CN106495233A - Rrinaceus earopaeuss shape needle-like ferroso-ferric oxide and preparation method thereof - Google Patents
Rrinaceus earopaeuss shape needle-like ferroso-ferric oxide and preparation method thereof Download PDFInfo
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 229940056319 ferrosoferric oxide Drugs 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000004202 carbamide Substances 0.000 claims abstract description 11
- 235000013877 carbamide Nutrition 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 8
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 239000006247 magnetic powder Substances 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 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 1
- 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
- 230000004044 response Effects 0.000 abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 14
- 239000000047 product Substances 0.000 description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229960004756 ethanol Drugs 0.000 description 4
- 238000013019 agitation Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 150000001805 chlorine compounds Chemical class 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000012456 homogeneous solution Substances 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229950000845 politef Drugs 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000376 reactant 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
- 230000008859 change Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 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
- 229910052742 iron Inorganic materials 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
- 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
- 241000289669 Erinaceus europaeus Species 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
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 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
- 229960002089 ferrous chloride Drugs 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
- 239000008187 granular material Substances 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
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- -1 iron ion Chemical class 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
- 239000004005 microsphere 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
- 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
- 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 Rrinaceus earopaeuss shape needle-like ferroso-ferric oxide and preparation method thereof, the preparation method comprises the steps：Step one, under stirring, anhydrous ferric chloride, sodium thiosulfate and carbamide are mixed with solvent, be obtained mixed solution；Step 2, the stirring after addition ZnO in mixed solution, are obtained suspension；Suspension is heated to 150 DEG C～180 DEG C by step 3, in a high voltage state, is incubated 8～12 hours；Step 4, it is cooled to cleaning after room temperature, dries, so as to the Fe 3 O 4 magnetic powder of needle-like is obtained.Obtained in of the invention, ferroso-ferric oxide specific surface area is high, need not add the materials such as template, convenient post-treatment, and reaction temperature is low, the response 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 are Fe3O4, with a cube inverse spinel structure, due to its unique physical chemistry
Matter, shows the purposes different from conventional material, such as pollution administration, magnetic recording material, magnetic fluid, medicine, face 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
Remove water pollution.
In recent years, the preparation method of the ferroso-ferric oxide of the method synthesis different structure for having document report different, for example
Using solvent method iron chloride as source of iron, lauryl mercaptan does precipitant and is prepared for monodispersity as emulsifying agent, sodium acetate
There is the Fe of hierarchy3O4Microsphere, and for example someone ferric acetyl acetonade is dissolved in containing 1,2- hexadecane diols, phenylate, Oleic acid
In the mixed solvent of oleyl amine, backflow at 150 DEG C has been obtained monodispersity Fe of the particle diameter less than 20nm3O4Particle.
Although possess certain Fe in prior art3O4Preparation method, but the Fe for preparing3O4Particle 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 to change synthesis condition3O4Pattern and synthesis Rrinaceus earopaeuss shape
The Fe of needle-like3O4Report is seldom.
Content of the invention
(1) technical problem for solving
For the deficiencies in the prior art, the invention provides a kind of Rrinaceus earopaeuss shape needle-like ferroso-ferric oxide and preparation method thereof,
With the Fe for overcoming prior art to prepare3O4The low technical problem of specific surface area.
(2) technical scheme
For realizing that object above, the present invention are achieved by the following technical programs：
On the one hand, The present invention gives a kind of preparation method of Rrinaceus earopaeuss shape needle-like ferroso-ferric oxide, the preparation method bag
Include following steps：
Step one, under stirring, anhydrous ferric chloride, sodium thiosulfate and carbamide are mixed with solvent, be obtained
Mixed solution；
Step 2, the stirring after addition ZnO in mixed solution, are obtained suspension；
Suspension is heated to 150 DEG C～180 DEG C by step 3, in a high voltage state, is incubated 8～12 hours；
Step 4, it is cooled to cleaning after room temperature, dries, so as to the Fe 3 O 4 magnetic powder of needle-like is obtained.
The mol ratio difference of anhydrous ferric chloride further, in the mixed solution, sodium thiosulfate, carbamide and solvent
For 1：1～2：2～4：10～14.
Further, the ZnO in step 2 is 0.1～0.2 with the mol ratio of anhydrous ferric chloride：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 two in 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
Very little it is 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 distribution of sizes is excellent
Elect 0.2～1.2 micron as.
The formation mechanism of the present invention is as follows：
1st, partial oxidation ferrum is reduced into ferrous 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, can participate in Fe (OH) under this system3Generate：
2FeCl3+3ZnO+3H2O=2Fe (OH)3+3ZnCl2.
3rd, 160 DEG C or so are heated in a high voltage state, carbamide 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, and 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 Rrinaceus earopaeuss 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 carbamide as raw material by hydro-thermal method and ZnO
Synthesis needle-like ferroso-ferric oxide, during the course of the reaction, it is not necessary to add dispersant and surfactant, and prepared specific surface area is
The ferroso-ferric oxide of 45～70m2/g, 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 response 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.
Description of the drawings
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
Accompanying drawing to be used needed for having technology description is 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 the SEM photograph of ferroso-ferric oxide Fe3O4 prepared by embodiment 3；
Fig. 2 is the XRD spectra of ferroso-ferric oxide Fe3O4 prepared by embodiment 3.
Specific embodiment
Purpose, technical scheme and advantage for making the embodiment of the present invention is clearer, below in conjunction with the embodiment of the present invention
In accompanying drawing, to the embodiment of the present invention in technical scheme be clearly and completely described, it is clear that described embodiment is
The a part of embodiment of the present invention, rather than whole embodiments.Embodiment in based on 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 Rrinaceus earopaeuss shape needle-like ferroso-ferric oxide, comprises the steps：
1st, 1mmol anhydrous ferric chlorides, 1mmol sodium thiosulfate and 2mmol carbamide are dissolved in 10ml deionized waters,
Homogeneous solution is obtained under magnetic stirring.
2nd, 0.1mmolZnO is subsequently adding, and magnetic agitation 10min obtains suspension；
3rd, suspension is added in the politef autoclave inner bag that volume is 50ml, in the pressure of 12MPa
Under, 150 DEG C are heated in baking oven, are incubated 8 hours.
4th, autoclave takes out reactant after naturally cooling to room temperature, and product is alternately each using deionized water and ethanol
Cleaning 3 times, collects precipitate using externally-applied magnetic field, product is transferred to 50 DEG C of the vacuum drying oven hour of drying 3 then, is obtained
Black ferroferric oxide Magnaglo of the specific surface area for 45m2/g.
Embodiment 2：
The embodiment of the present invention 2 proposes a kind of preparation method of Rrinaceus earopaeuss shape needle-like ferroso-ferric oxide, comprises the steps：
1st, 1mmol anhydrous ferric chlorides, 2mmol sodium thiosulfate and 4mmol carbamide are dissolved in 14ml deionized waters,
Homogeneous solution is obtained under magnetic stirring,
2nd, 0.2mmolZnO is subsequently adding, and magnetic agitation 15min obtains suspension；
3rd, suspension is added in the politef autoclave inner bag that volume is 50ml, in the pressure of 15MPa
Under, 180 DEG C are heated in baking oven, are incubated 12 hours.
4th, autoclave takes out reactant after naturally cooling to room temperature, and product is alternately each using deionized water and ethanol
Cleaning 5 times, collects precipitate using externally-applied magnetic field, product is transferred to 70 DEG C of the vacuum drying oven hour of drying 5 then, is obtained
Black ferroferric oxide Magnaglo of the specific surface area for 64m2/g.
Embodiment 3：
The embodiment of the present invention 3 proposes a kind of preparation method of Rrinaceus earopaeuss shape needle-like ferroso-ferric oxide, comprises the steps：
1st, 1mmol anhydrous ferric chlorides, 1.3mmol sodium thiosulfate and 2.6mmol carbamide are dissolved in 8ml deionized waters
In 4ml dehydrated alcohol mixed solutions,
2nd, obtain homogeneous solution under magnetic stirring, be subsequently adding 0.13mmolZnO, magnetic agitation 12min is suspended
Liquid；
3rd, suspension is added in the politef autoclave inner bag that volume is 50ml, in the pressure of 14MPa
Under be heated to 160 DEG C in baking oven, be incubated 10 hours.
4th, autoclave takes out reactant after naturally cooling to room temperature, and product is alternately each using deionized water and ethanol
Cleaning 4 times, collects precipitate using externally-applied magnetic field, product is transferred to 60 DEG C of the vacuum drying oven hour of drying 4 then, is obtained
Specific surface area is 70m2/g black ferroferric oxide Magnaglos.
The Rrinaceus earopaeuss shape needle-like ferroso-ferric oxide prepared by embodiment 3 carries out SEM observations and XRD analysis.
With reference to Fig. 1, knowable to SEM photograph, the yield of products therefrom is very big, and specific surface area is high, and granule is in needle-like and whole
Body distribution presents Rrinaceus earopaeuss shape, and aciculiform ferroso-ferric oxide length dimension is distributed in 1.0 microns.
With reference to Fig. 2, knowable to XRD (X-ray diffraction) spectrogram, products therefrom is ferroso-ferric oxide Fe3O4 phase crystal structures
(JCPDS card no.01-089-0688).
In sum, a kind of ferroso-ferric oxide of Rrinaceus earopaeuss shape needle-like high-specific surface area and its system are embodiments provided
Preparation Method.Possesses following beneficial effect：
1st, the embodiment of the present invention is by the use of anhydrous ferric chloride, sodium thiosulfate and carbamide as raw material, by hydro-thermal method and ZnO
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 obtained and compares table
Area is the ferroso-ferric oxide of 45～70m2/g, 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 response time is short, anti-
Answer process is simple, inexpensive.
3rd, embodiment of the present invention preparation process 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 not enough good, specific surface
The low problem of product.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any those familiar with the art the invention discloses technical scope in, technology according to the present invention scheme and its
Inventive concept equivalent or change in addition, should all be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of Rrinaceus earopaeuss shape needle-like ferroso-ferric oxide, it is characterised in that the preparation method comprises the steps：
Step one, under stirring, anhydrous ferric chloride, sodium thiosulfate and carbamide are mixed with solvent, be obtained mixing
Solution；
Step 2, the stirring after addition ZnO in mixed solution, are obtained suspension；
Suspension is heated to 150 DEG C～180 DEG C by step 3, in a high voltage state, is incubated 8～12 hours；
Step 4, it is cooled to cleaning after room temperature, dries, so as to the Fe 3 O 4 magnetic powder of needle-like is obtained.
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 sulfate, carbamide and solvent is respectively 1：1～2：2～4：10～14.
3. preparation method according to claim 2, it is characterised in that the ZnO in step 2 and anhydrous ferric chloride mole
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
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 two in liquid.
9. the ferroso-ferric oxide that prepared by the preparation method in a kind of employing claim 1-8 described in any one.
10. ferroso-ferric oxide according to claim 9, it is characterised in that the specific surface area of the ferroso-ferric oxide is 45
～70m2/g；The length dimension of the ferroso-ferric oxide is distributed in 0.1～2 micron.
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| CN201611267441.3A CN106495233B (en) | 2016-12-31 | 2016-12-31 | Hedgehog shape needle-like ferroso-ferric oxide and preparation method thereof |
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| CN106495233B CN106495233B (en) | 2017-10-24 |
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| CN111760569A (en) * | 2020-07-08 | 2020-10-13 | 合肥工业大学 | Composite photo-Fenton catalyst, preparation method and application |
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| CN111760569A (en) * | 2020-07-08 | 2020-10-13 | 合肥工业大学 | Composite photo-Fenton catalyst, preparation method and application |
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