CN108046334A - A kind of preparation method and applications of nanometer of classification hollow ball-shape iron oxide - Google Patents
A kind of preparation method and applications of nanometer of classification hollow ball-shape iron oxide Download PDFInfo
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- CN108046334A CN108046334A CN201711411161.XA CN201711411161A CN108046334A CN 108046334 A CN108046334 A CN 108046334A CN 201711411161 A CN201711411161 A CN 201711411161A CN 108046334 A CN108046334 A CN 108046334A
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 50
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004202 carbamide Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 27
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- 239000002086 nanomaterial Substances 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 17
- 235000019441 ethanol Nutrition 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 claims description 2
- 239000003344 environmental pollutant Substances 0.000 claims description 2
- 231100000719 pollutant Toxicity 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 24
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000012545 processing Methods 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 3
- 230000001681 protective effect Effects 0.000 abstract description 3
- 229910052742 iron Inorganic materials 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 150000002823 nitrates Chemical class 0.000 abstract 1
- 238000002441 X-ray diffraction Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 8
- IQUPABOKLQSFBK-UHFFFAOYSA-N 2-nitrophenol Chemical compound OC1=CC=CC=C1[N+]([O-])=O IQUPABOKLQSFBK-UHFFFAOYSA-N 0.000 description 7
- 230000015556 catabolic process Effects 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
- 229910002651 NO3 Inorganic materials 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 239000006227 byproduct Substances 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007783 nanoporous material Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000006228 supernatant Substances 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
- C01G49/06—Ferric oxide (Fe2O3)
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- B01J35/39—
-
- 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
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The invention discloses the preparation method and applications of a kind of nanometer of classification hollow ball-shape iron oxide, belong to material science and field of environment engineering.By the way that nine water ferric nitrates are dissolved in urea, ethanol system, it is placed in autoclave, controlling reaction temperature and time, by one-step synthesis, forms nanometer and be classified spherical iron oxide（α ﹣ Fe2O3）.First passage Control architecture agent of the present invention --- the amount of urea to synthesize the iron oxide of the unique classification hollow ball-shape structure of pattern, then is gone out by different temperature calcinations the iron oxide of the special pattern in different gaps；Source of iron is cheap, environmentally protective, can effectively remove organic pollution, provides a kind of easy, efficient method for the processing of organic pollution, with good economic efficiency and environmental benefit can carry out large-scale production and application.
Description
Technical field
The invention belongs to material science and field of environment engineering, and in particular to a kind of nanometer is classified hollow ball-shape iron oxide
Preparation method and applications.
Background technology
Now, the energy crisis and environmental pollution that industrialization development is brought have evolved into global problem, exploitation and selection
Effectively practical pollution control technology is the important topic of current environmental area.In numerous pollution control technologies, photocatalysis
Oxidation technology is because have the features such as oxidability is strong, and selectivity is small, mild condition, non-secondary pollution, it is considered to be most should
One of pollution control technology with prospect.On the other hand, solar energy is inexhaustible, cleanliness without any pollution, based on Solar use
Photocatalysis technology is our final goal.
Fe2O3It can be widely used in the fields such as sensor, magnetic material, medicine and catalysis.As photochemical catalyst, with TiO2
Etc. wide bandgap semiconductor materials compare, Fe2O3Biggest advantage be that band gap is about 2.2eV, the maximum of photoresponse swashs
Wavelength is sent out as 600nm or so, compared with TiO2UV areas absorbing wavelength 380nm long, it is higher to the utilization rate of sunlight, close to 40%；
Secondly Fe2O3Nontoxic and pollution-free, of low cost and chemical stability is good, while nanometer Fe2O3That stablizes with good is super hydrophilic
Performance is conducive to infiltration of the polar substances on its surface, for improving the efficiency of heterogeneous catalytic reaction, has important application
Value.Nanometer Fe2O3Except having common Fe2O3The characteristics of outside, since nanoparticle size is small, also with some special property
Matter, if any higher surface energy, large specific surface area, dispersiveness is high, has the characteristics that good absorption and screen effect to visible ray.
In recent years, with environmental problem and energy problem become increasingly conspicuous and the development of nanometer technology and photocatalysis technology, increasingly
More domestic and foreign scholars focus on research sight in the synthesis and photocatalytic applications of nano-sized iron oxide.
The content of the invention
It is an object of the invention to be directed to existing iron oxide（α ﹣ Fe2O3）It is insufficient existing for preparation method, it is closed by a step
Into formation nano-sized iron oxide（α ﹣ Fe2O3）, then FeOCl low temperature calcination obtained into the mutually identical Fe of object2O3Nano material.
This synthetic method is of low cost, environmentally protective, can effectively remove organic pollution, and removal rate is high, is the processing of organic pollution
Provide a kind of easy, efficient method, with good economic efficiency and environmental benefit.
To achieve the above object, the present invention adopts the following technical scheme that：
Nanometer classification hollow ball-shape iron oxide（α ﹣ Fe2O3）Preparation, including following raw material：Urea, ferric nitrate, hydrochloric acid, ethyl alcohol.
Specifically, the nanometer classification hollow ball-shape iron oxide（α ﹣ Fe2O3）Preparation method, comprise the following steps：
（1）Urea is dissolved in the mixed solution of ethyl alcohol and hydrochloric acid（The volume ratio of ethyl alcohol and hydrochloric acid is 12:1）In, it stirs at room temperature
Dissolving；
（2）In step（1）Obtained solution adds in ferric iron source（Fe（NO3）3·9H2O）, continue to stir；
（3）By step（2）Obtained solution is poured into autoclave, is placed in 160 ~ 180 DEG C of 0.5 ~ 5 h of isothermal reaction and is carried out perseverance
Temperature reaction；
（4）By step（3）Solution furnace cooling after reaction, is centrifuged, washs, dries（60~90 ℃）Until moisture is complete
Full volatilization, obtains Fe2O3；
（5）By step（4）The Fe being dried to obtain2O3Be placed in Muffle furnace, calcined in air atmosphere, control heating rate 1 ~
2 ℃·min-1, 400 ~ 600 DEG C of calcining heat, 1 ~ 3h of soaking time, obtain nanometer classification hollow ball-shape Fe2O3。
The Fe（NO3）3·9H2The concentration of O is the mol/L of 0.1 mol/L ~ 1.0.
The Fe prepared according to above-mentioned technical proposal2O3Nano material applied to the processing of organic pollution, is shown good
Removal effect.
It has particular application as：Pending organic pollution is placed in light reaction container, then by prepared nano material
It puts into pollutant, 0.5 h of dark reaction；Condensed water is followed by, opens the natural light irradiation solution of experimental provision, and is stirred,
Reaction time is controlled within 2 h, the sampling of same time interval.
The remarkable advantage of the present invention is：
（1）Preparation method one-step synthesis：Using solvent-thermal method, by one-step synthesis, low temperature calcination can obtain Fe2O3Nanometer material
Material；Technological operation is simple, at low cost；
（2）Pattern：Different from material prepared by other synthetic methods, it is porous classification hollow ball-shape structure, there is larger ratio table
Area shows significant effect to the processing of organic pollution；
（3）It is environmentally protective：Iron is cheap compared with other precious metal elements as a kind of environmentally friendly element, and derives from a wealth of sources,
Fe obtained2O3Nano-porous materials show significant effect to the processing of organic pollution.
Description of the drawings
Fig. 1 is comparative example 1 ~ 2 of the present invention, Fe made from embodiment 1 ~ 32O3The XRD diagram of nanometer classification hollow ball-shape material；
Fig. 2 is Fe made from comparative example 1 of the present invention2O3The SEM figures of nanometer classification hollow ball-shape material；
Fig. 3 is Fe made from comparative example 2 of the present invention2O3The SEM figures of nanometer classification hollow ball-shape material；
Fig. 4 is Fe made from the embodiment of the present invention 12O3The SEM figures of nanometer classification hollow ball-shape material；
Fig. 5 is Fe made from the embodiment of the present invention 22O3The SEM figures of nanometer classification hollow ball-shape material；
Fig. 6 is Fe made from the embodiment of the present invention 32O3The SEM figures of nanometer classification hollow ball-shape material；
Fig. 7 is the o-nitrophenol removal rate curve that application examples obtains.
Specific embodiment
With reference to the accompanying drawings and embodiments, the object, technical solution and advantage of the application are further illustrated, makes the application
It becomes apparent from understanding.It should be appreciated that specific embodiment described herein is not used to limit this hair only to explain the present invention
It is bright.
Comparative example 1
Fe2O3The preparation of nanometer classification hollow ball-shape material：
（1）The urea of 0.12 g is dissolved in 0.5 mL hydrochloric acid（12 mol/L）In the mixed solution of the ethyl alcohol of 6 mL, at room temperature
Stirring；
（2）The Fe of 1.212 g is added in above-mentioned solution（NO3）3·9H2O stirs 0.5h；
（3）Above-mentioned solution is poured into the autoclave of 100 mL, be placed in 170 DEG C of baking oven, after 1 h of heat preservation will react
Solution furnace cooling, centrifuge, and wash 3 times with ethyl alcohol and deionized water and obtain Fe2O3；
（4）By Fe2O3Nano material is placed in thermostatic drying chamber, dry under the conditions of 80 DEG C, until moisture volatilizees completely, is obtained
Fe2O3Nanometer classification hollow ball-shape material.
According to comparative example 1, by product X-ray diffraction analysis object phase, X-ray diffraction such as Fig. 1：a）Shown, analysis is true
Earnest is mutually Fe2O3；Scanning electron microscope such as Fig. 2.
Comparative example 2
Fe2O3The preparation of nanometer classification hollow ball-shape material：
（1）The urea of 0.36 g is dissolved in 0.5 mL hydrochloric acid（12M）In the mixed solution of the ethyl alcohol of 6 mL, stir at room temperature；
（2）The Fe of 1.212 g is added in above-mentioned solution（NO3）3·9H2O stirs 0.5h；
（3）Above-mentioned solution is poured into the autoclave of 100 mL, be placed in 170 DEG C of baking oven, after 1 h of heat preservation will react
Solution furnace cooling, centrifuge, and wash 3 times with ethyl alcohol and deionized water and obtain Fe2O3；
（4）By Fe2O3Nano material is placed in thermostatic drying chamber, dry under the conditions of 80 DEG C, until moisture volatilizees completely, is obtained
Fe2O3Nanometer classification hollow ball-shape material.
According to comparative example 2, by product X-ray diffraction analysis object phase, X-ray diffraction such as Fig. 1：b）Shown, analysis is true
Earnest is mutually Fe2O3；Scanning electron microscope is as shown in Figure 3.
Embodiment 1
Fe2O3The preparation of nanometer classification hollow ball-shape material：
（1）The urea of 0.36 g is dissolved in 0.5 mL hydrochloric acid（12M）In the mixed solution of the ethyl alcohol of 6 mL, stir at room temperature；
（2）The Fe of 1.212 g is added in above-mentioned solution（NO3）3·9H2O stirs 0.5h；
（3）Above-mentioned solution is poured into the autoclave of 100 mL, be placed in 170 DEG C of baking oven, after 1 h of heat preservation will react
Solution furnace cooling, centrifuge, and wash 3 times with ethyl alcohol and deionized water and obtain Fe2O3；
（4）By Fe2O3Nano material is placed in thermostatic drying chamber, dry under the conditions of 80 DEG C, until moisture volatilizees completely, is obtained
Fe2O3Nanometer classification hollow ball-shape material；
（5）By dried Fe2O3It is placed in Muffle furnace, is calcined in air atmosphere, 2 DEG C of min of control heating rate-1, forge
400 DEG C of temperature is burnt, 2 h of soaking time obtains Fe2O3Nano material.
According to embodiment 1, by product X-ray diffraction analysis object phase, X-ray diffraction such as Fig. 1：c）Shown, analysis is true
Earnest is mutually Fe2O3；Scanning electron microscope is as shown in Figure 4.
Embodiment 2
Fe2O3The preparation of nanometer classification hollow ball-shape material：
（1）The urea of 0.36 g is dissolved in 0.5 mL hydrochloric acid（12M）In the mixed solution of the ethyl alcohol of 6 mL, stir at room temperature；
（2）The Fe of 1.212 g is added in above-mentioned solution（NO3）3·9H2O stirs 0.5h；
（3）Above-mentioned solution is poured into the autoclave of 100 mL, be placed in 170 DEG C of baking oven, after 1 h of heat preservation will react
Solution furnace cooling, centrifuge, and wash 3 times with ethyl alcohol and deionized water and obtain Fe2O3；
（4）By Fe2O3Nano material is placed in thermostatic drying chamber, dry under the conditions of 80 DEG C, until moisture volatilizees completely, is obtained
Fe2O3Nano material；
（5）By dried Fe2O3It is placed in Muffle furnace, is calcined in air atmosphere, 2 DEG C of min of control heating rate-1, forge
500 DEG C of temperature is burnt, 2 h of soaking time obtains Fe2O3Nanometer classification hollow ball-shape material.
According to embodiment 2, by product X-ray diffraction analysis object phase, X-ray diffraction such as Fig. 1：d）Shown, analysis is true
Earnest is mutually Fe2O3；Scanning electron microscope is as shown in Figure 5.
Embodiment 3
Fe2O3The preparation of nanometer classification hollow ball-shape material：
（1）The urea of 0.36 g is dissolved in 0.5 mL hydrochloric acid（12M）In the mixed solution of the ethyl alcohol of 6 mL, stir at room temperature；
（2）The Fe of 1.212 g is added in above-mentioned solution（NO3）3·9H2O stirs 0.5h；
（3）Above-mentioned solution is poured into the autoclave of 100 mL, be placed in 170 DEG C of baking oven, after 1 h of heat preservation will react
Solution furnace cooling, centrifuge, and wash 3 times with ethyl alcohol and deionized water and obtain Fe2O3；
（4）By Fe2O3Nano material is placed in thermostatic drying chamber, dry under the conditions of 80 DEG C, until moisture volatilizees completely, is obtained
Fe2O3Nanometer classification hollow ball-shape material；
（5）By dried Fe2O3It is placed in Muffle furnace, is calcined in air atmosphere, 2 DEG C of min of control heating rate-1, forge
600 DEG C of temperature is burnt, 2 h of soaking time obtains Fe2O3Nano material.
According to embodiment 3, by product X-ray diffraction analysis object phase, X-ray diffraction such as Fig. 1：e）Shown, analysis is true
Earnest is mutually Fe2O3, scanning electron microscope is as shown in Figure 6.Calcining heat is higher, and nano material hole is fewer, because warm
Degree is high, and hole is merged.
Application examples
By the Fe of 1 ~ 3 gained of comparative example 2 and embodiment2O3Nanometer classification hollow ball-shape material is for removing organic pollution, specifically
Step is as follows：
（1）Prepare 30 mgL-1Ortho-nitrophenyl phenol solution, and be divided into identical 4 parts；
（2）By in ortho-nitrophenyl phenol solution injection light reaction vessel, then Fe prepared by comparative example 2 and embodiment 1 ~ 32O3Nanometer
Classification hollow ball-shape material is put into respectively in above-mentioned 4 parts of solution, controls the Fe of input2O3Concentration is 0.2 gL-1；
（3）It is reacted under dark condition（Dark reaction）Stir 0.5h, sampling；Lamp is opened after 0.5h, while accesses condensed water,
Stirring；
（4）Timing is 0 since illumination, is sampled by the different periods, centrifuges, takes supernatant, use ultraviolet-visible
Spectrophotometric measures o-nitrophenol concentration, calculates the removal rate of different time sections o-nitrophenol.
According to the data of above application example, o-nitrophenol removal rate curve as shown in Figure 7 is obtained.As can be seen from FIG. 7,
Fe made from comparative example 22O3The removal rate of nano material light degradation o-nitrophenol 2h is about 78%；Fe made from embodiment 12O3
The removal rate of nano material light degradation o-nitrophenol 2h is about 86%；Fe made from embodiment 32O3Nano material light degradation neighbour's nitre
The removal rate of base phenol 2h is about 96%；Fe made from embodiment 22O3The removal rate of nano material light degradation o-nitrophenol 2h is about
For 99%.
Calcining assists in removing the impurity on sample, more hole is formed simultaneously, beneficial to degradation of contaminant；It is but warm
Du Taigao, some holes can be sintered fusion, be unfavorable for degrading instead, such as Fig. 6（600℃）With Fig. 5（500℃）Comparison.Temperature is too
Formation that is low and being unfavorable for hole, degradation property is poor, such as Fig. 4（400℃）With Fig. 5（500℃）It compares.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification should all belong to the covering scope of the present invention.
Claims (8)
1. the preparation method of a kind of nanometer of classification hollow ball-shape iron oxide, it is characterised in that：Comprise the following steps：
（1）Urea is dissolved in the mixed solution of ethyl alcohol and hydrochloric acid, at room temperature stirring and dissolving；
（2）In step（1）Obtained solution adds in ferric iron source, continues to stir；
（3）By step（2）Obtained solution is poured into autoclave, carries out isothermal reaction；
（4）By step（3）Solution furnace cooling after reaction, be centrifuged, wash and dry until moisture volatilize completely, obtain
To Fe2O3；
（5）By step（4）The Fe being dried to obtain2O3It is placed in Muffle furnace, is calcined in air atmosphere, control heating rate, forge
Temperature and soaking time are burnt, obtains the nanometer classification hollow ball-shape Fe2O3。
2. the preparation method of nanometer classification hollow ball-shape iron oxide according to claim 1, it is characterised in that：Step（1）
In the ethyl alcohol and the mixed solution of hydrochloric acid, the volume ratio of ethyl alcohol and hydrochloric acid is 12:1.
3. the preparation method of nanometer classification hollow ball-shape iron oxide according to claim 1, it is characterised in that：Step（2）
The ferric iron source is Fe（NO3）3·9H2O, concentration are the mol/L of 0.1 mol/L ~ 1.0.
4. the preparation method of nanometer classification hollow ball-shape iron oxide according to claim 1, it is characterised in that：Step（3）
The isothermal reaction is specially：In 160 ~ 180 DEG C of 0.5 ~ 5h of isothermal reaction.
5. the preparation method of nanometer classification hollow ball-shape iron oxide according to claim 1, it is characterised in that：Step（4）
The drying temperature is 60 ~ 90 DEG C.
6. the preparation method of nanometer classification hollow ball-shape iron oxide according to claim 1, it is characterised in that：Step（5）
During middle calcining, heating rate is 1 ~ 2 DEG C of min-1, calcining heat is 400 ~ 600 DEG C, and soaking time is 1 ~ 3 h.
7. a kind of classification of the nanometer as made from claim 1-6 any one of them preparation methods hollow ball-shape iron oxide is answered
With, it is characterised in that：The nanometer classification hollow ball-shape iron oxide is used for the removal of organic pollution.
8. application according to claim 7, it is characterised in that：Pending organic pollution is placed in light reaction container
In, then prepared nano material put into pollutant, 0.5 h of dark reaction；Condensed water is followed by, opens experimental provision
Natural light irradiation solution, and stir, the reaction time is controlled within 2 h, the sampling of same time interval.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN112479262A (en) * | 2020-11-27 | 2021-03-12 | 重庆理工大学 | Method for preparing iron oxide and preparing pyruvic acid by catalyzing lactic acid |
| CN112479262B (en) * | 2020-11-27 | 2023-09-26 | 重庆理工大学 | Method for preparing ferric oxide and preparing pyruvic acid by catalyzing lactic acid |
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