CN105923629A - Method for preparing transition metal composite hetero atom doped porous carbon material through dipping, recrystallizing and carbonizing biomasses - Google Patents
Method for preparing transition metal composite hetero atom doped porous carbon material through dipping, recrystallizing and carbonizing biomasses Download PDFInfo
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Abstract
The invention provides a method for preparing a transition metal composite hetero atom doped porous carbon material through dipping, recrystallizing and carbonizing biomasses. The method comprises the following steps: immersing the biomasses in an aqueous solution of metal salt, and carrying out refrigeration vacuum drying on the immersed biomasses to recrystalize the metal salt in apertures of the biomasses in order to obtain a product A; and 2, placing the product A in a tubular furnace, and carrying out high temperature calcining to carbonize the biomasses at a high temperature and realize a metal salt decomposition reaction in order to obtain the transition metal composite hetero atom doped porous carbon material. The non-noble metal modified biomass carbon material is prepared from the biomasses through using the porous structure of the biomasses. Compared with routine high temperature carbonization, dipping recrystallization carbonization can synchronously realize activation and perforation, so the porous carbon prepared in the invention has a large specific surface area and good conductivity, thereby the porous carbon material still has strong energy storage and release ability under a high current density.
Description
Technical field
The present invention relates to a kind of transition metal compound-preparation method of Heteroatom doping porous carbon materials.
Background technology
In recent years, material with carbon element, as a kind of inexpensive and stable material, is paid close attention to by people, by
It is widely used in the fields such as gas separation, purifying water process, catalytic chromatography analysis, energy storage and photocatalysis.
And the electric property of original material with carbon element is relatively weak, up to the present, the electric capacity of traditional active carbon material
Basic at 100-200F g-1.Due to sp2Hydridization material with carbon element have abundant can be at material surface free migration
Pi-electron, heteroatomic incorporation can change the electronegativity of connected carbon atom, thus is conducive to improving its electricity
Learn performance.In order to improve doping material with carbon element chemical property, by changing the selection of presoma, by different
Hetero atom is incorporated in material with carbon element, such as: N, S, B, I, P etc., and control condition improves heteroatomic simultaneously
Content, regulates and controls the type of miscellaneous element.Study the miscellaneous constituent content showing singly to adulterate material with carbon element limited, be unfavorable for
The raising of material property.In order to improve the content of miscellaneous element, sight is turned to and adulterates more and be co-doped with by researchers
Miscellaneous, improve the content of miscellaneous element whereby, and utilize the cooperative effect between different miscellaneous element to make material
Chemical property strengthened.Report prepares exotic atom doping material with carbon element synthetic method at present has: heat treatment
Method, vapour deposition process, hydro-thermal method, arc discharge, plasma method etc., the major defect of these methods is
High to equipment requirements, simultaneous reactions condition requires harshness, the material causing synthesizing relatively costly, unfavorable
In industrialized production, it is less useful for the commercialization of product.
In order to improve the electric capacity of material with carbon element, transition metal oxide such as (Co further3O4、MnO2、NiO、Fe3O4
Deng) due to it, there is high ratio capacitance, substantial amounts of redox reaction can occur, thus and material with carbon element
It is combined, see (Carbon, 2007,45 (7): 2365-2373), yet with oxo transition metal
The poorly conductive of compound, the chemical property of therefore prepared composite still needs to improve.
Summary of the invention
It is an object of the invention to provide a kind of obtained porous carbon and there is bigger specific surface area, good
Electric conductivity, the most still have the storage of strong energy and releasability, step is simple, low cost,
Maneuverable dipping recrystallization carbonization biomass are prepared transition metal and are combined Heteroatom doping porous carbon materials
Method.
The object of the present invention is achieved like this:
Step one: biomass are immersed in the aqueous solution of slaine, the biomass economy freezing vacuum after immersion
The method being dried makes slaine recrystallization in the hole of biomass obtain product A;
Step 2: inserted by product A in tube furnace and carry out high-temperature calcination, at high temperature makes biomass generation carbon
Change reaction, slaine decomposition reaction occurs simultaneously, obtain the porous of the compound Heteroatom doping simultaneously of transition metal
Material with carbon element.
The present invention can also include:
1, described biomass are Hericium erinaceus (Bull. Ex Fr.) Pers., Auricularia, straw, bean curd powder, rice hulls, wood flour or Sargassum.
2, during the aqueous solution of described slaine is the nitrate of Fe, Co, Ni or Mn, phosphate or sulfate
The mixture of one or more.
3, the concentration of the aqueous solution of described slaine is 0.05~2mol L-1。
4, described high-temperature calcination is to calcine 10~180 minutes in a vacuum or inert atmosphere, and calcining heat is
600~1100 DEG C.
Compared with prior art, the present invention has a following beneficial effect:
(1) present invention uses biomass to be raw material, utilizes biomass porous structure, prepares base metal and repaiies
The biomass carbon material of decorations, compared with conventional high temperature carbonization, employing dipping recrystallization method carbonization can be in carbonization
During can synchronize realize activation perforate purpose, thus prepare porous carbon there is bigger specific surface area,
Good electric conductivity, the most still has strong energy storage and releasability.
(2) present invention utilizes containing heteroatomic metal salt solution as carbonization medium, it is achieved at biomass thermal
Solve in carbonisation and synchronize controlled nonmetal (N, P, S etc.) hetero atom that introduces in material with carbon element skeleton, simultaneously
By metal (Fe, Co, Ni, Mn etc.) and material with carbon element In-situ reaction, finally give transition metal compound simultaneously
The carbon-based material of hetero atom codope, compared with conventional doping method, one-step method of the present invention introduces transition gold
Belonging to compound and Heteroatom doping, step is simple, and low cost easily operates, and reactant purity is high, transition gold
The introducing belonged to is possible not only to improve the electric conductivity of carbon-based material, and can also increase its fake capacitance, widens its electricity
Pressure window, increases substantially its energy density, has preferable application prospect.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the Heteroatom doping porous carbon materials that embodiment 1 obtains.
Fig. 2 is that embodiment 1 obtains Heteroatom doping porous carbon materials at 5mV s-1Sweep the cyclic voltammogram under speed.
Fig. 3 is that embodiment 1 obtains Heteroatom doping porous carbon materials at 1A g-1Discharge and recharge under electric current density
Figure.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.Following example will assist in this area
Technical staff be further appreciated by the present invention, but limit the present invention the most in any form.It should be pointed out that,
To those skilled in the art, without departing from the inventive concept of the premise, it is also possible to if making
Dry deformation and improvement.These broadly fall into protection scope of the present invention.
Embodiment 1, Co is combined the preparation of N doped porous carbon material:
Weigh the Hericium erinaceus (Bull. Ex Fr.) Pers. of 4g, be immersed in 0.5mol L-1Co(NO3)2Aqueous solution in 12h, will soak after
Hericium erinaceus (Bull. Ex Fr.) Pers. lyophilisation, insert in tube furnace, under Ar atmosphere, with 5 DEG C of min-1Heating rate liter
To 850 DEG C, constant temperature 60min, clean the removal of impurity with distilled water after cooling, centrifugal drying obtains hetero atom and mixes
Miscellaneous porous carbon materials.
Utilize scanning electron microscope that prepared Heteroatom doping porous carbon materials is carried out physicochemical property table
Levying, Fig. 1 shows, prepared Heteroatom doping porous carbon materials is laminated structure, above load C o granule.
Gained material with carbon element Fig. 3 shows, carries out it at 1A g-1Charge-discharge test under electric current density, 1A g-1Electric discharge
Under electric current density, specific capacity is 200F g-1。
Embodiment 2, Ni is combined the preparation of N doped porous carbon material:
Weigh the Hericium erinaceus (Bull. Ex Fr.) Pers. of 4g, be immersed in 0.5mol L-1Ni(NO3)2Aqueous solution in 12h, will soak after
Hericium erinaceus (Bull. Ex Fr.) Pers. lyophilisation, insert in tube furnace, under Ar atmosphere, with 5 DEG C of min-1Heating rate liter
To 850 DEG C, constant temperature 60min, clean the removal of impurity with distilled water after cooling, centrifugal drying obtains hetero atom and mixes
Miscellaneous porous carbon materials.
Embodiment 3, the preparation of Co composite S doped porous carbon material:
Weigh the Hericium erinaceus (Bull. Ex Fr.) Pers. of 4g, be immersed in 0.5mol L-1CoSO4Aqueous solution in 12h, will soak after
Hericium erinaceus (Bull. Ex Fr.) Pers. lyophilisation, insert in tube furnace, under Ar atmosphere, with 5 DEG C of min-1Heating rate liter
To 850 DEG C, constant temperature 60min, clean the removal of impurity with distilled water after cooling, centrifugal drying obtains hetero atom and mixes
Miscellaneous porous carbon materials.
Embodiment 4, the preparation of Ni composite S doped porous carbon material:
Weigh the Hericium erinaceus (Bull. Ex Fr.) Pers. of 4g, be immersed in 0.5mol L-1NiSO4Aqueous solution in 12h, by soak after
Hericium erinaceus (Bull. Ex Fr.) Pers. lyophilisation, inserts in tube furnace, under Ar atmosphere, with 5 DEG C of min-1Heating rate rise to
850 DEG C, constant temperature 60min, clean the removal of impurity with distilled water after cooling, centrifugal drying obtains Heteroatom doping
Porous carbon materials.
Claims (9)
1. one kind impregnates recrystallization carbonization biomass and prepares transition metal and be combined Heteroatom doping porous carbon materials
Method, is characterized in that:
Step one: biomass are immersed in the aqueous solution of slaine, the biomass economy freezing vacuum after immersion
The method being dried makes slaine recrystallization in the hole of biomass obtain product A;
Step 2: inserted by product A in tube furnace and carry out high-temperature calcination, at high temperature makes biomass generation carbon
Change reaction, slaine decomposition reaction occurs simultaneously, obtain the porous of the compound Heteroatom doping simultaneously of transition metal
Material with carbon element.
Dipping recrystallization carbonization biomass the most according to claim 1 are prepared transition metal and are combined hetero atom
The method of doped porous carbon material, is characterized in that: described biomass are Hericium erinaceus (Bull. Ex Fr.) Pers., Auricularia, straw, bean curd
Powder, rice hulls, wood flour or Sargassum.
Dipping recrystallization carbonization biomass the most according to claim 1 and 2 are prepared transition metal and are combined miscellaneous
The method of atom doped porous carbon materials, is characterized in that: the aqueous solution of described slaine be Fe, Co, Ni or
The mixture of one or more in the nitrate of Mn, phosphate or sulfate.
Dipping recrystallization carbonization biomass the most according to claim 1 and 2 are prepared transition metal and are combined miscellaneous
The method of atom doped porous carbon materials, is characterized in that: the concentration of the aqueous solution of described slaine is 0.05~2
mol·L-1。
Dipping recrystallization carbonization biomass the most according to claim 3 are prepared transition metal and are combined hetero atom
The method of doped porous carbon material, is characterized in that: the concentration of the aqueous solution of described slaine is 0.05~2
mol·L-1。
Dipping recrystallization carbonization biomass the most according to claim 1 and 2 are prepared transition metal and are combined miscellaneous
The method of atom doped porous carbon materials, is characterized in that: described high-temperature calcination is in a vacuum or inert atmosphere
Calcining 10~180 minutes, calcining heat is 600~1100 DEG C.
Dipping recrystallization carbonization biomass the most according to claim 3 are prepared transition metal and are combined hetero atom
The method of doped porous carbon material, is characterized in that: described high-temperature calcination is to calcine in a vacuum or inert atmosphere
10~180 minutes, calcining heat was 600~1100 DEG C.
Dipping recrystallization carbonization biomass the most according to claim 4 are prepared transition metal and are combined hetero atom
The method of doped porous carbon material, is characterized in that: described high-temperature calcination is to calcine in a vacuum or inert atmosphere
10~180 minutes, calcining heat was 600~1100 DEG C.
Dipping recrystallization carbonization biomass the most according to claim 5 are prepared transition metal and are combined hetero atom
The method of doped porous carbon material, is characterized in that: described high-temperature calcination is to calcine in a vacuum or inert atmosphere
10~180 minutes, calcining heat was 600~1100 DEG C.
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CN106783213A (en) * | 2016-12-23 | 2017-05-31 | 宁海县浙工大海洋研究院 | Metal and the mesoporous carbon nano-composite material preparation method of metal oxide quantum dot |
CN106914265A (en) * | 2017-03-06 | 2017-07-04 | 南京师范大学 | A kind of method for preparing N doping porous nano carbon material as carbon source gel method with biomass |
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