CN108975306A - Aoxidize biomass porous carbon material of Fe2O3 doping and preparation method thereof and the application as magnetic material - Google Patents
Aoxidize biomass porous carbon material of Fe2O3 doping and preparation method thereof and the application as magnetic material Download PDFInfo
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- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 44
- 239000002028 Biomass Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000000696 magnetic material Substances 0.000 title claims abstract description 11
- 241000196252 Ulva Species 0.000 claims abstract description 47
- 238000007598 dipping method Methods 0.000 claims abstract description 20
- 230000003647 oxidation Effects 0.000 claims abstract description 19
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 19
- 238000004042 decolorization Methods 0.000 claims abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 11
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012298 atmosphere Substances 0.000 claims abstract description 7
- 239000011261 inert gas Substances 0.000 claims abstract description 7
- 238000003763 carbonization Methods 0.000 claims abstract description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 20
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 16
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 11
- 229960000583 acetic acid Drugs 0.000 claims description 10
- 239000012362 glacial acetic acid Substances 0.000 claims description 10
- KEQXNNJHMWSZHK-UHFFFAOYSA-L 1,3,2,4$l^{2}-dioxathiaplumbetane 2,2-dioxide Chemical compound [Pb+2].[O-]S([O-])(=O)=O KEQXNNJHMWSZHK-UHFFFAOYSA-L 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 229910006297 γ-Fe2O3 Inorganic materials 0.000 abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052799 carbon Inorganic materials 0.000 abstract description 6
- 210000003850 cellular structure Anatomy 0.000 abstract description 4
- 241000195493 Cryptophyta Species 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 6
- 239000012153 distilled water Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 229910001566 austenite Inorganic materials 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000003795 desorption Methods 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
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 229910052573 porcelain Inorganic materials 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- 229920001661 Chitosan Polymers 0.000 description 1
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000002122 magnetic nanoparticle Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004736 wide-angle X-ray diffraction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- 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]
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic 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
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention provides a kind of oxidation Fe2O3 doping biomass porous carbon material, spreads unchecked algae Enteromorpha as carbon source using east China sea area summer, is prepared by calcining carbonization under decolorization, iron nitrate solution dipping and atmosphere of inert gases.The biomass porous carbon material of the oxidation Fe2O3 doping (γ-Fe2O3@MSBC) have reticular structure, there is cellular structure abundant, higher specific surface area and saturation magnetic intensity, it can be used as magnetic material and have good application prospect in other fields.In addition, the porous carbon materials preparation process is simple and convenient, it is low in cost, and it is easily achieved tonnage grade industrialized production.
Description
Technical field
The invention belongs to porous carbon materials technical fields, and in particular to a kind of novel oxidized biomass porous carbon materials of Fe2O3 doping
Material and preparation method thereof and as magnetic material application.
Background technique
Porous carbon materials have flourishing pore structure, good chemical stability, biggish specific surface area, superior because of it
Acid and alkali-resistance and unique Electronic Transport of Two Benzene etc., in electrode material, absorption, separation, sensing, gas storage and catalyst carrier
There is potential application value in equal fields, are the polyporous materials in carbon nanomaterial family by height and extensive concern.
In porous carbon materials preparation, the selection of presoma focuses mostly in chemical reagent, such as phenolic resin, furtural, aromatic compound
Deng.In order to obtain more cheap preparation cost, traditional chemistry is replaced using the biomass or biomass castoff of low cost
Reagent is used to prepare multifunctional C material and has become research hotspot.
Porous carbon large specific surface area is widely used adsorbent material, in order to make porous carbon materials operation more just
Victory, it is more easy to separate and recover, it can be combined with magnetic nano-particle, magnetic porous carbon composite is made.It is existing
The source of carbon material is mainly glucose, chitosan and active carbon etc. in magnetic porous composite material, and following development trend is
By resource renewable in nature and cheap, such as sawdust, stalk, excrement of animals change give up into treasured, make carbon materials
The main source of material.In recent years, due to Global climate change, water eutrophication etc., ocean large ocean algae is caused
(Enteromorpha) green tide is broken out.A large amount of Enteromorpha floatings gather bank, block the fairway, while destroying marine ecosystems, seriously threaten
Inshore fishing, tourist industry development.
The present invention prepares novel porous carbon material as raw material using Enteromorpha, is able to achieve the recycling of Enteromorpha, will be it
Prevention and cure of pollution open up path.The biomass porous carbon material of oxidation Fe2O3 doping being prepared have cellular structure abundant, compared with
High specific surface area and saturation magnetic intensity, application value with higher.
Summary of the invention
It is an object of that present invention to provide a kind of novel oxidized biomass porous carbon materials of Fe2O3 doping, with duct abundant
Structure, higher specific surface area and saturation magnetic intensity, can be used as magnetic material and have good application prospect in other fields.
Another object of the present invention is the provision of the preparation method of the above-mentioned biomass porous carbon material of oxidation Fe2O3 doping, and
Its application as magnetic material.
To achieve the above object, the present invention adopts the following technical scheme:
It is a kind of aoxidize the biomass porous carbon material of Fe2O3 doping preparation method the Enteromorpha Jing Guo decolorization is impregnated in nitre
In sour ferrous solution, then calcining is carbonized to get the oxidation biomass porous carbon material of Fe2O3 doping is arrived under atmosphere of inert gases.
The preparation method of the above-mentioned biomass porous carbon material of oxidation Fe2O3 doping, specifically comprises the following steps:
1) clean, dry Enteromorpha is immersed in decolorising agent and becomes milk white gel in 65-85 DEG C of decolorization to Enteromorpha
Shape, it is cleaned after decolorization, dry to obtain Enteromorpha presoma (APEP)；
Wherein, decolorising agent is the mixed aqueous solution containing sodium hypochlorite and glacial acetic acid, and the concentration of sodium hypochlorite is in decolorising agent
0.10-0.15 mol L-1, the molar ratio of sodium hypochlorite and glacial acetic acid is 1:1；
2) Enteromorpha presoma is placed in 5 mol L of concentration 0.2-0.-1Iron nitrate solution in impregnate 12-36h, dipping terminates
By the dipping Enteromorpha (Fe for cleaning, being dried to obtain Fe2O3 doping3+@APEP)；
3) by the dipping Enteromorpha of Fe2O3 doping, 550-650 DEG C of calcining is carbonized 2- under atmosphere of inert gases in vacuum tube furnace
5h to get to oxidation the biomass porous carbon material of Fe2O3 doping (γ-Fe2O3@MSBC).The biomass porous carbon materials of oxidation Fe2O3 doping
Expect the biomass carbon skeleton with reticulated porous structures, iron oxide γ-Fe is distributed in surface2O3Nanoparticle.
Specifically, in step 1), clean, dry Enteromorpha is immersed in de- to obtain preferable decolorization effect
In toner, after mixing evenly, it is placed in air dry oven in 75 DEG C of constant temperature decolorization 1h；Aforementioned operation is repeated until Enteromorpha becomes
At milk white gel shape.It is further preferred that the concentration of sodium hypochlorite is in decolorising agent with 0.13 mol L in step 1)-1It is advisable.
Further, in order to obtain preferable dipping effect, in step 2, Enteromorpha presoma is placed in concentration 0.2mol
L-1Iron nitrate solution in impregnate and be advisable for 24 hours.
It is further preferred that the dipping Enteromorpha of Fe2O3 doping is calcined under atmosphere of inert gases in 600 DEG C in step 3)
Carbonization 2h is advisable.
The present invention provides the biomass porous carbon materials of oxidation Fe2O3 doping being prepared using above-mentioned preparation method.
Application the present invention also provides the above-mentioned biomass porous carbon material of oxidation Fe2O3 doping as magnetic material.
To efficiently use renewable resource, the marine algae Enteromorpha that the present invention is spread unchecked using Deposits in Eastern Coastal China summer is carbon
Source is carbonized through decoloration, metal salt solution dipping, calcining, prepares magnetic oxygenated Fe2O3 doping and have the novel of reticular structure
Biomass porous carbon material (γ-Fe2O3@MSBC), preparation process route is as shown in Figure 5.
Compared to the prior art, beneficial effects of the present invention are as follows:
The present invention is impregnated by simple decolorization, metal salt solution for the first time using Enteromorpha as raw material and calcining carbonization is prepared into
To the biomass porous carbon material of magnetic oxygenated Fe2O3 doping.The method of the present invention raw material is cheap and easy to get, and preparation process operation is convenient, is easy to
Realize tonnage grade industrialized production, and the biomass porous carbon material being prepared has cellular structure abundant, higher ratio
Surface area and higher magnetic intensity can be used as magnetic material and have good application prospect in other fields.
Detailed description of the invention
Fig. 1 is that embodiment 1 prepares gained γ-Fe2O3The stereoscan photograph of@MSBC；
Fig. 2 is that embodiment 1 prepares gained γ-Fe2O3The nitrogen adsorption of@MSBC/desorption isotherm figure；
Fig. 3 is that embodiment 1 prepares gained γ-Fe2O3The X ray diffracting spectrum of@MSBC；
Fig. 4 is that embodiment 1 prepares gained γ-Fe2O3The hysteresis loop figure of@MSBC；
Fig. 5 is preparation process route map of the present invention.
Specific embodiment
Technical solution of the present invention is further discussed in detail with reference to embodiments, but protection scope of the present invention
It is not limited thereto.
In following embodiments, the major experimental reagent and instrument used are listed below:
Sodium hypochlorite, glacial acetic acid, ferric nitrate (Fe (NO3)3·9H2O), GZX-9030 MBE type digital display air dry oven,
BSA22AS type single-deck electronic balance, vacuum tube furnace, Zeiss Ultra Plus field emission scanning electron microscope, D8
Advance diffractometer (Cu K α, λ=1.54), MicromeriticsTristar3000 adsorption instrument.
Embodiment 1
A kind of preparation method aoxidizing the biomass porous carbon material of Fe2O3 doping, specifically comprises the following steps:
1) it in coastal collection Enteromorpha, is dried for standby after cleaning；
2) 1.5 mL glacial acetic acid are taken, 2 g sodium hypochlorite are weighed, 195 mL distilled water are added and are made into decolorising agent.Then Enteromorpha is soaked
Bubble is sufficiently stirred in decolorising agent and is placed on constant temperature decoloration 1 hour in 75 DEG C of air dry ovens；Then repeat aforesaid operations until
Enteromorpha becomes milk white gel shape completely (general two to three times).3 ~ 4 times wash with distilled water, at this time most of starch,
Pectin is removed, the Enteromorpha after being decolourized, then vacuum dried acquisition Enteromorpha presoma (APEP), spare；
3) Enteromorpha presoma is placed in 0.2 mol L of concentration-1Ferric nitrate Fe (NO3)336h is impregnated in solution, after dipping
Wash with distilled water to remove unadsorbed metal ion, then vacuum dried is to obtain the dipping Enteromorpha (Fe of Fe2O3 doping afterwards3+@
APEP)；
4) the dipping Enteromorpha of Fe2O3 doping is placed in porcelain Noah's ark, then 600 DEG C of calcinings under nitrogen atmosphere in vacuum tube furnace
Carbonization 2 hours finally obtains the oxidation biomass porous carbon material γ-Fe of Fe2O3 doping2O3@MSBC。
Characterization experiment
To the above-mentioned biomass porous carbon material γ-Fe of the oxidation Fe2O3 doping being prepared2O3The structure and performance of@MSBC carries out table
Sign, it is specific as follows.
(1) scanning electron microscope characterizes: stereoscan photograph is as shown in Figure 1, preparation gained γ-Fe2O3@MSBC has netted knot
Structure, surface are dispersed with ferric oxide nano particles.The internal gutter of the biomass porous carbon material of oxidation Fe2O3 doping is intricate, hole
Diameter is not of uniform size, is greatly improved the specific surface area of material.
(2) nitrogen adsorption/desorption isotherm: the nitrogen adsorption of Fig. 2/desorption isotherm figure shows that typical IV type is bent
Line, and it is accompanied by apparent H2 type hysteresis loop.According to the desorption branch of curve, the ratio of material is calculated by BET and BJH formula
Surface area and pore volume are respectively 595.3 m2 g-1With 0.76 cm3 g-1, thus illustrate γ-Fe2O3@MSBC ratio with higher
Surface area and pore volume are conducive to provide more reaction site and big payload capacity for guest molecule.
(3) X ray diffracting spectrum: Fig. 3 is γ-Fe2O3The Wide angle X-ray diffraction figure of@MSBC, wherein 6 diffraction maximum difference
220,311,400,422,511 and 440 faces (JCPDS card: 89-5892) of corresponding maghemite phase.Should the result shows that: more
Successful growth has gone out iron oxide (γ-Fe in the carbon structure of hole2O3) nanoparticle.
(4) hysteresis loop: from the hysteresis loop of Fig. 4: γ-Fe2O3The remanent magnetism and coercivity of@MSBC is close to 0, says
The bright material is superparamagnetism.The material saturation magnetization is 26.7 emu g-1, have quick magnetic response to magnet, can expire
The needs of sufficient Magneto separate, to be used as magnetic material.
Embodiment 2
A kind of preparation method aoxidizing the biomass porous carbon material of Fe2O3 doping, specifically comprises the following steps:
1) clean, dry Enteromorpha is immersed in decolorising agent, is sufficiently stirred and is placed on constant temperature decoloration in 65 DEG C of air dry ovens
Processing, until Enteromorpha becomes milk white gel shape, 4 times wash with distilled water after decolorization, then vacuum dried acquisition
Enteromorpha presoma (APEP)；
Wherein, decolorising agent is the mixed aqueous solution containing sodium hypochlorite and glacial acetic acid, and the concentration of sodium hypochlorite is 0.15 in decolorising agent
mol L-1, the molar ratio of sodium hypochlorite and glacial acetic acid is 1:1；
2) Enteromorpha presoma is placed in 0.3 mol L of concentration-1Iron nitrate solution in impregnate for 24 hours, distilled water is used after dipping
Cleaning is to remove unadsorbed metal ion, then the vacuum dried dipping Enteromorpha (Fe for obtaining Fe2O3 doping3+@APEP)；
3) the dipping Enteromorpha of Fe2O3 doping is placed in porcelain Noah's ark, then 550 DEG C of calcinings under nitrogen atmosphere in vacuum tube furnace
Be carbonized 5h, finally obtains the oxidation biomass porous carbon material of Fe2O3 doping (γ-Fe2O3@MSBC).
Embodiment 3
A kind of preparation method aoxidizing the biomass porous carbon material of Fe2O3 doping, specifically comprises the following steps:
1) clean, dry Enteromorpha is immersed in decolorising agent, is sufficiently stirred and is placed on constant temperature decoloration in 85 DEG C of air dry ovens
Processing, until Enteromorpha becomes milk white gel shape, 3 times wash with distilled water after decolorization, vacuum dried acquisition again
Enteromorpha presoma (APEP)；
Wherein, decolorising agent is the mixed aqueous solution containing sodium hypochlorite and glacial acetic acid, and the concentration of sodium hypochlorite is 0.10 in decolorising agent
mol L-1, the molar ratio of sodium hypochlorite and glacial acetic acid is 1:1；
2) Enteromorpha presoma is placed in 0. 5 mol L of concentration-1Iron nitrate solution in impregnate 12h, with distillation after dipping
Water is cleaned to remove unadsorbed metal ion, then the vacuum dried dipping Enteromorpha (Fe for obtaining Fe2O3 doping3+@APEP)；
3) the dipping Enteromorpha of Fe2O3 doping is placed in porcelain Noah's ark, then 650 DEG C of calcinings under nitrogen atmosphere in vacuum tube furnace
Be carbonized 3h, finally obtains the oxidation biomass porous carbon material of Fe2O3 doping (γ-Fe2O3@MSBC).
To sum up, the present invention prepares the biomass of reticulated porous structures using the Enteromorpha that Eastern China seas summer spreads unchecked as raw material
Carbon material, and growth in situ magnetic ferric oxide nano particles.This method is simple to operation, low in cost, it is easy to accomplish tonnage grade
Industrialized production.Preparation gained magnetic composite has cellular structure abundant, higher specific surface area and magnetic intensity, can use
Make magnetic material and has good application prospect in other fields.
It should be noted last that: technical solution of the present invention that the above embodiments are only illustrative and not limiting is any right
The equivalent replacement and do not depart from the modification of spirit and scope of the invention or locally replace that the present invention carries out, should all cover in this hair
Within bright protective scope of the claims.
Claims (7)
1. a kind of preparation method for aoxidizing the biomass porous carbon material of Fe2O3 doping, which is characterized in that by the waterside Jing Guo decolorization
Tongue fur is impregnated in iron nitrate solution, and then calcining carbonization is biomass porous to get oxidation Fe2O3 doping is arrived under atmosphere of inert gases
Carbon material.
2. aoxidizing the preparation method of the biomass porous carbon material of Fe2O3 doping according to claim 1, which is characterized in that including such as
Lower step:
1) clean, dry Enteromorpha is immersed in decolorising agent and becomes milk white gel in 65-85 DEG C of decolorization to Enteromorpha
Shape, it is cleaned after decolorization, dry to obtain Enteromorpha presoma；
Wherein, decolorising agent is the mixed aqueous solution containing sodium hypochlorite and glacial acetic acid, and the concentration of sodium hypochlorite is in decolorising agent
0.10-0.15 mol L-1, the molar ratio of sodium hypochlorite and glacial acetic acid is 1:1；
2) Enteromorpha presoma is placed in 5 mol L of concentration 0.2-0.-1Iron nitrate solution in impregnate 12-36h, dipping terminates
By the dipping Enteromorpha for cleaning, being dried to obtain Fe2O3 doping；
3) the dipping Enteromorpha of Fe2O3 doping is carbonized 2-5h in 550-650 DEG C of calcining under atmosphere of inert gases to get oxidation is arrived
The biomass porous carbon material of Fe2O3 doping.
3. aoxidizing the preparation method of the biomass porous carbon material of Fe2O3 doping according to claim 2, which is characterized in that step 1)
In, the concentration of sodium hypochlorite is 0.13 mol L in decolorising agent-1。
4. aoxidizing the preparation method of the biomass porous carbon material of Fe2O3 doping according to claim 2, which is characterized in that step 2
In, Enteromorpha presoma is placed in 0.2 mol L of concentration-1Iron nitrate solution in impregnate for 24 hours.
5. aoxidizing the preparation method of the biomass porous carbon material of Fe2O3 doping according to claim 2, which is characterized in that step 3)
In, by the dipping Enteromorpha of Fe2O3 doping in 600 DEG C of calcinings carbonization 2h under atmosphere of inert gases.
6. the biomass porous carbon material of oxidation Fe2O3 doping being prepared using any preparation method of claim 1 to 5.
7. application of the oxidation biomass porous carbon material of Fe2O3 doping as magnetic material described in claim 6.
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