CN108046334B - 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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- CN108046334B CN108046334B CN201711411161.XA CN201711411161A CN108046334B CN 108046334 B CN108046334 B CN 108046334B CN 201711411161 A CN201711411161 A CN 201711411161A CN 108046334 B CN108046334 B CN 108046334B
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 46
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 33
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 32
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 10
- 239000004202 carbamide Substances 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 26
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- 235000019441 ethanol Nutrition 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 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
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 23
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 8
- 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
- 238000000034 method Methods 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 230000001681 protective effect Effects 0.000 abstract description 3
- 229910052742 iron Inorganic materials 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 150000002823 nitrates Chemical class 0.000 abstract 1
- 239000002086 nanomaterial Substances 0.000 description 16
- 238000002441 X-ray diffraction Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- 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
- 238000005516 engineering process Methods 0.000 description 6
- 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
- 238000000926 separation method 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
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 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
- 239000003054 catalyst Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007812 deficiency Effects 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
- 239000003344 environmental pollutant 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
- 239000002105 nanoparticle Substances 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
- 231100000719 pollutant Toxicity 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
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
Classifications
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- 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Iron (AREA)
- Catalysts (AREA)
Abstract
The invention discloses the preparation method and applications that a kind of nanometer is classified 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, in ethanol system, it is placed in autoclave, controls reaction temperature and time, by one-step synthesis, form nanometer and be classified spherical iron oxide (α ﹣ Fe2O3).First passage of the present invention controls template --- the amount of urea, the iron oxide of the unique classification hollow ball-shape structure of Lai Hecheng pattern, then goes 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 pollutant, provides a kind of easy, efficient method for the processing of organic pollutant, 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 technique
Now, industrialization development bring energy crisis and environmental pollution 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 because having oxidability strong, the small, mild condition of selectivity, it is without secondary pollution the features such as, it is considered to be most answer
With one of the pollution control technology of 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
Sending out wavelength is 600nm or so, compared with TiO2The area UV absorbing wavelength 380nm long, it is higher to the utilization rate of sunlight, close to 40%；
Secondly Fe2O3Nontoxic and pollution-free, low in cost and chemical stability is good, while nanometer Fe2O3With good and stable super hydrophilic
Performance, being conducive to polar substances in the infiltration on its surface has important application for improving the efficiency of heterogeneous catalytic reaction
Value.Nanometer Fe2O3In addition to common Fe2O3The characteristics of outside, since nanoparticle size is small, also have some special property
Matter, if any higher surface energy, large specific surface area, dispersibility is high, has the characteristics that good absorption and screen effect to visible light.
In recent years, with environmental problem and energy problem become increasingly conspicuous and the development of nanotechnology and photocatalysis technology, increasingly
More domestic and foreign scholars focus on research sight in the synthesis and photocatalytic applications of nano iron oxide.
Summary of the invention
It is an object of the invention to be directed to existing iron oxide (α ﹣ Fe2O3) deficiency existing for preparation method, pass through a step and closes
At formation nano iron oxide (α ﹣ Fe2O3), then FeOCl low temperature calcination is obtained into the mutually identical Fe of object2O3Nano material.
This synthetic method is low in cost, environmentally protective, can effectively remove organic pollutant, and removal rate is high, is the processing of organic pollutant
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:
Nanometer classification hollow ball-shape iron oxide (α ﹣ Fe2O3) preparation, including following raw material: urea, ferric nitrate, hydrochloric acid, second
Alcohol.
Specifically, the nanometer is classified hollow ball-shape iron oxide (α ﹣ Fe2O3) preparation method, comprising the following steps:
(1) urea is dissolved in the mixed solution (volume ratio of ethyl alcohol and hydrochloric acid is 12:1) of ethyl alcohol and hydrochloric acid, at room temperature
Stirring and dissolving；
(2) ferric iron source (Fe(NO is added in the solution that step (1) obtains3)3·9H2O), continue to stir；
(3) solution that step (2) obtains is poured into autoclave, be placed in 160 ~ 180 DEG C of 0.5 ~ 5 h of isothermal reaction into
Row isothermal reaction；
(4) by the solution furnace cooling after step (3) reaction, (60 ~ 90 DEG C) are centrifuged, wash, dried until water
Divide volatilization completely, obtains Fe2O3；
(5) Fe for being dried to obtain step (4)2O3It is placed in Muffle furnace, is calcined in air atmosphere, control heating speed
1 ~ 2 DEG C of min of rate-1, 400 ~ 600 DEG C of calcination temperature, 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 the above technical scheme2O3Nano material is shown good applied to the processing of organic pollutant
Removal effect.
Concrete application are as follows: organic pollutant to be processed is placed in light reaction container, then by prepared nano material
It puts into pollutant, 0.5 h of dark reaction；It is followed by condensed water, opens the natural light irradiation solution of experimental provision, and is stirred,
Reaction time controls within 2 h, the sampling of same time interval.
Remarkable advantage of the invention is:
(1) preparation method one-step synthesis: solvent-thermal method is used, by one-step synthesis, low temperature calcination can be obtained Fe2O3It receives
Rice material；Technological operation is simple, at low cost；
(2) pattern: being porous classification hollow ball-shape structure different from the material of other synthetic methods preparation, has biggish
Specific surface area shows significant effect to the processing of organic pollutant；
(3) environmentally protective: iron is cheap compared with other precious metal elements as a kind of environmentally friendly element, and source
Extensively, Fe obtained2O3Nano-porous materials show significant effect to the processing of organic pollutant.
Detailed description of the invention
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 figure of nanometer classification hollow ball-shape material；
Fig. 3 is Fe made from comparative example 2 of the present invention2O3The SEM figure of nanometer classification hollow ball-shape material；
Fig. 4 is Fe made from the embodiment of the present invention 12O3The SEM figure of nanometer classification hollow ball-shape material；
Fig. 5 is Fe made from the embodiment of the present invention 22O3The SEM figure of nanometer classification hollow ball-shape material；
Fig. 6 is Fe made from the embodiment of the present invention 32O3The SEM figure 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 objects, technical solutions and advantages of the application are further illustrated, makes the application
It is more clear clear.It should be appreciated that described herein, specific examples are only used to explain the present invention, is not used to limit this hair
It is bright.
Comparative example 1
Fe2O3The preparation of nanometer classification hollow ball-shape material:
(1) urea of 0.12 g is dissolved in the mixed solution of 0.5 mL hydrochloric acid (12 mol/L) and the ethyl alcohol of 6 mL, room
The lower stirring of temperature；
(2) Fe(NO of 1.212 g is added in above-mentioned solution3)3·9H2O stirs 0.5h；
(3) above-mentioned solution is poured into the autoclave of 100 mL, is placed in 170 DEG C of baking oven, 1 h of heat preservation will be anti-
Solution furnace cooling after answering, centrifuge separation, 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
To 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: shown in a), 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) urea of 0.36 g is dissolved in the mixed solution of 0.5 mL hydrochloric acid (12M) and the ethyl alcohol of 6 mL, is stirred at room temperature
It mixes；
(2) Fe(NO of 1.212 g is added in above-mentioned solution3)3·9H2O stirs 0.5h；
(3) above-mentioned solution is poured into the autoclave of 100 mL, is placed in 170 DEG C of baking oven, 1 h of heat preservation will be anti-
Solution furnace cooling after answering, centrifuge separation, 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
To 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: shown in b), 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) urea of 0.36 g is dissolved in the mixed solution of 0.5 mL hydrochloric acid (12M) and the ethyl alcohol of 6 mL, is stirred at room temperature
It mixes；
(2) Fe(NO of 1.212 g is added in above-mentioned solution3)3·9H2O stirs 0.5h；
(3) above-mentioned solution is poured into the autoclave of 100 mL, is placed in 170 DEG C of baking oven, 1 h of heat preservation will be anti-
Solution furnace cooling after answering, centrifuge separation, 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
To Fe2O3Nanometer classification hollow ball-shape material；
(5) by the Fe after drying2O3It is placed in Muffle furnace, is calcined in air atmosphere, control 2 DEG C of min of heating rate-1, 400 DEG C of calcination temperature, 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: shown in c), 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) urea of 0.36 g is dissolved in the mixed solution of 0.5 mL hydrochloric acid (12M) and the ethyl alcohol of 6 mL, is stirred at room temperature
It mixes；
(2) Fe(NO of 1.212 g is added in above-mentioned solution3)3·9H2O stirs 0.5h；
(3) above-mentioned solution is poured into the autoclave of 100 mL, is placed in 170 DEG C of baking oven, 1 h of heat preservation will be anti-
Solution furnace cooling after answering, centrifuge separation, 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
To Fe2O3Nano material；
(5) by the Fe after drying2O3It is placed in Muffle furnace, is calcined in air atmosphere, control 2 DEG C of min of heating rate-1, 500 DEG C of calcination temperature, 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: shown in d), 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) urea of 0.36 g is dissolved in the mixed solution of 0.5 mL hydrochloric acid (12M) and the ethyl alcohol of 6 mL, is stirred at room temperature
It mixes；
(2) Fe(NO of 1.212 g is added in above-mentioned solution3)3·9H2O stirs 0.5h；
(3) above-mentioned solution is poured into the autoclave of 100 mL, is placed in 170 DEG C of baking oven, 1 h of heat preservation will be anti-
Solution furnace cooling after answering, centrifuge separation, 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
To Fe2O3Nanometer classification hollow ball-shape material；
(5) by the Fe after drying2O3It is placed in Muffle furnace, is calcined in air atmosphere, control 2 DEG C of min of heating rate-1, 600 DEG C of calcination temperature, 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: shown in e), analysis is true
Earnest is mutually Fe2O3, scanning electron microscope is as shown in Figure 6.Calcination temperature is higher, and nano material hole is fewer, because warm
Degree is high, and hole is fused together.
Application examples
By comparative example 2 and the resulting Fe of embodiment 1 ~ 32O3Nanometer classification hollow ball-shape material has for removing organic pollutant
Steps are as follows for body:
(1) 30 mgL are prepared-1Ortho-nitrophenyl phenol solution, and be divided into identical 4 parts；
(2) by ortho-nitrophenyl phenol solution injection light reaction vessel, then Fe prepared by comparative example 2 and embodiment 1 ~ 32O3
Nanometer classification hollow ball-shape material is put into respectively in above-mentioned 4 parts of solution, and the Fe of investment is controlled2O3Concentration is 0.2 gL-1；
(3) (dark reaction) is reacted under dark condition stirs 0.5h, sampling；Lamp is opened after 0.5h, while being accessed cold
Condensate, stirring；
(4) since illumination timing be 0, be sampled by the different periods, be centrifuged, take supernatant, with it is ultraviolet-
Visible spectrophotometer surveys o-nitrophenol concentration, calculates the removal rate of different time sections o-nitrophenol.
According to the data of above application examples, 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
It is 99%.
Calcining assists in removing the impurity on sample, is formed simultaneously more hole, is conducive to degradation of contaminant；But it is warm
Du Taigao, some holes can be sintered fusion, be unfavorable for degrading instead, such as Fig. 6 (600 DEG C) and (500 DEG C) of Fig. 5 comparisons.Temperature is too
Formation that is low and being unfavorable for hole, degradation property is poor, if Fig. 4 (400 DEG C) is compared with Fig. 5 (500 DEG C).
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, is all covered by the present invention.
Claims (2)
1. the preparation method of a kind of nanometer of classification hollow ball-shape iron oxide, it is characterised in that: the following steps are included:
(1) urea is dissolved in the mixed solution of ethyl alcohol and hydrochloric acid, at room temperature stirring and dissolving；The mixing of the ethyl alcohol and hydrochloric acid is molten
In liquid, the volume ratio of ethyl alcohol and hydrochloric acid is 12:1；
(2) ferric iron source is added in the solution that step (1) obtains, continues to stir；The ferric iron source is
Fe(NO3)3·9H2O, concentration are the mol/L of 0.1 mol/L ~ 1.0；
(3) solution that step (2) obtains is poured into autoclave, in 160 ~ 180 DEG C of 0.5 ~ 5h of isothermal reaction；
(4) by step (3) reaction after solution furnace cooling, be centrifuged, wash and dry until moisture volatilize completely, obtain
To Fe2O3；
(5) Fe for being dried to obtain step (4)2O3It is placed in Muffle furnace, is calcined in air atmosphere, control heating rate, forge
Temperature and soaking time are burnt, the nanometer classification hollow ball-shape Fe is obtained2O3；
Above-mentioned heating rate is 1 ~ 2 DEG C of min-1, calcination temperature is 400 ~ 600 DEG C, and soaking time is 1 ~ 3 h.
2. 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.
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| CN102452687A (en) * | 2010-10-26 | 2012-05-16 | 南开大学 | Method for preparing porous nanometer alpha-Fe2O3 hollow spheres and application of hollow spheres to low-temperature alcohol sensitivity |
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| CN102452687A (en) * | 2010-10-26 | 2012-05-16 | 南开大学 | Method for preparing porous nanometer alpha-Fe2O3 hollow spheres and application of hollow spheres to low-temperature alcohol sensitivity |
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