CN106564873B - A kind of big micro-diplopore film carbon material and preparation method thereof - Google Patents
A kind of big micro-diplopore film carbon material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of big micro-diplopore film carbon materials and preparation method thereof, it is template using hollow sphere calcium carbonate, load poly-dopamine film, intermediate product CaO@S-HFGB is obtained under high temperature cabonization, then CaO@S-HFGB is washed with water to neutrality and filters to obtain filter cake, by filtration cakes torrefaction, big micro-diplopore film carbon material is made.Hollow sphere calcium carbonate used in the present invention decomposes the CO of release during high temperature cabonization2With efficient reaming effect, the problem of avoiding secondary carbonization and need to introduce expanding agent, one step carbonization can be obtained porous carbon materials S-HFGB；Preparation method of the invention is simple, process energy-saving and environment friendly, has great application potential in industrialization.
Description
Technical field
The invention belongs to material chemistry technical fields, and in particular to a kind of big micro-diplopore film carbon material and its preparation side
Method.
Background technique
Porous carbon materials are as a kind of environmentally friendly material, since its is cheap, high-specific surface area, pore structure can
The advantages that modified and excellent thermal stability, make its gas absorption, supercapacitor, in terms of have
Very big application potential.And the porous carbon materials with special appearance structure, in application sides such as gas separation, medicament slow release, catalysis
The excellent properties that face is shown make its correlation be prepared into the research hotspot of scientists.
Hard template method is a kind of common method for being effectively synthesized porous carbon materials, generally there is following steps composition：(1)
Carbon matrix precursor is immersed in template；(2) it allows presoma to polymerize on template, specific morphology is obtained by high temperature cabonization
Carbon material；(3) template in carbon material is removed；(4) expanding agent is added in specific morphology carbon material, carries out high temperature cabonization expansion
The porous carbon materials with special appearance are made in hole.Common spherical template agent has silica, ferroso-ferric oxide etc., but deposits
The problems such as template difficulty removes, carbon material pattern easily collapses after removal.In addition, being needed in traditional hard template method
The effect of by carburising step twice and expanding agent being added, can be only achieved carbon material reaming, has seriously affected product yield and energy
Consumption.
Calcium carbonate is a kind of common inorganic material, has many advantages, such as cheap, nontoxic, good biocompatibility.
The calcium carbonate products of different-shape can be prepared using processing method, the difference of crystallization condition, can be used as template be applied to it is more
In the preparation of hole carbon material.Dopamine (dopamine) is a kind of biological neural mediator, and under aqueous conditions, it can be molten
Oxidation-cross-linking reaction occurs under the action of solution oxygen, forms the compound thin layer of poly-dopamine that strength is attached to solid material surface
(PDA), it can be used as the presoma of special appearance carbon material.
The disclosure of background above technology contents is only used for auxiliary and understands design and technical solution of the invention, not necessarily
The prior art for belonging to present patent application, no tangible proof show above content present patent application the applying date
In disclosed situation, above-mentioned background technique should not be taken to the novelty and creativeness of evaluation the application.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of big micro-diplopore film carbon materials and preparation method thereof, to solve
The removal of conventional template agent difficulty, the cumbersome problem of carbonization reaming program.The present invention is during high temperature cabonization, composite material CaCO3@
Calcium carbonate in PDA not only acts as pattern supporting role, the CO of pyrolytic release2Also there is efficient reaming effect；This hair
Bright method solves the problems, such as that the difficult removal of traditional spheroidal template, pattern are easily collapsed, while avoiding secondary carbonization and needing to introduce
The problem of expanding agent.
In order to solve the above technical problems, the present invention uses following technical scheme：
For this purpose, the present invention proposes a kind of big micro-diplopore film carbon material, it is template, load using hollow sphere calcium carbonate
Poly-dopamine film obtains intermediate product CaO@S-HFGB under high temperature cabonization, CaO@S-HFGB is then washed with water to neutrality
And filter cake is filtered to obtain, by filtration cakes torrefaction, big micro-diplopore film carbon material is made.
The present invention also provides a kind of preparation methods of big micro-diplopore film carbon material, include the following steps：
(1) synthesis of hollow sphere calcium carbonate
Aqueous povidone solution 600mL, calcium chloride water 800mL, aqueous sodium carbonate 800mL are prepared respectively
With sodium dodecyl sulfate aqueous solution 600mL, four kinds of different solutions seal respectively to be stirred evenly；Taking two parts of volumes is 300mL
Prepared polyvinylpyrrolidonesolution solution is added in prepared calcium chloride solution and sodium carbonate liquor simultaneously respectively,
Under 20 DEG C of water bath conditions, it is vigorously stirred 0.5h；Then prepared sodium dodecyl sulfate solution is added to above-mentioned sodium carbonate
Solution is vigorously stirred 0.5h；Above-mentioned calcium chloride solution is added in the mixed solution of sodium carbonate, at 20 DEG C of bath temperature, is stirred
Mix revolving speed 300rmin-1Under conditions of, react 2h；Reaction rear slurry is filtered, is washed with dehydrated alcohol and deionization
It washs, in triplicate, hollow sphere calcium carbonate is made in 80 DEG C of vacuum drying 5h for the above operation；
(2)CaCO3The preparation of@PDA composite material
Dopamine saline solution 100mL, hollow sphere calcium carbonate aqueous solution 50mL are prepared respectively, and by 0.75mL ammonia
Water, 40mL ethyl alcohol, the alkaline solution that 90mL deionized water is prepared, three kinds of different solutions seal respectively to stir evenly；It will configure
Calcium carbonate aqueous solution be added into DOPA amine salt aqueous solution, at 15~25 DEG C of bath temperature, 150~300r of speed of agitator
min-1Under conditions of, react 0.5h；Prepared alkaline solution is added in above-mentioned dopamine mixed salt solution, reaction temperature
It is remained unchanged with revolving speed, reacts 20h；Reaction rear slurry is filtered, is washed with deionized, 80 DEG C of vacuum drying 5h, is made
Obtain CaCO3@PDA composite material；
(3) preparation of big micro-diplopore film carbon material
Weigh the CaCO of certain mass3@PDA composite sample is placed in tube furnace, under the protection of nitrogen, is carried out high
Temperature carbonization, obtains intermediate product CaO S-HFGB, is washed with deionized water to neutrality, and filter cake is finally put into 80 DEG C true
Dry 5h, is made big micro-diplopore film carbon material in empty drying box.
Further, the concentration of aqueous povidone solution described in step (1) is 20gL-1。
Further, the concentration of calcium chloride water described in step (1) is 0.1molL-1。
Further, the concentration of aqueous sodium carbonate described in step (1) is 0.1molL-1。
Further, the concentration 0.05molL of sodium dodecyl sulfate aqueous solution described in step (1)-1。
Further, the concentration of dopamine saline solution described in step (2) is 3~7gL-1。
Further, the concentration of hollow sphere calcium carbonate aqueous solution described in step (2) is 8gL-1。
Further, steps of processing is taken in the washing of reaction rear slurry described in step (2), will reaction rear slurry with having
Machine filter film is filtered, and when filtrate is down to half in funnel, supplement deionized water is to full bucket, and the above operation is in triplicate；It will filter
Cake is dissolved in deionized water, is slowly stirred 4h, and film is washed with water and is filtered, and is repeated twice by first time suction filtration process, finally will
Filter cake is put into 80 DEG C of vacuum oven dry 5h.
Further, high temperature cabonization program described in step (3) includes the following steps：
(a) temperature-rise period：With 2~10 DEG C of min-1Speed by CaCO3@PDA composite sample rises to 700 from room temperature
~900 DEG C；
(b) thermostatic process：By CaCO3@PDA composite sample is in 700~900 DEG C of 1~3h of holding；
(c) temperature-fall period：By presoma from 700~900 DEG C of cooled to room temperatures.
Compared with prior art, the present invention having the advantages that：
(1) present invention resolves into calcium oxide and carbon dioxide after high temperature cabonization using hollow sphere calcium carbonate as template,
Calcium oxide can be removed with water, solves the problems, such as the removal of later period template difficulty；
(2) the hollow sphere calcium carbonate used in the present invention decomposes the CO of release during high temperature cabonization2With height
The problem of imitating reaming effect, avoiding secondary carbonization and need to introduce expanding agent, one step carbonization can be obtained porous carbon materials S-
HFGB；
(3) one step carbonization of the invention, is carbonized compared to two traditional steps and sends out, and product yield is higher；
(4) product of preparation of the invention, structure novel has big micro-diplopore structure, and specific surface area is higher；
(5) preparation method of the invention is simple, process energy-saving and environment friendly, has greatly application latent in industrialization
Energy.
Detailed description of the invention
Fig. 1 is one hollow sphere calcium carbonate of the embodiment of the present invention and SEM and the TEM figure of S-HFGB；
Fig. 2 is S-HFGB constituent content analysis figure after one composite material CaO@S-HFGB of the embodiment of the present invention and washing；
Fig. 3 is the XRD diagram of one hollow sphere calcium carbonate of the embodiment of the present invention, CaO@S-HFGB and S-HFGB；
Fig. 4 is one hollow sphere calcium carbonate of the embodiment of the present invention, CaCO3The TG of@PDA schemes；
Fig. 5 is the N of one S-HFGB of the embodiment of the present invention2Adsorption-desorption figure.
Specific embodiment
With reference to embodiment and compares attached drawing invention is further described in detail.It is emphasized that
Following the description is only exemplary, the range and its application being not intended to be limiting of the invention.
Embodiment 1
A kind of preparation method of big micro-diplopore film carbon material, includes the following steps：
(1) synthesis of hollow sphere calcium carbonate
Compound concentration 20gL respectively-1Polyvinylpyrrolidone (PVP) aqueous solution 600mL, concentration 0.1molL-1's
Calcium chloride (CaCl2) aqueous solution 800mL, concentration 0.1molL-1Sodium carbonate (Na2CO3) aqueous solution 800mL and concentration
0.05mol·L-1Dodecyl sodium sulfate (SDS) aqueous solution 600mL, four kinds of different solutions seal respectively to stir evenly；Take two
Part (each 300mL) prepared PVP solution, is added to prepared CaCl simultaneously respectively2Solution and Na2CO3In solution, 20
Under DEG C water bath condition, it is vigorously stirred 0.5h；Then prepared SDS solution is added to above-mentioned Na2CO3Solution is vigorously stirred
0.5h；By above-mentioned CaCl2Na is added in solution2CO3Mixed solution in, at 20 DEG C of bath temperature, speed of agitator 300rmin-1
Under conditions of, react 2h；Reaction rear slurry is filtered, is washed with dehydrated alcohol and deionized water, the above operation repeats three
Secondary, hollow sphere calcium carbonate product is made in 80 DEG C of vacuum drying 5h；
(2)CaCO3The preparation of@PDA composite material
Compound concentration is 5gL-1DOPA amine salt (DA) aqueous solution 100mL, concentration 8gL-1Hollow sphere calcium carbonate is water-soluble
Liquid 50mL, i.e. weight ratio are 1.25DA/1.0CaCO3DOPA amine salt and hollow sphere calcium carbonate, and by 0.75mL ammonia
Water, 40mL ethyl alcohol, the weakly alkaline solution that 90mL deionized water is prepared, three kinds of different solutions seal respectively to stir evenly；It will configuration
Good calcium carbonate aqueous solution is added into DOPA amine salt aqueous solution, at 20 DEG C of bath temperature, speed of agitator 200rmin-1Item
Under part, 0.5h is reacted；Prepared weakly alkaline solution is added in above-mentioned dopamine mixed salt solution, reaction temperature and revolving speed
It remains unchanged, reacts 20h；Reaction rear slurry is filtered, is washed with deionized, 80 DEG C of vacuum drying 5h, is made
CaCO3@PDA composite material；
(3) preparation of big micro-diplopore film carbon material
Weigh the CaCO of certain mass3@PDA sample is placed in tube furnace, under the protection of nitrogen, carries out high temperature cabonization,
Carbonization Conditions are：With 5 DEG C of min-1Speed by CaCO3@PDA sample rises to 700 DEG C, constant temperature 1h, then natural cooling from room temperature
To room temperature；Intermediate product CaO S-HFGB is obtained, is washed with deionized water to neutrality, it is final to obtain carbon material S-HFGB-
1。
Embodiment 2
In addition to following variations, remaining is the same as embodiment 1.
Compound concentration is 3gL-1DOPA amine salt (DA) aqueous solution 100mL, concentration 8gL-1Hollow sphere calcium carbonate is water-soluble
Liquid 50mL, i.e. weight ratio are 0.75DA/1.0CaCO3DOPA amine salt and hollow sphere calcium carbonate, and by 0.75mL ammonia
Water, 40mL ethyl alcohol, the weakly alkaline solution that 90mL deionized water is prepared, three kinds of different solutions seal respectively to stir evenly；It will configuration
Good calcium carbonate aqueous solution is added into DOPA amine salt aqueous solution, at 15 DEG C of bath temperature, speed of agitator 150rmin-1Item
Under part, 0.5h is reacted；Prepared weakly alkaline solution is added in above-mentioned dopamine mixed salt solution, reaction temperature and revolving speed
It remains unchanged, intermediate product CaCO is made in reaction 20h3@PDA；
Weigh the CaCO of certain mass3@PDA sample is placed in tube furnace, under the protection of nitrogen, carries out high temperature cabonization,
Carbonization Conditions are：With 2 DEG C of min-1Speed by CaCO3@PDA sample rises to 800 DEG C, constant temperature 2h, then natural cooling from room temperature
To room temperature；Intermediate product CaO S-HFGB is obtained, is washed with deionized water to neutrality, it is final to obtain carbon material S-HFGB-
2。
Embodiment 3
In addition to following variations, remaining is the same as embodiment 1.
Compound concentration is 6gL-1DOPA amine salt (DA) aqueous solution 100mL, concentration 8gL-1Hollow sphere calcium carbonate is water-soluble
Liquid 50mL, i.e. weight ratio are 1.5DA/1.0CaCO3DOPA amine salt and hollow sphere calcium carbonate, and by 0.75mL ammonium hydroxide,
40mL ethyl alcohol, the weakly alkaline solution that 90mL deionized water is prepared, three kinds of different solutions seal respectively to stir evenly；It will be configured
Calcium carbonate aqueous solution is added into DOPA amine salt aqueous solution, at 25 DEG C of bath temperature, speed of agitator 300rmin-1Under conditions of,
React 0.5h；Prepared weakly alkaline solution is added in above-mentioned dopamine mixed salt solution, reaction temperature and revolving speed are kept
Constant, intermediate product CaCO is made in reaction 20h3@PDA；
Weigh the CaCO of certain mass3@PDA sample is placed in tube furnace, under the protection of nitrogen, carries out high temperature cabonization,
Carbonization Conditions are：With 10 DEG C of min-1Speed by CaCO3@PDA sample rises to 900 DEG C, constant temperature 3h, then natural cooling from room temperature
To room temperature；Intermediate product CaO S-HFGB is obtained, is washed with deionized water to neutrality, it is final to obtain carbon material S-HFGB-
3。
Instance analysis
As shown in Figure 1, S-HFGB porous carbon materials prepared by the present invention, the appearance structure with hollow sphere, show mould
Plate agent calcium carbonate has resolved into calcium oxide completely and has been washed with water removal, and pattern does not collapse after wash water.The wherein bright grain of SEM chart
The hollow sphere calcium carbonate that diameter is about 5 μm is mutually piled up by many uniform particle diameters, orderly aligned platy particle.
As shown in Fig. 2, its phosphorus content of S-HFGB prepared by the present invention is up to 84.5%；Wherein CaO@S-HFGB and washing after
Calcium element content in S-HFGB, respectively 15.3% and 0.26%, show that calcium oxide is washed with water removal completely.
As shown in figure 3, hollow sphere calcium carbonate prepared by the present invention is calcite type, and intermediate product CaO@S-HFGB
Characteristic peak of the XRD spectrum without calcium carbonate calcite type, shows CaCO3Calcium carbonate in@PDA resolves into calcium oxide completely.
The wherein XRD diagram of S-HFGB, upper with characteristic peak is graphitized at 26 ° and 44 °, (002) and (100) crystal face shows that S-HFGB has
There is part carbonization structure.
As shown in figure 4, hollow sphere calcium carbonate prepared by the present invention and CaCO3@PDA decomposition temperature, respectively 605 DEG C and
675 DEG C, wherein CaCO3@PDA weight-loss ratio under conditions of greenhouse rises to 900 DEG C is about 55%.
As shown in figure 5, the N of S-HFGB prepared by the present invention2Adsorption/desorption figure, and its thus obtain the pore structure of material
As shown in table 1.Know that S-HFGB has high-specific surface area and big micro-diplopore structure, BET are respectively with Langmuir specific surface area
719.9m2·g-1, 955.6m2·g-1, wherein micropore ratio is 26.08%.
The pore structure parameter of 1 S-HFGB of table
It would be recognized by those skilled in the art that above description make numerous accommodations be it is possible, so embodiment and attached
Figure is intended merely to describe one or more particular implementations.
It is counted as example embodiment of the invention although having been described and describing, it will be apparent to those skilled in the art that
It can be variously modified and is replaced, without departing from spirit of the invention.Furthermore it is possible to make many modifications with will be special
Condition of pledging love is fitted to religious doctrine of the invention, without departing from invention described herein central concept.So the present invention is unrestricted
In specific embodiment disclosed herein, but the present invention may further include belonging to all embodiments of the scope of the invention and its being equal
Object.
Claims (9)
1. a kind of preparation method of big micro-diplopore film carbon material, it is characterised in that：The big micro-diplopore film carbon material is
It is template using hollow sphere calcium carbonate, loads poly-dopamine film, intermediate product CaO@S- is obtained under high temperature cabonization
HFGB is then washed with water CaO@S-HFGB to neutrality and filters to obtain filter cake, filtration cakes torrefaction is made；
The preparation method of the big micro-diplopore film carbon material, includes the following steps：
(1) synthesis of hollow sphere calcium carbonate
Aqueous povidone solution 600mL, calcium chloride water 800mL, aqueous sodium carbonate 800mL and ten are prepared respectively
Dialkyl sulfonates aqueous solution 600mL, four kinds of different solutions seal respectively to stir evenly；Taking two parts of volumes is that 300mL is prepared
Good polyvinylpyrrolidonesolution solution is added in prepared calcium chloride solution and sodium carbonate liquor, simultaneously respectively at 20 DEG C
Under water bath condition, it is vigorously stirred 0.5h；Then prepared sodium dodecyl sulfate solution is added to above-mentioned sodium carbonate liquor,
It is vigorously stirred 0.5h；Above-mentioned calcium chloride solution is added in the mixed solution of sodium carbonate, at 20 DEG C of bath temperature, speed of agitator
300r·min-1Under conditions of, react 2h；Reaction rear slurry is filtered, is washed with dehydrated alcohol and deionized water, it is above
In triplicate, hollow sphere calcium carbonate is made in 80 DEG C of vacuum drying 5h for operation；
(2)CaCO3The preparation of@PDA composite material
Dopamine saline solution 100mL, hollow sphere calcium carbonate aqueous solution 50mL are prepared respectively, and by 0.75mL ammonium hydroxide,
40mL ethyl alcohol, the alkaline solution that 90mL deionized water is prepared, three kinds of different solutions seal respectively to stir evenly；By configured carbon
Sour calcium aqueous solution is added into DOPA amine salt aqueous solution, at 15~25 DEG C of bath temperature, 150~300rmin of speed of agitator-1's
Under the conditions of, react 0.5h；Prepared alkaline solution is added in above-mentioned dopamine mixed salt solution, reaction temperature and revolving speed
It remains unchanged, reacts 20h；Reaction rear slurry is filtered, is washed with deionized, 80 DEG C of vacuum drying 5h, is made
CaCO3@PDA composite material；
(3) preparation of big micro-diplopore film carbon material
Weigh the CaCO of certain mass3@PDA composite sample is placed in tube furnace, under the protection of nitrogen, carries out pyrocarbon
Change, obtains intermediate product CaO S-HFGB, washed with deionized water to neutrality, finally do the vacuum that filter cake is put into 80 DEG C
Dry 5h, is made big micro-diplopore film carbon material in dry case.
2. the preparation method of big micro-diplopore film carbon material according to claim 1, which is characterized in that institute in step (1)
The concentration for stating aqueous povidone solution is 20gL-1。
3. the preparation method of big micro-diplopore film carbon material according to claim 1, which is characterized in that institute in step (1)
The concentration for stating calcium chloride water is 0.1molL-1。
4. the preparation method of big micro-diplopore film carbon material according to claim 1, which is characterized in that institute in step (1)
The concentration for stating aqueous sodium carbonate is 0.1molL-1。
5. the preparation method of big micro-diplopore film carbon material according to claim 1, which is characterized in that institute in step (1)
State the concentration 0.05molL of sodium dodecyl sulfate aqueous solution-1。
6. the preparation method of big micro-diplopore film carbon material according to claim 1, it is characterised in that：Institute in step (2)
The concentration for stating dopamine saline solution is 3~7gL-1。
7. the preparation method of big micro-diplopore film carbon material according to claim 1, it is characterised in that：Institute in step (2)
The concentration for stating hollow sphere calcium carbonate aqueous solution is 8gL-1。
8. the preparation method of big micro-diplopore film carbon material according to claim 1, it is characterised in that：Institute in step (2)
It states reaction rear slurry washing and takes steps of processing, reaction rear slurry is filtered with organic filter membrane, when filtrate in funnel
Supplement deionized water is to full bucket when being down to half, and the above operation is in triplicate；Filter cake is dissolved in deionized water, is slowly stirred
4h is washed with water film and is filtered, and is repeated twice by first time suction filtration process, is finally put into filter cake in 80 DEG C of vacuum oven
Dry 5h.
9. the preparation method of big micro-diplopore film carbon material according to claim 1, it is characterised in that：Institute in step (3)
High temperature cabonization program is stated to include the following steps：
(a) temperature-rise period：With 2~10 DEG C of min-1Speed by CaCO3@PDA composite sample rises to 700 from room temperature~
900℃；
(b) thermostatic process：By CaCO3@PDA composite sample is in 700~900 DEG C of 1~3h of holding；
(c) temperature-fall period：By CaCO3@PDA composite sample is from 700~900 DEG C of cooled to room temperatures.
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