CN109939643A - α-Fe2O3Adulterate the preparation method and applications of charcoal - Google Patents
α-Fe2O3Adulterate the preparation method and applications of charcoal Download PDFInfo
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Abstract
The present invention relates to a kind of α-Fe2O3Adulterate the preparation method and applications of charcoal.The present invention is directed to overcome the shortcomings of prior art iron oxide catalyzing and degrading pollutant, for the attainment of one's purpose, the technical solution of the present invention is as follows: charcoal is added in green vitriol solution first, NaOH solution, which is added dropwise, makes solution alkaline, then reacts under quick magnetic agitation, stands, washing precipitating, again overnight by the drying of gained precipitating, finally the solid high-temperature after drying is calcined, obtains reddish dark brown doping solid powder.α-Fe produced by the present invention2O3Charcoal is adulterated as catalyst and is applied to organic pollutant process field.The present invention improves absorption property, stability and the dispersibility of composite material and the Oxidative Degradation to organic dyestuff, raw material environment-protecting clean, cheap.
Description
Technical field
The invention belongs to sewage treatment fields, and in particular to a kind of α-Fe2O3Adulterate the preparation method and α-of charcoal
Fe2O3Adulterate the application of charcoal catalytic treatment organic pollutant.
Background technique
The substance that the most common bioanalysis of wastewater treatment is poor to biodegradability at present, relative molecular mass is from thousands of to tens of thousands of
Processing is more difficult, and chemical oxidation can improve the biodegradability of the pollutant by its direct mineralising or by oxidation, together
When also to having very big advantage in terms of the processing of the micro harmful chemical such as Environmental estrogen.Chemical oxidization method is to utilize chemistry
The strong oxidizing property of oxidant, by waste water inorganic matter and organic matter exhaustive oxidation at nontoxic small-molecule substance or gas, from
And achieve the purpose that processing.Common chemical oxidizing agent is O3、H2O2、ClO2Deng these oxidants are all strong oxygen under normal conditions
Agent can aoxidize Some Organic Pollutants in the solution.However, that but there are still oxidabilities is not strong and selective equal scarce
Point, it is difficult to meet the requirements.
Ferriferous oxide mainly includes the hydroxide of iron and the oxide of iron, is widely present in natural environment.Wherein, three
Two iron etc. are aoxidized due to cheap and easy to get, and there is more stable physicochemical properties, the extensive concern by researcher.Traditional
Iron oxide catalysis needs to be aided with the oxidizing substances such as hydrogen peroxide, ozone to achieve the purpose that catalytic degradation organic pollutant.Oxidation
Agent consumption is larger, and degradation speed is slow, is not able to satisfy industry degradation and requires.
Bloodstone (α-Fe2O3) it is a kind of environmental-friendly n-type semiconductor, have relatively narrow forbidden bandwidth (2.2 eV),
Corresponding excitation wavelength is 560 nm, can efficiently use 40% sunlight, is caused extensively in the field of optical-electronic-Fenton catalysis
General concern.However, its quantum efficiency is low, photocatalytic activity is restricted.In order to improve α-Fe2O3Photocatalytic activity, can be with
It takes α-Fe2O3The compound mode with other semiconductor materials, when the semiconductor material with different conduction bands and forbidden bandwidth
When being combined with each other, α-Fe not only can be improved2O3To the response range of light, and due to having delayed the compound of electron hole pair,
Catalyst is improved to the degradation capability of organic dyestuff.
Charcoal has biggish specific surface area, flourishing pore structure and oxygen-containing functional group abundant, these oxygen-containing officials
(such as carboxyl, phenolic hydroxyl group, acid anhydrides), which can be rolled into a ball, makes charcoal have good characterization of adsorption, therefore has stronger ion complexation energy
Power, can with the inorganic heavy metal ion in water, soil or deposit occur complexing and be adsorbed on surface and with water body,
Generation acts between heavy metal, organic pollutant in soil.
Doping is exactly by α-Fe2O3Pass through the methods of hydro-thermal or co-precipitation group with certain material with large specific surface area
It is combined, improves absorption property, stability and the dispersibility of composite material, in visible light action, improve α-Fe2O3
To the absorption and utilization rate of visible light.Light induced electron efficiently produces, and improves oxidation of the composite material to organic dyestuff
Degradation property.By α-Fe2O3α-Fe can be reduced with charcoal doping2O3In electron-hole recombinations, inhibit to reunite, realization follows
Ring utilizes, and improves catalyst to the degradation capability of organic dyestuff.
Summary of the invention
The invention aims to provide a kind of α-Fe2O3Adulterate the preparation method of charcoal, α-Fe obtained2O3Doping
Charcoal is applied in the processing of the organic pollutants such as treatment of domestic sewage advanced and Industrial Wastewater Treatment, and the prior art is overcome to aoxidize
The deficiency of iron catalyzing and degrading pollutant improves absorption property, stability and the dispersibility of composite material and to organic dyestuff
Oxidative Degradation.
In order to achieve the above object, a kind of α-Fe provided by the invention2O3Adulterate charcoal preparation method, successively include
Following steps:
(1) charcoal is added in green vitriol solution, the mass ratio of green vitriol and charcoal is 1:0.5
~3；
(2) NaOH solution is added dropwise under magnetic stirring, when solution alkaline and pH=9, stops that NaOH solution is added dropwise；
(3) 40 min are reacted under quick magnetic agitation, precipitate solution left standstill, outwell supernatant, are rushed repeatedly with deionized water
It washes, until the pH value of filtrate is in neutrality, and no longer contains sodium ion and sulfate ion；
(4) precipitating obtained by step 3 is put into drying box at 70 DEG C and is dried overnight；
(5) solid after drying is transferred in crucible, is placed in Muffle furnace at 600 DEG C and is calcined, finally obtained dark red
Brown adulterates solid powder.
Charcoal in above-mentioned steps 1 is made of orange peel, stalk or cornstalk.
The condition calcined in above-mentioned steps 5 are as follows: temperature program: 10 DEG C/min rises to 600 DEG C, keeps the temperature 120min, drops naturally
It warms to room temperature.
According to α-Fe made from above-mentioned preparation method2O3Adulterate application of the charcoal as catalyst treatment organic pollutant
The beneficial effects of the present invention are:
1) for the present invention using charcoal as precursor liquid, charcoal has biggish specific surface area, flourishing pore structure and abundant
Oxygen-containing functional group becomes the pollutant in cheap, efficient adsorbent removal or control environment, charcoal and active carbon phase
Than not needing to activate, energy consumption is greatly reduced, the wastes such as orange peel, stalk, cornstalk, which are realized, turns waste into wealth, environment-protecting clean；
2) present invention is in 600 DEG C of progress high-temperature calcinations.α-Fe2O3It adulterates with charcoal, with the raising of maturing temperature, is conducive to
The formation of charcoal central hole structure makes α-Fe so that the quantity of micropore increases2O3Biological carbon composite specific surface area is adulterated to increase
Greatly；But when temperature rises to 700 DEG C, temperature is too high to cause micropore hole wall ablation, and cavity collapses, and makes α-Fe2O3It is compound to adulterate charcoal
Material specific surface area reduces, therefore under 600 DEG C of calcination conditions, α-Fe2O3The specific surface area for adulterating biological carbon composite reaches
Maximum increases the active sites points of reaction, enhances its adsorption capacity to organic dyestuff, enhance its catalytic performance；
3) NaOH solution is added, adjusts solution ph, is conducive to iron oxide generation, iron oxide is catalytically decomposed hydrogen peroxide and generates hydroxyl
Free radical, raising photo-catalysis capability can also further speed up the circulation of iron ion and further increase α-Fe to realize2O3Work
Property.
4) of the invention by α-Fe2O3It is adulterated with charcoal, substantially increases α-Fe2O3Absorption property, stability and dispersion
Property.
5) α-Fe produced by the present invention2O3Adulterate the solid reagent that biological Pd/carbon catalyst is safety and stability, convenient transportation and valence
Lattice are cheap.
6) α-Fe produced by the present invention2O3Biological Pd/carbon catalyst is adulterated in degradation process, replaces ultraviolet light with sunlight,
Promote H while reducing energy consumption2O2Generation, further improve degradation efficiency.
7) present invention replaces Fe with solid phase iron ion catalyst2+, the generation of iron sludge is avoided, does not easily cause secondary dirt
Dye, and ensure that the stability of catalyst.
Detailed description of the invention
Fig. 1 is preparation flow figure of the invention；
Fig. 2 is α-Fe prepared by the embodiment of the present invention 12O3Adulterate the XRD diagram of charcoal photochemical catalyst powder；
Fig. 3 is α-Fe prepared by the embodiment of the present invention 12O3Adulterate the degradation curve of charcoal photocatalyst for degrading methylene blue
Figure.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, but embodiments of the present invention include
But it is not limited to the range of following embodiment expression.
A kind of α-Fe2O3Adulterate charcoal preparation method, successively the following steps are included:
1,0.1 g charcoal is added in green vitriol solution, the mass ratio of green vitriol and charcoal is
1:0.5 ~ 3；
2,3 mol/L NaOH solutions are added dropwise under magnetic stirring, when solution alkaline and pH=9, stop being added dropwise
NaOH solution；
3,40 min are reacted under quick magnetic agitation, precipitate solution left standstill, outwell supernatant, are rushed repeatedly with deionized water
It washes, until the pH value of filtrate is in neutrality, and no longer contains sodium ion and sulfate ion；
4, precipitating obtained by step 3 is put into drying box at 70 DEG C and is dried overnight；
5, the solid after drying is transferred in crucible, is placed in Muffle furnace at 600 DEG C and is calcined, finally obtain dark red palm fibre
Color adulterates solid powder, the condition of calcining are as follows: temperature program: 10 DEG C/min rises to 600 DEG C, keeps the temperature 120min, is naturally cooling to
Room temperature.
Embodiment:
A kind of α-Fe2O3Adulterate the preparation method of charcoal, the specific steps are as follows:
1,0.1 g charcoal is added in the green vitriol solution that 5ml concentration is 0.02 g/ml, seven hydrated sulfuric acids are sub-
The mass ratio of iron and charcoal is 1:1；
2,3 mol/L NaOH solutions are added dropwise under magnetic stirring, when solution alkaline and pH=9, stop being added dropwise
NaOH solution；
3,40 min are reacted under quick magnetic agitation, precipitate solution left standstill, outwell supernatant, are rushed repeatedly with deionized water
It washes, until the pH value of filtrate is in neutrality, and no longer contains sodium ion and sulfate ion；
4, precipitating obtained by step 3 is put into drying box at 70 DEG C and is dried overnight；
5, the solid after drying is transferred in crucible, is placed in Muffle furnace at 600 DEG C and is calcined, finally obtain dark red palm fibre
Color adulterates solid powder, the condition of calcining are as follows: temperature program: 10 DEG C/min rises to 600 DEG C, keeps the temperature 120min, is naturally cooling to
Room temperature.
Referring to table 1, modifying the mass ratio of green vitriol and charcoal in above-mentioned steps 1 is 1:2,2:1,1:3, is obtained
To embodiment 2 ~ 4.
Table 1: green vitriol and charcoal mass ratio in embodiment
| Embodiment | Mass ratio |
| 1 | 1:1 |
| 2 | 1:2 |
| 3 | 2:1 |
| 4 | 1:3 |
Fig. 1 is α-Fe2O3Adulterate the process flow of charcoal photochemical catalyst preparation method.
Fig. 2 is the XRD diagram that embodiment 1 prepares product.As can be seen from Figure 2 wherein Fig. 2 of sample prepared by the present embodiment
(a) the curve position at more each peak and peak type goodness of fit compared with PDF card (JCPDS33-0664) is high, prepared by determination
Sample is single pure phase α-Fe2O3.Fig. 2 (b) is homemade charcoal (BC), and the wideization degree of XRD is high, illustrates that sample is nothing
The amorphous substance of setting.Fig. 2 (c) is the XRD spectra of composite sample, is compared with Fig. 2 (a), finds α-Fe2O3Adulterate charcoal with
Pure α-Fe2O3Diffraction maximum it is almost the same, only intensity is opposite weakens, and this is mainly due to the additions of charcoal so that α-
Fe2O3Diffraction peak intensity weaken, cause spectral line occur amorphous peak packet.It is from XRD diagram it can also be seen that the knot of the material
Crystalline substance and object are mutually preferable.
Fig. 3 is product α-Fe prepared in embodiment2O3Adulterate charcoal degradation of methylene blue waste water from dyestuff curve graph.
Degradation process is as follows:
α-Fe prepared by embodiment 1-42O3Charcoal is adulterated as catalyst, taking 200 mL concentration is the methylene of 20 mg/L
Base indigo plant solution, adjusting its pH is 3, and prepared 0.1 g of catalyst is added and 6 ‰ H are added by several times2O21 mL of solution, in high-pressure mercury
Lamp, which provides, carries out 60 min of degradation experiment under visible light conditions.The mass ratio of green vitriol and charcoal chooses 1 respectively:
1,1:2,2:1,1:3,3:1.Filtered reaction solution is taken, measures absorbance when wavelength is 664 nm.
It can be seen that α-the Fe of embodiment preparation2O3Charcoal photochemical catalyst is adulterated when the degradation efficiency in solar irradiation 1h
Reach 75% or more, wherein embodiment 1-3 degradation efficiency reaches 90% or more.Embodiment 1 is optimum embodiment.
Claims (4)
1. a kind of α-Fe2O3Adulterate charcoal preparation method, successively the following steps are included:
(1) charcoal is added in green vitriol solution, the mass ratio of green vitriol and charcoal is 1:0.5
~3；
(2) NaOH solution is added dropwise under magnetic stirring, when solution alkaline and pH=9, stops that NaOH solution is added dropwise；
(3) 40 min are reacted under quick magnetic agitation, precipitate solution left standstill, outwell supernatant, are rushed repeatedly with deionized water
It washes, until the pH value of filtrate is in neutrality, and no longer contains sodium ion and sulfate ion；
(4) precipitating obtained by step 3 is put into drying box at 70 DEG C and is dried overnight；
(5) solid after drying is transferred in crucible, is placed in Muffle furnace at 600 DEG C and is calcined, finally obtained dark red
Brown adulterates solid powder.
2. α-Fe according to claim 12O3Adulterate the preparation method of charcoal, it is characterised in that:
The condition calcined in the step 5 are as follows: temperature program: 10 DEG C/min rises to 600 DEG C, keeps the temperature 120min, is naturally cooling to
Room temperature.
3. α-Fe according to claim 22O3Adulterate the preparation method of charcoal, it is characterised in that:
Charcoal in the step 1 is made of orange peel, stalk or cornstalk.
4. α-Fe made from preparation method as described in claim 12O3Charcoal is adulterated as catalyst treatment organic pollutant
Application.
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Cited By (9)
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| CN111018084A (en) * | 2019-12-23 | 2020-04-17 | 大连理工大学 | Biochar-goethite heterogeneous Fenton oxidation method applied to ofloxacin wastewater treatment |
| CN112547015A (en) * | 2020-12-07 | 2021-03-26 | 西安工业大学 | Preparation method and application of PEI modified biochar |
| CN113004902A (en) * | 2021-02-09 | 2021-06-22 | 西安工程大学 | Method for preparing biochar by co-pyrolyzing bentonite and metal |
| CN113145076A (en) * | 2021-05-13 | 2021-07-23 | 沈阳农业大学 | Preparation method of modified biochar and modified biochar |
| CN113426448A (en) * | 2021-06-04 | 2021-09-24 | 浙江科技学院 | Preparation method and application of novel biochar-based tar cracking catalyst |
| CN113634243A (en) * | 2021-07-08 | 2021-11-12 | 郑州大学 | Preparation and application of moxa-carbon ferric oxide |
| CN114177915A (en) * | 2021-11-30 | 2022-03-15 | 国网福建省电力有限公司电力科学研究院 | Preparation method and application of adsorption-catalysis bifunctional porous material |
| CN114515566A (en) * | 2022-01-18 | 2022-05-20 | 燕山大学 | Application of functional protein ferric oxide composite material in oxidation complex-breaking complex-state heavy metal |
| CN114832823A (en) * | 2022-05-13 | 2022-08-02 | 辽宁石油化工大学 | Ball-milled ferroferric oxide @ biochar cathode material as well as preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111018084A (en) * | 2019-12-23 | 2020-04-17 | 大连理工大学 | Biochar-goethite heterogeneous Fenton oxidation method applied to ofloxacin wastewater treatment |
| CN112547015A (en) * | 2020-12-07 | 2021-03-26 | 西安工业大学 | Preparation method and application of PEI modified biochar |
| CN113004902A (en) * | 2021-02-09 | 2021-06-22 | 西安工程大学 | Method for preparing biochar by co-pyrolyzing bentonite and metal |
| CN113145076A (en) * | 2021-05-13 | 2021-07-23 | 沈阳农业大学 | Preparation method of modified biochar and modified biochar |
| CN113145076B (en) * | 2021-05-13 | 2023-05-02 | 沈阳农业大学 | Preparation method of modified biochar and modified biochar |
| CN113426448A (en) * | 2021-06-04 | 2021-09-24 | 浙江科技学院 | Preparation method and application of novel biochar-based tar cracking catalyst |
| CN113634243A (en) * | 2021-07-08 | 2021-11-12 | 郑州大学 | Preparation and application of moxa-carbon ferric oxide |
| CN113634243B (en) * | 2021-07-08 | 2024-04-05 | 郑州大学 | Preparation and application of moxa-charcoal ferric oxide |
| CN114177915A (en) * | 2021-11-30 | 2022-03-15 | 国网福建省电力有限公司电力科学研究院 | Preparation method and application of adsorption-catalysis bifunctional porous material |
| CN114515566A (en) * | 2022-01-18 | 2022-05-20 | 燕山大学 | Application of functional protein ferric oxide composite material in oxidation complex-breaking complex-state heavy metal |
| CN114832823A (en) * | 2022-05-13 | 2022-08-02 | 辽宁石油化工大学 | Ball-milled ferroferric oxide @ biochar cathode material as well as preparation method and application thereof |
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