍合金复合材料，不仅综合了埃洛石中空管状结构和其稳定的矿物结构特征，而且制备的纳米尺寸铁镍合金在稳定性与分散性方面的性能得到了有效提高，扩大了其应用前景。本发明制备的埃洛石-铁镍合金复合材料利用了埃洛石管状结构特点，将其作为纳米反应器，降低了铁、镍纳米颗粒被氧化的程度且限制了磁性颗粒之间的团聚，制备出磁能积更高、剩磁对温度依赖小、磁化特性优良的铁镍合金，可广泛应用于吸波材料、硬质合金、合金镀层等行业。
具体实施方式
以下对本发明进行具体阐述。
一种埃洛石-铁镍合金复合材料，由铁镍合金插层埃洛石得到；所述的埃洛石(HNTs)是一种天然铝硅酸盐管状粘土矿物，由高岭石片层在天然条件下卷曲而成；铁镍合金颗粒均匀分布于埃洛石层间。
一种所述的埃洛石-单质铁复合材料的制备方法，第一步是将埃洛石分散于氯化铁、氯化镍六水合物混合溶液中，加热促进金属离子水解，产生酸性环境。
具体反应如下：
氢离子进入埃洛石内管，与铝氧八面体层反应，酸化生成无定型铝氧化物以及铝离子，酸蚀扩大埃洛石管内径。反应完成后将混合体系过滤，得到液相和固体，记为取液相①和固体①。
第二步是制备咪唑啉改性的埃洛石。将步骤一的固体①分散于羟乙基两性咪唑啉表面活性剂溶液中，碱性溶液条件下羟乙基两性咪唑啉能有效降低埃洛石表面能，且其带负电，埃洛石管内带正电，磁力搅拌充分接触，通过静电吸附作用，润湿性较好的羟乙基两性咪唑啉迅速在埃洛石管内铺展开来得到改性后的埃洛石（固体②）。
第三步是将液相①与固体②充分混合，使溶液中带正电的氢氧化铁胶体、铁离子、镍离子与附着在埃洛石管内的羟乙基两性咪唑啉充分接触，反应生成有机金属络合物。
第四步是通过水合肼的还原作用将三价铁和二价镍还原生成铁镍单质。水合肼分子量较小，渗透性优异，在搅拌作用下可充分进入埃洛石纳米管管内与三价铁和二价镍作用，将其还原生成铁镍合金，水洗干燥固相即可得到埃洛石-铁镍合金复合材料。
所述的制备方法，步骤如下：
1）取10g粒径分布为0.1～200μm的埃洛石，加入50～100mL FeCl3浓度为3～5.67mol/L、NiCl2.6H2O浓度为0.33～0.81 mol/L混合溶液，80～120℃回流反应10～30h，反应完成后将混合体系过滤，取液相，记为液相①，取过滤后固体水洗三次，60℃真空干燥，记为固体①；
2）取1～3g羧乙基两性咪唑啉溶于50～100mL亚砜溶剂，加入固体①，超声20min，室温磁力搅拌20～40h，过滤回收固体，水洗三次，40～60℃烘干，磨细备用，记为固体②；
3）取固体②与液相①均匀混合，室温抽真空磁力搅拌20～30min，重复两次，过滤回收固体，水洗三次，记为固体③；
4）取固体③分散于浓度为2～4mol/L的水合肼水溶液中，室温磁力搅拌10～30min，过滤回收固体，水洗三次，40～60℃真空干燥即得到埃洛石-铁镍合金复合材料。
所述的亚砜溶剂为二甲基亚砜或癸基甲基亚砜，作为溶解和促渗体系。
以下结合实施例进一步对本发明做进一步的阐述。
实施例1
1）取10g粒径分布为0.1～200μm的埃洛石，加入50～100mL FeCl3浓度为3～5.67mol/L、NiCl2.6H2O浓度为0.33～0.81 mol/L混合溶液，80～120℃回流反应10～30h，反应完成后将混合体系过滤，取液相，记为液相①，取过滤后固体水洗三次，60℃真空干燥，记为固体①；
2）取1～3g羧乙基两性咪唑啉溶于50～100mL二甲基亚砜溶剂，加入固体①，超声20min，室温磁力搅拌20～40h，过滤回收固体，水洗三次，40～60℃烘干，磨细备用，记为固体②；
3）取固体②与液相①均匀混合，室温抽真空磁力搅拌20～30min，重复两次，过滤回收固体，水洗三次，记为固体③；
4）取固体③分散于浓度为2～4mol/L的水合肼水溶液中，室温磁力搅拌10～30min，过滤回收固体，水洗三次，40～60℃真空干燥即得到埃洛石-铁镍合金复合材料。
实施例2
1）取10g粒径分布为0.1～200μm的埃洛石，加入50～100mL FeCl3浓度为3～5.67mol/L、NiCl2.6H2O浓度为0.33～0.81 mol/L混合溶液，80～120℃回流反应10～30h，反应完成后将混合体系过滤，取液相，记为液相①，取过滤后固体水洗三次，60℃真空干燥，记为固体①；
2）取1～3g羧乙基两性咪唑啉溶于50～100mL癸甲基亚砜溶剂，加入固体①，超声20min，室温磁力搅拌20～40h，过滤回收固体，水洗三次，40～60℃烘干，磨细备用，记为固体②；
3）取固体②与液相①均匀混合，室温抽真空磁力搅拌20～30min，重复两次，过滤回收固体，水洗三次，记为固体③；
4）取固体③分散于浓度为2～4mol/L的水合肼水溶液中，室温磁力搅拌10～30min，过滤回收固体，水洗三次，40～60℃真空干燥即得到埃洛石-铁镍合金复合材料。
实施例3
1）取10g粒径分布为0.1～200μm的埃洛石，加入50～100mL FeCl3浓度为3～5.67mol/L、NiCl2.6H2O浓度为0.33～0.81 mol/L混合溶液，80～120℃回流反应10～30h，反应完成后将混合体系过滤，取液相，记为液相①，取过滤后固体水洗三次，60℃真空干燥，记为固体①；
2）取1～3g羧乙基两性咪唑啉溶于50～100mL二甲基亚砜溶剂，加入固体①，超声20min，室温磁力搅拌20～40h，过滤回收固体，水洗三次，40～60℃烘干，磨细备用，记为固体②；
3）取固体②与液相①均匀混合，室温抽真空磁力搅拌20～30min，重复两次，过滤回收固体，水洗三次，记为固体③；
4）取固体③分散于浓度为2～4mol/L的水合肼水溶液中，室温磁力搅拌10～30min，过滤回收固体，水洗三次，40～60℃真空干燥即得到埃洛石-铁镍合金复合材料。
实施例4
1）取10g粒径分布为0.1～200μm的埃洛石，加入50～100mL FeCl3浓度为3～5.67mol/L、NiCl2.6H2O浓度为0.33～0.81 mol/L混合溶液，80～120℃回流反应10～30h，反应完成后将混合体系过滤，取液相，记为液相①，取过滤后固体水洗三次，60℃真空干燥，记为固体①；
2）取1～3g羧乙基两性咪唑啉溶于50～100mL癸甲基亚砜溶剂，加入固体①，超声20min，室温磁力搅拌20～40h，过滤回收固体，水洗三次，40～60℃烘干，磨细备用，记为固体②；
3）取固体②与液相①均匀混合，室温抽真空磁力搅拌20～30min，重复两次，过滤回收固体，水洗三次，记为固体③；
4）取固体③分散于浓度为2～4mol/L的水合肼水溶液中，室温磁力搅拌10～30min，过滤回收固体，水洗三次，40～60℃真空干燥即得到埃洛石-铁镍合金复合材料。
实施例5
1）取10g粒径分布为0.1～200μm的埃洛石，加入50～100mL FeCl3浓度为3～5.67mol/L、NiCl2.6H2O浓度为0.33～0.81 mol/L混合溶液，80～120℃回流反应10～30h，反应完成后将混合体系过滤，取液相，记为液相①，取过滤后固体水洗三次，60℃真空干燥，记为固体①；
2）取1～3g羧乙基两性咪唑啉溶于50～100mL二甲基亚砜溶剂，加入固体①，超声20min，室温磁力搅拌20～40h，过滤回收固体，水洗三次，40～60℃烘干，磨细备用，记为固体②；
3）取固体②与液相①均匀混合，室温抽真空磁力搅拌20～30min，重复两次，过滤回收固体，水洗三次，记为固体③；
4）取固体③分散于浓度为2～4mol/L的水合肼水溶液中，室温磁力搅拌10～30min，过滤回收固体，水洗三次，40～60℃真空干燥即得到埃洛石-铁镍合金复合材料。
实施例6
1）取10g粒径分布为0.1～200μm的埃洛石，加入50～100mL FeCl3浓度为3～5.67mol/L、NiCl2.6H2O浓度为0.33～0.81 mol/L混合溶液，80～120℃回流反应10～30h，反应完成后将混合体系过滤，取液相，记为液相①，取过滤后固体水洗三次，60℃真空干燥，记为固体①；
2）取1～3g羧乙基两性咪唑啉溶于50～100mL癸甲基亚砜溶剂，加入固体①，超声20min，室温磁力搅拌20～40h，过滤回收固体，水洗三次，40～60℃烘干，磨细备用，记为固体②；
3）取固体②与液相①均匀混合，室温抽真空磁力搅拌20～30min，重复两次，过滤回收固体，水洗三次，记为固体③；
4）取固体③分散于浓度为2～4mol/L的水合肼水溶液中，室温磁力搅拌10～30min，过滤回收固体，水洗三次，40～60℃真空干燥即得到埃洛石-铁镍合金复合材料。
实施例7
1）取10g粒径分布为0.1～200μm的埃洛石，加入50～100mL FeCl3浓度为3～5.67mol/L、NiCl2.6H2O浓度为0.33～0.81 mol/L混合溶液，80～120℃回流反应10～30h，反应完成后将混合体系过滤，取液相，记为液相①，取过滤后固体水洗三次，60℃真空干燥，记为固体①；
2）取1～3g羧乙基两性咪唑啉溶于50～100mL二甲基亚砜溶剂，加入固体①，超声20min，室温磁力搅拌20～40h，过滤回收固体，水洗三次，40～60℃烘干，磨细备用，记为固体②；
3）取固体②与液相①均匀混合，室温抽真空磁力搅拌20～30min，重复两次，过滤回收固体，水洗三次，记为固体③；
4）取固体③分散于浓度为2～4mol/L的水合肼水溶液中，室温磁力搅拌10～30min，过滤回收固体，水洗三次，40～60℃真空干燥即得到埃洛石-铁镍合金复合材料。
Claims (4)
1.一种埃洛石-铁镍合金复合材料，其特征在于，由铁镍合金插层埃洛石得到；所述的埃洛石是一种天然铝硅酸盐管状粘土矿物，由高岭石片层在天然条件下卷曲而成；铁镍合金颗粒均匀分布于埃洛石层间。
2.一种根据权利要求1所述的埃洛石-单质铁复合材料的制备方法，其特征在于，
将埃洛石分散于氯化铁、氯化镍六水合物混合溶液中，加热促进金属离子水解，产生酸性环境，氢离子进入埃洛石内管，与铝氧八面体层反应，酸化生成无定型铝氧化物以及铝离子，酸蚀扩大埃洛石管内径；利用羧乙基两性咪唑啉对金属离子络合形成可溶性有机金属络合物，可溶性有机金属络合物在埃洛石内壁铺展开来，真空环境经水合肼还原处理，得到铁镍合金插层的复合材料。
3.根据权利要求2所述的制备方法，其特征在于，步骤如下：
1）取10g粒径分布为0.1～200μm的埃洛石，加入50～100mL 混合溶液，其中FeCl3浓度为3～5.67mol/L，NiCl2.6H2O浓度为0.33～0.81 mol/L，80～120℃回流反应10～30h，反应完成后将混合体系过滤，取液相，记为液相①，取过滤后固体水洗三次，60℃真空干燥，记为固体①；
2）取1～3g羧乙基两性咪唑啉溶于50～100mL亚砜溶剂，加入固体①，超声20min，室温磁力搅拌20～40h，过滤回收固体，水洗三次，40～60℃烘干，磨细备用，记为固体②；
3）取固体②与液相①均匀混合，室温抽真空磁力搅拌20～30min，重复两次，过滤回收固体，水洗三次，记为固体③；
4）取固体③分散于浓度为2～4mol/L的水合肼水溶液中，室温磁力搅拌10～30min，过滤回收固体，水洗三次，40～60℃真空干燥即得到埃洛石-铁镍合金复合材料。
4.根据权利要求2所述的制备方法，其特征在于，所述的亚砜溶剂为二甲基亚砜或癸基甲基亚砜，作为溶解和促渗体系。
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