CN106495233B - Hedgehog shape needle-like ferroso-ferric oxide and preparation method thereof - Google Patents
Hedgehog shape needle-like ferroso-ferric oxide and preparation method thereof Download PDFInfo
- Publication number
- CN106495233B CN106495233B CN201611267441.3A CN201611267441A CN106495233B CN 106495233 B CN106495233 B CN 106495233B CN 201611267441 A CN201611267441 A CN 201611267441A CN 106495233 B CN106495233 B CN 106495233B
- Authority
- CN
- China
- Prior art keywords
- preparation
- ferroso
- ferric oxide
- needle
- suspension
- 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.)
- Active
Links
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 229940056319 ferrosoferric oxide Drugs 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 241000027355 Ferocactus setispinus Species 0.000 title description 2
- 241000289669 Erinaceus europaeus Species 0.000 claims abstract description 13
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004202 carbamide Substances 0.000 claims abstract description 11
- 239000000725 suspension Substances 0.000 claims abstract description 11
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims abstract description 10
- 235000019345 sodium thiosulphate Nutrition 0.000 claims abstract description 10
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 9
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 239000006247 magnetic powder Substances 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims 2
- 238000002156 mixing Methods 0.000 claims 1
- 229910052938 sodium sulfate Inorganic materials 0.000 claims 1
- 235000011152 sodium sulphate Nutrition 0.000 claims 1
- 125000000446 sulfanediyl group Chemical group *S* 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- -1 iron ion Chemical class 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 206010013786 Dry skin Diseases 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 150000001805 chlorine compounds Chemical class 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000012456 homogeneous solution Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 231100001261 hazardous Toxicity 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 230000007096 poisonous effect Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 229910001868 water Inorganic materials 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 description 1
- BTOOAFQCTJZDRC-UHFFFAOYSA-N 1,2-hexadecanediol Chemical class CCCCCCCCCCCCCCC(O)CO BTOOAFQCTJZDRC-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- UXKUODQYLDZXDL-UHFFFAOYSA-N fulminic acid Chemical compound [O-][N+]#C UXKUODQYLDZXDL-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 239000011553 magnetic fluid Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- 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
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- 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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/45—Aggregated particles or particles with an intergrown morphology
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Iron (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention discloses a kind of hedgehog shape needle-like ferroso-ferric oxide and preparation method thereof, the preparation method comprises the following steps：Step 1: under stirring, anhydrous ferric chloride, sodium thiosulfate and urea are mixed with solvent, mixed solution is made；Stirred Step 2: being added into mixed solution after ZnO, suspension is made；Step 3: in a high voltage state, suspension is heated into 150 DEG C~180 DEG C, 8~12 hours are incubated；Clean, dry Step 4: being cooled to after room temperature, so that the Fe 3 O 4 magnetic powder of needle-like is made.Ferroso-ferric oxide specific surface area produced by the present invention is high, without adding the materials such as template, convenient post-treatment, and reaction temperature is low, the reaction time is short, reaction process is simple, inexpensive, and environmental protection.
Description
Technical field
The present invention relates to field of material technology, and in particular to a kind of hedgehog type needle-like ferroso-ferric oxide and preparation method thereof.
Background technology
Ferroso-ferric oxide, molecular formula is Fe3O4, with a cube inverse spinel structure, due to its unique physical chemistry
Matter, the purposes different from conventional material, such as pollution administration, magnetic recording material, magnetic fluid, medicine, face are shown at numerous aspects
The fields such as material are widely used.In terms of pollution administration, due to outstanding catalytic decomposition performance and absorption property, good
Magnetic is easy to reclaim, and ferroso-ferric oxide has become the study hotspot in terms of environment in recent years improvement, by by extensive with making a return journey
Except water pollution.
In recent years, there is the preparation method of the ferroso-ferric oxide of the different method synthesis different structure of document report, for example
Using solvent method iron chloride as source of iron, lauryl mercaptan does precipitating reagent and is prepared for monodispersity as emulsifying agent, sodium acetate
Fe with hierarchy3O4Microballoon, and for example someone ferric acetyl acetonade is dissolved in containing 1,2- hexadecane diols, phenylate, oleic acid
With the in the mixed solvent of oleyl amine, the monodispersity Fe that particle diameter is less than 20nm has been made in backflow at 150 DEG C3O4Particle.
Although possessing certain Fe in the prior art3O4Preparation method, but the Fe prepared3O4Particle morphology is not outstanding enough,
Performance is not good enough, and specific surface area is not big enough, and regulates and controls Fe to how changing synthesis condition3O4Pattern and synthesis hedgehog shape
The Fe of needle-like3O4Report is seldom.
The content of the invention
(1) technical problem solved
In view of the shortcomings of the prior art, the invention provides a kind of hedgehog shape needle-like ferroso-ferric oxide and preparation method thereof,
To overcome Fe prepared by prior art3O4The low technical problem of specific surface area.
(2) technical scheme
To realize object above, the present invention is achieved by the following technical programs：
On the one hand, The present invention gives a kind of preparation method of hedgehog shape needle-like ferroso-ferric oxide, the preparation method bag
Include following steps：
Step 1: under stirring, anhydrous ferric chloride, sodium thiosulfate and urea are mixed with solvent, it is made
Mixed solution；
Stirred Step 2: being added into mixed solution after ZnO, suspension is made；
Step 3: in a high voltage state, suspension is heated into 150 DEG C~180 DEG C, 8~12 hours are incubated；
Clean, dry Step 4: being cooled to after room temperature, so that the Fe 3 O 4 magnetic powder of needle-like is made.
Further, in the mixed solution anhydrous ferric chloride, sodium thiosulfate, the mol ratio difference of urea and solvent
For 1：1~2：2~4：10~14.
Further, in step 2 ZnO and the mol ratio of anhydrous ferric chloride is 0.1~0.2：1；The time of stirring is 10
~15min.
Further, the pressure of the high pressure in step 3 is 12MPa~15MPa.
Further, the temperature of the drying in step 4 is 50~70 DEG C, and the time is 3~5 hours.
Further, the wash number in step 4 is 3~5 times.
Further, the solvent is one or both of deionized water or ethanol solution.
On the other hand, The present invention gives a kind of ferroso-ferric oxide prepared using preparation method described above.
Further, the specific surface area of the ferroso-ferric oxide is 45~70m2/g；The length ruler of the ferroso-ferric oxide
It is very little to be distributed in 0.1~2 micron.
The length dimension distribution of the ferroso-ferric oxide of the present invention is preferably 0.15~1.5 micron, and further Size Distribution is excellent
Elect 0.2~1.2 micron as.
The formation mechanism of the present invention is as follows：
1st, partial oxidation iron is reduced into frerrous chloride by sodium thiosulfate, and its reaction equation is as follows：
2FeCl3+2Na2S2O3=2NaCl+2FeCl2+Na2S4O6；
So that iron ion is in coexisting state with ferrous ion in system.
2nd, the mechanism of ZnO regulation and control：
ZnO has both sexes, and Fe (OH) can be participated under this system3Generation：
2FeCl3+3ZnO+3H2O=2Fe (OH)3+3ZnCl2。
3rd, 160 DEG C or so are heated in a high voltage state, urea slowly decomposes release ammonia, its reaction equation is as follows：
CO(NH2)2=NH3+HCNO；
The ammonia of generation is soluble in water, produces weakly alkaline environment：
NH3+H2O=NH4 ++OH-。
4th, at high temperature under high pressure, ferroso-ferric oxide is generated, its reaction equation is as follows：
Fe2++2Fe3++8OH-=Fe3O4+4H2O；
Or Fe (OH)2+2Fe(OH)3=Fe3O4+4H2O。
(3) beneficial effect
The invention provides a kind of ferroso-ferric oxide of hedgehog shape needle-like high-specific surface area and preparation method thereof.Possess following
Beneficial effect：
1st, the present invention is regulated and controled by the use of anhydrous ferric chloride, sodium thiosulfate and urea as raw material by hydro-thermal method and ZnO
Needle-like ferroso-ferric oxide is synthesized, during the course of the reaction, it is not necessary to add dispersant and surfactant, and obtained specific surface area is
45~70m2/g ferroso-ferric oxide, improves the specific surface area of ferroso-ferric oxide.
2nd, the present invention need not add the materials such as template, convenient post-treatment, and reaction temperature is low, the reaction time is short, reaction process
Simply, inexpensive.
3rd, preparation process environmental protection of the present invention, is not used any poisonous and hazardous organic reagent.
4th, the present invention solves that process in traditional preparation methods is complicated, with high costs, pattern not enough good, specific surface area is low
Problem.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the accompanying drawing used required in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with
Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is ferroso-ferric oxide Fe3O4 prepared by embodiment 3 SEM photograph；
Fig. 2 is ferroso-ferric oxide Fe3O4 prepared by embodiment 3 XRD spectra.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention
In accompanying drawing, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is
A part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art
The every other embodiment obtained under the premise of creative work is not made, belongs to the scope of protection of the invention.
Embodiment 1：
The embodiment of the present invention 1 proposes a kind of preparation method of hedgehog shape needle-like ferroso-ferric oxide, comprises the following steps：
1st, 1mmol anhydrous ferric chlorides, 1mmol sodium thiosulfate and 2mmol urea are dissolved in 10ml deionized waters,
Homogeneous solution is obtained under magnetic stirring.
2 then add 0.1mmolZnO, magnetic agitation 10min, obtain suspension；
3rd, suspension is added in the polytetrafluoroethylene (PTFE) autoclave inner bag that volume is 50ml, in 12MPa pressure
Under, 150 DEG C are heated in baking oven, 8 hours are incubated.
4th, autoclave, which is naturally cooled to, takes out reactant after room temperature, product is each using deionized water and ethanol alternating
Cleaning 3 times, collects sediment using externally-applied magnetic field, product then is transferred into vacuum drying chamber 3 hours of 50 DEG C of dryings, obtained
Specific surface area is 45m2/g black ferroferric oxide Magnaglo.
Embodiment 2：
The embodiment of the present invention 2 proposes a kind of preparation method of hedgehog shape needle-like ferroso-ferric oxide, comprises the following steps：
1st, 1mmol anhydrous ferric chlorides, 2mmol sodium thiosulfate and 4mmol urea are dissolved in 14ml deionized waters,
Homogeneous solution is obtained under magnetic stirring,
2 then add 0.2mmolZnO, magnetic agitation 15min, obtain suspension；
3rd, suspension is added in the polytetrafluoroethylene (PTFE) autoclave inner bag that volume is 50ml, in 15MPa pressure
Under, 180 DEG C are heated in baking oven, 12 hours are incubated.
4th, autoclave, which is naturally cooled to, takes out reactant after room temperature, product is each using deionized water and ethanol alternating
Cleaning 5 times, collects sediment using externally-applied magnetic field, product then is transferred into vacuum drying chamber 5 hours of 70 DEG C of dryings, obtained
Specific surface area is 64m2/g black ferroferric oxide Magnaglo.
Embodiment 3：
The embodiment of the present invention 3 proposes a kind of preparation method of hedgehog shape needle-like ferroso-ferric oxide, comprises the following steps：
1st, 1mmol anhydrous ferric chlorides, 1.3mmol sodium thiosulfate and 2.6mmol urea are dissolved in 8ml deionized waters
In 4ml absolute ethyl alcohol mixed solutions,
2nd, homogeneous solution is obtained under magnetic stirring, is then added 0.13mmolZnO, magnetic agitation 12min, is suspended
Liquid；
3rd, suspension is added in the polytetrafluoroethylene (PTFE) autoclave inner bag that volume is 50ml, in 14MPa pressure
Under be heated to 160 DEG C in baking oven, be incubated 10 hours.
4th, autoclave, which is naturally cooled to, takes out reactant after room temperature, product is each using deionized water and ethanol alternating
Cleaning 4 times, collects sediment using externally-applied magnetic field, product then is transferred into vacuum drying chamber 4 hours of 60 DEG C of dryings, obtained
Specific surface area is 70m2/g black ferroferric oxide Magnaglos.
The hedgehog shape needle-like ferroso-ferric oxide prepared to embodiment 3 carries out SEM observations and XRD analysis.
Reference picture 1, it was found from SEM photograph, the yield of products therefrom is very big, and specific surface area is high, and particle is in needle-like, and whole
Body distribution shows hedgehog shape, and aciculiform ferroso-ferric oxide length dimension is distributed in 1.0 microns.
Reference picture 2, it was found from XRD (X-ray diffraction) spectrogram, products therefrom is ferroso-ferric oxide Fe3O4 phase crystal structures
(JCPDS card no.01-089-0688)。
In summary, the embodiments of the invention provide a kind of ferroso-ferric oxide of hedgehog shape needle-like high-specific surface area and its system
Preparation Method.Possesses following beneficial effect：
1st, the embodiment of the present invention passes through hydro-thermal method and ZnO by the use of anhydrous ferric chloride, sodium thiosulfate and urea as raw material
To regulate and control synthesis needle-like ferroso-ferric oxide, during the course of the reaction, it is not necessary to add dispersant and surfactant, and it is made and compares table
Area is 45~70m2/g ferroso-ferric oxide, improves the specific surface area of ferroso-ferric oxide.
2nd, the embodiment of the present invention need not add the materials such as template, convenient post-treatment, and reaction temperature is low, the reaction time is short, anti-
Answer that technique is simple, inexpensive.
3rd, preparation process of embodiment of the present invention environmental protection, is not used any poisonous and hazardous organic reagent.
4th, the embodiment of the present invention solves that process in traditional preparation methods is complicated, with high costs, pattern is not good enough, compare surface
The low problem of product.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (8)
1. a kind of preparation method of hedgehog shape needle-like ferroso-ferric oxide, it is characterised in that the preparation method comprises the following steps：
Step 1: under stirring, anhydrous ferric chloride, sodium thiosulfate and urea are mixed with solvent, mixing is made
Solution；
Stirred Step 2: being added into mixed solution after ZnO, suspension is made；
Step 3: in a high voltage state, suspension is heated into 150 DEG C~180 DEG C, 8~12 hours are incubated；
Clean, dry Step 4: being cooled to after room temperature, so that the Fe 3 O 4 magnetic powder of needle-like is made.
2. preparation method according to claim 1, it is characterised in that anhydrous ferric chloride in the mixed solution, thio
The mol ratio of sodium sulphate, urea and solvent is respectively 1：1~2：2~4：10~14.
3. preparation method according to claim 2, it is characterised in that mole of ZnO and anhydrous ferric chloride in step 2
Than for 0.1~0.2：1；The time of stirring is 10~15min.
4. the preparation method according to claim 1 or 2 or 3, it is characterised in that the pressure of the high pressure in step 3 is
12MPa~15MPa.
5. preparation method according to claim 4, it is characterised in that the temperature of the drying in step 4 is 50~70 DEG C,
Time is 3~5 hours.
6. the preparation method according to claim 1 or 2 or 3, it is characterised in that the temperature of the drying in step 4 is 50~
70 DEG C, the time is 3~5 hours.
7. the preparation method according to claim 1 or 2 or 3, it is characterised in that the wash number in step 4 is 3~5
It is secondary.
8. the preparation method according to claim 1 or 2 or 3, it is characterised in that the solvent is that deionized water or ethanol are molten
One or both of liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611267441.3A CN106495233B (en) | 2016-12-31 | 2016-12-31 | Hedgehog shape needle-like ferroso-ferric oxide and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611267441.3A CN106495233B (en) | 2016-12-31 | 2016-12-31 | Hedgehog shape needle-like ferroso-ferric oxide and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106495233A CN106495233A (en) | 2017-03-15 |
| CN106495233B true CN106495233B (en) | 2017-10-24 |
Family
ID=58334894
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611267441.3A Active CN106495233B (en) | 2016-12-31 | 2016-12-31 | Hedgehog shape needle-like ferroso-ferric oxide and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106495233B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111760569A (en) * | 2020-07-08 | 2020-10-13 | 合肥工业大学 | Composite photo-Fenton catalyst, preparation method and application |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102001712A (en) * | 2010-12-16 | 2011-04-06 | 苏州康立达纳米生物工程有限公司 | Method for preparing superparamagnetic Fe3O4 nano particle based on thermal decomposition of template |
| CN102153146B (en) * | 2011-04-18 | 2015-06-17 | 中国科学院化学研究所 | Method for controllably preparing hydroxyl oxidize iron, iron sesquioxide and ferroferric oxide |
| CN105381802B (en) * | 2015-12-23 | 2018-10-02 | 哈尔滨工业大学 | One kind preparing dandelion shape Fe based on heterogeneous nucleation means3O4The methods and applications of@ZnO nucleocapsid compounds |
-
2016
- 2016-12-31 CN CN201611267441.3A patent/CN106495233B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN106495233A (en) | 2017-03-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103539210B (en) | A kind of preparation method of cobalt molybdate crystallite | |
| CN102275986A (en) | Controllable hydro-thermal preparation method for titanium dioxide nanobelts of different crystal forms | |
| CN105271405B (en) | A kind of material based on bismuthyl carbonate or oxidation bismuth nanotube and preparation method thereof | |
| CN101746837B (en) | Preparation method of cobalt sulfide micro tube with hiberarchy structure | |
| CN106379924A (en) | Nano magnesium-aluminum hydrotalcite and preparation method thereof | |
| CN101798120B (en) | Method for producing nanometer iron oxide red by utilizing ferrous chloride recovered from waste acid washing liquor | |
| Badnore et al. | Effect of pH on sonication assisted synthesis of ZnO nanostructures: Process details | |
| CN104150541B (en) | A kind of grain of rice shape α-Fe 2o 3the preparation method of nanometer powder | |
| CN103288136A (en) | Hydrothermal synthesis method of shape-controllable molybdenum dioxide submicrocrystals | |
| CN107745133A (en) | A kind of inexpensive environment-friendly preparation method thereof of Nanometer Copper | |
| CN106495233B (en) | Hedgehog shape needle-like ferroso-ferric oxide and preparation method thereof | |
| Mao et al. | The coprecipitation formation study of iron oxide nanoparticles with the assist of a gas/liquid mixed phase fluidic reactor | |
| CN103318974A (en) | Preparation method of ferroferric oxide magnetic carrier | |
| CN104495884B (en) | basic magnesium carbonate and preparation method thereof | |
| CN103880093B (en) | Hollow spherical nickel bicarbonate aggregate | |
| CN102616840A (en) | Method for preparing transition metal oxide nano single crystal with specific exposed crystal faces through stripping nanosheets | |
| CN102328960B (en) | Synthesis method of trimanganese tetroxide material with 3D (three-dimensional) flower-shaped structure | |
| CN104030363B (en) | A kind of preparation method of ferriferrous oxide nano-particle | |
| CN101805017B (en) | Preparation method of rutile type titanium dioxide nano particle | |
| CN109133192B (en) | A kind of Transition-metal dichalcogenide material and preparation method thereof | |
| CN104988576B (en) | The preparation method of alkali magnesium sulfate crystal whisker | |
| Xing et al. | Surfactant-free fabrication of Fe3O4 nanospheres with selective shape | |
| CN103145535A (en) | Diethylene glycol ferrous alkoxide with three-dimensional pattern multi-stage structure and preparation method thereof | |
| CN106517264B (en) | A kind of preparation method of petal-shaped magnesium hydroxide | |
| CN105543975A (en) | Method for synthesizing calcium carbonate nanocrystal whiskers on basis of sodium carboxymethyl cellulose and potassium chloride |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | 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 |