CN104138743B - Method for preparing algae base magnetic activated carbon material and application of algae base magnetic activated carbon material - Google Patents
Method for preparing algae base magnetic activated carbon material and application of algae base magnetic activated carbon material Download PDFInfo
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- CN104138743B CN104138743B CN201410350570.3A CN201410350570A CN104138743B CN 104138743 B CN104138743 B CN 104138743B CN 201410350570 A CN201410350570 A CN 201410350570A CN 104138743 B CN104138743 B CN 104138743B
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Abstract
The invention discloses a method for preparing an algae base magnetic activated carbon material and the application of the algae base magnetic activated carbon material. According to the method, the preparing process and the magnetizing process of the activated carbon material are synchronized, a one-pot mode is adopted, drying, smashing, sieving and other preprocessing and activating processes are not needed, the steps of washing, drying and activator removing and the like are not needed after carbonization, a ferric salt solution is directly carbonized into ferroferric oxide nanometer particles in the preparing process, the ferroferric oxide nanometer particles are loaded to the surface of the activated carbon material, the operation is simple and easy to carry out, the preparing period is short, cost is low, mass production can be achieved, and due to the fact that the environmental pollutant of blue algae is utilized in the preparing process, dual environment benefits are achieved. The prepared algae base magnetic activated carbon material has large specific surface area and porosity, can efficiently adsorb methylene blue or methylene blue or bisphenol A in wastewater, has superparamagnetism and can be quickly separated from a liquid phase system after adsorption, and recycling is facilitated.
Description
Technical field
The invention belongs to environmental protection and comprehensive utilization of resources field, and in particular to one kind is with blue-green algae as containing carbon raw material
Material, by Process Duty ferroferric oxide nano granules such as immersion, charings the preparation side of algae base magnetic active carbon material is prepared
Method and obtained algae base magnetic active carbon material and application.
Background technology
Activated carbon makes it extensively apply in adsorbing domain due to larger specific surface area and loose structure.Although in absorption side
Face is with the obvious advantage, but activated carbon high-volume using due to some engineering roadblocks suffered hinder, such as recycle problem and
Regeneration cost problem etc..Therefore in the urgent need to seeking a kind of simple and easy to do method realizing the quick separating of activated carbon.If energy
It is enough that absorbent charcoal material imparting magnetic just can be realized into efficiently separating between activated carbon and waste water, consequently facilitating recycling.
At present, using natural material the research of magnetic active carbon material has been prepared for raw material, wherein, discarded stalk（Referring to：Open and pay
Shen;Liu Zhengang;Wu Jianzhi. the new technology of preparing C-Fe shell-core magnetic active carbon by utilizing waste biomasses. application for a patent for invention
Number: 200910080168.7.）, pericarp, bark（Referring to：Chen Baoliang;Chen Zaiming. a kind of magnetic biological carbon adsorbing material
Preparation method and its usage. application for a patent for invention number: 200910100973.1）Deng biological material through a series of process
The magnetic active carbon material for obtaining the oxide of load iron content is widely studied.But the preparation method in both patents, needs
Add alkaline-earth metal or reconcile PH and activate, and further carrying out washing treatment is also needed to after carbonizing, preparation process is more complicated,
Cost is greatly increased.
At the same time, recently as economic fast-developing, industrial scale expanding day, substantial amounts of Industry Waste
Water, sanitary sewage and agricultural irrigation water-break etc. enter lake, cause water body in lake obvious eutrophic state, nitrogen, phosphorus occur
Deng nutriment severe overweight, ultimately result in blue-green alga bloom and frequently break out, the productive life of people is caused to have a strong impact on, and work as
When Cells of Blue-green Algae ruptures or be dead, toxin will be released in water, mainly include hepatotoxin and neurotoxin, and they are known
Meeting invasion and attack liver and nerve toxin, to health produce harm.Therefore, need badly and lake blue algae is administered, but mesh
The improvement of front blue-green algae still suffers from many difficult problems, and situation allows of no optimist.If can be made full use of, huge economy can be produced
With environmental benefit.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method and application of algae base magnetic active carbon material, should
Preparation method with blue-green algae as raw material, simple without the need for pre-treatment and subsequent wash step in preparation process, manufacturing cycle
It is short, it is with low cost, it is possible to achieve a large amount of productions, and absorbent charcoal material prepared by the method has superparamagnetism, and magnetic is uniform,
With good absorption property.
It is an object of the invention to provide a kind of preparation method of algae base magnetic active carbon material, the preparation method includes following
Step：
A. blue-green algae is soaked into 12-24h in the solution of iron precursor；
B. it is dried after the blue-green algae after immersion is separated；
C. dried blue-green algae is carried out into high temperature carbonization, is cooled down, as algae base magnetic active carbon material.
A kind of preparation method of algae base magnetic active carbon material, the preparation method is comprised the following steps：
A. blue-green algae is soaked into 12-24h in iron precursor solution, the blue-green algae is 0.5- with the amount ratio of iron precursor solution
2g:6-60mL, and the concentration of iron precursor solution is 5-50mg/mL；
B. the blue-green algae after immersion is separated and is dried 4-8h after 30-80 DEG C；
C. by dried blue-green algae under nitrogen protection, charing 0.5-2h is carried out in 500-900 DEG C of high temperature, is cooled down, obtained final product
Algae base magnetic active carbon material.
The blue-green algae is 1g with the amount ratio of iron precursor solution:30mL, the concentration of the iron precursor solution is 10mg/mL.
Soak time in step a is 18h.
Baking temperature in step b is 50 DEG C, and drying time is 6h.
Carbonization temperature in step c is 800 DEG C, and carbonization time is 1h.
The iron precursor is iron ammonium oxalate, iron chloride or ferric nitrate.
With algae base magnetic active carbon material obtained in the preparation method of above-mentioned algae base magnetic active carbon material.
Methylene blue of the above-mentioned algae base magnetic active carbon material in waste water is removed, the application in methyl orange or bisphenol-A.
As the biological materials such as blue-green algae and stalk, pericarp, bark, also containing more carbon, and containing in a large number may be used
With the group of chelated metal ions, be easy to prepare metallic compound composite, therefore, it can using blue algae collecting process and as
One kind prepares magnetic active carbon material containing carbon source materials.Blue-green algae this environmental contaminants are effectively utilized simultaneously, with dual
Environmental benefit.
Algae base magnetic active carbon material prepared by the present invention has very high specific surface area and porous, can be to pollution
Thing is effectively adsorbed.With very strong magnetic, due to the ferroferric oxide nano granules that iron precursor is generated in carbonization process
The surface of algae is carried on securely, can be in use effectively separated and be reused.In materials process is prepared,
Can change and load on algae base magnetic active carbon material by the concentration of the iron precursor solution of change immersion blue-green algae and time
The amount of ferroferric oxide nano granules, the size in resulting materials aperture and specific surface area size.
It is an advantage of the current invention that：(1) what is proposed prepares algae base magnetic active carbon material by the use of blue-green algae as raw material
Thinking, successfully make use of this environmental contaminants product of blue-green algae, while adopting blue-green algae for raw material, abundance is with low cost,
Realize environmental benefit and economic benefit；(2) present invention achieves the preparation of absorbent charcoal material and the synchronization of tax magnetic process, adopt
Prepared by " one kettle way ", without the need for drying, pre-treatment and the activation process such as crush, sieve, and need not wash after charing, be dried to remove
The steps such as activator, magnetic-particle is prepared in preparation process without alkali lye regulation pH generation ferric hydroxide precipitates are added dropwise, and
It is directly to pass through iron salt solutions in carbonization process while preparing the magnetic-particle of nano shape, process is simple, excellent adsorption,
It is easily isolated.(3) magnetic active carbon material obtained in has unique network structure, and magnetic nanoparticle is connected with each other, blue-green algae
Inlay wherein, with larger specific surface area and preferable stability and absorption property, and the algae base magnetic active carbon for preparing
Material character is stablized, and with superparamagnetism, with magnet can quick separating be reclaimed from liquid-phase system by it, can repeat profit
With；(4) the algae base magnetic active carbon material for preparing has high efficiency of additive capability to pollutant, can be applicable to water environment pollution control
Field.
Description of the drawings
Fig. 1 is the SEM figures of algae base magnetic active carbon material in embodiment 1.
Fig. 2 is the hysteresis graph of algae base magnetic active carbon material in embodiment 1.
Fig. 3 is the XRD of algae base magnetic active carbon material in embodiment 1.
Fig. 4 is the SEM figures of algae base magnetic active carbon material in embodiment 2.
Fig. 5 is the hysteresis graph of algae base magnetic active carbon material in embodiment 2.
Fig. 6 is the SEM figures of algae base magnetic active carbon material in embodiment 3.
Fig. 7 is the hysteresis graph of algae base magnetic active carbon material in embodiment 3.
Fig. 8 is the curve map that algae base magnetic active carbon material adsorbs water Methylene Blue in embodiment 4.
Fig. 9 is the curve map of methyl orange in algae base magnetic active carbon material absorption water in embodiment 5.
Figure 10 is the curve map of bisphenol-A in algae base magnetic active carbon material absorption water in embodiment 6.
Specific embodiment
With reference to specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples.Institute
State method and be conventional method if no special instructions.The raw material can be obtained if no special instructions from open commercial sources.
The preparation of embodiment 1, algae base magnetic active carbon material
The blue-green algae collected from Taihu Lake is rinsed with running water.1g blue-green algaes are immersed in into the grass that 30mL concentration is 10mg/mL
18h in sour iron ammonium salt solution, centrifugation is dried 6h at 50 DEG C, tiles afterwards in crucible, in being put into atmosphere furnace, in nitrogen
1h is carbonized in 800 DEG C under protection, room temperature is then naturally cooled to, black powder, as algae base magnetic active carbon material is obtained.
Gained algae base magnetic active carbon material ESEM（SEM）And X-ray diffraction（XRD）Characterized, and used magnetic
Stagnant curve map reflects its magnetic size.Fig. 1 is the SEM figures of the algae base magnetic active carbon material.Fe as seen from Figure 13O4Nanometer
Particle is relatively evenly distributed in the surface of algae, and hole is relatively obvious.Fig. 2 is the B-H loop of the algae base magnetic active carbon material
Figure, its saturation magnetization is 15.60emu g-1, magnetic is preferable.Fig. 3 is the XRD spectrum of algae base magnetic active carbon material.Fig. 3
Show, the peak position (220), (311), (400), (422), (511) and (440) of the material respectively with pure Fe3O4Nano-particle phase
It coincide.This shows Fe3O4Nano-particle successfully loads to absorbent charcoal material surface.
The preparation of embodiment 2, algae base magnetic active carbon material
The blue-green algae collected from Taihu Lake is rinsed with running water.0.5g blue-green algaes are immersed in into the chlorine that 6mL concentration is 5mg/mL
Change ferrous solution in 12h, 4h is then dried at 30 DEG C, tile afterwards in crucible, in being put into atmosphere furnace, under nitrogen protection in
500 DEG C of charing 0.5h, then naturally cool to room temperature, obtain black powder, as algae base magnetic active carbon material.
Gained algae base magnetic active carbon material ESEM（SEM）Characterized, and reflected its magnetic with hysteresis graph
Property size.Fig. 4 is the SEM figures of algae base magnetic active carbon material.The Fe for generating as seen from Figure 43O4Nano particle it is less and compared with
It is little, and minimal amount is carried on the surface of algae.Fig. 5 is the hysteresis graph of the algae base magnetic active carbon material, and its saturated magnetization is strong
Spend for 10.77emu g-1, magnetic is weaker with respect to the magnetic of the material in embodiment 1.
The preparation of embodiment 3, algae base magnetic active carbon material
The blue-green algae collected from Taihu Lake is rinsed with running water.2g blue-green algaes are immersed in into the nitre that 60mL concentration is 50mg/mL
24h in sour ferrous solution, is then dried 8h at 80 DEG C, tiles afterwards in crucible, in being put into atmosphere furnace, under nitrogen protection in
900 DEG C of charing 2h, then naturally cool to room temperature, obtain black powder, as algae base magnetic active carbon material.
Gained algae base magnetic active carbon material ESEM（SEM）Characterized, and reflected its magnetic with hysteresis graph
Property size.Fig. 6 is the SEM figures of the algae base magnetic active carbon material.The Fe for generating as seen from Figure 63O4Nano particle it is more and
Size is larger, and almost all is covered in the surface of algae, and distribution of pores is not obvious.Fig. 7 is the algae base magnetic active carbon material
Hysteresis graph, its saturation magnetization is 15.91emu g-1, magnetic is most strong.
Embodiment 4, the experiment of the adsorption applications of algae base magnetic active carbon material
Take 0.2g L-1Algae base magnetic active carbon material obtained by the preparation of embodiment 1, input concentration is 20 mg L-1Asia
In methyl blue waste water, through 10 h, the absorption of absorbent charcoal material basically reaches balance, as shown in figure 8, adsorption efficiency is reachable
85.26%.After the completion of absorption, the algae base magnetic active carbon material can be isolated from liquid-phase system in seconds with magnet,
Separate after activation to methylene blue second adsorption, adsorption efficiency is up to 81.37%.Illustrate the algae base magnetic active carbon material to dye
Material has stronger absorption property and can reuse, and the application in terms of dye wastewater treatment is feasible.
Embodiment 5, the experiment of the adsorption applications of algae base magnetic active carbon material
Take 0.2g L-1Algae base magnetic active carbon material obtained by the preparation of embodiment 2, input concentration is 20 mg L-1First
In base orange waste water, through 10 h, the absorption of absorbent charcoal material basically reaches balance, as shown in figure 9, adsorption efficiency is reachable
66.59%.After the completion of absorption, the algae base magnetic active carbon material can be isolated from liquid-phase system in seconds with magnet,
Separate after activation to methyl orange second adsorption, adsorption efficiency is up to 62.64%.Illustrate the algae base magnetic active carbon material in dyestuff
Application in terms of wastewater treatment is feasible.
Embodiment 6, the experiment of the adsorption applications of algae base magnetic active carbon material
Take 0.2g L-1Algae base magnetic active carbon material obtained by the preparation of embodiment 3, input concentration is 20 mg L-1It is double
In phenol A waste water, through 10 h, the absorption of absorbent charcoal material basically reaches balance, and as shown in Figure 10, adsorption efficiency is reachable
59.16%.After the completion of absorption, the algae base magnetic active carbon material can be isolated from liquid-phase system in seconds with magnet,
Separate after activation to bisphenol-A second adsorption, adsorption efficiency is up to 56.25%.Illustrate the algae base magnetic active carbon material in organic matter
Application in terms of pollutant effluents process is feasible.
Claims (8)
1. a kind of preparation method of algae base magnetic active carbon material, it is characterised in that：The preparation method is comprised the following steps：
A. blue-green algae is soaked into 12-24h in iron precursor solution, the blue-green algae is 0.5-2g with the amount ratio of iron precursor solution: 6-
60mL, and the concentration of iron precursor solution is 5-50mg/mL；
B. the blue-green algae after immersion is separated and is dried 4-8h after 30-80 DEG C；
C. by dried blue-green algae under nitrogen protection, charing 0.5-2h is carried out in 500-900 DEG C of high temperature, is cooled down, obtain final product algae base
Magnetic activated carbons material.
2. a kind of preparation method of algae base magnetic active carbon material according to claim 1, it is characterised in that：The blue-green algae with
The amount ratio of iron precursor solution is 1g:30mL, the concentration of the iron precursor solution is 10mg/mL.
3. a kind of preparation method of algae base magnetic active carbon material according to claim 1, it is characterised in that：Step a
In soak time be 18h.
4. a kind of preparation method of algae base magnetic active carbon material according to claim 1, it is characterised in that：Step b
In baking temperature be 50 DEG C, drying time is 6h.
5. a kind of preparation method of algae base magnetic active carbon material according to claim 1, it is characterised in that：Step c
In carbonization temperature be 800 DEG C, carbonization time is 1h.
6. a kind of preparation method of algae base magnetic active carbon material according to claim 1, it is characterised in that：The iron precursor
For iron ammonium oxalate, iron chloride or ferric nitrate.
7. lived according to the algae base magnetic that the preparation method of any one algae base magnetic active carbon material in claim 1-6 is obtained
Property Carbon Materials.
8. algae base magnetic active carbon material according to claim 7 remove waste water in methylene blue, methyl orange or double
The application of phenol A.
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| CN107243323B (en) * | 2017-06-27 | 2020-05-08 | 王建军 | Magnetic bamboo fiber based activated carbon material and preparation method and application thereof |
| CN107215869A (en) * | 2017-06-28 | 2017-09-29 | 淮阴工学院 | A kind of biomass pyrolytic prepares magnetic active carbon and the method rich in synthesis gas gas |
| CN107337204A (en) * | 2017-06-28 | 2017-11-10 | 淮阴工学院 | Biomass pyrolytic, which is combined, prepares magnetic active carbon and the method rich in synthesis gas gas |
| CN108101142B (en) * | 2017-12-20 | 2021-07-09 | 华东交通大学 | Biomass charcoal ammonia nitrogen treatment material and preparation method thereof |
| CN108671886A (en) * | 2018-04-25 | 2018-10-19 | 中国矿业大学 | A kind of magnetic active carbon adsorbent and the preparation method and application thereof based on abandoned biomass |
| CN108439398A (en) * | 2018-05-30 | 2018-08-24 | 蒋春霞 | A method of preparing activated carbon using cyanobacteria |
| CN108840334A (en) * | 2018-09-03 | 2018-11-20 | 新奥石墨烯技术有限公司 | Modified activated carbon and its preparation method and application |
| CN109589913A (en) * | 2018-11-09 | 2019-04-09 | 广州润方环保科技有限公司 | A kind of magnetic bio charcoal and the preparation method and application thereof of quick removal methylene blue |
| CN109920999A (en) * | 2019-03-22 | 2019-06-21 | 广西师范大学 | A kind of cyanobacteria base anode material and preparation method thereof for lithium-sulfur cell |
| CN109876810B (en) * | 2019-03-26 | 2020-07-24 | 中国科学院生态环境研究中心 | Preparation method and application of magnetic microalgae-based biochar |
| CN109942699A (en) * | 2019-04-24 | 2019-06-28 | 南阳师范学院 | A method of fat-reducing peptide is prepared using bloom blue algae |
| CN110272085B (en) * | 2019-07-30 | 2023-02-24 | 江南大学 | Modified blue algae biochar composite material and application thereof in treatment of electroplating wastewater |
| CN111204817B (en) * | 2020-01-15 | 2021-06-01 | 李立欣 | Magnetic composite carbon prepared from harmful algal bloom and plastic and preparation method thereof |
| CN114477698B (en) * | 2022-02-11 | 2023-01-03 | 江南大学 | Application of ferric chloride mediated cyanobacteria-based biochar in removing zero-valent mercury in flue gas |
| CN115055161B (en) * | 2022-06-20 | 2023-10-13 | 南京林业大学 | Preparation method of magnetic activated carbon, magnetic activated carbon and application of magnetic activated carbon |
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| US8097185B2 (en) * | 2002-02-26 | 2012-01-17 | University Of Utah Research Foundation | Magnetic activated carbon particles for adsorption of solutes from solution |
| CN101298327B (en) * | 2008-01-24 | 2011-03-16 | 云南大学 | Blue algae bloom activated char and preparation thereof |
| CN101847481A (en) * | 2009-03-25 | 2010-09-29 | 中国科学院生态环境研究中心 | Novel process for preparing C-Fe shell-core magnetic active carbon by utilizing waste biomasses |
| CN101891188B (en) * | 2010-03-22 | 2012-06-27 | 中国科学院等离子体物理研究所 | Method for preparing nano active carbon spheres by using blue-green algae residue |
| CN101830460B (en) * | 2010-05-26 | 2012-05-30 | 中国科学技术大学苏州研究院 | Active carbon particles and preparation method thereof |
| CN103055813B (en) * | 2013-01-11 | 2014-12-31 | 福建工程学院 | Preparation method of formed magnetic black carbon |
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