CN108455595A - The preparation method of porous carbon materials - Google Patents
The preparation method of porous carbon materials Download PDFInfo
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- CN108455595A CN108455595A CN201810175626.4A CN201810175626A CN108455595A CN 108455595 A CN108455595 A CN 108455595A CN 201810175626 A CN201810175626 A CN 201810175626A CN 108455595 A CN108455595 A CN 108455595A
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Abstract
The invention discloses a kind of preparation methods of porous carbon materials.The preparation method comprises the following steps：Orange peel is cleaned, crushed, is dried；The orange peel after drying is weighed, 2~5 h are pre-oxidized at 200~300 DEG C；According to activator:Orange peel=2~5 after pre-oxidation：Orange peel after activator and pre-oxidation is mixed, is stirred, impregnated later, obtain mixture by 1 mass ratio；The mixture is risen to 500~700 DEG C under an inert atmosphere, is warming up to 800~900 DEG C later with 10 DEG C/min, 2~4 h are to get product for heat preservation.The raw materials used in the present invention is cheap, and preparation process is simple, and prepared product has high-specific surface area, mesoporous and excellent chemical property.
Description
Technical field
The present invention relates to carbon material preparing technical fields, and in particular to a kind of preparation method of porous carbon materials.
Background technology
Porous carbon refers to using carbon as basic framework and the substance with different size holes, has both had carbon material chemistry steady
Qualitative height, good conductivity, it is cheap the advantages that, and have because of the introducing of pore structure than table and accumulate big, pore passage structure is controllable,
The features such as aperture is adjustable.
Porous carbon materials are widely used as the adsorbent of pigment, heavy metal particles and toxic gas etc. because of its advantage, change
The electrode material etc. of catalyst and lithium ion battery, fuel cell and ultracapacitor in reaction.Wherein, it determines more
The key factor of hole carbon material performance is the size of its specific surface area and porosity.
In general, the raw material for preparing porous carbon is petroleum product, coal, trees etc., such raw material has high excellent of phosphorus content
Point, still, a large amount of uses can damage the ecological balance, pollute the environment.
Therefore, it is urgent to provide a kind of preparation methods of the porous carbon materials i.e. with social benefit and with economic benefit.
Invention content
The technical problem to be solved in the present invention is to provide a kind of at low cost, environmental-friendly and excellent product property porous
The preparation method of carbon material.
In order to solve the above technical problems, the present invention adopts the following technical scheme that：
Since orange has a large amount of VC and sour-sweet mouthfeel, and it is that people like and often edible one of fruit is still eaten
After being finished orange, life waste material orange peel is will produce, orange peel can merely be given up money again as domestic refuse to handle
Useless power.Therefore, the present invention prepares porous carbon material using orange peel as charcoal source, the method both taken full advantage of waste with
It is energy saving, and can produce and have excellent performance, have the porous carbon material of high added value.
Specific technical solution is as follows：
A kind of preparation method of porous carbon materials is designed, is included the following steps：
（1）Orange peel is cleaned, crushed, is dried；
（2）By step（1）Orange peel after middle drying pre-oxidizes 2~5 h at 200~300 DEG C；
（3）According to activator:Orange peel=2~5 after pre-oxidation：1 mass ratio, by activator and step（2）Middle pre-oxidation
Orange peel afterwards is mixed, is stirred, and is impregnated later, and mixture is obtained；
（4）By step（3）Middle gained mixture rises to 500~700 DEG C under an inert atmosphere, is warming up to later with 10 DEG C/min
800~900 DEG C, keep the temperature 2~4 h；
（5）By step（4）Products therefrom is washed to neutrality, dry later to get.
Preferably, in the step（3）In, the activator is phosphoric acid or zinc chloride.
Preferably, in the step（3）In, when the activator is solid, mixed with the orange peel after the pre-oxidation
Before conjunction, by the activator water dissolution；After being mixed with dipping with the orange peel after the pre-oxidation, it is dried.
Preferably, in the step（3）In, the dip time control is 12~14h.
Preferably, in the step（5）In, the product and mixed in hydrochloric acid are stirred, carry out being washed to neutrality later.
Preferably, the inert atmosphere is selected from least one of ammonia, nitrogen, hydrogen, argon gas.
Compared with prior art, the beneficial technical effect of the present invention lies in：
1. the orange peel using biology base of the invention initiative as charcoal source, both takes full advantage of waste with energy saving,
Can produce again high added value, meet the multi-field porous carbon material used.
2. the porous charcoal prepared by the present invention has high specific surface area and flourishing pore structure.
3. the porous charcoal prepared by the present invention has good charge-discharge performance and high specific capacitance value.
4. present invention process is simple, it is environmentally friendly, there are society and economical effects.
Description of the drawings
Fig. 1 is the XRD diagram of the porous carbon materials prepared by embodiment 2-5；
Fig. 2 is the XRD diagram of the porous carbon materials prepared by embodiment 6-9；
Fig. 3 is the SEM figures of the porous carbon materials after embodiment 1 pre-oxidizes；
Fig. 4 is the SEM figures of the porous carbon materials prepared by embodiment 2-5；
Fig. 5 is the SEM figures of the porous carbon materials prepared by embodiment 6-9；
Fig. 6 is the adsorption/desorption isotherms figure of the porous carbon materials prepared by embodiment 2-5；
Fig. 7 is the graph of pore diameter distribution of the porous carbon materials prepared by embodiment 2-5；
Fig. 8 is the adsorption/desorption isotherms figure of the porous carbon materials prepared by embodiment 6-9；
Fig. 9 is the graph of pore diameter distribution of the porous carbon materials prepared by embodiment 6-9；
Figure 10 is the constant current charge-discharge test chart of porous carbon materials the 2nd cycle and the 20th cycle prepared by embodiment 4；
Figure 11 is the constant current charge-discharge test chart of porous carbon materials the 2nd cycle and the 20th cycle prepared by embodiment 8.
Specific implementation mode
Illustrate the specific implementation mode of the present invention with reference to the accompanying drawings and examples, but following embodiment is used only in detail
It describes the bright present invention in detail, does not limit the scope of the invention in any way.
Involved instrument and equipment is routine instrument device unless otherwise instructed in the examples below；Involved
Material and reagent are purchased from conventional chemical reagent shop unless otherwise instructed；Involved test, preparation method, such as without especially
Illustrate, is conventional method.
The pre-oxidation of 1 orange peel of embodiment
Orange peel is cleaned, crush after be put into electric drying oven with forced convection and fully dried, weigh it is dry after orange
Skin is placed in Muffle furnace, and 3 h are pre-oxidized at 250 DEG C, and the quality of electronic balance weighing orange peel is used after being cooled to room temperature.4 groups
Pre-oxidation yield such as the following table 1 of orange peel, wherein pre-oxidation yield=（Orange before quality/pre-oxidation of orange peel after pre-oxidation
The quality of skin）×100%：
。
Orange peel after embodiment 2 is pre-oxidized using embodiment 1 prepares porous carbon materials
Phosphoric acid solution is measured in small beaker with pipette, phosphoric acid volume is converted into quality, according to phosphoric acid:After pre-oxidation
Orange peel=2：The phosphoric acid solution is mixed with the orange peel after pre-oxidation in embodiment 1, is stirred by 1 mass ratio, it
After impregnate 12 h, obtain mixture, the mixture be put into porcelain boat, the porcelain boat is placed in tube furnace, in nitrogen gas
600 DEG C are risen under atmosphere, is warming up to 900 DEG C later with 10 DEG C/min, are kept the temperature 3 h to be carbonized, are cooled to room temperature.Later,
It is 7 or so by the product circulation warm water washing after charing to pH, obtained sample is named as OPAC-H3PO4-2。
Orange peel after embodiment 3 is pre-oxidized using embodiment 1 prepares porous carbon materials
As different from Example 2：Phosphoric acid and the mass ratio of the orange peel after pre-oxidation are 3：1, remaining with 2 phase of embodiment
Together, obtained sample is named as OPAC-H3PO4-3。
Orange peel after embodiment 4 is pre-oxidized using embodiment 1 prepares porous carbon materials
As different from Example 2：Phosphoric acid and the mass ratio of the orange peel after pre-oxidation are 4：1, remaining with 2 phase of embodiment
Together, obtained sample is named as OPAC-H3PO4-4。
Orange peel after embodiment 5 is pre-oxidized using embodiment 1 prepares porous carbon materials
As different from Example 2：Phosphoric acid and the mass ratio of the orange peel after pre-oxidation are 5：1, remaining with 2 phase of embodiment
Together, obtained sample is named as OPAC-H3PO4-5。
Charing yield such as the following table 2 of porous charcoal prepared by embodiment 2,3,4,5, wherein
（Molecule is that sample passes through water after carbonizing in above-mentioned formula
Wash, dry after activated carbon product quality）：
。
Orange peel after embodiment 6 is pre-oxidized using embodiment 1 prepares porous carbon materials
The orange peel after being pre-oxidized in embodiment 1 is weighed by assay balance, according to ZnCl2：The matter of orange peel after pre-oxidation
Amount is than being 2:1, weigh ZnCl2, with distilled water stirring and dissolving, then it is uniformly mixed with the orange peel after pre-oxidation, impregnates 12 h
After be put into baking oven to fall moisture evaporation, so that activator is entered material internal and uniformly spread, obtain mixture, by the mixture
It is put into porcelain boat, the porcelain boat is placed in tube furnace, rise to 600 DEG C in a nitrogen atmosphere, heated up later with 10 DEG C/min
To 900 DEG C, 3 h are kept the temperature to be carbonized, are cooled to room temperature.The product after charing is placed in the conical flask of 50 mL later,
It takes the hydrochloric acid solution of 20 mL 20% to be placed in the conical flask with pipette again, is sufficiently mixed stirring, is rushed later with circulating hot water
It is 7 that suction filtration, which is washed, to pH, and the product after washing is placed in baking oven dry 12 h later, is weighed after being cooled to room temperature, by what is obtained
Sample is named as OPAC-ZnCl2-2。
Orange peel after embodiment 7 is pre-oxidized using embodiment 1 prepares porous carbon materials
As different from Example 6：ZnCl2Mass ratio with the orange peel after pre-oxidation is 3：1, remaining with 6 phase of embodiment
Together, obtained sample is named as OPAC-ZnCl2-3。
Orange peel after embodiment 8 is pre-oxidized using embodiment 1 prepares porous carbon materials
As different from Example 6：ZnCl2Mass ratio with the orange peel after pre-oxidation is 4：1, remaining with 6 phase of embodiment
Together, obtained sample is named as OPAC-ZnCl2-4。
Orange peel after embodiment 9 is pre-oxidized using embodiment 1 prepares porous carbon materials
As different from Example 6：ZnCl2Mass ratio with the orange peel after pre-oxidation is 5：1, remaining with 6 phase of embodiment
Together, obtained sample is named as OPAC-ZnCl2-5。
Charing yield such as the following table 3 of porous charcoal prepared by embodiment 6,7,8,9, wherein
（Molecule is that sample passes through water after carbonizing in above-mentioned formula
Wash, dry after activated carbon product quality）：
。
Embodiment 10 carries out XRD tests to the porous carbon materials prepared by embodiment 2-9
The D8 ADVANCE types X-ray diffractometers produced using German Bruker companies are to the porous carbon prepared by embodiment 2-9
Material is tested, and scanning angle is set as 10-90 °, sweep speed be set as 0.04 °/, embodiment 2-5 test results are for example attached
Fig. 1, embodiment 6-9 test result such as attached drawing 2.
It can be seen that from attached drawing 1,2, each sample occurs a larger peak, this peak value at 25 ° or so in 2 θ angles
It coincide substantially with the angle of arrival at the crystal diffraction peak of irregular graphite charcoal, shows that obtained sample is most of unformed
The charcoal of structure and a certain number of irregular graphite charcoal crystallizations.And have also appeared one when 2 θ angles are at 45 ° or so
The peak intensity that peak, the peak value at this peak occur when compared to 2 θ being 25 ° is much smaller, in peak area comparison, 25 ° strong diffraction maximum
Peak area is about 3 times of 45 ° of weak absorbing peak areas.Reason is analyzed, the appearance of 45 ° of diffraction maximums may be since porous charcoal is in work
Catalytic oxidation occurs for the carbon atom and activator that distortion of lattice is caused during change, in graphite microcrystal, and distortion elimination is made to lead
The small absorption peak caused.
Embodiment 11 carries out SEM tests to the product prepared by embodiment 1-9
The table of the product prepared by Quanta 250 model scanning electron microscope observation embodiment 1-9 using FEI Co. of Czech
Face pattern.Sample prepared by Example 1-9 is ground to agate mortar can be by the metallic sieve of 200 mesh, then with conduction
Sample is fixed on sample stage by glue, after metal spraying processing, is opened electronic scanner microscope and is entered working condition, be put into sample, lead to
Cross mobile example platform, adjustment amplification factor, adjustment obtain suitable image and finally take pictures the surface shape for preserving and obtaining each sample
Looks, embodiment 1 pre-oxidize after orange peel SEM test results such as attached drawing 3, the orange peel base porous carbon prepared by embodiment 2-5
The SEM test results of material such as attached drawing 4, the SEM test results such as attached drawing 5 of the porous carbon materials prepared by embodiment 6-9.
It can be seen that from attached drawing 3, the compact structure of the orange peel sample surfaces after pre-oxidation.
It can be seen that from attached drawing 5, sample OPAC-ZnCl2- 2 surface is smooth, and duct is clear, there is apparent duct
Structure mainly exists in, in the form of macropore；Sample OPAC-ZnCl2- 3 gullies increase, aperture smaller, and duct lines is clear；
Sample OPAC-ZnCl2- 4 and sample OPAC-ZnCl2- 5 structures are similar, have abundant central hole structure and are in flakey, and level
It is numerous.
Embodiment 12 carries out specific surface area and opening size test to the porous charcoal prepared by embodiment 2-9
Use the specific surface area pore size determination instrument for the 2QDS-MP-30 that Kang Ta instrument companies of the U.S. produce.Weigh 50 mg embodiments
Porous carbon material prepared by 2-9, in 250 DEG C of 12 h of vacuum outgas, liquid nitrogen manufactures ultra-low temperature surroundings, carries out nitrogen adsorption, desorption
Test.
The adsorption/desorption isotherms such as attached drawing 6 of porous carbon material prepared by embodiment 2-5, graph of pore diameter distribution such as attached drawing 7 are more
The pore structure parameter of hole Carbon Materials such as the following table 4：
。
By attached drawing 6 it can be seen that the thermoisopleth of 4 groups of samples prepared by embodiment 2-5 belongs to IV class adsorption isotherm,
Absorption occurs mainly in pressure larger part, illustrates that material internal is mainly mesoporous, and concentration is compared in distribution.Mesoporous capillary attraction
Generated desorption hysteresis circle is more apparent, also indirect proof a large amount of presence of mesoporous.
It can be obtained from 4 data of upper table, the sample prepared by embodiment 2-5 has larger specific surface area.Wherein embodiment 2
Prepared porous carbon materials OPAC-H3PO4- 2 specific surface area and pore volume has reached 1758 m2/ g and 1.2890 cm3/g。
In conjunction with attached drawing 7 can obtain made from porous carbon material be typical mesopore material, have very least a portion of microcellular structure, and mesoporous
Size mainly in 4.5 nm or so.
The adsorption/desorption isotherms such as attached drawing 8 of porous carbon material prepared by embodiment 6-9, graph of pore diameter distribution such as attached drawing 9 are more
The pore structure parameter of hole Carbon Materials such as the following table 5：
。
Embodiment 12 carries out electrochemical property test to the porous carbon material prepared by embodiment 4,8
Porous carbon materials prepared by embodiment 4,8 are dried, according to porous carbon materials:Polytetrafluoroethylene (PTFE):Carbon black=84:8:8
Mass ratio, the porous carbon materials, polytetrafluoroethylene (PTFE), carbon black are mixed, a small amount of ethyl alcohol is added afterwards and is mixed.It waits mixing
After closing uniformly, it is pressed into thin slice, material disk is made with round card punch.Nickel foam is pressed into sequin with tablet press machine, use is anhydrous
After ethyl alcohol washing by soaking, 12h is placed in oven and dried after 1 h is washed in supersonic wave cleaning machine.The material disk is put into
On nickel foam disk after the drying, 30 s are kept under the pressure of 5 MPa with tablet press machine, finally dry constant weight in an oven
12 h, obtain pole piece, and button-shaped capacitor is made in the pole piece.Using the new Weir Electronics Co., Ltd. production in Shenzhen
CT-3008W-5V5mA-S4 battery test systems carry out constant current charge-discharge test, and data collection interval is 2 s, is followed in total
Ring 20 times.Test condition is the potassium hydroxide electrolyte of 6 mol/L, and charging and discharging currents density is 0.1 A/g, voltage range 0-
1 V。
The 2nd cycle of porous carbon material and the constant current charge-discharge test chart of the 20th this cycle prepared by embodiment 4 is for example attached
Figure 10.The constant current charge-discharge test chart of orange peel base porous carbon material the 2nd cycle and the 20th cycle prepared by embodiment 8
Such as attached drawing 11.
By attached drawing 10,11 it is found that carrying out constant current charge-discharge test to porous carbon material, wherein the change of voltage at any time
Changing has linear relationship, and charging curve is substantially similar to isosceles triangle to discharge curve.After 20 charge-discharge tests,
Constant current charge-discharge curvilinear figure is held essentially constant, and discharge curve voltage drop is smaller, influence of the multiple charge and discharge to material property
Substantially it can ignore, there is good chemical property cyclical stability, illustrate that material possesses good capacitance characteristic, electrode
Reaction is mainly the charge transfer reaction on double layer capacity.When charging curve is changed into discharge curve, as time increases
The reduction of voltage significantly reduces, and illustrates that the internal resistance of material is smaller, is adapted to do electrode material in performance.
The specific capacitance of constant current charge-discharge test uses formulaIt calculates, in formula：I：Electric discharge electricity
Stream, A；Δt：Discharge time, s；ΔU：Voltage drop, V；m：Average quality, g, result of calculation such as the following table 6：
。
It can be seen that from upper table 6, sample made embodiment 2-9 has larger specific surface area and specific capacitance, and in cycle 20
There is specific capacitance value after secondary is a little promoted, be since the chemical property of material after multiple cycle charge-discharge tends towards stability state,
Big hole path is got through in transmission of materials energy, utmostly excites the storing up electricity performance of material.But it fluctuates on the whole
Amount is little, and then reflects the excellent chemical property of sample, is a kind of good storing up electricity material.
The present invention is described in detail above in conjunction with drawings and examples, still, those of skill in the art
Member is it is understood that without departing from the purpose of the present invention, can also carry out each design parameter in above-described embodiment
Change, forms multiple specific embodiments, is the common variation range of the present invention, is no longer described in detail one by one herein.
Claims (6)
1. a kind of preparation method of porous carbon materials, includes the following steps：
（1）Orange peel is cleaned, crushed, is dried；
（2）By step（1）Orange peel after middle drying pre-oxidizes 2~5 h at 200~300 DEG C；
（3）According to activator：Orange peel=2~5 after pre-oxidation：1 mass ratio, by activator and after the pre-oxidation of upper step
Orange peel is mixed, is stirred, and is impregnated later, and mixture is obtained；
（4）By step（3）Middle gained mixture is warming up to 500~700 DEG C under atmosphere of inert gases, later again with 10 DEG C/
Min is warming up to 800~900 DEG C, keeps the temperature 2~4 h；
（5）By step（4）Products therefrom is washed to neutrality, dry later to get.
2. the preparation method of porous carbon materials according to claim 1, which is characterized in that in the step（3）In, it is described
Activator is phosphoric acid or zinc chloride.
3. the preparation method of porous carbon materials according to claim 1, which is characterized in that in the step（3）In, it is described
When activator is solid, before being mixed with the orange peel after the pre-oxidation, by the activator water dissolution；With it is described pre-
After orange peel after oxidation is mixed with dipping, it is dried.
4. the preparation method of porous carbon materials according to claim 1, which is characterized in that in the step（3）In, it is described
Dip time control is 12~14h.
5. the preparation method of porous carbon materials according to claim 1, which is characterized in that in the step（5）In, first will
Products therefrom and mixed in hydrochloric acid stirring, carry out being washed to neutrality later.
6. the preparation method of porous carbon materials according to claim 1, which is characterized in that the inert gas be ammonia,
At least one of nitrogen, hydrogen, argon gas.
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| CN113511654A (en) * | 2021-04-16 | 2021-10-19 | 中国科学院山西煤炭化学研究所 | Capacitance carbon and preparation method thereof |
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Application publication date: 20180828 |