CN101780952A - Method for preparing loading functional oxide porous carbon - Google Patents

Method for preparing loading functional oxide porous carbon Download PDF

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Publication number
CN101780952A
CN101780952A CN201010133489A CN201010133489A CN101780952A CN 101780952 A CN101780952 A CN 101780952A CN 201010133489 A CN201010133489 A CN 201010133489A CN 201010133489 A CN201010133489 A CN 201010133489A CN 101780952 A CN101780952 A CN 101780952A
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chloride
acetate
ch3coo
nitrate
porous carbon
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刘庆雷
朱申敏
张荻
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Shanghai Jiaotong University
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Shanghai Jiaotong University
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Priority to CN201010133489A priority Critical patent/CN101780952A/en
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Priority to PCT/GB2011/050621 priority patent/WO2011117657A2/en
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02CCAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00Capture or disposal of greenhouse gases
    • Y02C20/40Capture or disposal of greenhouse gases of CO2

Abstract

The invention relates to a method for preparing a loading functional oxide porous carbon, which belongs to the technical field of carbon material. The method comprises the following steps of: selecting biomass material, and carbonizing at the temperature of 400-1000 DEG C in vacuum or on inert condition; preparing porous carbon by a physical activating or chemical activating process according to the requirement on the pore structure by the carbonized porous carbon; immersing the porous carbon into a precursor solution of an element M, cleaning many times with distilled water, and drying; roasting on the porous carbon at the temperature of 300-1000 DEG C in vacuum or on inert atmosphere, and then the active carbon of the loading functional oxide MxOy is prepared. The active carbon of the loading functional oxide MxOy prepared by the invention has the special pore structure of the biomass, also has the functions performed by the oxides, and has important application value in water treatment, hydrogen storage, photocatalysis, fuel cells and relevant fields.

Description

The preparation method of loading functional oxide porous carbon
Technical field
That the present invention relates to is a kind of preparation method of carbon materials technical field, is specially a kind of preparation method of loading functional oxide porous carbon.
Background technology
Porous charcoal is a kind of important carbon materials, has pore texture prosperity, characteristics that specific surface area is high, has very strong adsorptive power for inorganic or organic substance and colloidal solid etc. in gas, the solution.Therefore, traditional porous charcoal mainly is used to gas or water treatment.Active carbon adsorption mainly is a porosity characteristic of utilizing gac, makes objectionable impurities in gas or the solution be attracted to activated carbon surface and is removed.Wherein, gac can be divided into physical adsorption and chemisorption to the absorption of pollutent, and is wherein most based on physical adsorption.In recent years, a lot of scholars more and more pay attention to the effect of activated carbon surface functional group, by utilizing strong acid or highly basic activated carbon surface are carried out chemical modification, thereby improve the chemisorption of gac.
Yet there is great potential in the application of porous charcoal in some high-new industrial circles.Because advantages such as porous charcoal has porosity height, good corrosion resistance, electrochemical stability is good, high-temperature stability is good; can be used as catalyzer and other functional material carriers, therefore have application potential widely at industrial circles such as environment protection, water treatment and energy storage.In recent years, a lot of scholars more and more pay attention to the modification of porous charcoal, by to porous charcoal surface and internal surface loading functional organic or inorganic particle or film, realize the application of porous charcoal in fields such as environment protection, water treatment and energy storage.
Find that through literature search as Chinese patent CN1695797, name is called: " preparation method of absorbent charcoal loading titanium dioxide photocatalyst " to prior art.What this technical characterstic was to adopt is Metalorganic Chemical Vapor Deposition, comprising: absorbent charcoal carrier is carried out nitric acid treatment, be downloaded in the quartz reactor that fills gac, with TiO by the titanium precursor thing of rare gas element with heating 2Deposit to activated carbon surface, under protection of inert gas, calcine again.This technology can realize the TiO of porous carbon material 2Load, yet the TiO of prepared material 2Only be carried on the porous charcoal surface, do not enter inside, hole, and this technical matters output is lower.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of preparation method of loading functional oxide porous carbon is provided.The porous charcoal carrier of the present invention's preparation not only has the pattern of biomass fineness and optional, controlled vesicular structure, and effectively realizes the load of functional oxide compound on porous charcoal carrier hole surface, realizes the integrated of pattern, vesicular structure and oxide compound function.Simultaneously, raw material sources are wide, and are with low cost, and the technique means versatility is good.
The present invention is achieved by the following technical solutions, the present invention makes full use of the pattern of the fineness that natural plant material has and meticulous vesicular structure characteristics, utilize the abundant non-metallic element C of vegetable material institute inherent, through non-oxidation pyroprocessing, dip treating and assembling, secondary non-oxidation pyroprocessing, prepare porous carbon material with biomass graded porous fine structure and loading functional oxide.
The present invention includes following steps:
The first step is selected biological material, under vacuum or the inert conditions and carbonization in 400-1000 ℃ of temperature range;
Second step according to the needs to pore structure, was adopted physically activated or chemical activating process with the porous charcoal of gained after the carbonization, prepared porous charcoal;
Described physically activated employing is at CO 2, in water vapour or the air atmosphere, 300-1000 ℃ following thermal treatment 1-12 hour; Described chemical activation adopts activator KOH, ZnCl 2Or Fe (NO 3) 2With the raw material of wood-charcoal material by weight 1: (0.1-5) behind the uniform mixing, in vacuum or inert atmosphere 300-1000 ℃ following thermal treatment 1-12 hour.
The porous charcoal of the 3rd step with gained is impregnated in the precursor solution of element M, cleans for several times drying with distilled water;
The 4th step promptly got the loading functional oxide M with porous charcoal 300-1000 ℃ of roasting under vacuum or inert atmosphere of gained xO yGac.
Described loading functional oxide M xO y, wherein: M is one or more among metal Ti, Fe, Ni, Co, Zn, Cu, Mn, Zr, Cr, Al, Sn, Y, Ce, La, Pb, Pd, Ru, Sr, In, Ga, Bi and the nonmetal Si, and X is 1,2 or 3, and Y is 1,2,3 or 4.
Described biological material refers to a kind of in agricultural waste material or the waterplant material, and wherein agricultural waste material refers to one or more in stalk, rice husk, shell, cotton fibre, fruit stone, straw, corn ear, wood chip, bamboo and the wild rice stem leaf; The waterplant material refers to a kind of in algae and the Herba Eichhorniae.
Described element M is an organic or inorganic salt, refers to a kind of in nitrate, chlorate, vitriol, acetate and the alkoxide of element M.
Described element M refers to iron nitrate [Fe (NO especially 3) 3], Xiao Suangu [Co (NO 3) 2], nickelous nitrate [Ni (NO 3) 2], zinc nitrate [Zn (NO 3) 2], cerous nitrate [Ce (NO 3) 3], cupric nitrate [Cu (NO 3) 2], aluminum nitrate [Al (NO 3) 3], Yttrium trinitrate [Y (NO 3) 3], manganous nitrate [Mn (NO 3) 2], zirconium nitrate [Zr (NO 3) 2], chromium nitrate [Cr (NO 3) 3], lanthanum nitrate [La (NO 3) 3], nitric acid tin [Sn (NO 3) 2], lead nitrate [Pb (NO 3) 2], Palladous nitrate [Pd (NO 3) 2], nitric acid ruthenium [Ru (NO 3) 3], strontium nitrate [Sr (NO 3) 2], indium nitrate [In (NO 3) 3], gallium nitrate [Ga (NO 3) 3], Bismuth trinitrate [Bi (NO 3) 3], titanous chloride [TiCl 3], titanium tetrachloride [TiCl 4], zinc chloride [ZnCl 2], Cerium II Chloride [CeCl 3], cupric chloride [CuCl 2], aluminum chloride [AlCl 3], tin tetrachloride [SnCl 4], Yttrium trichloride [YCl 3], Manganous chloride tetrahydrate [MnCl 2], zirconium chloride [ZrCl 2], chromium chloride [CrCl 3], iron(ic) chloride [FeCl 3], iron protochloride [FeCl 2], nickelous chloride [NiCl 2], cobalt chloride [CoCl 2], Lanthanum trichloride [LaCl 3], lead chloride [PbCl 3], Palladous chloride [PdCl 2], ruthenium chloride [RuCl 3], strontium chloride [SrCl 2], indium chloride [InCl 3], gallium chloride [GaCl 3], bismuth chloride [BiCl 3], titanium sulfate [Ti (SO 4) 2], Tai-Ace S 150 [Al 2(SO 4) 3], zinc sulfate [ZnSO 4], ferrous sulfate [FeSO 4], chromium sulphate [Cr 2(SO 4) 3], single nickel salt [NiSO 4], copper sulfate [CuSO 4], palladous sulfate [Pd 2(SO 4) 3], cerous sulfate [Ce 2(SO 4) 3], indium sulfate [In 2(SO 4) 3], manganous sulfate [MnSO 4], gallium sulfate [Ga 2(SO 4) 3], bismuth sulfate [Bi 2(SO 4) 3], acetate [Zn (CH 3COO) 2], cerous acetate [Ce (CH 3COO) 3], venus crystals [Cu (CH 3COO) 2], aluminum acetate [Al (CH 3COO) 3], yttium acetate [Y (CH 3COO) 3], manganous acetate [Mn (CH 3COO) 2], zirconium acetate [Zr (CH 3COO) 2], ferrous acetate [Fe (CH 3COO) 2], ironic acetate [Fe (CH 3COO) 3], nickelous acetate [Ni (CH 3COO) 2], cobaltous acetate [Co (CH 3COO) 2], lanthanum acetate [La (CH 3COO) 3], lead acetate [Pb (CH 3COO) 2], acid chloride [Pd (CH 3COO) 2], ruthenium acetate [Ru (CH 3COO) 3], strontium acetate [Sr (CH 3COO) 2], indium acetate [In (CH 3COO) 3], acetate gallium [Ga (CH 3COO) 3], bismuth acetate [Bi (CH 3COO) 3], tetrabutyl titanate [C 16H 36O 4Ti], metatitanic acid [H 2Ti 2O 3], isopropyl titanate [C 12H 28O 4Ti] and tetraethoxy [C 8H 20O 4Si] in a kind of.
Described functional oxide M xO y, refer to TiO 2, Fe 3O 4, Fe 2O 3, FeO, NiO, Ni 2O 3, Co 3O 4, CoO, ZnO, CuO, MnO, MnO 2, ZrO 2, Cr 2O 3, CrO 2, Al 2O 3, SnO 2, Y 2O 3, CeO 2, La 2O 3, PbO, PbO 2, PdO, PdO 2, RuO 2, RuO 4, SrO, SrO 2, In 2O 3, Ga 2O 3, Bi 2O 3And SiO 2In one.
The present invention makes full use of the porous charcoal that the characteristics preparation of natural plants material in pattern, material and structure has meticulous pattern of biomass and constructional feature, and be template parcel or loading functional oxide compound with it, satisfy the application of porous carbon material in new functional area.The characteristics of vegetable material are that pattern is meticulous different, all are rich in the C elemental composition, and have the classifying porous fine structure of micron order to the nano level uniqueness.The present invention is according to the application direction difference, and preferred configuration, the vegetable material that structure is useful are starting material, in conjunction with physics/chemical activation method, can prepare the porous charcoal of the meticulous pattern of hereditary vegetable material, and its pore structure is adjustable controlled by the charing of non-oxygen atmosphere.Porous charcoal with different-shape and Different Pore Structures is a template, utilize it to enrich the duct, surface or hole inside with functional oxide in-situ is grown and wrapped up or be carried on porous charcoal can make the advanced porous charcoal base functional composite material that has both functional oxide compound advantage and porous charcoal structural advantages.The present invention is starting material with the biomass of occurring in nature, inherits its classifying porous meticulous pattern and structure, and its component that makes a variation realizes the synchronous heredity of pattern, 26S Proteasome Structure and Function.
The present invention can obtain to have the porous charcoal of meticulous pattern of starting material and structure by the control to preferred, the thermal decomposition process and the activating process of material of vegetable origin, and Controlled Pore Structure.At different industrial application targets, can on preferred porous charcoal template, further introduce functional oxide compound, thus preparation porous charcoal base functional composite material.In this invention preparation process, can effectively control the aperture and the pore distribution of porous carbon material.Gac in the traditional sense often has a large amount of micropores since the aperture less (<2nm), thereby be difficult to realize the assembling or the load of functional oxide material.The present invention is by the preferred biomass materials kind, and the mesopore/macropore ratio by technology controlling and process realization porous carbon material has guaranteed that porous charcoal had both had bigger specific surface area, and the mesopore/macropore ratio of higher proportion is arranged again.The present invention adopts, and biomass with low cost, wide material sources are starting material, can be applied to fields, forward position such as environment protection, water treatment, photochemical catalysis and energy storage.
Embodiment
Below embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment one
Choosing dry rice husk is starting material, and clean dry is also pulverized, and its heat-up rate with 1 ℃/minute under vacuum condition is risen to 400 ℃ of carbonizations, is incubated 6 hours.The porous charcoal of gained after the carbonization is pulverized the back mix with 0.1: 1 mass ratio with KOH, the heat-up rate with 5 ℃/minute under nitrogen protection atmosphere rises to 1000 ℃ of activation 1 hour.Porous charcoal after the activation be impregnated in 12h in the Titanium Nitrate solution, filter to take out and clean for several times drying with distilled water.Impregnated porous charcoal is risen to 1000 ℃ and be incubated 0.5 hour with 20 ℃/minute heat-up rate under nitrogen protection atmosphere, can make load TiO 2Porous carbon composite material.This matrix material can reach pure TiO to the catalytic effect of methylene blue 23 efficiency-timed fruits of material.
Embodiment two
Choosing the drying wheat stalk is starting material, and clean dry is also pulverized, and its heat-up rate with 10 ℃/minute under vacuum condition is risen to 1000 ℃ of carbonizations, is incubated 0.5 hour.The porous charcoal of gained after the carbonization is pulverized back and ZnCl 2Mix with 3: 1 mass ratioes, the heat-up rate with 10 ℃/minute under nitrogen protection atmosphere rises to 650 ℃ of activation 6 hours.Porous charcoal after the activation be impregnated in 12h in the nitric acid solution of tin, filter to take out and clean for several times drying with distilled water.Impregnated porous charcoal is risen to 400 ℃ and be incubated 3 hours with 10 ℃/minute heat-up rate under nitrogen protection atmosphere, can make load SnO 2Porous carbon composite material.
Embodiment three
Choosing dry coconut husk is starting material, and clean dry is also pulverized, and its heat-up rate with 20 ℃/minute under vacuum condition is risen to 1000 ℃ of carbonizations, is incubated 2 hours.The porous charcoal of gained after the carbonization is pulverized the back mix with 3: 1 mass ratioes with KOH, the heat-up rate with 10 ℃/minute under nitrogen protection atmosphere rises to 300 ℃ of activation 12 hours.Porous charcoal after the activation be impregnated in 12h in the nickel nitrate solution, filter to take out and clean for several times drying with distilled water.Impregnated porous charcoal is risen to 400 ℃ and be incubated 6 hours with 1 ℃/minute heat-up rate under nitrogen protection atmosphere, can make the porous carbon composite material of load NiO.
Embodiment four
Choosing dry bamboo is starting material, and clean dry is also pulverized, and its heat-up rate with 5 ℃/minute under vacuum condition is risen to 650 ℃ of carbonizations, is incubated 3.5 hours.The porous charcoal of gained after the carbonization is pulverized the back mix with 3: 1 mass ratioes with KOH, the heat-up rate with 5 ℃/minute under nitrogen protection atmosphere rises to 900 ℃ of activation 5 hours.Porous charcoal after the activation be impregnated in 12h in the ironic acetate solution, filter to take out and clean for several times drying with distilled water.Impregnated porous charcoal is risen to 300 ℃ and be incubated 6 hours with 1 ℃/minute heat-up rate under nitrogen protection atmosphere, can make load Fe 3O 4Porous carbon composite material.This matrix material has superparamagnetism, under the effect of externally-applied magnetic field, can separate from solution, can be used for the returnability water purification material.
Embodiment five
Choosing dry cotton fibre is starting material, and clean dry is also pulverized, and its heat-up rate with 15 ℃/minute under vacuum condition is risen to 650 ℃ of carbonizations, is incubated 4 hours.The porous charcoal of gained after the carbonization is pulverized the back mix with 5: 1 mass ratioes with KOH, the heat-up rate with 15 ℃/minute under nitrogen protection atmosphere rises to 900 ℃ of activation 3 hours.Porous charcoal after the activation be impregnated in 12h in the venus crystals solution, filter to take out and clean for several times drying with distilled water.Impregnated porous charcoal is risen to 600 ℃ and be incubated 1 hour with 10 ℃/minute heat-up rate under nitrogen protection atmosphere, can make the porous carbon composite material of Supported CuO.

Claims (8)

1. the preparation method of a loading functional oxide porous carbon is characterized in that, comprises the steps:
The first step is selected biological material, under vacuum or the inert conditions and carbonization in 400-1000 ℃ of temperature range;
Second step according to the needs to pore structure, was adopted physically activated or chemical activating process with the porous charcoal of gained after the carbonization, prepared porous charcoal;
The porous charcoal of the 3rd step with gained is impregnated in the precursor solution of element M, cleans for several times drying with distilled water;
The 4th step promptly got the loading functional oxide M with porous charcoal 300-1000 ℃ of roasting under vacuum or inert atmosphere of gained xO yGac.
2. the preparation method of loading functional oxide porous carbon according to claim 1 is characterized in that, described physically activated employing is at CO 2, in water vapour or the air atmosphere, 300-1000 ℃ following thermal treatment 1-12 hour.
3. the preparation method of loading functional oxide porous carbon according to claim 1 is characterized in that, described chemical activation adopts activator KOH, ZnCl 2Or Fe (NO 3) 2With the raw material of wood-charcoal material by weight 1: (0.1-5) behind the uniform mixing, in vacuum or inert atmosphere 300-1000 ℃ following thermal treatment 1-12 hour.
4. the preparation method of loading functional oxide porous carbon according to claim 1 is characterized in that, described loading functional oxide M xO y, wherein: M is one or more among metal Ti, Fe, Ni, Co, Zn, Cu, Mn, Zr, Cr, Al, Sn, Y, Ce, La, Pb, Pd, Ru, Sr, In, Ga, Bi and the nonmetal Si, and x is 1,2 or 3, and Y is 1,2,3 or 4.
5. the preparation method of loading functional oxide porous carbon according to claim 1 is characterized in that, described functional oxide M xO y, refer to TiO 2, Fe 3O 4, Fe 2O 3, FeO, NiO, Ni 2O 3, Co 3O 4, CoO, ZnO, CuO, MnO, MnO 2, ZrO 2, Cr 2O 3, CrO 2, Al 2O 3, SnO 2, Y 2O 3, CeO 2, La 2O 3, PbO, PbO 2, PdO, PdO 2, RuO 2, RuO 4, SrO, SrO 2, In 2O 3, Ga 2O 3, Bi 2O 3And SiO 2In one.
6. the preparation method of loading functional oxide porous carbon according to claim 1, it is characterized in that, described biological material, refer to a kind of in agricultural waste material or the waterplant material, wherein agricultural waste material refers to one or more in stalk, rice husk, shell, cotton fibre, fruit stone, straw, corn ear, wood chip, bamboo and the wild rice stem leaf; The waterplant material refers to a kind of in algae and the Herba Eichhorniae.
7. the preparation method of loading functional oxide porous carbon according to claim 1 is characterized in that, described element M is an organic or inorganic salt, refers to a kind of in nitrate, chlorate, vitriol, acetate and the alkoxide of element M.
8. according to the preparation method of claim 1 or 7 described loading functional oxide porous carbons, it is characterized in that, described element M refers to iron nitrate [Fe (NO3) 3], Xiao Suangu [Co (NO3) 2], nickelous nitrate [Ni (NO3) 2], zinc nitrate [Zn (NO3) 2], cerous nitrate [Ce (NO3) 3], cupric nitrate [Cu (NO3) 2], aluminum nitrate [Al (NO3) 3], Yttrium trinitrate [Y (NO3) 3], manganous nitrate [Mn (NO3) 2], zirconium nitrate [Zr (NO3) 2], chromium nitrate [Cr (NO3) 3], lanthanum nitrate [La (NO3) 3], nitric acid tin [Sn (NO3) 2], lead nitrate [Pb (NO3) 2], Palladous nitrate [Pd (NO3) 2], nitric acid ruthenium [Ru (NO3) 3], strontium nitrate [Sr (NO3) 2], indium nitrate [In (NO3) 3], gallium nitrate [Ga (NO3) 3], Bismuth trinitrate [Bi (NO3) 3], titanous chloride [TiCl3], titanium tetrachloride [TiCl4], zinc chloride [ZnCl2], Cerium II Chloride [CeCl3], cupric chloride [CuCl2], aluminum chloride [AlCl3], tin tetrachloride [SnCl4], Yttrium trichloride [YCl3], Manganous chloride tetrahydrate [MnCl2], zirconium chloride [ZrCl2], chromium chloride [CrCl3], iron(ic) chloride [FeCl3], iron protochloride [FeCl2], nickelous chloride [NiCl2], cobalt chloride [CoCl2], Lanthanum trichloride [LaCl3], lead chloride [PbCl3], Palladous chloride [PdCl2], ruthenium chloride [RuCl3], strontium chloride [SrCl2], indium chloride [InCl3], gallium chloride [GaCl3], bismuth chloride [BiCl3], titanium sulfate [Ti (SO4) 2], Tai-Ace S 150 [Al2 (SO4) 3], zinc sulfate [ZnSO4], ferrous sulfate [FeSO4], chromium sulphate [Cr2 (SO4) 3], single nickel salt [NiSO4], copper sulfate [CuSO4], palladous sulfate [Pd2 (SO4) 3], cerous sulfate [Ce2 (SO4) 3], indium sulfate [In2 (SO4) 3], manganous sulfate [MnSO4], gallium sulfate [Ga2 (SO4) 3], bismuth sulfate [Bi2 (SO4) 3], acetate [Zn (CH3COO) 2], cerous acetate [Ce (CH3COO) 3], venus crystals [Cu (CH3COO) 2], aluminum acetate [Al (CH3COO) 3], yttium acetate [Y (CH3COO) 3], manganous acetate [Mn (CH3COO) 2], zirconium acetate [Zr (CH3COO) 2], ferrous acetate [Fe (CH3COO) 2], ironic acetate [Fe (CH3COO) 3], nickelous acetate [Ni (CH3COO) 2], cobaltous acetate [Co (CH3COO) 2], lanthanum acetate [La (CH3COO) 3], lead acetate [Pb (CH3COO) 2], acid chloride [Pd (CH3COO) 2], ruthenium acetate [Ru (CH3COO) 3], strontium acetate [Sr (CH3COO) 2], indium acetate [In (CH3COO) 3], acetate gallium [Ga (CH3COO) 3], bismuth acetate [Bi (CH3COO) 3], tetrabutyl titanate [C16H36O4Ti], metatitanic acid [H2Ti2O3], a kind of in isopropyl titanate [C12H28O4Ti] and the tetraethoxy [C8H2OO4Si].
CN201010133489A 2010-03-26 2010-03-26 Method for preparing loading functional oxide porous carbon Pending CN101780952A (en)

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