CN108862399A - A kind of preparation method of monodispersed micron order hexagon oxidation iron plate - Google Patents

A kind of preparation method of monodispersed micron order hexagon oxidation iron plate Download PDF

Info

Publication number
CN108862399A
CN108862399A CN201811137011.9A CN201811137011A CN108862399A CN 108862399 A CN108862399 A CN 108862399A CN 201811137011 A CN201811137011 A CN 201811137011A CN 108862399 A CN108862399 A CN 108862399A
Authority
CN
China
Prior art keywords
hexagon
solution
iron plate
preparation
micron order
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201811137011.9A
Other languages
Chinese (zh)
Other versions
CN108862399B (en
Inventor
李晓宇
胡新芳
邵明星
刘爽
荆象阳
傅敏
岳增武
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
State Grid Corp of China SGCC
Electric Power Research Institute of State Grid Shandong Electric Power Co Ltd
Original Assignee
State Grid Corp of China SGCC
Electric Power Research Institute of State Grid Shandong Electric Power Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by State Grid Corp of China SGCC, Electric Power Research Institute of State Grid Shandong Electric Power Co Ltd filed Critical State Grid Corp of China SGCC
Priority to CN201811137011.9A priority Critical patent/CN108862399B/en
Publication of CN108862399A publication Critical patent/CN108862399A/en
Application granted granted Critical
Publication of CN108862399B publication Critical patent/CN108862399B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/02Oxides; Hydroxides
    • C01G49/06Ferric oxide (Fe2O3)
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer

Abstract

The invention discloses a kind of preparation methods of monodispersed micron order hexagon oxidation iron plate, include the following steps:Step 1 configures reaction solution;The primary product of reddish violet is made in step 2, solvent-thermal method;Step 3, heat treatment obtains bronzing iron oxide in Muffle furnace.Innovatively use methanol-water mixed solution system, polyvinylpyrrolidone is used to carry out auxiliary control as pattern and dispersibility of the surfactant to product, using Iron trichloride hexahydrate as source of iron, carries out solvent thermal reaction and prepare micron order hexagon oxidation iron plate.The micron order regular hexagon oxidation iron plate unicity of preparation is good, and of uniform size, good dispersion, surface is smooth, and preparation step is simple, can have good application prospect in fields such as electrode material, catalyst, functional paint, air-sensitives with large-scale industrial production.

Description

A kind of preparation method of monodispersed micron order hexagon oxidation iron plate
Technical field
The present invention relates to inorganic material to synthesize field, and specifically a kind of monodispersed micron order hexagon aoxidizes iron plate Preparation method.
Background technique
Iron oxide is important magnetic material, catalyst, polishing material, battery material, red pigment, colorant, function Coating, gas sensitive.It is widely used in medical treatment, the energy, telecommunication, measurement instrument industry, paint, rubber, plastics, cosmetics, enamel, skin The fields such as leather, magnetic alloy, catalysis industry and gas sensor.Such as:In terms of medicine, the micron iron oxide of dopen Nano particle Suspension is used for medical magnetic resonance radiography;In terms of electrochemistry, there is the performance of the LiFePO4/C positive electrode based on micron iron oxide Research;In terms of chemical industry, about the report for using micron suspension of ferric oxide powder to wash pickling exhaust gas;Catalysis aspect, it is related In using micron ferric oxide and potassium carbonate as the application of the catalyst for phenylethylene dehydrogenation of raw material.
The preparation method of iron oxide micron particles material is mainly dry and wet at present.Wet process mainly has:It is hydro-thermal method, strong Compel Hydrolyze method, sol-gal process, colloid chemistry methods, microemulsion method and chemical precipitation method etc..Dry method mainly has:Flame thermal decomposition, Vapor deposition, low-temperature plasma chemical vapour deposition technique, solid phase method and laser thermal decomposition method.
The wet process generallyd use is to react suitable iron salt solutions with soda bath, is passed through air at normal temperature and is allowed to complete Portion becomes ferric hydroxide colloid solution, and gradually oxide deposition generates iron oxide micron particles.Dry method generallys use nitric acid and iron plate Reaction generates ferrous nitrate, through crystallisation by cooling, dehydration and drying, polished calcining, then oxidation is made through washing, drying, crushing Iron.
An important factor for microscopic appearance and structure size of iron oxide are its performance and application, therefore the tune of morphology and size Control is always the research emphasis of iron oxide material.It is desirable that obtaining novel iron oxide micron by control reaction condition etc. Grain has unique pattern, the corresponding new performance applications for having electrochemistry, catalysis etc..For being mixed in methanol-water It is had not yet seen in the prior art in solution system with the iron oxide material that solvent-thermal method prepares micron order hexagon.
Summary of the invention
The present invention is exactly to provide a kind of monodispersed micron order hexagon to solve deficiencies of the prior art The preparation method of iron plate is aoxidized, methanol-water mixed solution system is innovatively used, uses polyvinylpyrrolidone as table Face activating agent carries out auxiliary control to the pattern and dispersibility of product, and using Iron trichloride hexahydrate as source of iron, it is anti-to carry out solvent heat Micron order hexagon oxidation iron plate should be prepared.The micron order regular hexagon oxidation iron plate unicity of preparation is good, of uniform size, dispersion Property is good, and surface is smooth, and preparation step is simple, can be with large-scale industrial production, in electrode material, catalyst, functional paint, gas There is good application prospect in quick equal fields.
The technical scheme adopted by the invention to solve the technical problem is that:
A kind of preparation method of monodispersed micron order hexagon oxidation iron plate, includes the following steps:
Step 1:Iron trichloride hexahydrate is dissolved in methanol solution, stirring adds appropriate polyethylene up to being completely dissolved Pyrrolidones continues stirring until being completely dissolved, and obtains the transparent uniform solution that ferric chloride concn is 0.035-0.045mol/L; Polyvinylpyrrolidone is surfactant, and additional amount meets corresponding reaction and requires.
In deionized water by sodium hydroxide dissolution, it stirs to being completely dissolved, obtains transparent sodium hydrate aqueous solution, The solubility of middle sodium hydroxide is 0.8-1.0mol/L;
By the sodium hydroxide of preparation, solution is added dropwise in above-mentioned ferric chloride solution under magnetic stirring, ferric chloride solution and Sodium hydroxide solution volume proportion is 2.5-3.5:1, continue magnetic agitation 40-60 minutes.
Step 2:The liquid that step 1 is obtained is transferred in the reaction kettle of polytetrafluoroethyllining lining, is maintained at 150-180 DEG C heating 10-20 hours.It is opened after reaction kettle at room temperature natural cooling, by reaction product methanol solution and deionized water Centrifuge washing 3-5 times respectively, the primary product of reddish violet is obtained after drying;
Step 3:Product obtained in step 2 is heated 1.5-2 hours at 480-550 DEG C, removes remaining surface Hydroxyl etc. obtains regular hexagon oxidation iron plate russet after exhaustive oxidation.
The transparent uniform solution concentration of iron chloride is 0.04mol/L in the step 1, and the concentration of the sodium hydroxide is 0.83mol/L;Ferric chloride solution and sodium hydroxide solution volume proportion are 3 in the step 1:1.
The beneficial effects of the invention are as follows:
1, size shape is uniform, good dispersion, and side length is about 3.5~3.8*103Nanometer, thickness are about 200~380 to receive Rice.Particle surface is flat and smooth, fine and close pore-free.
2, methanol-water mixed solution system is innovatively used, uses polyvinylpyrrolidone as surfactant Pattern and dispersibility to product carry out auxiliary control, and using Iron trichloride hexahydrate as source of iron, progress solvent thermal reaction prepares micro- Meter level hexagon aoxidizes iron plate.The micron order regular hexagon oxidation iron plate unicity of preparation is good, of uniform size, good dispersion, table Face is smooth, and preparation step is simple, can be led with large-scale industrial production in electrode material, catalyst, functional paint, air-sensitive etc. There is good application prospect in domain.
Detailed description of the invention
Fig. 1 and Fig. 2 is the stereoscan photograph that micron order hexagon prepared by the embodiment of the present invention 1 aoxidizes iron plate.
Specific embodiment
For a better understanding of the present invention, a specific embodiment of the invention is explained in detail with reference to the accompanying drawing.
Embodiment 1
It weighs 0.5g Iron trichloride hexahydrate to be added in 38ml methanol, be stirred under magnetic stirring to being completely dissolved, then weigh 1g Polyvinylpyrrolidone is added, and continues stirring to being completely dissolved.It separately weighs 0.5g sodium hydroxide to be added in 15mL water, magnetic agitation To being completely dissolved.The aqueous solution of sodium hydroxide is added dropwise to the methanol solution of Iron trichloride hexahydrate obtained above under stiring In.Then aforesaid liquid is transferred in the reaction kettle of polytetrafluoroethyllining lining, reacts 16 hours at 160 DEG C, at room temperature from It is so cooling.Reaction product is poured into centrifuge tube, deionized water and methanol wash 4 times respectively, are then placed in 55 DEG C of baking ovens and protect It holds 24 hours and dries, place into Muffle furnace and keep aoxidizing to get to micron-sized regular hexagon russet for 2 hours for 500 DEG C Iron plate.
Embodiment 2
It weighs 0.6g Iron trichloride hexahydrate to be added in 45ml methanol, be stirred under magnetic stirring to being completely dissolved, then weigh 0.8g polyvinylpyrrolidone is added, and continues stirring to being completely dissolved.It separately weighs 0.6g sodium hydroxide to be added in 18mL water, magnetic force Stirring is to being completely dissolved.The methanol that Iron trichloride hexahydrate obtained above is added dropwise in the aqueous solution of sodium hydroxide under stiring is molten In liquid.Then aforesaid liquid is transferred in the reaction kettle of polytetrafluoroethyllining lining, reacts 10 hours at 170 DEG C, at room temperature Natural cooling.Reaction product is poured into centrifuge tube, deionized water and methanol wash 5 times respectively, are then placed in 60 DEG C of baking ovens It keeps drying for 12 hours, places into Muffle furnace and kept for 2 hours to get micron-sized regular hexagon oxygen russet is arrived for 480 DEG C Change iron plate.
Embodiment 1
It weighs 0.5g Iron trichloride hexahydrate to be added in 52ml methanol, be stirred under magnetic stirring to being completely dissolved, then weigh 1g Polyvinylpyrrolidone is added, and continues stirring to being completely dissolved.It separately weighs 0.5g sodium hydroxide to be added in 15mL water, magnetic agitation To being completely dissolved.The aqueous solution of sodium hydroxide is added dropwise to the methanol solution of Iron trichloride hexahydrate obtained above under stiring In.Then aforesaid liquid is transferred in the reaction kettle of polytetrafluoroethyllining lining, reacts 16 hours at 180 DEG C, at room temperature from It is so cooling.Reaction product is poured into centrifuge tube, deionized water and methanol wash 4 times respectively, are then placed in 55 DEG C of baking ovens and protect It holds 24 hours and dries, place into Muffle furnace and keep aoxidizing to get to micron-sized regular hexagon russet for 2 hours for 550 DEG C Iron plate.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention, It should be equivalent substitute mode, be included within the scope of the present invention.

Claims (2)

1. a kind of preparation method of monodispersed micron order hexagon oxidation iron plate, characterized in that the method includes following steps Suddenly:
Step 1:Iron trichloride hexahydrate is dissolved in methanol solution, stirring adds appropriate polyvinyl pyrrole up to being completely dissolved Alkanone continues stirring until being completely dissolved, and obtains the transparent uniform solution that ferric chloride concn is 0.035-0.045mol/L;
In deionized water by sodium hydroxide dissolution, it stirs to being completely dissolved, obtains transparent sodium hydrate aqueous solution, wherein hydrogen The solubility of sodium oxide molybdena is 0.8-1.0mol/L;
By the sodium hydroxide of preparation, solution is added dropwise in above-mentioned ferric chloride solution under magnetic stirring, ferric chloride solution and hydrogen-oxygen Change sodium solution volume proportion is 2.5-3.5:1, continue magnetic agitation 40-60 minutes.
Step 2:The liquid that step 1 is obtained is transferred in the reaction kettle of polytetrafluoroethyllining lining, is maintained at 150-180 DEG C and is added It is 10-20 hours hot, it is opened after reaction kettle at room temperature natural cooling, reaction product methanol solution and deionized water is distinguished Centrifuge washing 3-5 times obtains the primary product of reddish violet after drying;
Step 3:Product obtained in step 2 is heated 1.5-2 hours at 480-550 DEG C, removes the hydroxyl of remaining surface, Regular hexagon oxidation iron plate russet is obtained after exhaustive oxidation.
2. a kind of preparation method of monodispersed micron order hexagon oxidation iron plate according to claim 1, characterized in that The transparent uniform solution concentration of iron chloride is 0.04mol/L in the step 1, and the concentration of the sodium hydroxide is 0.83mol/ L;Ferric chloride solution and sodium hydroxide solution volume proportion are 3 in the step 1:1.
CN201811137011.9A 2018-09-28 2018-09-28 Preparation method of monodisperse micron-sized hexagonal iron oxide sheet Active CN108862399B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811137011.9A CN108862399B (en) 2018-09-28 2018-09-28 Preparation method of monodisperse micron-sized hexagonal iron oxide sheet

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811137011.9A CN108862399B (en) 2018-09-28 2018-09-28 Preparation method of monodisperse micron-sized hexagonal iron oxide sheet

Publications (2)

Publication Number Publication Date
CN108862399A true CN108862399A (en) 2018-11-23
CN108862399B CN108862399B (en) 2021-03-19

Family

ID=64324599

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811137011.9A Active CN108862399B (en) 2018-09-28 2018-09-28 Preparation method of monodisperse micron-sized hexagonal iron oxide sheet

Country Status (1)

Country Link
CN (1) CN108862399B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112661194A (en) * 2020-12-24 2021-04-16 厦门大学 Preparation method of uniform flaky ferric oxide with adjustable size
CN112919548A (en) * 2021-03-09 2021-06-08 陕西科技大学 Purple luster iron oxide flaky particles and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112661194A (en) * 2020-12-24 2021-04-16 厦门大学 Preparation method of uniform flaky ferric oxide with adjustable size
CN112661194B (en) * 2020-12-24 2023-05-23 厦门大学 Preparation method of uniform flaky ferric oxide with adjustable size
CN112919548A (en) * 2021-03-09 2021-06-08 陕西科技大学 Purple luster iron oxide flaky particles and preparation method thereof
CN112919548B (en) * 2021-03-09 2023-08-08 晶瓷(北京)新材料科技有限公司 Purple glossy iron oxide flaky particles and preparation method thereof

Also Published As

Publication number Publication date
CN108862399B (en) 2021-03-19

Similar Documents

Publication Publication Date Title
CN104888753B (en) A kind of stannic disulfide/titanium dioxide composite photocatalyst and preparation method thereof
CN109705646A (en) A kind of titanium dioxide compounded mix and preparation method thereof, reflective heat-insulation paint
CN102060330B (en) Method for synthetizing bismuth molybdate octahedral nanoparticle by microwave radiation heating
CN104925867B (en) A kind of nanometer wolframic acid caesium powder body and preparation method and application
CN105838115B (en) A kind of preparation method of graphene-based Electro-conductive pearlescent pigment
CN108862399A (en) A kind of preparation method of monodispersed micron order hexagon oxidation iron plate
CN101205078B (en) Method for preparing cerium dioxide nano-tube
CN108480657A (en) A kind of bismuth nanometer sheet, preparation method and its application
CN106866992B (en) A kind of preparation method of the titania modified polyacrylate dispersion of hollow spheres
Zhao et al. Preparation of nanosized anatase TiO2-coated illite composite pigments by Ti (SO4) 2 hydrolysis
CN106744728A (en) A kind of method that room temperature liquid phase method prepares SnSe micron balls
CN107032391B (en) A kind of method of the nanocrystalline morphology and size regulation of stannic disulfide
CN104282913A (en) Sheet-shaped porous carbon cladded ZnO nano composite material as well as preparation method and application thereof
CN105460983A (en) Method for preparing nickel cobaltate nano material for super capacitor
CN106356522B (en) A kind of electrochemically stable efficient storage lithium Li3VO4The low-temperature microwave synthetic method of hollow Nano cube
CN113443650B (en) Method for preparing nano titanate by utilizing self-release of crystal water
CN108557886B (en) A kind of reaction kettle, a kind of vanadium dioxide nano powder and preparation method thereof
CN110292920A (en) The preparation method of the doping cerium dioxide porous bead of zirconium
CN108609652A (en) A method of preparing Zirconium dioxide nano powder using fused salt
CN109110750A (en) The method for preparing graphene using expanded graphite
CN106732588B (en) The catalyst and its preparation method and application of Cr (VI) in a kind of conversion aqueous solution
CN104047015A (en) Method for preparing high-purity alumina powder by alternating current electrolysis
CN105347377A (en) Preparation method for high-purity flaky alumina
CN109517217A (en) A kind of tungsten-doped vanadium dioxide/graphene complex and the preparation method and application thereof
CN101805017B (en) Preparation method of rutile type titanium dioxide nano particle

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant