CN101973542A - Preparation method of porous carbon material for supercapacitor - Google Patents
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Abstract
The invention provides a preparation method of porous carbon materials for a supercapacitor, in the preparation method, with refinery coke or pitch coke as raw materials and composite alkali metal hydroxide as an activating agent, the porous carbon material is prepared by using a two-stage activation process. The obtained porous carbon material has a specific surface area of 1500-1800m2/g, has good adsorptive property and narrow aperture distribution, and the aperture distribution can be regulated according to requirements. A supercapacitor electrode made of the porous carbon materials has the characteristics of high capacity, high power, long cycle life, and the like. The preparation method has the characteristics of low hydroxid usage, simple production technology, and the like and is convenient to practicability.
Description
Technical field
The present invention relates to the preparation method of porous carbon material, particularly the ultracapacitor preparation method of porous carbon material.
Background technology
Porous carbon material is as the electrode materials of ultracapacitor, and its performance depends primarily on inner pore structure, comprises pore size distribution, hole shape and pore volume etc., and the control punch structure is the key point that obtains the high-performance porous charcoal effectively.The porous charcoal of the KOH chemical activation method preparation that development in recent years is got up has characteristics such as specific surface area is big, electrical capacity height, but its pore size distribution concentrates in the following range of micropores of 2nm, and only being suitable for inorganicss such as H2SO4 or KOH is electrolytical aqueous super capacitor.In addition,, not only cause the waste of KOH, and need to handle a large amount of alkaline waste waters because the usage quantity of KOH is 3 ~ 5 times of carbonaceous raw material, also very harsh to the requirement of producing.Continuous expansion along with the supercapacitor applications field, organic system ultracapacitor with height ratio capacity and high-specific-power becomes the main flow in market, also to the structure and the performance of required porous charcoal, particularly the pore volume in the 2-5nm scope in the porous charcoal pore size distribution is had higher requirement simultaneously.In order to improve the pore volume in the 2-5nm scope in the porous charcoal pore size distribution, people have been developed catalytic activation method, polymer blending charring, template charring and organic gel method etc., but all exist specific surface area lower, thereby the low problem of ultracapacitor specific storage of preparation.
More existing patents of invention have been introduced the preparation method of relevant porous charcoal therewith.
CN101648706 has announced a kind of production method of activated carbon for super capacitors; petroleum coke powder is broken to the powder of 200～500 order sizes; mix by mass ratio 1: 2.5～5 with potassium hydroxide again; grinding obtains mixed powder; then mixed powder is carried out 400～500 ℃ of following charings and 800～900 ℃ of activation down successively; charing and activation are all carried out under protection of inert gas, and product grinds and promptly gets activated carbon for super capacitors after cooling, cleaning, oven dry.The usage quantity of this method KOH is bigger, the production cost height, and prepared gac only is suitable for aqueous super capacitor.
CN101525132 has announced a kind of activated carbon for super capacitors and preparation method thereof.Described activated carbon for super capacitors is raw material with starch, makes through charing, activation.But carbonized material and potassium hydroxide solid weight proportion up to 1: 4～8.The production cost height, prepared gac only is suitable for aqueous super capacitor.
CN101177266 has announced a kind of preparation method of active carbon electrode material for super capacitor.With the hard fruit shell is raw material, is placed in the ZnCl2 solution through fragmentation, fully stirs the back 110-120 ℃ of oven dry down.Heat-activated under nitrogen atmosphere and CO2 atmosphere respectively then.The specific surface area of this method preparation only is about 1200m2/g, and is not only lower than electric capacity, and the Cl2 that produces in the production process has greater environmental impacts.
Summary of the invention
The present invention aims to provide the preparation method of the high ultracapacitor of a kind of specific surface area height, the pore volume of pore size distribution in the 2-5nm scope with porous carbon material, and is more higher than capacitance, chemical property is excellent.
Implementation of the present invention is as follows:
A kind of ultracapacitor may further comprise the steps with the preparation method of porous carbon material,
For improving refinery coke or pitch coke, need carry out oxide treatment to refinery coke and pitch coke to the adsorptive power of complex hydroxide.This oxidizing solution is 10% H2O2 solution or 10% NaNO3 solution among the present invention.In addition, described refinery coke or pitch coke can also be crushed to particle diameter≤100 μ m among the present invention, join then in the filtrate of replenishing behind the new liquid, and described additional new liquid is 15% H2O2 solution, 15% NaNO3 solution, magnitude of recruitment be about remaining H2O2 solution or NaNO3 solution quality 30 ~ 50%, thereby utilize this filtrate of replenishing behind new liquid that refinery coke and pitch coke are carried out oxide treatment.
Preferably, ultracapacitor of the present invention is with the preparation method of porous carbon material, the C/H(hydrocarbon atom of described refinery coke or pitch coke than) and ash content meet the following conditions: 10.0≤C/H≤30.0, ash content≤0.3%.
Preferably, the ultracapacitor of the present invention preparation method of porous carbon material, described composite alkali metal oxyhydroxide is the mixture of potassium hydroxide or sodium hydroxide and calcium hydroxide.
Preferably, the ultracapacitor of the present invention preparation method of porous carbon material, the mass ratio of potassium hydroxide or sodium hydroxide and calcium hydroxide is 2:(1 ~ 1.5 in the described composite alkali metal oxyhydroxide).
Preferably, the ultracapacitor of the present invention preparation method of porous carbon material, described composite alkali metal oxyhydroxide need carry out melting mixing and cooling granulation in advance, and particle diameter is not more than 5mm.
Preferably, ultracapacitor of the present invention needs first activation products are carried out granulation before re-activation is handled with the preparation method of porous carbon material, and particle shape is sphere or cylindricality, and particle diameter is 2 ~ 5mm.
Preferably, the ultracapacitor of the present invention preparation method of porous carbon material, re-activation must be heated to temperature by the temperature rise rate of 1 ~ 5 ℃/min when being 500 ℃ ~ 600 ℃ when handling, begin to feed water vapour, the water vapour flow is 0.5 ~ 1 L/h, and continuing temperature rise rate by 1 ~ 5 ℃/min when feeding water vapour, to be heated to temperature be 800 ℃ ~ 1000 ℃, and the soak time under this temperature is 0.5 ~ 1h.
The present invention is improved on traditional KOH chemical activation method basis, with the single KOH activator of the mixture replacing of potassium hydroxide or sodium hydroxide and calcium hydroxide, reduces the consumption of activator simultaneously significantly.I.e. its synergistic activation effect by potassium or sodium element and calcium constituent in potassium hydroxide or sodium hydroxide and the calcium hydroxide congruent melting compound and be aided with the activation of water vapour, on the basis that keeps the porous charcoal high specific surface area, improve the pore volume in the 2-5nm scope in the porous charcoal.
The present invention can be by selecting suitable refinery coke or pitch coke, change complex hydroxide kind with the carbonaceous raw material proportioning and be aided with relevant steam activation technology, can regulate the pore structure of porous carbon material in the larger context, and then obtain organic system electrode of super capacitor porous carbon material than bigger serface, senior middle school's porosity.
Description of drawings
Fig. 1 is the step synoptic diagram for preparing ultracapacitor with the method for porous carbon material of the present invention;
Fig. 2 uses the graph of pore diameter distribution of porous carbon material for the ultracapacitor of the present invention's preparation.
Embodiment
As shown in Figure 1, the ultracapacitor for preparing of the present invention comprises that with the method for porous carbon material as shown in the figure step 1 is to step 5.Give further instruction below in conjunction with specific embodiments.
Get refinery coke 100 g, join in the H2O2 solution of 2000ml10%, mixed the back dipping 4 hours, filter the back and deviate from remaining H2O2 solution with whizzer.The KOH that with refinery coke raw material after the above-mentioned oxidation and 150g mass ratio is 2:1.5 mixes with the mixture of Ca (OH) 2, slowly is heated to 300 ~ 350 ℃, stirring reaction 2 hours by the temperature rise rate of 2 ℃/min.After the granulation, in the tube furnace of packing into, being heated to temperature by the temperature rise rate of 2 ℃/min is 500 ℃, begins to feed water vapour and carries out re-activation and handle, and the water vapour flow is 0.5 L/h.Continuing temperature rise rate by 2 ℃/min, to be heated to temperature be 800 ℃, activates 1h under this temperature.Add the water repetitive scrubbing to pH≤10 after the product cooling to be activated, the HCl solution soaking of adding 10% 5 hours continues to add water washing to pH≤8, filters the back 100 ~ 110 ℃ of oven dry down, promptly gets the porous carbon material for preparing.
It is 5 ~ 10 μ m that above-mentioned porous carbon material is finely ground to particle diameter with ball mill, is warming up to 500 ℃ with 2 ℃/min speed again under the vacuum condition of 0.01MPa and carries out vacuum heat treatment, and the treatment time is 1h, finally obtains the electrode of super capacitor porous carbon material.
After tested, the tap density of above-mentioned porous carbon material is 0.42g/cm3, specific surface area is 1720 m2/g, pore volume is 1.3 cm3/g, mean pore size is 2.3 nm, and the ratio electric capacity when current density is 1 mA/cm2 in 1 mol/L Et4NBF4/PC organic electrolyte is 185 F/g, and current density increases 20 times, still reach 165F/g than electric capacity, show the favorable charge-discharge performance.
Get refinery coke 100 g, join in the NaNO3 solution of 2000ml10%, mixed the back dipping 6 hours, filter the back and deviate from remaining NaNO3 solution with whizzer.The KOH that with refinery coke raw material after the above-mentioned oxidation and 150g mass ratio is 2:1.5 mixes with the mixture of Ca (OH) 2, slowly is heated to 350 ℃, stirring reaction 2 hours by the temperature rise rate of 2 ℃/min.After the granulation, in the tube furnace of packing into, being heated to temperature by the temperature rise rate of 2 ℃/min is 600 ℃, begins to feed water vapour and carries out re-activation and handle, and the water vapour flow is 0.5 L/h.Continuing temperature rise rate by 2 ℃/min, to be heated to temperature be 800 ℃, activates 1h under this temperature.Add the water repetitive scrubbing to pH≤10 after the product cooling to be activated, the HCl solution soaking of adding 10% 5 hours continues to add water washing to pH≤8, filters the back 100 ~ 110 ℃ of oven dry down, promptly gets the porous carbon material for preparing.
It is 5 ~ 10 μ m that above-mentioned porous carbon material is finely ground to particle diameter with ball mill, is warming up to 500 ℃ with 2 ℃/min speed again under the vacuum condition of 0.01MPa and carries out vacuum heat treatment, and the treatment time is 1h, finally obtains the electrode of super capacitor porous carbon material.
After tested, the tap density of above-mentioned porous carbon material is 0.42g/cm3, specific surface area is 1720 m2/g, pore volume is 1.4 cm3/g, mean pore size is 2.4 nm, and the ratio electric capacity when current density is 1 mA/cm2 in 1 mol/L Et4NBF4/PC organic electrolyte is 180 F/g, and current density increases 20 times, still reach 160F/g than electric capacity, show the favorable charge-discharge performance.
Get pitch coke 100 g, join in the H2O2 solution of 1500ml10%, mixed the back dipping 5 hours, filter the back and deviate from remaining H2O2 solution with whizzer.The NaOH that with refinery coke raw material after the above-mentioned oxidation and 200g mass ratio is 2:1 mixes with the mixture of Ca (OH) 2, slowly is heated to 350 ℃, stirring reaction 3 hours by the temperature rise rate of 2 ℃/min.After the granulation, in the tube furnace of packing into, being heated to temperature by the temperature rise rate of 2 ℃/min is 600 ℃, begins to feed water vapour and carries out re-activation and handle, and the water vapour flow is 0.8 L/h.Continuing temperature rise rate by 2 ℃/min, to be heated to temperature be 900 ℃, activates 1.5h under this temperature.Add the water repetitive scrubbing to pH≤10 after the product cooling to be activated, the HCl solution soaking of adding 10% 5 hours continues to add water washing to pH≤8, filters the back 100 ~ 110 ℃ of oven dry down, promptly gets the porous carbon material for preparing.
It is 5 ~ 15 μ m that above-mentioned porous carbon material is finely ground to particle diameter with ball mill, is warming up to 500 ℃ with 2 ℃/min speed again under the vacuum condition of 0.01MPa and carries out vacuum heat treatment, and the treatment time is 1h, finally obtains the electrode of super capacitor porous carbon material.
After tested, the tap density of above-mentioned porous carbon material is 0.43g/cm3, specific surface area is 1760 m2/g, pore volume is 1.35 cm3/g, mean pore size is 2.3 nm, and the ratio electric capacity when current density is 1 mA/cm2 in 1 mol/L Et4NBF4/PC organic electrolyte is 182 F/g, and current density increases 20 times, still reach 160F/g than electric capacity, show the favorable charge-discharge performance.
Get pitch coke 100 g, join in the NaNO3 solution of 2000ml10%, mixed the back dipping 6 hours, filter the back and deviate from remaining NaNO3 solution with whizzer.The NaOH that with pitch coke raw material after the above-mentioned oxidation and 150g mass ratio is 2:1 mixes with the mixture of Ca (OH) 2, slowly is heated to 350 ℃, stirring reaction 3 hours by the temperature rise rate of 2 ℃/min.After the granulation, in the tube furnace of packing into, being heated to temperature by the temperature rise rate of 2 ℃/min is 600 ℃, begins to feed water vapour and carries out re-activation and handle, and the water vapour flow is 0.8 L/h.Continuing temperature rise rate by 2 ℃/min, to be heated to temperature be 850 ℃, activates 1.5h under this temperature.Add the water repetitive scrubbing to pH≤10 after the product cooling to be activated, the HCl solution soaking of adding 10% 5 hours continues to add water washing to pH≤8, filters the back 100 ~ 110 ℃ of oven dry down, promptly gets the porous carbon material for preparing.
It is 5 ~ 15 μ m that above-mentioned porous carbon material is finely ground to particle diameter with ball mill, is warming up to 600 ℃ with 2 ℃/min speed again under the vacuum condition of 0.01MPa and carries out vacuum heat treatment, and the treatment time is 1h, finally obtains the electrode of super capacitor porous carbon material.
After tested, the tap density of above-mentioned porous carbon material is 0.42g/cm3, specific surface area is 1720 m2/g, pore volume is 1.3 cm3/g, mean pore size is 2.2 nm, and the ratio electric capacity when current density is 1 mA/cm2 in 1 mol/L Et4NBF4/PC organic electrolyte is 184 F/g, and current density increases 20 times, still reach 158F/g than electric capacity, show the favorable charge-discharge performance.
Although embodiment of the present invention are open as above, but it is not restricted to listed utilization in specification sheets and the embodiment, it can be applied to various suitable the field of the invention fully, for those skilled in the art, can easily realize other modification, therefore under the universal that does not deviate from claim and equivalency range and limited, the legend that the present invention is not limited to specific details and illustrates here and describe.
Claims (8)
1. a ultracapacitor is characterized in that with the preparation method of porous carbon material: may further comprise the steps,
Step 1, refinery coke or pitch coke are crushed to particle diameter≤100 μ m, join then in the NaNO3 solution of a certain amount of 10% H2O2 solution or 10%, mix under the normal temperature of back and left standstill 4-8 hour, filter the back and deviates from remaining H2O2 solution or NaNO3 solution with whizzer, wherein the mass ratio of refinery coke or pitch coke and 10% H2O2 solution or 10% NaNO3 solution is 1:(1.5～2.5);
Step 2, the product of step 1 gained is mixed with composite alkali metal oxyhydroxide, heating makes the fusion of composite alkali metal oxyhydroxide carry out first activation treatment simultaneously, the mass ratio of described refinery coke or pitch coke and composite alkali metal oxyhydroxide is 1:(1～2), and first priming reaction condition is: 1 ~ 10 ℃/min of temperature rise rate, temperature of reaction is 300 ~ 350 ℃, and the reaction times is 1 ~ 4h;
Step 3, put into tube furnace after the step 2 products therefrom is granulated to the 50-200 order while hot, being heated to temperature by the temperature rise rate of 1 ~ 5 ℃/min is 500 ℃ ~ 600 ℃, begin to feed water vapour then and carry out the re-activation processing, and the water vapour flow is 0.5 ~ 1 L/h, continuing temperature rise rate by 1 ~ 5 ℃/min afterwards, to be heated to temperature be 800 ℃ ~ 1000 ℃, and soak time is 0.5 ~ 1h under this temperature;
Step 4, step 3 gained activation products are added water washing to pH≤10, add 10% HCl solution, soaked 5 ~ 8 hours, continue to add water washing, filter the back and dry down at 100 ~ 110 ℃ and make porous carbon material to pH≤8.
Step 5, the prepared porous carbon material of step 4 is carried out ball milling and screening, selecting particle diameter is the powder of 5 ~ 20 μ m, be that 0.01MPa ~ 0.03MPa, temperature rise rate are that 1 ~ 5 ℃/min, thermal treatment temp are that 450 ~ 700 ℃ and soaking time are to carry out vacuum high-temperature thermal treatment under the condition of 1 ~ 3h at pressure again, thereby make the electrode of super capacitor porous carbon material.
2. the ultracapacitor as claimed in claim 1 preparation method of porous carbon material, it is characterized in that: described refinery coke or pitch coke can also be crushed to particle diameter≤100 μ m, join the filtrate of replenishing behind the new liquid then, and described additional new liquid is 15% H2O2 solution, 15% NaNO3 solution, magnitude of recruitment be about remaining H2O2 solution or NaNO3 solution quality 30 ~ 50%.
3. ultracapacitor as claimed in claim 1 is characterized in that with the preparation method of porous carbon material: the C/H(hydrocarbon atom of described refinery coke or pitch coke than) and ash content meet the following conditions: 10.0≤C/H≤30.0, ash content≤0.3%.
4. the ultracapacitor as claimed in claim 1 preparation method of porous carbon material, it is characterized in that: described composite alkali metal oxyhydroxide is the mixture of potassium hydroxide or sodium hydroxide and calcium hydroxide.
5. the ultracapacitor as claimed in claim 4 preparation method of porous carbon material, it is characterized in that: the mass ratio of potassium hydroxide or sodium hydroxide and calcium hydroxide is 2:(1 ~ 1.5 in the described composite alkali metal oxyhydroxide).
6. the ultracapacitor as claimed in claim 1 preparation method of porous carbon material, it is characterized in that: described composite alkali metal oxyhydroxide need carry out melting mixing and cooling granulation in advance, and particle diameter is not more than 5mm.
7. the ultracapacitor as claimed in claim 1 preparation method of porous carbon material is characterized in that: need before re-activation is handled carry out granulation to first activation products, particle shape is sphere or cylindricality, and particle diameter is 2 ~ 5mm.
8. the ultracapacitor as claimed in claim 1 preparation method of porous carbon material, it is characterized in that: re-activation must be heated to temperature by the temperature rise rate of 1 ~ 5 ℃/min when being 500 ℃ ~ 600 ℃ when handling, begin to feed water vapour, the water vapour flow is 0.5 ~ 1 L/h, and continuing temperature rise rate by 1 ~ 5 ℃/min when feeding water vapour, to be heated to temperature be 800 ℃ ~ 1000 ℃, and the soak time under this temperature is 0.5 ~ 1h.
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