CN108862399B - A kind of preparation method of monodisperse micron hexagonal iron oxide sheet - Google Patents
A kind of preparation method of monodisperse micron hexagonal iron oxide sheet Download PDFInfo
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- CN108862399B CN108862399B CN201811137011.9A CN201811137011A CN108862399B CN 108862399 B CN108862399 B CN 108862399B CN 201811137011 A CN201811137011 A CN 201811137011A CN 108862399 B CN108862399 B CN 108862399B
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 12
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 12
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 12
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims abstract description 11
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims abstract description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 66
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 39
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 13
- 229940032296 ferric chloride Drugs 0.000 claims description 13
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000003760 magnetic stirring Methods 0.000 claims description 6
- 239000007795 chemical reaction product Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 2
- 239000012456 homogeneous solution Substances 0.000 claims 2
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 6
- 238000004729 solvothermal method Methods 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 229910052742 iron Inorganic materials 0.000 abstract description 3
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 abstract description 3
- 239000011259 mixed solution Substances 0.000 abstract description 3
- 239000004094 surface-active agent Substances 0.000 abstract description 3
- 229940067573 brown iron oxide Drugs 0.000 abstract 1
- 150000004687 hexahydrates Chemical class 0.000 abstract 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 15
- -1 enamel Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 230000005518 electrochemistry Effects 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 150000002505 iron Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910000901 LiFePO4/C Inorganic materials 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 229960004887 ferric hydroxide Drugs 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 1
- 238000001725 laser pyrolysis Methods 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 229910001004 magnetic alloy Inorganic materials 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000002595 magnetic resonance imaging Methods 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000001054 red pigment Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Iron (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Paints Or Removers (AREA)
- Catalysts (AREA)
Abstract
本发明公开了一种单分散的微米级六边形氧化铁片的制备方法，包括以下步骤：步骤一，配置反应溶液；步骤二，溶剂热法制得红紫色的初步产物；步骤三，马弗炉中加热处理得到红褐色氧化铁。创新性地采用了甲醇‑水混合溶液体系，使用聚乙烯吡咯烷酮作为表面活性剂对产物的形貌和分散性进行辅助控制，采用六水氯化铁作为铁源，进行溶剂热反应制备微米级六边形氧化铁片。制备的微米级正六边形氧化铁片单一性好，尺寸均匀，分散性好，表面光滑，制备步骤简单，可以大规模工业化生产，在电极材料、催化剂、功能涂料、气敏等领域都有很好的应用前景。
The invention discloses a preparation method of monodisperse micron-sized hexagonal iron oxide flakes, comprising the following steps: step 1, preparing a reaction solution; step 2, preparing a red-purple preliminary product by solvothermal method; step 3, muffle Heat treatment in a furnace to obtain reddish-brown iron oxide. The methanol-water mixed solution system is innovatively adopted, and polyvinylpyrrolidone is used as a surfactant to assist in controlling the morphology and dispersibility of the product, and ferric chloride hexahydrate is used as the iron source to conduct solvothermal reaction to prepare micron-sized hexahydrate. Edge-shaped iron oxide flakes. The prepared micron-sized regular hexagonal iron oxide flakes have good uniformity, uniform size, good dispersibility, smooth surface, simple preparation steps, and can be industrialized on a large scale. good application prospects.
Description
Technical Field
The invention relates to the field of inorganic material synthesis, in particular to a preparation method of monodisperse micron-sized hexagonal iron oxide sheets.
Background
Iron oxide is an important magnetic material, catalyst, polishing material, battery material, red pigment, colorant, functional coating and gas sensitive material. The method is widely applied to the fields of medical treatment, energy, telecommunication, instrument industry, paint, rubber, plastics, cosmetics, enamel, leather, magnetic alloy, catalytic industry, gas sensors and the like. For example: in the medical aspect, the micron ferric oxide mixed suspension doped with the nano particles is used for medical magnetic resonance imaging; in the aspect of electrochemistry, the performance research of the LiFePO4/C anode material based on micron ferric oxide is carried out; in the chemical industry, the report about washing the pickling waste gas by using micron iron oxide powder suspension; in the aspect of catalysis, the application of the ethylbenzene dehydrogenation catalyst which takes micron-sized ferric oxide and potassium carbonate as raw materials is disclosed.
At present, the preparation method of the iron oxide micron particle material is mainly a dry method and a wet method. The wet method mainly comprises the following steps: hydrothermal method, forced hydrolysis method, sol-gel method, colloid chemical method, micro-emulsion method, chemical precipitation method, etc. The dry method mainly comprises the following steps: flame pyrolysis, vapor deposition, low temperature plasma chemical vapor deposition, solid phase methods, and laser pyrolysis methods.
The wet process is usually adopted, which is to react proper amount of iron salt solution with caustic soda solution, introduce air at normal temperature to change the iron salt solution into ferric hydroxide colloid solution, and gradually oxidize and deposit to generate ferric oxide micron particles. The dry method generally adopts the reaction of nitric acid and iron sheets to generate ferrous nitrate, and the ferric oxide is prepared by cooling, crystallizing, dehydrating, drying, grinding, calcining, washing with water, drying and crushing.
The microscopic shape and the structural size of the iron oxide are important factors for the performance and the application of the iron oxide, so the shape and the size are always the key points for the research of the iron oxide material. We hope to obtain new ferric oxide micro-particles by controlling the reaction conditions, etc., with unique morphology, and corresponding new performance applications in electrochemistry, catalysis, etc. The prior art for preparing micron-scale hexagonal iron oxide materials in a methanol-water mixed solution system by a solvothermal method does not exist.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a preparation method of monodisperse micron-sized hexagonal iron oxide sheets. The prepared micron-sized regular hexagonal iron oxide sheet has the advantages of good unicity, uniform size, good dispersibility, smooth surface and simple preparation steps, can be industrially produced on a large scale, and has good application prospects in the fields of electrode materials, catalysts, functional coatings, gas sensitivity and the like.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of monodisperse micron-sized hexagonal iron oxide sheets comprises the following steps:
the method comprises the following steps: dissolving ferric chloride hexahydrate in methanol, stirring until the ferric chloride hexahydrate is completely dissolved, adding a proper amount of polyvinylpyrrolidone, and continuously stirring until the ferric chloride is completely dissolved to obtain a transparent uniform solution with the concentration of 0.035-0.045 mol/L; polyvinylpyrrolidone is used as a surfactant, and the addition amount of the polyvinylpyrrolidone meets the corresponding reaction requirement.
Dissolving sodium hydroxide in deionized water, stirring until the sodium hydroxide is completely dissolved to obtain a transparent sodium hydroxide aqueous solution, wherein the solubility of the sodium hydroxide is 0.8-1.0 mol/L;
dropwise adding the prepared sodium hydroxide into the ferric chloride solution under magnetic stirring, wherein the volume ratio of the ferric chloride solution to the sodium hydroxide solution is 2.5-3.5:1, and continuing to magnetically stir for 40-60 minutes.
Step two: transferring the liquid obtained in the step one to a reaction kettle with a polytetrafluoroethylene lining, and heating for 10-20 hours at the temperature of 150 ℃ and 180 ℃. Opening the reaction kettle after the reaction kettle is naturally cooled at room temperature, respectively centrifugally washing the reaction product for 3-5 times by using methanol and deionized water, and drying to obtain a reddish purple primary product;
step three: and heating the product obtained in the step two at 480-550 ℃ for 1.5-2 hours to remove the hydroxyl on the residual surface and the like, and completely oxidizing to obtain the reddish-brown regular hexagonal iron oxide sheet.
The concentration of the transparent uniform solution of ferric chloride in the first step is 0.04mol/L, and the concentration of sodium hydroxide is 0.83 mol/L; in the first step, the volume ratio of the ferric chloride solution to the sodium hydroxide solution is 3: 1.
The invention has the beneficial effects that:
1. uniform size and shape, good dispersibility, and side length of about 3.5-3.8 x 103And the thickness of the nano-particles is about 200 to 380 nanometers. The surface of the particles is smooth, compact and micro-freeAnd (4) a hole.
2. A methanol-water mixed solution system is innovatively adopted, polyvinylpyrrolidone is used as a surfactant to assist in controlling the morphology and the dispersibility of the product, ferric chloride hexahydrate is used as an iron source, and solvothermal reaction is carried out to prepare the micron-sized hexagonal iron oxide sheet. The prepared micron-sized regular hexagonal iron oxide sheet has the advantages of good unicity, uniform size, good dispersibility, smooth surface and simple preparation steps, can be industrially produced on a large scale, and has good application prospects in the fields of electrode materials, catalysts, functional coatings, gas sensitivity and the like.
Drawings
Fig. 1 and 2 are scanning electron micrographs of micron-sized hexagonal iron oxide sheets prepared in example 1 of the present invention.
Detailed Description
For a better understanding of the present invention, specific embodiments thereof are explained in detail below with reference to the accompanying drawings.
Example 1
0.5g of ferric chloride hexahydrate is weighed into 38ml of methanol, stirred under magnetic stirring until the ferric chloride is completely dissolved, 1g of polyvinylpyrrolidone is weighed into the solution, and the solution is continuously stirred until the polyvinylpyrrolidone is completely dissolved. 0.5g of sodium hydroxide was further weighed into 15mL of water and stirred magnetically until completely dissolved. An aqueous solution of sodium hydroxide was added dropwise to the above-prepared methanol solution of ferric chloride hexahydrate with stirring. Then transferring the liquid into a reaction kettle with a polytetrafluoroethylene lining, reacting for 16 hours at 160 ℃, and naturally cooling at room temperature. And pouring the reaction product into a centrifuge tube, washing with deionized water and methanol for 4 times respectively, then putting into a 55 ℃ oven for drying for 24 hours, and then putting into a muffle furnace for holding for 2 hours at 500 ℃ to obtain the micron-sized reddish-brown regular hexagonal iron oxide sheet.
Example 2
0.6g of ferric chloride hexahydrate is weighed into 45ml of methanol, stirred under magnetic stirring until the ferric chloride is completely dissolved, then 0.8g of polyvinylpyrrolidone is weighed into the solution, and the solution is continuously stirred until the polyvinylpyrrolidone is completely dissolved. 0.6g of sodium hydroxide was weighed into 18mL of water and stirred magnetically until completely dissolved. An aqueous solution of sodium hydroxide was added dropwise to the above-prepared methanol solution of ferric chloride hexahydrate with stirring. Then transferring the liquid into a reaction kettle with a polytetrafluoroethylene lining, reacting for 10 hours at 170 ℃, and naturally cooling at room temperature. And pouring the reaction product into a centrifuge tube, washing with deionized water and methanol for 5 times respectively, then putting into a 60 ℃ oven for drying for 12 hours, and then putting into a muffle furnace for holding for 2 hours at 480 ℃, thus obtaining the micron-sized reddish-brown regular hexagonal iron oxide sheet.
Example 3
0.5g of ferric chloride hexahydrate is weighed into 52ml of methanol, stirred under magnetic stirring until the ferric chloride is completely dissolved, 1g of polyvinylpyrrolidone is weighed into the mixture, and stirring is continued until the polyvinylpyrrolidone is completely dissolved. 0.5g of sodium hydroxide was further weighed into 15mL of water and stirred magnetically until completely dissolved. An aqueous solution of sodium hydroxide was added dropwise to the above-prepared methanol solution of ferric chloride hexahydrate with stirring. Then transferring the liquid into a reaction kettle with a polytetrafluoroethylene lining, reacting for 16 hours at 180 ℃, and naturally cooling at room temperature. And pouring the reaction product into a centrifuge tube, washing with deionized water and methanol for 4 times respectively, then putting into a 55 ℃ oven for drying for 24 hours, and then putting into a muffle furnace for drying for 2 hours at 550 ℃ to obtain the micron-sized reddish-brown regular hexagonal iron oxide sheet.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
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