CN106475040A - A kind of facile syntheesis of additive Mn iron oxide and its application - Google Patents
A kind of facile syntheesis of additive Mn iron oxide and its application Download PDFInfo
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- CN106475040A CN106475040A CN201611029191.XA CN201611029191A CN106475040A CN 106475040 A CN106475040 A CN 106475040A CN 201611029191 A CN201611029191 A CN 201611029191A CN 106475040 A CN106475040 A CN 106475040A
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 239000000654 additive Substances 0.000 title claims abstract description 48
- 230000000996 additive effect Effects 0.000 title claims abstract description 48
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 57
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000002086 nanomaterial Substances 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000011259 mixed solution Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 239000000243 solution Substances 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 229910052603 melanterite Inorganic materials 0.000 claims abstract description 7
- 239000000047 product Substances 0.000 claims description 20
- 238000005119 centrifugation Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 9
- 238000003837 high-temperature calcination Methods 0.000 claims description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 9
- 229910052573 porcelain Inorganic materials 0.000 claims description 9
- 238000001291 vacuum drying Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 6
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 5
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 5
- 239000012467 final product Substances 0.000 claims description 2
- 230000010355 oscillation Effects 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 7
- 239000000975 dye Substances 0.000 abstract description 6
- 239000002351 wastewater Substances 0.000 abstract description 6
- 238000000926 separation method Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- 238000011953 bioanalysis Methods 0.000 abstract description 2
- 238000009388 chemical precipitation Methods 0.000 abstract description 2
- 230000009881 electrostatic interaction Effects 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 239000011572 manganese Substances 0.000 description 40
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 23
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 23
- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 description 17
- 238000006243 chemical reaction Methods 0.000 description 14
- 238000002360 preparation method Methods 0.000 description 8
- 150000001336 alkenes Chemical class 0.000 description 6
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 6
- 239000006227 byproduct Substances 0.000 description 3
- 238000010025 steaming Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000005802 health problem Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002047 photoemission electron microscopy Methods 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
-
- 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
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Hydrology & Water Resources (AREA)
- Crystallography & Structural Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Compounds Of Iron (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of facile syntheesis of additive Mn iron oxide and its application, belong to absorption and the separation technology field of Wastewater Dyes；Under room temperature, PVP is added in the mixed solution of water and ethylene glycol, stirring and dissolving is to forming colourless transparent solution；By Mn (CH3COO)2·4H2O and FeSO4·7H2O is added in the mixed solution in the step (1), is stirred to being completely dissolved；By H2C2O4It is added in the mixed solution in the step (1), stirs to being completely dissolved；The solution obtained in step (2) and (3) slowly being mixed, being stirred at room temperature until mixing；The mixed solution obtained in step (4) is transferred in autoclave, and 12h is reacted at 120 DEG C；Composition is simple, and material non-toxic, inertia；The ferric oxide nano structure of additive Mn is mainly combined by electrostatic interaction with CR, compared to chemical precipitation method, bioanalysis etc., will not produce secondary pollution.
Description
Technical field
The present invention relates to the absorption of Wastewater Dyes and separation technology field, and in particular to a kind of letter of additive Mn iron oxide
It is easily-synthesized and its applies.
Background technology：
Congo red (CR) is a kind of important organic dyestuff, is widely used in many industry.But will be Congo red straight
Run in be put in natural stream networks and can cause serious environmental problem and health problem.It is currently used in the main side that CR is removed in water body
Method includes：Coagulation sedimentation, biological degradation method, ion-exchange, chemical oxidization method, nanof iotaltration and absorption method etc..At this
In a little methods, absorption method because its high efficiency, low cost, simple operation and other advantages and get most of the attention.The method is higher using having
Specific surface area or the adsorbent with surface specific functional groups, the method by physically or chemically adsorbing, to firm in waste water
Arnotto is effectively removed.The adsorbents such as activated carbon, nano composite material be all applied to Congo red in waste water remove, but
It is to fail to be widely used in wastewater treatment due to reasons such as high cost, the low or separation difficulties of the rate of adsorption.In recent years, have
The ferric oxide nano particles of special appearance are got most of the attention due to its larger specific surface and the higher ability for removing dyestuff.Certainly
In several iron oxide that so boundary is present, alpha-ferric oxide has most stable of thermodynamic state.Its stable chemical state and abundant
Reserves make which be expected to become a kind of cheap dye sorbent.A lot of scholars have carried out substantial amounts of in this field in recent years
Research work, is prepared for large quantities of alpha-ferric oxide nanostructures with different-shape, and has studied in detail its adsorption.
However, traditional alpha-ferric oxide nanostructure often absorption property is poor, therefore how to improve its absorption property just becomes restriction
The key factor of its later stage large-scale application.Recent correlative study shows that the doping of manganese is favorably improved which to dye molecule
And affinity and the adsorption capacity of heavy metal.Therefore, the alpha-ferric oxide of additive Mn in waste water Congo red be adsorbed with important
Researching value.
Content of the invention
For the problems referred to above, the technical problem to be solved in the present invention be provide a kind of facile syntheesis of additive Mn iron oxide and
Its application；Cost is relatively low, and raw material is easy to get, and absorption property is excellent, process is simple, can effectively reduce cost for wastewater treatment.
A kind of facile syntheesis of additive Mn iron oxide of the present invention, using the ferric oxide nano knot of hydro-thermal method synthesis additive Mn
Structure, concretely comprises the following steps：
1st, under room temperature, PVP is added in the mixed solution of water and ethylene glycol, stirring and dissolving is to colourless transparent solution；
2nd, by Mn (CH3COO)2·4H2O and FeSO4·7H2O is added in the mixed solution in the step (1), stirring
To being completely dissolved；
3rd, by H2C2O4It is added in the mixed solution in the step (1), stirs to being completely dissolved；
4th, the solution obtained in step (2) and (3) slowly being mixed, is stirred at room temperature until mixing；
5th, the mixed solution obtained in step (4) is transferred in autoclave, 12h is reacted at 120 DEG C；
6th, the product centrifugation that will be obtained in step (5), and distilled water is used, absolute ethanol washing for several times, is then placed
Dry in 60～80 DEG C of vacuum drying chamber；
7th, the desciccate obtained in step (6) is placed in porcelain boat, then in 400 DEG C of high-temperature calcinations in Muffle furnace
2h, obtains the ferric oxide nano structure of final product additive Mn.
Preferably, step 1 water and ethylene glycol volume ratio are 2:5.
Preferably, the step 2 mixing time 15-20 minute.
Preferably, the step 2Mn (CH3COO)2·4H2O and FeSO4·7H2The mol ratio of O is 1:4.
Preferably, the step 3 mixing time 15-20 minute.
Preferably, step 5 hydrothermal temperature is 200 DEG C, reaction time 12h；
Preferably, the step 6 centrifugation rotating speed is 9000r/min, baking temperature is 60 DEG C.
Preferably, when the step 7 is calcined, programming rate：1℃·min-1.
Application of the ferric oxide nano structure of additive Mn prepared by the method for the present invention in adsorbing separation CR, concrete process
Method is：The ferric oxide nano structure of additive Mn is added in the aqueous solution containing CR, water temperature is 25 DEG C, puts after ultrasonic 5min
In 25 DEG C of thermostats, constant temperature oscillation 24h, is centrifuged, and supernatant is removed.
Preferably, the initial total concentration of CR is 45.98～66.88mg/L in the control aqueous solution.
Beneficial effects of the present invention：Prepared by the ferric oxide nano structure of the additive Mn of the present invention convenient, and composition is simple, and material
Expect nontoxic, inertia；The ferric oxide nano structure of additive Mn is mainly combined by electrostatic interaction with CR, compared to chemical precipitation method,
Bioanalysis etc., will not produce secondary pollution；The ferric oxide nano structure of additive Mn has good adsorptivity to the CR in the aqueous solution
Can, the rate of adsorption is fast, and adsorbance is big, can be widely applied to the adsorbing separation of CR in waste water.
Description of the drawings
For ease of explanation, the present invention is embodied as and accompanying drawing is described in detail by following.
Fig. 1 is the X-ray powder diffraction figure of the ferric oxide nano structure of additive Mn prepared by embodiment 1；
Fig. 2 is the ferric oxide nano structure of additive Mn prepared by embodiment 1 to N under 77.5K2Adsorption desorption curve and
Size distribution curve；
Fig. 3 is the ferric oxide nano structure of additive Mn prepared by embodiment 1 at 25 DEG C to CR curve of adsorption kinetics figure；
Fig. 4 is the ferric oxide nano structure of additive Mn prepared by embodiment 1 at 25 DEG C to variable concentrations CR adsorption curve figure；
Specific embodiment
Below by specific embodiment, the present invention will be further elaborated, but the not limit to the scope of the present invention
System, on the basis of technical scheme, it is each that those skilled in the art are made by need not paying creative work
Modification or deformation are planted still within protection scope of the present invention.
Embodiment 1：
Reference picture 1- Fig. 4；The preparation method of the ferric oxide nano structure of additive Mn, using hydro-thermal method, with water/ethylene glycol/
PVP(PVP:Polyvinylpyrrolidone) mixed solution that constituted is solution, concretely comprises the following steps：
15g PVP is added in the mixed solution of 40ml water and 100ml ethylene glycol, stirring and dissolving, by 8mmol FeSO4·
7H2O+2mmol Mn(CH3COO)2·4H2O and 10mmol H2C2O4Above-mentioned mixed liquor is separately added into, is stirred to being completely dissolved, two
Person mixes, and equivalent is transferred in 7 autoclaves, and reactor is placed on temperature for isothermal reaction 12h, Zhi Houleng at 120 DEG C
But lower the temperature, reaction terminate after under the rotating speed of 6000r/min centrifugation 3min obtain product.By the product for obtaining respectively with steaming
Distilled water, for several times, the vacuum drying chamber for being then placed into 60 DEG C dries 12h to absolute ethanol washing.Products therefrom is placed in porcelain boat,
Then in 400 DEG C of high-temperature calcinations, 2 hours (atmosphere in Muffle furnace：Air；Programming rate：1℃·min-1), obtain additive Mn
Ferric oxide nano structure.The transmission electron microscope photo and high resolution transmission electron microscopy photo acceleration electricity of 200kV
It is pressed in what JEOL 2010 was obtained.Transmission electron microscope photo shows that the ferric oxide nano structure of the additive Mn has porous
Structure, its particle diameter are 3.51nm.Which is to N2Adsorption desorption curve, transmission electron micrograph and high-resolution transmitted electron aobvious
Micro mirror picture is respectively as shown in Fig. 2, Fig. 3 and Fig. 4.
The ferric oxide nano structure of the 6.4mg additive Mn of above-mentioned preparation is added in the 8ml aqueous solution containing CR, CR's
Concentration is 55.73mg/L, and after adsorbing 2h, the concentration of CR is 16.44mg/L, and clearance is 70.5%.
Embodiment 2：
The preparation method of the ferric oxide nano structure of additive Mn, using hydro-thermal method, with water/ethylene glycol/PVP (PVP:Poly- second
Alkene pyrrolidone) mixed solution that constituted is solution, concretely comprises the following steps：
15g PVP is added in the mixed solution of 40ml water and 100ml ethylene glycol, stirring and dissolving, by 9.5mmol
FeSO4·7H2O+0.5mmol Mn(CH3COO)2·4H2O and 10mmol H2C2O4Above-mentioned mixed liquor is separately added into, is stirred to complete
CL, the two mixing, equivalent are transferred in 7 autoclaves, and reactor is placed on temperature for isothermal reaction at 120 DEG C
12h, is cooled afterwards, reaction terminate after under the rotating speed of 6000r/min centrifugation 3min obtain product.The product that will be obtained
Thing uses distilled water respectively, and for several times, the vacuum drying chamber for being then placed into 60 DEG C dries 12h to absolute ethanol washing.By products therefrom
It is placed in porcelain boat, then in 400 DEG C of high-temperature calcinations, 2 hours (atmosphere in Muffle furnace：Air；Programming rate：1℃·min-1),
Obtain the ferric oxide nano structure of additive Mn.
Embodiment 3：
The preparation method of the ferric oxide nano structure of additive Mn, using hydro-thermal method, with water/ethylene glycol/PVP (PVP:Poly- second
Alkene pyrrolidone) mixed solution that constituted is solution, concretely comprises the following steps：
15g PVP is added in the mixed solution of 40ml water and 100ml ethylene glycol, stirring and dissolving, by 9mmol FeSO4·
7H2O+1mmol Mn(CH3COO)2·4H2O and 10mmol H2C2O4Above-mentioned mixed liquor is separately added into, is stirred to being completely dissolved, two
Person mixes, and equivalent is transferred in 7 autoclaves, and reactor is placed on temperature for isothermal reaction 12h, Zhi Houleng at 120 DEG C
But lower the temperature, reaction terminate after under the rotating speed of 6000r/min centrifugation 3min obtain product.By the product for obtaining respectively with steaming
Distilled water, for several times, the vacuum drying chamber for being then placed into 60 DEG C dries 12h to absolute ethanol washing.Products therefrom is placed in porcelain boat,
Then in 400 DEG C of high-temperature calcinations, 2 hours (atmosphere in Muffle furnace：Air；Programming rate：1℃·min-1), obtain additive Mn
Ferric oxide nano structure.
Embodiment 4：
The preparation method of the ferric oxide nano structure of additive Mn, using hydro-thermal method, with water/ethylene glycol/PVP (PVP:Poly- second
Alkene pyrrolidone) mixed solution that constituted is solution, concretely comprises the following steps：
15g PVP is added in the mixed solution of 40ml water and 100ml ethylene glycol, stirring and dissolving, by 8.5mmol
FeSO4·7H2O+1.5mmol Mn(CH3COO)2·4H2O and 10mmol H2C2O4Above-mentioned mixed liquor is separately added into, is stirred to complete
CL, the two mixing, equivalent are transferred in 7 autoclaves, and reactor is placed on temperature for isothermal reaction at 120 DEG C
12h, is cooled afterwards, reaction terminate after under the rotating speed of 6000r/min centrifugation 3min obtain product.The product that will be obtained
Thing uses distilled water respectively, and for several times, the vacuum drying chamber for being then placed into 60 DEG C dries 12h to absolute ethanol washing.By products therefrom
It is placed in porcelain boat, then in 400 DEG C of high-temperature calcinations, 2 hours (atmosphere in Muffle furnace：Air；Programming rate：1℃·min-1),
Obtain the ferric oxide nano structure of additive Mn.
Embodiment 5：
The preparation method of the ferric oxide nano structure of additive Mn, using hydro-thermal method, with water/ethylene glycol/PVP (PVP:Poly- second
Alkene pyrrolidone) mixed solution that constituted is solution, concretely comprises the following steps：
15g PVP is added in the mixed solution of 40ml water and 100ml ethylene glycol, stirring and dissolving, by 7.5mmol
FeSO4·7H2O+2.5mmol Mn(CH3COO)2·4H2O and 10mmol H2C2O4Above-mentioned mixed liquor is separately added into, is stirred to complete
CL, the two mixing, equivalent are transferred in 7 autoclaves, and reactor is placed on temperature for isothermal reaction at 120 DEG C
12h, is cooled afterwards, reaction terminate after under the rotating speed of 6000r/min centrifugation 3min obtain product.The product that will be obtained
Thing uses distilled water respectively, and for several times, the vacuum drying chamber for being then placed into 60 DEG C dries 12h to absolute ethanol washing.By products therefrom
It is placed in porcelain boat, then in 400 DEG C of high-temperature calcinations, 2 hours (atmosphere in Muffle furnace：Air；Programming rate：1℃·min-1),
Obtain the ferric oxide nano structure of additive Mn.
Embodiment 6：
The preparation method of the ferric oxide nano structure of additive Mn, using hydro-thermal method, with water/ethylene glycol/PVP (PVP:Poly- second
Alkene pyrrolidone) mixed solution that constituted is solution, concretely comprises the following steps：
15g PVP is added in the mixed solution of 40ml water and 100ml ethylene glycol, stirring and dissolving, by 7mmol FeSO4·
7H2O+3mmol Mn(CH3COO)2·4H2O and 10mmol H2C2O4Above-mentioned mixed liquor is separately added into, is stirred to being completely dissolved, two
Person mixes, and equivalent is transferred in 7 autoclaves, and reactor is placed on temperature for isothermal reaction 12h, Zhi Houleng at 120 DEG C
But lower the temperature, reaction terminate after under the rotating speed of 6000r/min centrifugation 3min obtain product.By the product for obtaining respectively with steaming
Distilled water, for several times, the vacuum drying chamber for being then placed into 60 DEG C dries 12h to absolute ethanol washing.Products therefrom is placed in porcelain boat,
Then in 400 DEG C of high-temperature calcinations, 2 hours (atmosphere in Muffle furnace：Air；Programming rate：1℃·min-1), obtain additive Mn
Ferric oxide nano structure.
Embodiment 7：
The preparation method of the ferric oxide nano structure of additive Mn, using hydro-thermal method, with water/ethylene glycol/PVP (PVP:Poly- second
Alkene pyrrolidone) mixed solution that constituted is solution, concretely comprises the following steps：
15g PVP is added in the mixed solution of 40ml water and 100ml ethylene glycol, stirring and dissolving, by 10mmol
FeSO4·7H2O and 10mmol H2C2O4Above-mentioned mixed liquor is separately added into, is stirred to being completely dissolved, the two mixing, equivalent are transferred to
In 7 autoclaves, reactor is placed on temperature for isothermal reaction 12h at 120 DEG C, is cooled afterwards, after reaction terminates
Under the rotating speed of 6000r/min, centrifugation 3min obtains product.The product for obtaining is used distilled water, absolute ethanol washing respectively
For several times, the vacuum drying chamber for being then placed into 60 DEG C dries 12h.Products therefrom is placed in porcelain boat, then in Muffle furnace in
400 DEG C of high-temperature calcinations, 2 hours (atmosphere：Air；Programming rate：1℃·min-1), obtain the ferric oxide nano structure of additive Mn.
Claims (10)
1. a kind of facile syntheesis of additive Mn iron oxide, it is characterised in that it synthesizes the ferric oxide nano of additive Mn using hydro-thermal method
Structure, concretely comprises the following steps：
(1) under room temperature, PVP is added in the mixed solution of water and ethylene glycol, stirring and dissolving is to colourless transparent solution；
(2) by Mn (CH3COO)2·4H2O and FeSO4·7H2O is added in the mixed solution in the step (1), is stirred to complete
CL；
(3) by H2C2O4It is added in the mixed solution in the step (1), stirs to being completely dissolved；
(4) solution obtained in step (2) and (3) slowly being mixed, is stirred at room temperature until mixing；
(5) mixed solution obtained in step (4) is transferred in autoclave, 12h is reacted at 120 DEG C；
(6) the product centrifugation that will be obtained in step (5), and distilled water is used, absolute ethanol washing for several times, is then placed into 60
Dry in～80 DEG C of vacuum drying chamber；
(7) desciccate obtained in step (6) is placed in porcelain boat, then in 400 DEG C of high-temperature calcination 2h in Muffle furnace, obtains
The ferric oxide nano structure of final product additive Mn.
2. the application after a kind of facile syntheesis of additive Mn iron oxide according to claim 1, it is characterised in that its place
Reason method is：The ferric oxide nano structure of additive Mn is added in the aqueous solution containing CR, water temperature is 25 DEG C, after ultrasonic 5min
Constant temperature oscillation 24h in 25 DEG C of thermostats is placed on, is centrifuged, supernatant is removed.
3. a kind of facile syntheesis of additive Mn iron oxide according to claim 1 and its application, it is characterised in that the step
Suddenly (1) water and ethylene glycol volume ratio are 2:5.
4. a kind of facile syntheesis of additive Mn iron oxide according to claim 1 and its application, it is characterised in that the step
Suddenly (2) mixing time 15-20 minute.
5. a kind of facile syntheesis of additive Mn iron oxide according to claim 1 and its application, it is characterised in that the step
Suddenly (2) Mn (CH3COO)2·4H2O and FeSO4·7H2The mol ratio of O is 1:4.
6. a kind of facile syntheesis of additive Mn iron oxide according to claim 1 and its application, it is characterised in that the step
Suddenly (3) mixing time 15-20 minute.
7. a kind of facile syntheesis of additive Mn iron oxide according to claim 1 and its application, it is characterised in that the step
Suddenly (5) hydrothermal temperature is 200 DEG C, reaction time 12h.
8. a kind of facile syntheesis of additive Mn iron oxide according to claim 1 and its application, it is characterised in that the step
Suddenly (6) centrifugation rotating speed is 9000r/min, and baking temperature is 60 DEG C.
9. a kind of facile syntheesis of additive Mn iron oxide according to claim 1 and its application, it is characterised in that the step
Suddenly when (7) calcine, programming rate：1℃·min-1.
10. the application after a kind of facile syntheesis of additive Mn iron oxide according to claim 2, it is characterised in that the control
In the aqueous solution processed, the initial total concentration of CR is 45.98～66.88mg/L.
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