CN108479724A - A kind of preparation method with high magnetic responsiveness iron-iron oxide@polyphosphazene magnetic nano chains - Google Patents
A kind of preparation method with high magnetic responsiveness iron-iron oxide@polyphosphazene magnetic nano chains Download PDFInfo
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- CN108479724A CN108479724A CN201810087254.XA CN201810087254A CN108479724A CN 108479724 A CN108479724 A CN 108479724A CN 201810087254 A CN201810087254 A CN 201810087254A CN 108479724 A CN108479724 A CN 108479724A
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- iron
- iron oxide
- polyphosphazene
- magnetic nano
- magnetic
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- IGHXQFUXKMLEAW-UHFFFAOYSA-N iron(2+) oxygen(2-) Chemical compound [O-2].[Fe+2].[Fe+2].[O-2] IGHXQFUXKMLEAW-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 229920002627 poly(phosphazenes) Polymers 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 230000004043 responsiveness Effects 0.000 title claims abstract description 22
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000002604 ultrasonography Methods 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 5
- 239000002253 acid Substances 0.000 claims abstract description 3
- 239000011230 binding agent Substances 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 20
- 239000007787 solid Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 235000019441 ethanol Nutrition 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 12
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical group CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 9
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical group [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 7
- 239000011591 potassium Substances 0.000 claims description 7
- 229910052700 potassium Inorganic materials 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 229910010277 boron hydride Inorganic materials 0.000 claims description 6
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims description 6
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 6
- 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 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 5
- -1 4,4 '-diaminodiphenyl ethers Chemical class 0.000 claims description 4
- 229920002873 Polyethylenimine Polymers 0.000 claims description 4
- VERMEZLHWFHDLK-UHFFFAOYSA-N benzene-1,2,3,4-tetrol Chemical compound OC1=CC=C(O)C(O)=C1O VERMEZLHWFHDLK-UHFFFAOYSA-N 0.000 claims description 4
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical compound B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- MQJKPEGWNLWLTK-UHFFFAOYSA-N Dapsone Chemical group C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=C1 MQJKPEGWNLWLTK-UHFFFAOYSA-N 0.000 claims description 3
- 150000002505 iron Chemical class 0.000 claims description 3
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims description 3
- 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 3
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 3
- 239000000178 monomer Substances 0.000 claims description 3
- QCDYQQDYXPDABM-UHFFFAOYSA-N phloroglucinol Chemical compound OC1=CC(O)=CC(O)=C1 QCDYQQDYXPDABM-UHFFFAOYSA-N 0.000 claims description 3
- 229960001553 phloroglucinol Drugs 0.000 claims description 3
- 239000012266 salt solution Substances 0.000 claims description 3
- XCJXQCUJXDUNDN-UHFFFAOYSA-N chlordene Chemical group C12C=CCC2C2(Cl)C(Cl)=C(Cl)C1(Cl)C2(Cl)Cl XCJXQCUJXDUNDN-UHFFFAOYSA-N 0.000 claims description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 2
- 239000012279 sodium borohydride Substances 0.000 claims description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 2
- KZTYYGOKRVBIMI-UHFFFAOYSA-N diphenyl sulfone Chemical compound C=1C=CC=CC=1S(=O)(=O)C1=CC=CC=C1 KZTYYGOKRVBIMI-UHFFFAOYSA-N 0.000 claims 4
- 238000006068 polycondensation reaction Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 16
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 24
- 238000013019 agitation Methods 0.000 description 12
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 12
- 238000000643 oven drying Methods 0.000 description 12
- 229910052742 iron Inorganic materials 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 241000209094 Oryza Species 0.000 description 3
- 235000007164 Oryza sativa Nutrition 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 235000009566 rice Nutrition 0.000 description 3
- OTEKOJQFKOIXMU-UHFFFAOYSA-N 1,4-bis(trichloromethyl)benzene Chemical compound ClC(Cl)(Cl)C1=CC=C(C(Cl)(Cl)Cl)C=C1 OTEKOJQFKOIXMU-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229910017135 Fe—O Inorganic materials 0.000 description 1
- 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 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 description 1
- QVYYOKWPCQYKEY-UHFFFAOYSA-N [Fe].[Co] Chemical compound [Fe].[Co] QVYYOKWPCQYKEY-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- ZSTLPJLUQNQBDQ-UHFFFAOYSA-N azanylidyne(dihydroxy)-$l^{5}-phosphane Chemical compound OP(O)#N ZSTLPJLUQNQBDQ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000013500 data storage Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000000609 electron-beam lithography Methods 0.000 description 1
- 229940056319 ferrosoferric oxide Drugs 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 description 1
- WTFXARWRTYJXII-UHFFFAOYSA-N iron(2+);iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Fe+2].[Fe+3].[Fe+3] WTFXARWRTYJXII-UHFFFAOYSA-N 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012673 precipitation polymerization Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/06—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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- 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
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/28—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of the platinum group metals, iron group metals or copper
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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- B01J35/33—Electric or magnetic properties
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- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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- Materials Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The present invention relates to a kind of preparation methods with high magnetic responsiveness iron iron oxide@polyphosphazene magnetic nano chains comprising following steps：1）Prepare one-dimensional iron iron oxide magnetic nano chain；2）Using prepared one-dimensional iron iron oxide magnetic nano chain as template, hexachlorocyclotriph,sphazene and comonomer are added in the presence of a solvent, and using triethylamine as acid binding agent, 0.5-1h is reacted in 20-80 DEG C under ultrasound condition, obtains iron iron oxide@polyphosphazene magnetic nano chains through Magneto separate, washing, drying after reaction.The method of the present invention is not required to directly prepare one-dimensional magnetic nanochain by externally-applied magnetic field；Preparation process is simple and convenient to operate, and is suitble to industrialized production, and the iron iron oxide@polyphosphazene magnetic nano chains prepared have 90 120 emu g‑1High magnetic responsiveness.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, and in particular to one kind has high magnetic responsiveness iron-iron oxide@poly-
The preparation method of phosphonitrile magnetic nano chain is mainly used for synthesizing one-dimensional magnetic Nano material.
Background technology
Come in the past few decades, field of nanometer material technology achieves incredible fast development.Therefore, a large amount of document
It reports and how to manufacture variously-shaped micron and nanostructure.Wherein, one-dimensional（1D）Structure, such as nanometer rods, pipe, fiber band,
Especially nano chain is most frequently studied, because they are such as drug sensors in modern development application, data storage,
Energy stores and conversion, the very important part such as catalysis.In addition, these materials play important work in basic research
With because they connect nanometer object and macrocosm.In addition, compared with nano particle, rodlike, tubulose, threadiness
Or linear nano material is capable of providing more active surfaces, because they will not form such densification as nano particle
Aggregate.However, the principal element for actually influencing their final performances is still their preparation method, and therefore, people
Still new, simple and cheap synthesis strategy is being found.
So far, many synthetic methods have been developed and have been applied successfully to production metal micro chain and nano chain
（Such as iron nano chain, nickel nano chain, cobalt nano chain）And binary metal alloy nano chain（Such as nickel cobalt nano chain, iron cobalt nanometer
Chain, iron nickel nano chain）.In general, they can be divided into three classes, including solid state technology, gaseous techniques and be based on liquid phase or molten
The technology of liquid.The micro-nano chain manufacturing method being firstly mentioned relates generally to electron beam lithography and ultrashort laser ablation, and
Two kinds of methods include chemical vapor deposition（CVD）, thermal decomposition, focus the methods of e-beam induced deposition molecular beam epitaxy.However,
Both methods is all fairly expensive and time-consuming.Moreover, they usually require considerably complicated equipment, do not allow to mass produce micro-
Rice or nano chain.Therefore, the third possible chain structure synthetic schemes is that the technology based on liquid or solution seemingly can
The most potential technology in terms of lower temperature and pressure is applied, and this method is at low cost, equipment is simple, and yield
It is high.
102502873 A of Chinese invention patent CN propose a kind of preparation method of one-dimensional magnetic nanochain, and being will be molten
The high magnetic responsiveness ferroso-ferric oxide of monodisperse prepared by the hot method of agent is that core passes through magnetic field using acrylic monomer as function monomer
Induce self assembly, prepared during precipitation polymerization clean surface, permalink one-dimensional magnetic nanochain, one-dimensional magnetic
A length of 2~14 μm of nano chain chain, magnetic saturation intensity are about 78.1 emu g-1.The one-dimensional magnetic nanochain that this method obtains
Preparation process is complicated, and obtained magnetic nano chain magnetic saturation intensity is relatively low.107282026 A of Chinese invention patent CN are carried
Go out with ferric iron, acetate, dispersant and organic amine or organic acid for raw material, has obtained magnetic nanometer composite material, the material
The material of chain structure can be obtained by hydrogen bond or induced by magnetic field again, the magnetic saturation intensity of gained composite material is 56.8 emu
g-1, there is still a need for external magnetic field inductions for this method, and step is complicated, and products therefrom magnetic saturation intensity is relatively low.In conclusion passing through letter
Single method is not required to externally-applied magnetic field induction, and the one-dimensional magnetic nanochain for directly preparing high magnetic saturation intensity is still huge chooses
War.
Invention content
Present invention aims to overcome that prior art defect, provides a kind of with high magnetic responsiveness iron-iron oxide@polyphosphazenes
The preparation method of magnetic nano chain, this method under the conditions of outer induced by magnetic field without carrying out, and preparation process is simple, operation side
Just, the magnetic saturation intensity of product is higher, is suitble to industrialized production.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of preparation method with high magnetic responsiveness iron-iron oxide@polyphosphazene magnetic nano chains comprising following steps：
1）Prepare one-dimensional iron-iron oxide magnetic nano chain；
2）Using prepared one-dimensional iron-iron oxide magnetic nano chain as template, chlordene ring is added in the presence of a solvent
Three phosphonitriles and comonomer, and using triethylamine as acid binding agent, 0.5-1h, reaction are reacted in 20-80 DEG C under ultrasound condition
After end iron-iron oxide polyphosphazene magnetic nano chain is obtained through Magneto separate, washing, drying.Prepare iron-iron oxide@of gained
Polyphosphazene magnetic nano chain has using iron-iron oxide as core, and using polyphosphazene as the nucleocapsid of shell, wherein iron-iron oxide is straight
For diameter in 30-100 nm, the thickness of polyphosphazene shell is 2-150 nm；Iron-iron oxide@polyphosphazene magnetic nano chains have 90-120
The magnetic saturation intensity of emu g-1.
Specifically, step 2）In, the solvent can be acetonitrile, tetrahydrofuran, ethyl alcohol, methanol or acetone etc..Per 50mg
One-dimensional iron-iron oxide magnetic nano chain in, the additive amount of solvent is 60-100ml, and the additive amount of triethylamine is 2-10ml.
Specifically, step 2）In, the comonomer can be 4,4'-diaminodiphenyl sulfone, 4,4 '-diamino hexichol
Ether, 4,4 '-dihydroxydiphenylsulisomers, to biphenol, phloroglucin, trihydroxy phenol, 4,4 '-dioxydiphenyl methanes or branched
Polyethyleneimine（Average molecular weight 600-5000）；The molar ratio of comonomer and hexachlorocyclotriph,sphazene is 1-6：1.
Specifically, step 2）In, the quality of one-dimensional iron-iron oxide magnetic nano chain used and hexachlorocyclotriph,sphazene is
1-2：1.
Further, step 1）Specially：Boron hydride is dissolved in solvent hexamethylene, then in mixture of ice and water
Mechanic whirl-nett reaction 0.1-0.5 h, reaction terminate to obtain fluffy solid, and ultrasound makes fluffy solid dissolve, and continues under stirring condition
Iron salt solutions are added and react 0.1-1 h, obtain one-dimensional iron-iron oxide magnetic nano chain.
Specifically, step 1）In, the boron hydride is potassium borohydride or sodium borohydride；The iron salt solutions are ferric iron
Salting liquid, such as ferric chloride hexahydrate aqueous solution, ferric sulfate aqueous solution or iron nitrate aqueous solution, the quality of boron hydride and molysite
Than for 0.5-0.9：1.
Compared to the prior art, the method for the present invention has the beneficial effect that：
1）The high magnetic responsiveness iron prepared in the present invention-iron oxide@polyphosphazene nano chains have core@shell structures, highly cross-linked
Polyphosphazene shell can form good protection to stratum nucleare iron-iron oxide；
2）The technique that the present invention prepares high magnetic responsiveness nano chain is relatively simple, and repeatability is strong, it is more to obtain product, reaction item
Part is easy to reach, low for equipment requirements, largely reduces production cost；
3）Using iron-iron oxide@polyphosphazene magnetic nano chains that the method for the present invention prepares gained has using iron-iron oxide as core,
Using polyphosphazene as the nucleocapsid of shell, wherein for the diameter of iron-iron oxide in 30-100 nm, the thickness of polyphosphazene shell is 2-150
nm；Iron-iron oxide@polyphosphazene magnetic nano chains have 90-120 emu g-1High magnetic saturation intensity, and it is steady with preferable heat
Qualitative and aqueous dispersion；
4）The method of the present invention is prepared in iron-iron oxide@polyphosphazene nano chains of gained, and polyphosphazene has stronger Dye Adsorption ability
And metallic coordination ability, iron-iron oxide@polyphosphazene nano chains can be made to be applied to environment adsorbing domain and catalytic field.
Description of the drawings：
Fig. 1 is the digital photograph for one-dimensional iron-iron oxide magnetic nano chain that embodiment 1 obtains；
Fig. 2 is the Fourier transform infrared spectroscopy figure for iron-iron oxide@polyphosphazene magnetic nano chains that embodiment 1 is prepared；
Fig. 3 is the energy spectrum diagram for iron-iron oxide@polyphosphazene magnetic nano chains that embodiment 1 is prepared；
Fig. 4 is the scanning electron microscope (SEM) photograph for iron-iron oxide@polyphosphazene magnetic nano chains that embodiment 1 is prepared；
Fig. 5 is one-dimensional iron-iron oxide magnetic nano chain that embodiment 1 is prepared and iron-iron oxide@polyphosphazene magnetic nano chains
Hysteresis loop（VSM）.
Specific implementation mode
Technical scheme of the present invention is further discussed in detail with reference to embodiments, but protection scope of the present invention
It is not limited thereto.
Embodiment 1
A kind of preparation method with high magnetic responsiveness iron-iron oxide@polyphosphazene magnetic nano chains, specifically includes following step
Suddenly：
1）Prepare one-dimensional iron-iron oxide magnetic nano chain；
By 1.0g potassium borohydrides, 50 milliliters of hexamethylenes, mechanical agitation dissolves in the flask of 250ml, and flask is then positioned over ice
Mechanical agitation about half an hour in aqueous mixtures（Rotating speed is about 700 rev/min）, react and terminate to obtain fluffy solid.It takes out and burns
Simultaneously ultrasound makes fluffy solid dissolve to bottle, continues to stir, the ferric chloride hexahydrate aqueous solution of 50 milliliter of 0.1 mol/L is added
（6H2O·FeCl3, 1.38g）, continue stir about and stop stirring in 30 minutes, sample is collected with magnet, after water, ethyl alcohol sequentially wash,
12 h of oven drying obtains one-dimensional iron-iron oxide magnetic nano chain；
2）The one-dimensional iron of 50 mg-iron oxide magnetic nano chain is taken, is added in the flask equipped with 70 ml acetonitriles, 80 DEG C, 40W ultrasound items
Under part, 25mg is added（0.000072 mol）Hexachlorocyclotriph,sphazene and 54mg（0.00022 mol）4,4'-diaminodiphenyl sulfone,
2 ml triethylamines are added after ultrasonic half an hour, reaction was completed after continuation ultrasonic half an hour.Magnet collects sample, each with water, ethyl alcohol
Washing three times, 40 DEG C of 12 h of oven drying are to get iron-iron oxide@polyphosphazene magnetic nano chains.Gained iron-iron oxide@polyphosphazenes
For magnetic nano chain thickness in 1-30nm, magnetic saturation intensity is 102 emu g-1。
Fig. 1 is step 1 in embodiment 1）The digital photograph of the one-dimensional iron-iron oxide magnetic nano chain of gained is prepared, it can in figure
Will become apparent from：Product is solid powder sample, and sample homogeneity is good, and sample size is larger.
Fig. 2 is the Fourier transform infrared spectroscopy for iron-iron oxide@polyphosphazene magnetic nano chains that embodiment 1 is prepared
Scheme, 3441 cm in figure-1Peak correspond to O-H keys, 1488 cm-1With 1591 cm-1Peak correspond to the aromatic rings of C=C, in figure
1287 cm-1With 1154 cm-1Corresponding is the resonance absorbing peak of O=S=O keys, 1184 cm-1Corresponding bands of a spectrum are the flexible of P=N
Vibration peak, 937 cm-1The stretching vibration peak of corresponding bands of a spectrum Ar-O-P, 500-700 cm-1Peak belong to the flexible peak of Fe-O,
Spectrum Analysis explanation：Polyphosphazene is successfully coated on iron-ferric oxide nano chain surface.
The energy spectrum diagram of the iron that Fig. 3 embodiments 1 are prepared-iron oxide@polyphosphazene magnetic nano chains.It can from energy spectrum diagram
Go out：Contained member is known as iron, oxygen, carbon, nitrogen, chlorine, phosphorus, sulphur in prepared product, it was demonstrated that iron-iron oxide polyphosphazene composite material
（Fe-Fe2O3@PZS）Successful preparation.
Fig. 4 is the scanning electron microscopic picture for iron-iron oxide@polyphosphazene magnetic nano chains that embodiment 1 is prepared, can in figure
Can be seen that：Sample structure is one-dimensional nano material.
Fig. 5 is that one-dimensional iron-iron oxide magnetic nano chain that embodiment 1 is prepared and iron-iron oxide@polyphosphazene magnetism are received
The hysteresis loop of rice chain（VSM）.As can be seen from the figure：The magnetic saturation intensity of prepared iron-iron oxide is 130 emu g-1
（Curve a in figure）, after coating polyphosphazene, the magnetic saturation intensity of iron-iron oxide@polyphosphazene nano chains is still up to 102 emu
g-1（Curve b in figure）.
Embodiment 2
A kind of preparation method with high magnetic responsiveness iron-iron oxide@polyphosphazene magnetic nano chains, specifically includes following step
Suddenly：
1）Prepare one-dimensional iron-iron oxide magnetic nano chain；
By 0.75g sodium borohydrides, 50 milliliters of hexamethylenes, mechanical agitation dissolves in the flask of 250ml, is then positioned over flask
Mechanical agitation about half an hour in mixture of ice and water（Rotating speed is about 700 rev/min）, react and terminate to obtain fluffy solid.It takes out
Simultaneously ultrasound makes fluffy solid dissolve to flask, continues to stir, the ferric chloride hexahydrate aqueous solution of 50 milliliter of 0.1 mol/L is added
（6H2O·FeCl3 1.38g）, continue stir about and stop stirring in 30 minutes, sample is collected with magnet, after water, ethyl alcohol sequentially wash,
12 h of oven drying obtains one-dimensional iron-iron oxide magnetic nano chain；
2）The one-dimensional iron of 50 mg-iron oxide magnetic nano chain is taken, is added in the flask equipped with 70 ml acetonitriles, 25 DEG C, 40W ultrasound items
Under part, 25mg is added（0.000072 mol）Hexachlorocyclotriph,sphazene and 54mg（0.000269 mol）4,4 '-diamino hexichol
2 ml triethylamines are added in ether after ultrasonic half an hour, reaction was completed after continuation ultrasonic half an hour.Magnet collects sample, with water, ethyl alcohol
Each washing three times, 40 DEG C of 12 h of oven drying are to get iron-iron oxide@polyphosphazene magnetic nano chains.Gained iron-poly- the phosphorus of iron oxide@
Nitrile magnetic nano chain thickness is about 20nm, and magnetic saturation intensity is 91 emu g-1。
Embodiment 3
A kind of preparation method with high magnetic responsiveness iron-iron oxide@polyphosphazene magnetic nano chains, specifically includes following step
Suddenly：
1）Prepare one-dimensional iron-iron oxide magnetic nano chain；
By 1.0g potassium borohydrides, 50 milliliters of hexamethylenes, mechanical agitation dissolves in the flask of 250ml, and flask is then positioned over ice
Mechanical agitation about half an hour in aqueous mixtures（Rotating speed is about 700 rev/min）, react and terminate to obtain fluffy solid.It takes out and burns
Simultaneously ultrasound makes fluffy solid dissolve to bottle, continues to stir, the ferric chloride hexahydrate aqueous solution of 50 milliliter of 0.1 mol/L is added
（6H2O·FeCl31.38g）, continue stir about and stop stirring in 30 minutes, sample is collected with magnet, after water, ethyl alcohol sequentially wash,
12 h of oven drying obtains one-dimensional iron-iron oxide magnetic nano chain；
2）The one-dimensional iron of 50 mg-iron oxide magnetic nano chain is taken, is added in the flask equipped with 70 ml acetonitriles, 30 DEG C, 40W ultrasound items
Under part, 50mg is added（0.000143 mol）Hexachlorocyclotriph,sphazene and 108mg（0.000856 mol）Phloroglucin, ultrasound half
2 ml triethylamines are added after hour, reaction was completed after continuation ultrasonic half an hour.Magnet collects sample, and three are respectively washed with water, ethyl alcohol
Time, 40 DEG C of 12 h of oven drying are to get iron-iron oxide@polyphosphazene magnetic nano chains.Gained iron-iron oxide@polyphosphazene magnetism is received
For rice chain thickness in 20-30nm, magnetic saturation intensity is 100 emu g-1。
Embodiment 4
A kind of preparation method with high magnetic responsiveness iron-iron oxide@polyphosphazene magnetic nano chains, specifically includes following step
Suddenly：
1）Prepare one-dimensional iron-iron oxide magnetic nano chain；
By 1.0g potassium borohydrides, 50 milliliters of hexamethylenes, mechanical agitation dissolves in the flask of 250ml, and flask is then positioned over ice
Mechanical agitation about half an hour in aqueous mixtures（Rotating speed is about 700 rev/min）, react and terminate to obtain fluffy solid.It takes out and burns
Simultaneously ultrasound makes fluffy solid dissolve to bottle, continues to stir, the ferric sulfate aqueous solution of 50 milliliter of 0.1 mol/L is added（Fe2(SO4) 3
1.99g）, continue stir about and stop stirring in 30 minutes, sample, after water, ethyl alcohol sequentially wash, oven drying 12 are collected with magnet
H obtains one-dimensional iron-iron oxide magnetic nano chain；
2）Take the one-dimensional iron of 50 mg-iron oxide magnetic nano chain, be added in the flask equipped with 70 ml tetrahydrofurans, 40 DEG C, 40W it is super
Under the conditions of sound, 25mg is added（0.000072 mol）Hexachlorocyclotriph,sphazene and 86mg（0.000143 mol）Branched polyethylene is sub-
Amine（Average molecular weight 600-5000）, 2 ml triethylamines are added after ultrasonic half an hour, continue after ultrasonic half an hour that reaction was completed.Magnetic
Iron collects sample, is respectively washed three times with water, ethyl alcohol, 40 DEG C of 12 h of oven drying are to get iron-iron oxide@polyphosphazene magnetic Nanos
Chain.For gained iron-iron oxide@polyphosphazene magnetic nano chain thickness in 10-15nm, magnetic saturation intensity is 98 emu g-1。
Embodiment 5
A kind of preparation method with high magnetic responsiveness iron-iron oxide@polyphosphazene magnetic nano chains, specifically includes following step
Suddenly：
1）Prepare one-dimensional iron-iron oxide magnetic nano chain；
By 1.0g potassium borohydrides, 50 milliliters of hexamethylenes, mechanical agitation dissolves in the flask of 250ml, and flask is then positioned over ice
Mechanical agitation about half an hour in aqueous mixtures（Rotating speed is about 700 rev/min）, react and terminate to obtain fluffy solid.It takes out and burns
Simultaneously ultrasound makes fluffy solid dissolve to bottle, continues to stir, the iron nitrate aqueous solution of 50 milliliter of 0.1 mol/L is added（Fe (NO3) 3
1.156g）, continue stir about and stop stirring in 30 minutes, sample, after water, ethyl alcohol sequentially wash, oven drying 12 are collected with magnet
H obtains one-dimensional iron-iron oxide magnetic nano chain；
2）The one-dimensional iron of 50 mg-iron oxide magnetic nano chain is taken, is added in the flask equipped with 70 ml acetonitriles, 50 DEG C, 40W ultrasound items
Under part, 25mg is added（0.000072 mol）Hexachlorocyclotriph,sphazene and 86mg（0.000143 mol）Branched polyethylene imine（It is flat
Average molecular weight 600-5000）, 2 ml triethylamines are added after ultrasonic half an hour, continue after ultrasonic half an hour that reaction was completed.Magnet is received
Collect sample, is respectively washed three times with water, ethyl alcohol, 40 DEG C of 12 h of oven drying are to get iron-iron oxide@polyphosphazene magnetic nano chains.Institute
Iron-iron oxide@polyphosphazene magnetic nano chain thickness is obtained in 20-30nm, magnetic saturation intensity is 90 emu g-1。
Embodiment 6
A kind of preparation method with high magnetic responsiveness iron-iron oxide@polyphosphazene magnetic nano chains, specifically includes following step
Suddenly：
1）Prepare one-dimensional iron-iron oxide magnetic nano chain；
By 1.0g potassium borohydrides, 50 milliliters of hexamethylenes, mechanical agitation dissolves in the flask of 250ml, and flask is then positioned over ice
Mechanical agitation about half an hour in aqueous mixtures（Rotating speed is about 700 rev/min）, react and terminate to obtain fluffy solid.It takes out and burns
Simultaneously ultrasound makes fluffy solid dissolve to bottle, continues to stir, the ferric chloride hexahydrate aqueous solution of 50 milliliter of 0.1 mol/L is added
（6H2O·FeCl3 1.38g）, continue stir about and stop stirring in 30 minutes, sample is collected with magnet, after water, ethyl alcohol sequentially wash,
12 h of oven drying obtains one-dimensional iron-iron oxide magnetic nano chain；
2）The one-dimensional iron of 50 mg-iron oxide magnetic nano chain is taken, is added and is equipped in 70 ml acetonitrile flasks, 60 DEG C, 40W ultrasound items
Under part, 25mg is added（0.000072 mol）Hexachlorocyclotriph,sphazene and 47mg（0.0000783 mol）Branched polyethylene imine
（Average molecular weight 600-5000）, 2 ml triethylamines are added after ultrasonic half an hour, continue after ultrasonic half an hour that reaction was completed.Magnet
Sample is collected, is respectively washed three times with water, ethyl alcohol, 40 DEG C of 12 h of oven drying are to get iron-iron oxide@polyphosphazene magnetic nano chains.
For gained iron-iron oxide@polyphosphazene magnetic nano chain thickness in 10-15nm, magnetic saturation intensity is 102 emu g-1。
Claims (6)
1. a kind of preparation method with high magnetic responsiveness iron-iron oxide@polyphosphazene magnetic nano chains, which is characterized in that including
Following steps：
1）Prepare one-dimensional iron-iron oxide magnetic nano chain；
2）Using prepared one-dimensional iron-iron oxide magnetic nano chain as template, chlordene ring is added in the presence of a solvent
Three phosphonitriles and comonomer, and using triethylamine as acid binding agent, 0.5-1h, reaction are reacted in 20-80 DEG C under ultrasound condition
After end iron-iron oxide polyphosphazene magnetic nano chain is obtained through Magneto separate, washing, drying.
2. the preparation method with high magnetic responsiveness iron-iron oxide@polyphosphazene magnetic nano chains according to claim 1,
It is characterized in that, step 2）In, the solvent is acetonitrile, tetrahydrofuran, ethyl alcohol, methanol or acetone.
3. the preparation method with high magnetic responsiveness iron-iron oxide@polyphosphazene magnetic nano chains according to claim 1,
It is characterized in that, step 2）In, the comonomer is 4,4'-diaminodiphenyl sulfone, 4,4 '-diaminodiphenyl ethers, 4,4 '-dihydroxies
Base diphenyl sulphone (DPS), to biphenol, phloroglucin, trihydroxy phenol, 4,4 '-dioxydiphenyl methanes or branched polyethylene imine；Altogether
Polycondensation monomer and the molar ratio range of hexachlorocyclotriph,sphazene are 1-6：1.
4. the preparation method with high magnetic responsiveness iron-iron oxide@polyphosphazene magnetic nano chains according to claim 1,
It is characterized in that, step 2）In, the mass ratio of one-dimensional iron-iron oxide magnetic nano chain used and hexachlorocyclotriph,sphazene is ranging from
1-2：1.
5. the preparation method with high magnetic responsiveness iron-iron oxide@polyphosphazene magnetic nano chains according to claim 1,
It is characterized in that, step 1）Specially：Boron hydride is dissolved in hexamethylene, then the mechanic whirl-nett reaction in mixture of ice and water
0.1-0.5 h, reaction terminate to obtain fluffy solid, and ultrasound makes fluffy solid dissolve, and it is molten to continue addition molysite under stirring condition
Liquid obtains one-dimensional iron-iron oxide magnetic nano chain.
6. the preparation method with high magnetic responsiveness iron-iron oxide@polyphosphazene magnetic nano chains according to claim 5,
It is characterized in that, step 1）In, the boron hydride is potassium borohydride or sodium borohydride；The iron salt solutions are ferric chloride hexahydrate
Aqueous solution, ferric sulfate aqueous solution or iron nitrate aqueous solution；The mass ratio of boron hydride and molysite is 0.5-0.9：1.
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