CN101973542B - 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 preparation method of porous carbon material for supercapacitor.
Background technology
Porous carbon material is as the electrode material of ultracapacitor, and its performance depends primarily on inner pore structure, comprises pore-size distribution, hole shape and pore volume etc., and the control hole structure is the key point that obtains the high-performance porous charcoal effectively.The porous charcoal of KOH chemical activation method that development in recent years is got up preparation has that specific area is large, the capacitance high, but its pore-size distribution concentrates in the following range of micropores of 2nm, only is suitable for take inorganic matters such as H2SO4 or KOH as electrolytical aqueous super capacitor.In addition, be 3 ~ 5 times of carbonaceous raw material due to the use amount of KOH, not only cause the waste of KOH, and need to process a large amount of alkaline waste waters, 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 structure and the performance of required porous charcoal, particularly the pore volume in 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 blend technique method, template charring and organic gel method etc., but all exist specific area lower, thereby the low problem of ultracapacitor specific capacity 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 with potassium hydroxide 1: 2.5 in mass ratio～5 again; grinding obtains mixed-powder; then mixed-powder is carried out activation under 400～500 ℃ of lower charings and 800～900 ℃ successively; charing and activation are all carried out under inert gas shielding, and product grinds and namely gets activated carbon for super capacitors after cooling, cleaning, oven dry.The use amount of the method KOH is larger, and production cost is high, and prepared active carbon 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 makes through charing, activation take starch as raw material.But the weight proportion of carbonized material and potassium hydroxide solid up to 1: 4～8.Production cost is high, and prepared active carbon only is suitable for aqueous super capacitor.
CN101177266 has announced a kind of preparation method of active carbon electrode material for super capacitor.Take hard fruit shell as raw material, be placed in ZnCl2 solution oven dry under 110-120 ℃ after fully stirring through fragmentation.Then heat-activated under nitrogen atmosphere and CO2 atmosphere respectively.The specific area of the method preparation is only the 1200m2/g left and right, and is not only lower than electric capacity, and the Cl2 that produces in production process has greater environmental impacts.
Summary of the invention
The present invention aims to provide the preparation method of the porous carbon material for supercapacitor that a kind of specific area is high, the pore volume of pore-size distribution in the 2-5nm scope is high, and is higher than capacitance, chemical property is excellent.
Implementation of the present invention is as follows:
A kind of preparation method of porous carbon material for supercapacitor comprises the following steps,
For improving petroleum coke or pitch coke to the adsorption capacity of complex hydroxide, need to carry out oxidation processes to petroleum coke and pitch coke.In the present invention, this oxidizing solution is 10% H2O2 solution or 10% NaNO3 solution.In addition, described petroleum coke or pitch coke can also be crushed to particle diameter≤100 μ m in the present invention, then join in the filtrate of replenishing after 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 after new liquid to carry out oxidation processes to petroleum coke and pitch coke.
Preferably, the preparation method of porous carbon material for supercapacitor of the present invention, the C/H(hydrocarbon atom ratio of described petroleum coke or pitch coke) and ash content meet the following conditions: 10.0≤C/H≤30.0, ash content≤0.3%.
Preferably, the preparation method of porous carbon material for supercapacitor of the present invention, described composite alkali metal hydroxide is the mixture of potassium hydroxide or NaOH and calcium hydroxide.
Preferably, the preparation method of porous carbon material for supercapacitor of the present invention, in described composite alkali metal hydroxide, the mass ratio of potassium hydroxide or NaOH and calcium hydroxide is 2:(1 ~ 1.5).
Preferably, the preparation method of porous carbon material for supercapacitor of the present invention, described composite alkali metal hydroxide need carry out melting mixing and cooling granulation in advance, and particle diameter is not more than 5mm.
Preferably, the preparation method of porous carbon material for supercapacitor of the present invention needs first activation products are carried out granulation before re-activation is processed, and grain shape is spherical or cylindricality, and particle diameter is 2 ~ 5mm.
Preferably, the preparation method of porous carbon material for supercapacitor of the present invention, in the time of must being heated to by the heating rate of 1 ~ 5 ℃/min temperature when re-activation is processed and being 500 ℃ ~ 600 ℃, begin to pass into steam, the steam flow is 0.5 ~ 1 L/h, and continuing heating rate by 1 ~ 5 ℃/min when passing into steam, to be heated to temperature be 800 ℃ ~ 1000 ℃, and the soak time at 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 NaOH and calcium hydroxide, significantly reduces the consumption of activator simultaneously.I.e. its synergistic activation effect by potassium or sodium element and calcium constituent in potassium hydroxide or NaOH and calcium hydroxide congruent melting compound and be aided with the activation of steam, on the basis that keeps the porous charcoal high specific surface area, improve the pore volume in the 2-5nm scope in porous charcoal.
The present invention can be by selecting suitable petroleum coke or pitch coke, change complex hydroxide kind and to the carbonaceous raw material proportioning and be aided with relevant steam activation technique, can regulate in the larger context the pore structure of porous carbon material, and then obtain the organic system electrode of super capacitor porous carbon material than bigger serface, high mesoporous.
Summary of the invention
Fig. 1 is the step schematic diagram for preparing the method for porous carbon material for supercapacitor of the present invention;
Fig. 2 is the graph of pore diameter distribution of the porous carbon material for supercapacitor for preparing of the present invention.
Embodiment
As shown in Figure 1, the method for preparing porous carbon material for supercapacitor of the present invention comprises that as shown in the figure step 1 is to step 5.Give below in conjunction with specific embodiments further instruction.
Get petroleum coke 100 g, join in the H2O2 solution of 2000ml10%, mix rear dipping 4 hours, deviate from remaining H2O2 solution with centrifuge after filtering.The KOH that with the petroleum coke raw material after 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 heating rate of 2 ℃/min.After granulation, in the tube furnace of packing into, being heated to temperature by the heating rate of 2 ℃/min is 500 ℃, begins to pass into steam and carries out re-activation and process, and the steam flow is 0.5 L/h.Continuing heating rate by 2 ℃/min, to be heated to temperature be 800 ℃, activates 1h at this temperature.Add the water cyclic washing after product to be activated is cooling to pH≤10, add 10% HCl solution to soak 5 hours, continue to add water washing to pH≤8, after filtering, oven dry under 100 ~ 110 ℃, namely get the porous carbon material of preparation.
It is 5 ~ 10 μ m that above-mentioned porous carbon material is finely ground to particle diameter with ball mill, then is warming up to 500 ℃ with 2 ℃/min speed carries out vacuum heat under the vacuum condition of 0.01MPa, and the processing 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 area is 1720 m2/g, pore volume is 1.3 cm3/g, average 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 good charge-discharge performance.
Get petroleum coke 100 g, join in the NaNO3 solution of 2000ml10%, mix rear dipping 6 hours, deviate from remaining NaNO3 solution with centrifuge after filtering.The KOH that with the petroleum coke raw material after 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 heating rate of 2 ℃/min.After granulation, in the tube furnace of packing into, being heated to temperature by the heating rate of 2 ℃/min is 600 ℃, begins to pass into steam and carries out re-activation and process, and the steam flow is 0.5 L/h.Continuing heating rate by 2 ℃/min, to be heated to temperature be 800 ℃, activates 1h at this temperature.Add the water cyclic washing after product to be activated is cooling to pH≤10, add 10% HCl solution to soak 5 hours, continue to add water washing to pH≤8, after filtering, oven dry under 100 ~ 110 ℃, namely get the porous carbon material of preparation.
It is 5 ~ 10 μ m that above-mentioned porous carbon material is finely ground to particle diameter with ball mill, then is warming up to 500 ℃ with 2 ℃/min speed carries out vacuum heat under the vacuum condition of 0.01MPa, and the processing 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 area is 1720 m2/g, pore volume is 1.4 cm3/g, average 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 good charge-discharge performance.
Get pitch coke 100 g, join in the H2O2 solution of 1500ml10%, mix rear dipping 5 hours, deviate from remaining H2O2 solution with centrifuge after filtering.The NaOH that with the petroleum coke raw material after 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 heating rate of 2 ℃/min.After granulation, in the tube furnace of packing into, being heated to temperature by the heating rate of 2 ℃/min is 600 ℃, begins to pass into steam and carries out re-activation and process, and the steam flow is 0.8 L/h.Continuing heating rate by 2 ℃/min, to be heated to temperature be 900 ℃, activates 1.5h at this temperature.Add the water cyclic washing after product to be activated is cooling to pH≤10, add 10% HCl solution to soak 5 hours, continue to add water washing to pH≤8, after filtering, oven dry under 100 ~ 110 ℃, namely get the porous carbon material of preparation.
It is 5 ~ 15 μ m that above-mentioned porous carbon material is finely ground to particle diameter with ball mill, then is warming up to 500 ℃ with 2 ℃/min speed carries out vacuum heat under the vacuum condition of 0.01MPa, and the processing 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 area is 1760 m2/g, pore volume is 1.35 cm3/g, average 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 good charge-discharge performance.
Get pitch coke 100 g, join in the NaNO3 solution of 2000ml10%, mix rear dipping 6 hours, deviate from remaining NaNO3 solution with centrifuge after filtering.The NaOH that with the pitch coke raw material after 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 heating rate of 2 ℃/min.After granulation, in the tube furnace of packing into, being heated to temperature by the heating rate of 2 ℃/min is 600 ℃, begins to pass into steam and carries out re-activation and process, and the steam flow is 0.8 L/h.Continuing heating rate by 2 ℃/min, to be heated to temperature be 850 ℃, activates 1.5h at this temperature.Add the water cyclic washing after product to be activated is cooling to pH≤10, add 10% HCl solution to soak 5 hours, continue to add water washing to pH≤8, after filtering, oven dry under 100 ~ 110 ℃, namely get the porous carbon material of preparation.
It is 5 ~ 15 μ m that above-mentioned porous carbon material is finely ground to particle diameter with ball mill, then is warming up to 600 ℃ with 2 ℃/min speed carries out vacuum heat under the vacuum condition of 0.01MPa, and the processing 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 area is 1720 m2/g, pore volume is 1.3 cm3/g, average 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 good charge-discharge performance.
Although embodiment of the present invention are open as above, but it is not restricted to listed utilization in specification and execution mode, 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 do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and the legend of describing.
Claims (3)
1. the preparation method of a porous carbon material for supercapacitor is characterized in that: comprises the following steps,
Step 1, pitch coke is crushed to particle diameter≤100 μ m, then joins a certain amount of 10% NaNO
3In solution, mix under rear normal temperature standing 4-8 hour, deviates from remaining NaNO with centrifuge after filtering
3Solution, wherein petroleum coke or pitch coke and 10% NaNO
3The mass ratio of solution is 1:(1.5～2.5);
Step 2, the product of step 1 gained is mixed with compound alkali, described compound alkali is the mixture of potassium hydroxide or NaOH and calcium hydroxide, heating makes compound alkali fusion carry out simultaneously first activation processing, the mass ratio of described pitch coke and compound alkali is 1:(1～2), and first priming reaction condition is: 1 ~ 10 ℃/min of heating rate, reaction temperature is 300 ~ 350 ℃, and the reaction time is 1 ~ 4h;
Step 3, after being granulated to the 50-200 order while hot, the step 2 products therefrom puts into tube furnace, being heated to temperature by the heating rate of 1～5 ℃/min is 500 ℃ ~ 600 ℃, then begin to pass into steam and carry out the re-activation processing, and the steam flow is 0.5 ~ 1L/h, continuing afterwards heating rate by 1 ~ 5 ℃/min, to be heated to temperature be 800 ℃ ~ 1000 ℃, and soak time is 0.5 ~ 1h at 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 to pH≤8, after filtering under 100 ~ 110 ℃ oven dry make porous carbon material;
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, heating rate are that 1 ~ 5 ℃/min, heat treatment temperature are that 450 ~ 700 ℃ and temperature retention time are to carry out vacuum high-temperature heat treatment under the condition of 1 ~ 3h at pressure again, thereby make the electrode of super capacitor porous carbon material;
Wherein, the hydrocarbon atom of described pitch coke meets the following conditions than C/H and ash content: 10.0≤C/H≤30.0, ash content≤0.3%;
Wherein, in the preparation method of described porous carbon material for supercapacitor, in described compound alkali, the mass ratio of potassium hydroxide or NaOH and calcium hydroxide is 2:(1～1.5).
2. the preparation method of porous carbon material for supercapacitor as claimed in claim 1, it is characterized in that: described compound alkali need carry out melting mixing and cooling granulation in advance, and particle diameter is not more than 5mm.
3. the preparation method of porous carbon material for supercapacitor as claimed in claim 1 is characterized in that: need before re-activation is processed carry out granulation to first activation products, grain shape is spherical or cylindricality, and particle diameter is 2 ~ 5mm.
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| CN104495842B (en) * | 2014-12-29 | 2017-05-24 | 新疆大学 | Method for preparing activated carbon by partially substituting potassium hydroxide by calcium hydroxide |
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| CN114122393A (en) * | 2021-11-11 | 2022-03-01 | 深圳市翔丰华科技股份有限公司 | Preparation method of high-power-density negative electrode material for lithium ion battery |
| CN114275782B (en) * | 2021-12-10 | 2023-07-28 | 海南大学 | Method for preparing full-microporous activated carbon by low-temperature alkali melting method |
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Address after: Nanshan District Xueyuan Road in Shenzhen city of Guangdong province 518057 No. 1001 Nanshan Chi Park Bl Building 5 floor Patentee after: TIG TECHNOLOGY CO., LTD. Address before: 518057 Guangdong city of Shenzhen province Nanshan District South Road 009 Chinese Technology Development Institute Technology Park building three, 202 building, room 206 Patentee before: Shenzhen City TIG New Energy Technologies Co., Ltd. |