CN110803703A - Magnetic carbon-coated iron carbide nano material and preparation method and application thereof - Google Patents
Magnetic carbon-coated iron carbide nano material and preparation method and application thereof Download PDFInfo
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- CN110803703A CN110803703A CN201911108994.8A CN201911108994A CN110803703A CN 110803703 A CN110803703 A CN 110803703A CN 201911108994 A CN201911108994 A CN 201911108994A CN 110803703 A CN110803703 A CN 110803703A
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- iron carbide
- magnetic carbon
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- coated iron
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- 229910001567 cementite Inorganic materials 0.000 title claims abstract description 140
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 135
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 133
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 113
- 238000002360 preparation method Methods 0.000 title claims abstract description 38
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 138
- 229910052742 iron Inorganic materials 0.000 claims abstract description 56
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000002243 precursor Substances 0.000 claims abstract description 33
- 239000003513 alkali Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 18
- 229910001868 water Inorganic materials 0.000 claims abstract description 16
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- 239000012298 atmosphere Substances 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 8
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 84
- 238000010438 heat treatment Methods 0.000 claims description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 17
- 239000013067 intermediate product Substances 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 14
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- 239000002105 nanoparticle Substances 0.000 claims description 12
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 8
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 4
- 239000000969 carrier Substances 0.000 claims description 4
- 238000006555 catalytic reaction Methods 0.000 claims description 4
- 238000004146 energy storage Methods 0.000 claims description 4
- 238000005984 hydrogenation reaction Methods 0.000 claims description 4
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 3
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000002253 acid Substances 0.000 abstract description 24
- 150000002505 iron Chemical class 0.000 abstract description 10
- 150000002500 ions Chemical class 0.000 abstract description 6
- 238000000197 pyrolysis Methods 0.000 abstract description 5
- 239000003575 carbonaceous material Substances 0.000 abstract description 3
- 238000002441 X-ray diffraction Methods 0.000 description 23
- 238000005406 washing Methods 0.000 description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 16
- 230000005540 biological transmission Effects 0.000 description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 description 7
- 230000005389 magnetism Effects 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 238000001000 micrograph Methods 0.000 description 6
- 239000012299 nitrogen atmosphere Substances 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 239000000706 filtrate Substances 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 230000005415 magnetization Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 238000005554 pickling Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- -1 citrate ions Chemical class 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 229960002413 ferric citrate Drugs 0.000 description 1
- 230000005308 ferrimagnetism Effects 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 229910052595 hematite Inorganic materials 0.000 description 1
- 239000011019 hematite Substances 0.000 description 1
- 159000000014 iron salts Chemical class 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 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 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
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- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/0036—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties showing low dimensional magnetism, i.e. spin rearrangements due to a restriction of dimensions, e.g. showing giant magnetoresistivity
- H01F1/0045—Zero dimensional, e.g. nanoparticles, soft nanoparticles for medical/biological use
- H01F1/0054—Coated nanoparticles, e.g. nanoparticles coated with organic surfactant
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Abstract
The invention belongs to the technical field of carbon materials, and particularly relates to a magnetic carbon-coated iron carbide nano material as well as a preparation method and application thereof. In the preparation method, the iron source is selected from one or more of magnetite, ferrous oxide, ferroferric oxide and reduced iron powder, the alkali source can be used as a catalyst to promote the iron source to be dissolved in water, the polycarboxyl complex reacts with the alkali source to generate polycarboxyl complex ions, the polycarboxyl complex ions then carry out complex reaction with the iron source, the iron element in the iron source is extracted and dissolved in the water to obtain a complex precursor, the complex precursor is roasted in an inert atmosphere for pyrolysis self-reduction to obtain the magnetic carbon-coated iron carbide nano material, and the iron salt is not needed to be used as the iron source, so that the problems that the iron salt is needed to be used for preparing the existing magnetic carbon-coated iron carbide nano material, a large amount of acid and alkali is needed to be used for preparing the iron salt, the process flow is long, and the cost is.
Description
Technical Field
The invention belongs to the technical field of carbon materials, and particularly relates to a magnetic carbon-coated iron carbide nano material as well as a preparation method and application thereof.
Background
The magnetic carbon-coated iron carbide nano material is used as a carbon material, and has wide application prospects in the fields of microwave absorption, hydrogenation catalysis, catalyst carriers, energy storage and the like. The nanoscale iron carbide particles are uniformly dispersed in the carbon layer, so that the magnetic carbon-coated iron carbide nano material has high performance and stability, and on one hand, the function of the nano iron carbide particles is fully exerted; on the other hand, the carbon layer coated outside the iron carbide not only can play a role in isolating the nano particles and preventing the nano particles from agglomerating at high temperature so as to improve the thermal stability of the nano particles, but also can avoid the corrosion of acid-base environment to the iron carbide by adjusting the coating degree and thickness of the carbon layer.
However, at present, high-purity ferric salts such as ferric nitrate, ferric chloride, ferric sulfate and ferric citrate are mostly adopted to prepare the magnetic carbon-coated iron carbide nano material, a large amount of acid and alkali are needed in the industrial process of the ferric salt, the process flow is long, the quality requirement of the ferric salt is high, a large amount of waste gas is generated during the preparation of the ferric salt, the environmental pressure is high, and the cost is high. Therefore, a method for preparing magnetic carbon-coated iron carbide nano-materials without using iron salts is urgently sought.
Disclosure of Invention
In view of the above, the invention provides a magnetic carbon-coated iron carbide nano material, and a preparation method and an application thereof, and aims to solve the problems that iron salt is required to be used for preparing the existing magnetic carbon-coated iron carbide nano material, a large amount of acid and alkali is required to be used for preparing the iron salt, the process flow is long, and the cost is high.
The specific technical scheme of the invention is as follows:
a preparation method of a magnetic carbon-coated iron carbide nano material comprises the following steps:
a) carrying out heating reaction on an iron source, a polycarboxyl complex and an alkali source in water to obtain an intermediate product;
b) drying the intermediate product to obtain a complex precursor, and roasting the complex precursor at 550-800 ℃ in an inert atmosphere to obtain a magnetic carbon-coated iron carbide nano material;
wherein the iron source is selected from one or more of magnetite, ferrous oxide, ferroferric oxide and reduced iron powder;
the molar ratio of the iron element in the iron source to the carboxyl in the polycarboxyl complex is 1: 3-1: 10.
Preferably, the polycarboxy complex of step a) is selected from one or more of citric acid, ethylenediaminetetraacetic acid, tartaric acid and nitrilotriacetic acid.
Preferably, the alkali source is selected from one or more of potassium hydroxide, sodium hydroxide, aqueous ammonia, ethylenediamine, ethanolamine, and calcium hydroxide.
Preferably, the pH value of a reaction system formed by the iron source, the polycarboxyl complex, the alkali source and water in the step a) is 2-10.
Preferably, the temperature of the heating reaction in the step a) is 40-100 ℃;
the heating reaction time is 1-6 h.
Preferably, the roasting time in the step b) is 2-10 h;
the heating rate before roasting is 1-30 ℃/min.
Preferably, the drying temperature in the step b) is 60-170 ℃;
the drying time is 12-120 h.
The invention also provides a magnetic carbon-coated iron carbide nano material prepared by the preparation method of the technical scheme.
Preferably, the particle size of the magnetic carbon-coated iron carbide nano material is 4 nm-29 nm;
the thickness of the carbon layer in the magnetic carbon-coated iron carbide nano material is 0.6 nm-1.2 nm.
The invention also provides the magnetic carbon-coated iron carbide nano material prepared by the preparation method in the technical scheme and/or the application of the magnetic carbon-coated iron carbide nano material in the technical scheme in the fields of microwave absorption, hydrogenation catalysis, catalyst carriers or energy storage.
In summary, the invention provides a preparation method of a magnetic carbon-coated iron carbide nano material, which comprises the following steps: a) carrying out heating reaction on an iron source, a polycarboxyl complex and an alkali source in water to obtain an intermediate product; b) drying the intermediate product to obtain a complex precursor, and roasting the complex precursor at 550-800 ℃ in an inert atmosphere to obtain a magnetic carbon-coated iron carbide nano material; wherein the iron source is selected from one or more of magnetite, ferrous oxide, ferroferric oxide and reduced iron powder; the molar ratio of the iron element in the iron source to the carboxyl in the polycarboxyl complex is 1: 3-1: 10. According to the invention, the iron source is selected from one or more of magnetite, ferrous oxide, ferroferric oxide and reduced iron powder, the alkali source can be used as a catalyst to promote the iron source to be dissolved in water, the polycarboxyl complex reacts with the alkali source to generate polycarboxyl complex ions, the polycarboxyl complex ions then undergo a complex reaction with the iron source, iron elements in the iron source are extracted and dissolved in water to obtain a complex precursor, the complex precursor is roasted in an inert atmosphere to carry out pyrolysis self-reduction, and the magnetic carbon-coated iron carbide nano material is obtained without using iron salt as the iron source, so that the problems that iron salt is required to be used for preparing the existing magnetic carbon-coated iron carbide nano material, a large amount of acid and alkali is required to be used for preparing the iron salt, the process flow is longer, and the cost is higher are.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 is an XRD standard spectrum of iron carbide and graphitic carbon;
FIG. 2 is an XRD spectrum of the magnetic carbon-coated iron carbide nanomaterial prepared in example 1;
FIG. 3 is an XRD (X-ray diffraction) spectrum of the magnetic carbon-coated iron carbide nano-material prepared in example 1 after acid washing;
FIG. 4 is a TEM image of the magnetic carbon-coated iron carbide nanomaterial prepared in example 1 at a baking temperature of 500 ℃;
FIG. 5 is a TEM image of the magnetic carbon-coated iron carbide nanomaterial prepared in example 1 at a baking temperature of 600 deg.C;
FIG. 6 is a transmission electron microscope image of the magnetic carbon-coated iron carbide nanomaterial prepared in example 1 after acid washing at a baking temperature of 500 ℃;
FIG. 7 is a transmission electron microscope image of the magnetic carbon-coated iron carbide nanomaterial prepared in example 1 after acid washing at a baking temperature of 600 ℃;
FIG. 8 is a scanning electron microscope photograph of a magnetic carbon-coated iron carbide nanomaterial prepared at a baking temperature of 600 ℃ in example 1;
FIG. 9 is an XRD spectrum of the magnetic carbon-coated iron carbide nanomaterial prepared in example 2 after acid washing;
FIG. 10 is an XRD spectrum of the magnetic carbon-coated iron carbide nanomaterial prepared in example 3 after acid washing;
FIG. 11 is an XRD spectrum of the magnetic carbon-coated iron carbide nanomaterial prepared in example 4 after acid washing;
FIG. 12 is an XRD pattern of the magnetic carbon-coated iron carbide nanomaterial prepared in example 5 after acid washing;
FIG. 13 is an XRD pattern of the magnetic carbon-coated iron carbide nanomaterial prepared in example 6 after acid washing;
FIG. 14 is a hysteresis regression curve of the magnetic carbon-coated iron carbide nanomaterial prepared in example 2 at a molar ratio of iron element to citric acid of 1:3 before pickling;
FIG. 15 is a hysteresis regression curve of the magnetic carbon-coated iron carbide nanomaterial prepared in example 2 in which the molar ratio of iron element to citric acid in magnetite is 1:3 after acid washing.
Detailed Description
The invention provides a magnetic carbon-coated iron carbide nano material as well as a preparation method and application thereof, which are used for solving the problems that the preparation of the existing magnetic carbon-coated iron carbide nano material needs to use ferric salt, and the preparation of the ferric salt needs to adopt a large amount of acid and alkali, so that the process flow is longer and the cost is higher.
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A preparation method of a magnetic carbon-coated iron carbide nano material comprises the following steps:
a) carrying out heating reaction on an iron source, a polycarboxyl complex and an alkali source in water to obtain an intermediate product;
b) drying the intermediate product to obtain a complex precursor, and roasting the complex precursor at 550-800 ℃ in an inert atmosphere to obtain a magnetic carbon-coated iron carbide nano material;
wherein the iron source is selected from one or more of magnetite, ferrous oxide, ferroferric oxide and reduced iron powder, and is more preferably magnetite and/or ferroferric oxide;
the molar ratio of the iron element in the iron source to the carboxyl in the polycarboxyl complex is 1: 3-1: 10, and more preferably 1: 4-1: 5.
In the embodiment of the invention, an alkali source can be used as a catalyst to promote the dissolution of an iron source in water, firstly, a polycarboxyl complex reacts with the alkali source to generate polycarboxyl complex ions, the polycarboxyl complex ions then react with the iron source in a complex manner, iron elements in the iron source are extracted and dissolved in water to obtain a complex precursor, and the complex precursor is roasted in an inert atmosphere to carry out pyrolysis self-reduction, so that the magnetic carbon-coated iron carbide nano material is obtained. The magnetic carbon-coated iron carbide nano material prepared by the preparation method has saturation magnetization of 38.09emu/g and superparamagnetism; the outer layer of the iron carbide nano-particles is wrapped by a carbon layer, so that the iron carbide nano-particles have excellent corrosion resistance and stable magnetism; in addition, the preparation method has simple process and can be used for large-scale preparation.
Magnetite is a kind of ferrimagnetism mineral, it is rich in ferriferrous oxide, produce in metamorphic ore deposit and endogenous deposit, the reserve is huge in our country, distribute extensively, become hematite or limonite after oxidizing, it is the main raw materials of ironmaking. Currently, magnetite is mainly used for iron making, but iron making needs to be carried out by reducing magnetite with carbon monoxide at high temperature for refining, the current iron making process consumes extremely large energy, a large amount of waste gas and waste residues are generated in the iron making process, certain environmental protection pressure exists, and the risk problems of poisoning, explosion and the like exist in the reduction with carbon monoxide.
In the embodiment of the invention, the iron source can be magnetite, iron elements can be extracted from the magnetite under mild conditions, filtering and drying are preferably carried out to obtain a complex precursor, and then the complex precursor is roasted to obtain the magnetic carbon-coated iron carbide nano material. The method adopts cheap natural magnetite resources as an iron source, provides a new way for the application of magnetite, and directly prepares the magnetic carbon-coated iron carbide nano material by utilizing the magnetite, thereby having very important industrial application value. In addition, the preparation method can avoid intermediate smelting and preparation and purification of iron salt when the iron source is derived from natural minerals.
In the embodiment of the invention, the method for extracting the iron element from the magnetite is simple and mild, the process route for preparing the magnetic carbon-coated iron carbide nano material is simple, the large-scale production is easy to implement, the stability and feasibility of the operation are high, the industrial iron making of natural magnetite and the deep processing process of iron salt industry are avoided, and the method has the characteristics of energy conservation, environmental protection and the like. The iron carbide nano particles in the magnetic carbon-coated iron carbide nano material prepared by the preparation method can reach below 10nm and are uniformly distributed in the carbon layer, the particle size of the iron carbide nano particles and the thickness of the coated carbon layer can be adjusted according to needs, and the magnetic hysteresis loop is determined to show that the magnetic carbon-coated iron carbide nano material prepared by the preparation method has good magnetism.
In an embodiment of the invention, the polycarboxy complex of step a) is selected from one or more of citric acid, ethylenediaminetetraacetic acid, tartaric acid and nitrilotriacetic acid;
the alkali source is one or more selected from potassium hydroxide, sodium hydroxide, ammonia water, ethylenediamine, ethanolamine and calcium hydroxide, preferably a mixture of sodium hydroxide and ammonia water.
When the polycarboxyl complex is citric acid, the citric acid reacts with an alkali source to generate citrate ions, the citrate ions then undergo a complexing reaction with an iron source, and the iron element is extracted from the iron source based on the following reactions:
H3C6H5O7+OH-→H2C6H5O7 -+H2O
H2C6H5O7 -+Fe→FeC6H5O7 -+H2
H2C6H5O7 -+FeO→FeC6H5O7 -+H2O
3H2C6H5O7 -+Fe3O4→FeC6H5O7 -+2FeC6H5O7+2H2O+2OH-
in the embodiment of the invention, the step a) is specifically as follows: adding water into an iron source and citric acid, stirring, adding an alkali source, and carrying out heating reaction to obtain an intermediate product.
The pH value of a reaction system formed by the iron source, the polycarboxyl complex, the alkali source and water in the step a) is 2-10, and preferably 3-6.
In the embodiment of the invention, the temperature of the heating reaction in the step a) is 40-100 ℃, and more preferably 85 ℃;
the heating reaction time is 1-6 h, preferably 3-5 h, so that the iron source is completely dissolved in the reaction system.
In the embodiment of the invention, the roasting time in the step b) is 2-10 h;
the roasting temperature is preferably 550-700 ℃;
the heating rate before roasting is 1-30 deg.C/min, preferably 1-10 deg.C/min.
In the embodiment of the invention, the drying temperature in the step b) is 60-170 ℃, preferably 100-120 ℃;
the drying time is 12-120 h, preferably 24-120 h.
The invention also provides a magnetic carbon-coated iron carbide nano material prepared by the preparation method of the technical scheme.
The magnetic carbon-coated iron carbide nano material prepared by the preparation method has saturation magnetization of 38.09emu/g and superparamagnetism; in addition, the outer layer of the iron carbide nano particles in the magnetic carbon-coated iron carbide nano material is coated by a carbon layer, so that the magnetic carbon-coated iron carbide nano material has excellent corrosion resistance and stable magnetism.
In the embodiment of the invention, the magnetic carbon-coated iron carbide nano material is of a core-shell structure, and the particle size of the magnetic carbon-coated iron carbide nano material is 4-29 nm;
the thickness of the carbon layer in the magnetic carbon-coated iron carbide nano material is 0.6 nm-1.2 nm, and the carbon layer is a graphite carbon layer.
The invention also provides the magnetic carbon-coated iron carbide nano material prepared by the preparation method in the technical scheme and/or the application of the magnetic carbon-coated iron carbide nano material in the technical scheme in the fields of microwave absorption, hydrogenation catalysis, catalyst carriers or energy storage.
In the embodiment of the invention, when the magnetic carbon-coated iron carbide nano material is applied to the catalyst carrier, the catalyst can be recovered through magnetism due to the magnetism of the magnetic carbon-coated iron carbide nano material, so that the recovery rate of the catalyst is increased.
For a further understanding of the invention, reference will now be made in detail to the following examples.
In the specific example, magnetite was purchased from the analytical test center of Shandong province, and the iron content was 62.55 wt%.
Example 1
In this embodiment, the preparation of the magnetic carbon-coated iron carbide nanomaterial by using different roasting temperatures specifically comprises:
1.836g of magnetite and 15g of citric acid (C) are weighed out6H8O7) Putting the mixture into 50ml of deionized water, adding concentrated ammonia water to adjust the pH value to 2, heating the mixture at 100 ℃ for reaction until the iron source is completely dissolved (67-83% of the mass of the magnetite), then filtering the mixture, and collecting filtrate to obtain an intermediate product.
Drying the intermediate product at 60 ℃ for 120 hours to obtain a brownish black fluffy complex precursor, and roasting the complex precursor in a nitrogen atmosphere at 500 ℃, 550 ℃, 600 ℃, 700 ℃ and 800 ℃ for 12 hours respectively, wherein the heating rate before roasting is 1 ℃/min, so as to obtain the magnetic carbon-coated iron carbide nano material.
XRD analysis was performed on the magnetic carbon-coated iron carbide nanomaterial prepared in this example, and the result is shown in fig. 2. The magnetic carbon-coated iron carbide nanomaterial is subjected to acid washing by using a 10 wt% dilute sulfuric acid solution, and an XRD (X-ray diffraction) spectrogram of the acid-washed magnetic carbon-coated iron carbide nanomaterial is shown in figure 3. Fig. 2 and fig. 3 show that the magnetic carbon-coated iron carbide nanomaterial can be prepared at a baking temperature of 550-800 ℃, when the baking temperature is above 550 ℃, an XRD spectrogram of the magnetic carbon-coated iron carbide nanomaterial obviously shows a diffraction peak of metal iron carbide, and the diffraction peak still exists after acid washing, which indicates that the carbon-coated iron carbide nanomaterial prepared at the baking temperature of 550-800 ℃ has a good carbon-coating degree.
As a result of transmission electron microscope analysis of the magnetic carbon-coated iron carbide nanomaterial obtained at the firing temperatures of 500 ℃ and 600 ℃, see fig. 4 and 5, fig. 4 is a transmission electron microscope image of the magnetic carbon-coated iron carbide nanomaterial obtained at the firing temperature of 500 ℃ in example 1, and fig. 5 is a transmission electron microscope image of the magnetic carbon-coated iron carbide nanomaterial obtained at the firing temperature of 600 ℃ in example 1. The magnetic carbon-coated iron carbide nanomaterial prepared at the baking temperatures of 500 ℃ and 600 ℃ is pickled with a 10 wt% dilute sulfuric acid solution and then analyzed by a transmission electron microscope, and the results are shown in fig. 6 and 7, fig. 6 is a transmission electron microscope image of the magnetic carbon-coated iron carbide nanomaterial prepared in example 1 at the baking temperature of 500 ℃ after pickling, and fig. 7 is a transmission electron microscope image of the magnetic carbon-coated iron carbide nanomaterial prepared in example 1 at the baking temperature of 600 ℃ after pickling. Fig. 5 and 7 show that the carbon-coated iron carbide nanomaterial with a typical core-shell structure is formed by pyrolysis self-reduction through roasting at 600 ℃ in an inert atmosphere, reducing gas is decomposed by citric acid at high temperature, an iron carbide precursor can be self-reduced, and the particle size of the prepared magnetic carbon-coated iron carbide nanomaterial is 4-29 nm, which indicates that the magnetic carbon-coated iron carbide nanomaterial with a smaller particle size can be prepared by the preparation method provided by the invention. And when the product of the iron carbide is roasted at 500 ℃, the iron carbide is not completely wrapped by carbon, and the iron carbide is dissolved by dilute sulfuric acid after acid washing, so that the honeycomb-shaped carbon shell structure aggregate shown in figure 5 is left.
The SEM analysis of the magnetic carbon-coated iron carbide nanomaterial prepared at a baking temperature of 600 ℃ is performed, and the result is shown in fig. 8, where fig. 8 shows that the complex precursor is gradually converted into a spherical particle aggregate through high-temperature pyrolysis self-reduction in an inert atmosphere, and has a fluffy structure and a large number of voids.
Example 2
In this embodiment, the preparation of the magnetic carbon-coated iron carbide nanomaterial is performed, and the molar ratio of the iron element to the citric acid in the magnetite is different, which specifically includes:
respectively mixing the iron element and the citric acid in the magnetite according to a molar ratio of 1: 2. 1: 3. 1: 4. 1: 5. 1: 8 weighing 0.918g and 5.00g of magnetite, 0.918g and 7.50g of citric acid, 0.918g and 10.00g of magnetite, 0.918g and 12.50g of citric acid and 0.918g and 20g of citric acid from the magnetite, respectively placing the materials into 50ml of deionized water, adding sodium hydroxide to adjust the pH value to 5, heating at 40 ℃ for reaction until the iron source is completely dissolved (67-83% of the mass of the magnetite), filtering, and collecting filtrate to obtain an intermediate product.
Drying the intermediate product at 170 ℃ for 12 hours to obtain a brownish black fluffy complex precursor, roasting the complex precursor at 700 ℃ for 2 hours in a nitrogen atmosphere at a heating rate of 10 ℃/min before roasting to obtain the magnetic carbon-coated iron carbide nano material, carrying out acid washing by using a 10 wt% dilute sulfuric acid solution, and obtaining the XRD spectrogram of the magnetic carbon-coated iron carbide nano material after acid washing as shown in figure 9. Fig. 9 shows that the molar ratio of iron element to citric acid in magnetite is 1: 2 to 1: 8, decomposing the reducing gas by citric acid at high temperature, and self-reducing the iron carbide precursor, wherein a diffraction peak of the iron carbide is obviously shown in fig. 9, and when the molar ratio of the iron element in the magnetite to the citric acid is 1: 2, diffraction peaks of the iron carbide are very dispersed, the average particle size of the magnetic carbon-coated iron carbide nano material is calculated to be about 7.8-11.9 nm according to an XRD spectrogram through a Scherrer formula (Scherrer formula), and when the molar ratio of iron elements to citric acid in magnetite is 1: when the carbon content is more than 5, more carbon residues are easily caused by excessive citric acid, and the amorphous carbon coating peak begins to gradually rise.
Example 3
In this embodiment, the preparation of the magnetic carbon-coated iron carbide nanomaterial is performed by using different iron sources, which specifically includes:
1.836g of ferroferric oxide (Fe) is weighed out respectively3O4) 1.332g of reduced iron powder (Fe) or 3g of magnetite and 15g of citric acid are placed in 50ml of deionized water, concentrated ammonia water is added to adjust the pH value to 4, heating reaction is carried out for 24h at 60 ℃ until the iron source is completely dissolved, when the iron source is the magnetite, filtration is needed to collect filtrate, drying is carried out for 72 h at 100 ℃ to obtain a complex precursor, the complex precursor is roasted for 2h at 700 ℃ in a nitrogen atmosphere, the heating rate before roasting is 5 ℃/min to obtain the magnetic carbon-coated iron carbide nano material, acid washing is carried out by adopting 10 wt% of dilute sulfuric acid solution, and the XRD spectrogram of the acid-washed magnetic carbon-coated iron carbide nano material is shown in figure 9.
Fig. 10 shows that when the iron source is magnetite, reduced iron powder, or ferroferric oxide, citric acid decomposes the reducing gas at high temperature, and can self-reduce the iron carbide precursor, fig. 10 shows the diffraction peak of iron carbide, and the diffraction peak is very dispersed, and the average particle size of the magnetic carbon-coated iron carbide nanomaterial calculated by using Scherrer formula (Scherrer formula) under different iron sources is about 8nm, which indicates that the particle size of the magnetic carbon-coated iron carbide nanomaterial is less affected by the iron source.
Example 4
In this embodiment, the preparation of the magnetic carbon-coated iron carbide nanomaterial is performed by using different polycarboxyl complexes, which specifically includes:
1.836g of magnetite and 20.856g of ethylenediaminetetraacetic acid (C) were weighed out10H16N2O8) Or 15g of citric acid is put into 50ml of deionized water, potassium hydroxide is added to adjust the pH value to 10, heating reaction is carried out at 40 ℃ until the iron source is completely dissolved, then filtration is carried out, and the filtrate is collected to obtain an intermediate product.
Drying the intermediate product at 120 ℃ for 48 hours to obtain a complex precursor, roasting the complex precursor at 700 ℃ for 8 hours in a nitrogen atmosphere at a heating rate of 5 ℃/min before roasting to obtain the magnetic carbon-coated iron carbide nanomaterial, carrying out acid washing by using a 10 wt% dilute sulfuric acid solution, and referring to an XRD (X-ray diffraction) spectrogram of the acid-washed magnetic carbon-coated iron carbide nanomaterial to be shown in figure 11. Fig. 11 shows that the polycarboxyl complex is citric acid and ethylenediaminetetraacetic acid, both of which can decompose reducing gas at high temperature, and self-reduce the iron carbide precursor, fig. 11 shows the diffraction peak of the iron carbide obviously, and the diffraction peak is very diffuse, and the average particle size of the magnetic carbon-coated iron carbide nano material calculated by using Scherrerformula is 7.8 nm.
Example 5
In this embodiment, the preparation of the magnetic carbon-coated iron carbide nanomaterial is performed by using different alkali sources, which specifically includes:
1.836g of ferroferric oxide (Fe) is weighed3O4) And 15g of citric acid, placing the mixture into 50ml of deionized water, adding sodium hydroxide or ammonia water to adjust the pH value to 5, heating the mixture at 90 ℃ to react until the iron source is completely dissolved, drying the mixture at 80 ℃ for 100 hours to obtain a complex precursor (xerogel), roasting the complex precursor at 700 ℃ for 0.5 hour in a nitrogen atmosphere at the heating rate of 30 ℃/min before roasting to obtain a magnetic carbon-coated iron carbide nano material, carrying out acid washing by using a 10 wt% dilute sulfuric acid solution, and obtaining an XRD spectrogram of the acid-washed magnetic carbon-coated iron carbide nano material, referring to fig. 12. The results show that the corresponding XRD pattern clearly shows diffraction peaks of iron carbide and is very diffuse using sodium hydroxide as an alkali source, and the magnetism calculated by ScherrerformulaThe average particle size of the carbon-coated iron carbide nano material is about 13nm, while the average particle size of the magnetic carbon-coated iron carbide nano material obtained by using ammonia water as an alkali source is 18nm, which shows that different alkali sources have great influence on the iron carbide nano particles prepared by the preparation method.
Example 6
In this embodiment, the preparation of the magnetic carbon-coated iron carbide nanomaterial is performed, and a carbon source is added or not added except for citric acid, which specifically includes:
1.836g of magnetite and 15g of citric acid are weighed, added or not added with 15g D-glucose (C6H12O6), placed in 50ml of deionized water, added with ethanolamine to adjust the pH value to 3, heated at 80 ℃ for reaction until the iron source is completely dissolved, filtered, and the filtrate is collected to obtain an intermediate product.
Drying the intermediate product at 120 ℃ for 48 hours to obtain a complex precursor, roasting the complex precursor at 700 ℃ for 1 hour in a nitrogen atmosphere at a heating rate of 20 ℃/min before roasting to obtain the magnetic carbon-coated iron carbide nanomaterial, carrying out acid washing by using a 10 wt% dilute sulfuric acid solution, and referring to an XRD (X-ray diffraction) spectrogram of the acid-washed magnetic carbon-coated iron carbide nanomaterial to be shown in figure 13. The result shows that the added glucose is used as a carbon source, the corresponding XRD spectrogram obviously shows the diffraction peak of the iron carbide and is very dispersive, the average grain diameter of the magnetic carbon-coated iron carbide nano material calculated by using the Scherrer formula is about 9.5nm, and the preparation of the iron carbide nano particles can be carried out by using the added carbon source, so that the coating degree of the iron carbide nano particle carbon layer is changed.
Example 7
In the embodiment, the magnetic carbon-coated iron carbide nano material prepared in example 2 in which the molar ratio of the iron element to the citric acid in the magnetite is 1:3 is subjected to magnetic testing, a testing instrument is a vibration sample magnetometer (Quantum design SQUID-VSM), and the magnetic field intensity range provided by the testing instrument is-20 kOe<H<20 kOe. The hysteresis regression curves of the magnetic carbon-coated iron carbide nanomaterial before and after acid washing were tested at room temperature, and the results, as shown in fig. 14 and 15, indicate that the saturation magnetization of the magnetic carbon-coated iron carbide nanomaterial reaches 38.09emu/g, and the magnetic carbon-coated iron carbide nanomaterial has the characteristics ofSuperparamagnetism; after washing, the magnetic carbon-coated iron carbide nano material still keeps certain magnetism (10 wt% H50 times of the weight of the magnetic carbon-coated iron carbide nano material)2SO45 washes) with a saturation magnetization of 6.74 emu/g.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of a magnetic carbon-coated iron carbide nano material is characterized by comprising the following steps:
a) carrying out heating reaction on an iron source, a polycarboxyl complex and an alkali source in water to obtain an intermediate product;
b) drying the intermediate product to obtain a complex precursor, and roasting the complex precursor at 550-800 ℃ in an inert atmosphere to obtain a magnetic carbon-coated iron carbide nano material;
wherein the iron source is selected from one or more of magnetite, ferrous oxide, ferroferric oxide and reduced iron powder;
the molar ratio of the iron element in the iron source to the carboxyl in the polycarboxyl complex is 1: 3-1: 10.
2. The method of claim 1, wherein the polycarboxy complex of step a) is selected from one or more of citric acid, ethylenediaminetetraacetic acid, tartaric acid, and nitrilotriacetic acid.
3. The method according to claim 1, wherein the alkali source in step a) is one or more selected from potassium hydroxide, sodium hydroxide, aqueous ammonia, ethylenediamine, ethanolamine, and calcium hydroxide.
4. The method according to claim 1, wherein the reaction system formed by the iron source, the polycarboxy complex, the alkali source and water in step a) has a pH of 2 to 10.
5. The preparation method according to claim 1, wherein the temperature of the heating reaction in the step a) is 40 ℃ to 100 ℃;
the heating reaction time is 1-6 h.
6. The preparation method of claim 1, wherein the roasting time in the step b) is 2-10 h;
the heating rate before roasting is 1-30 ℃/min.
7. The method for preparing the nano-particles according to claim 1, wherein the drying temperature in the step b) is 60-170 ℃;
the drying time is 12-120 h.
8. A magnetic carbon-coated iron carbide nanomaterial characterized by being produced by the production method according to any one of claims 1 to 7.
9. The magnetic carbon-coated iron carbide nanomaterial according to claim 8, wherein the magnetic carbon-coated iron carbide nanomaterial has a particle size of 4nm to 29 nm;
the thickness of the carbon layer in the magnetic carbon-coated iron carbide nano material is 0.6 nm-1.2 nm.
10. The magnetic carbon-coated iron carbide nano material prepared by the preparation method of any one of claims 1 to 7 and/or the magnetic carbon-coated iron carbide nano material of any one of claims 8 to 9 is applied to the fields of microwave absorption, hydrogenation catalysis, catalyst carriers or energy storage.
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