CN103979530A - Method for preparing porous carbon for electrochemical capacitor from egg white used as raw material - Google Patents
Method for preparing porous carbon for electrochemical capacitor from egg white used as raw material Download PDFInfo
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- CN103979530A CN103979530A CN201410258484.XA CN201410258484A CN103979530A CN 103979530 A CN103979530 A CN 103979530A CN 201410258484 A CN201410258484 A CN 201410258484A CN 103979530 A CN103979530 A CN 103979530A
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- egg white
- electrochemical capacitor
- porous carbon
- raw material
- acid
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Abstract
The invention discloses a method for preparing a porous carbon material for an electrochemical capacitor from egg white used as a raw material, and belongs to the technical field of novel energy sources. The preparation method comprises the following steps: firstly adding neutral salts or an organic solvent into egg white used as the raw material to separate out protein, and carrying out high-temperature pre-carbonization on the protein so as to obtain a carbon precursor; then obtaining the high-performance porous carbon material for the supercapacitor by use of an alkali metal hydroxide activation method, wherein egg white is taken as a raw material. The method disclosed by the invention is capable of using biological materials and has the advantages of novel raw materials, low cost and wide sources, the porous carbon material prepared has the advantages of rich microporous/mesoporous multi-level pore structures, high specific surface area and excellent electrochemical capacitance performance and has broad application prospects in the field of electrochemical capacitors.
Description
Technical field
The invention belongs to technical field of new energies, be specifically related to the preparation method of porous carbon material for a kind of electrochemical capacitor.
Background technology
Electrochemical capacitor is called again ultracapacitor, is a kind of novel power-type electronic devices and components.It has the features such as specific energy is high, specific power is high and have extended cycle life, be widely used in the numerous areas such as microcomputer standby power supply, solar charger, warning device, household electrical appliance, camera flashlamp and aerospace high impulse producer, especially in electromobile field, caused extensive attention.
Porous carbon material is as one of main electrode material of electrochemical capacitor, and its energy storage mechanism is realized its efficient storage lotus by forming electric double layer capacitance.At present, the porous carbon material for electrochemical capacitor mainly concentrates on gac, activated carbon fiber, charcoal-aero gel, carbon nanotube and template charcoal etc.Due to the plurality of advantages such as its high-specific surface area, high porosity, production technique be simple and cheap, porous carbon material is subject to investigator always to be favored, and becomes one of commercial electrochemical capacitor electrode material.Because the raw material sources of porous carbon material are extensive, Chinese scholars is selected different carbonaceous presomas, through specific heat treatment process preparation, is had the porous charcoal of certain specific surface area and pore size distribution, and then is applied to the research of electrochemical capacitor.
Porous charcoal almost can be prepared with any carbonaceous material, as: timber, sawdust, coal, peat class, shell, fruit stone, bagasse, oil waste material, waste or used plastics, Leather Waste, damaged tire, papermaking waste material and municipal wastes etc.The production technique of different material is difference slightly also, but is all to carry out charing and follow-up activation after modulation.The method of activation has two kinds of physically activated and chemical activations.Wherein, physically activated is mainly at water vapour, CO
2under the existence of air, in 700-1000 ℃, heat-treat.Chemical activation is to utilize some acid or alkali to carry out chemical etching, to increase pore structure, specific surface area and the surface functional group of material, or with tensio-active agent, material is carried out to chemical modification, to improve the wetting property of electrolytic solution in material, thereby carries high specific capacitance.Due to its unique advantage, chemical activation and modification ratio are physically activated to be applied more generally.
Egg is food very common in a kind of human lives, but regrettably, up to now, also about usining egg white, does not prepare the relevant report of porous charcoal as raw material.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides a kind of method of egg white as raw material making electrochemical capacitor use porous carbon material of take, intention is novel, and prepared porous carbon material has and enriches multistage micro/meso porous pore passage structure, high-specific surface area and the good advantages such as electrochemical capacitor characteristic.
A kind of egg white that utilizes of the present invention is made the method for porous carbon material for electrochemical capacitor for raw material, comprises the following steps:
(1) in egg white liquid, add neutral salt or organic solvent to separate out albumen, the albumen obtaining is placed in vacuum drying oven and is dried;
Described neutral salt is one or more in chlorate, vitriol and nitrate; Described organic solvent is one or both mixing of dehydrated alcohol, acetone;
(2) after the dried protein material of step (1) is ground, put into tube furnace, in rare gas element, with 1～10 ℃/min of speed speed, be warmed up to pre-carbonization temperature, at this temperature, be incubated after 2h, obtain carbon precursor;
Described rare gas element is one or more in nitrogen, argon gas, helium; Described pre-carbonization temperature is 450～600 ℃;
(3) carbon precursor step (2) being obtained evenly mixes by a certain percentage with alkali metal hydroxide, then in rare gas element, with speed, 1～10 ℃/min is warmed up to activation temperature, and be incubated 1～10h, under this activation temperature, carbon precursor is carried out to activation treatment, obtain activation products;
Described carbon precursor and the mass ratio of alkali metal hydroxide are 1:2～5; Described alkali metal hydroxide is the mixture of the one or both in potassium hydroxide, sodium hydroxide; Described rare gas element is one or more in nitrogen, argon gas, helium; Described activation temperature is 700～1000 ℃;
(4) acid neutralization for the activation products that step (3) obtained, then extremely neutral by washed with de-ionized water, dry, after grinding, obtain electrochemical capacitor porous charcoal;
Described acid is one or more in hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid.
As a kind of optimization, in described step (1), with organic solvent, separate out albumen, this organic solvent is dehydrated alcohol; In described step (2), rare gas element is nitrogen, and pre-carbonization temperature is 600 ℃; In described step (3), the mass ratio of carbon precursor and alkali metal hydroxide is 1:3, and alkali metal hydroxide is potassium hydroxide, and rare gas element is nitrogen, and activation temperature is 800 ℃; In described step (4), acid is hydrochloric acid.
Compared with prior art, the present invention has following technique effect:
(1) intention is novel, utilizes a kind of brand-new biological material to prepare electrochemical capacitor porous carbon material, and abundant raw material and cheap and easy to get, is conducive to industrialized realization;
(2) the concrete special mechanics of biological tissue of egg white is the important prerequisite of preparing high specific surface area in use for electrochemical capacitor porous charcoal, is that activator forms the basis of enriching multistage micro/meso porous structure in charcoal forerunner;
(3) electrochemical capacitor that prepared by the present invention with porous carbon material have abundant micro-/Jie's multi-stage artery structure and high-specific surface area (1450m
2g
-1), large and high rate performance is good by its prepared porous carbon electrode specific storage; Experiment showed, that prepared porous carbon material is in 6M KOH aqueous electrolyte, its specific discharge capacity is 347F g
-1; And with 1M (C
2h
5)
4nBF
4/ Propylene carbonate solution is electrolytic solution, and the symmetrical electrochemical capacitor of button that the porous carbon material that makes of take is assembled as electrode has high-energy-density density and good specific power characteristic.
Accompanying drawing explanation
Fig. 1 is the Ar adsorption desorption hysteresis loop figure of prepared porous carbon material in the embodiment of the present invention 1;
From figure, Ar adsorption desorption hysteresis loop shape can be found out, with the prepared porous carbon material of egg white, has abundant mesoporous and micropore canals structure.By this figure, can calculate its specific surface area is 1450m
2g
-1.
Fig. 2 is the pore size distribution curve figure of prepared porous carbon material in the embodiment of the present invention 1;
As can be seen from this figure, the main aperture of prepared porous carbon material is mainly distributed between 0.5-4nm.
Fig. 3 is specific storage graphic representation under the different current densities of prepared porous carbon material in the embodiment of the present invention 1;
As can be seen from this figure, prepared porous carbon material is in the electrolytic solution of 6M KOH, at 0.2A g
-1current density under, it is 347F g than electric capacity
-1.When current density is brought up to 10A g
-1time, its quality still can remain on 160F g than electric capacity
-1.
Fig. 4 is the Ragone graphic representation of prepared porous carbon material in embodiment 2 in the embodiment of the present invention 1;
As can be seen from the figure, with 1M (C
2h
5)
4nBF
4/ Propylene carbonate solution is electrolytic solution, and the porous carbon material making is that specific energy and the specific power density of the symmetrical electrochemical capacitor of button of electrode assembling one-tenth can reach 16Wh kg respectively
-1with 3750W kg
-1.
Embodiment
The following examples will be further described the present invention, but not thereby limiting the invention.
Embodiment 1
In Ma'an Mountain food market, buy common egg, get the egg white solution of two pieces of eggs in beaker, toward pouring 200mL dehydrated alcohol in beaker, separate out albumen, the albumen of separating out is after 60 ℃ of oven dry of vacuum drying oven, get 10g and be placed in quartz boat, speed with 5 ℃/min in being connected with the tube furnace of nitrogen is warmed up to 600 ℃, insulation 2h.Then the carbon precursor above-mentioned pre-charing being obtained in mass ratio 1:3 and activator fully mixes, and activator is potassium hydroxide, then under nitrogen atmosphere, with the speed of 5 ℃/min, is warmed up to 800 ℃ and activates, and soak time is 2h.By 0.1mol salt acid elution for above-mentioned activation products, then by washed with de-ionized water to neutrality, be dried, obtain porous charcoal.As shown in Figure 1, the specific surface area of gained porous charcoal is 1450m
2g
-1.
Get the prepared porous charcoal of 7mg, in active substance: the ratio of acetylene black: tetrafluoroethylene=7:2:1 is evenly mixed, and then the pressure with 20MPa is pressed onto mixture on nickel foam collector, makes electrode of super capacitor.In 6M KOH electrolytic solution, carry out electro-chemical test.Wherein foam nickel electrode is working electrode, and saturated calomel electrode is reference electrode, and platinum wire electrode is to electrode.As shown in Figure 3, prepared porous carbon material is at 0.2A g
-1ratio electric capacity under current density reaches 347F g
-1, when current density is 10A g
-1time, its quality still can remain on 160F g than electric capacity
-1, illustrate that this electrode has good high rate performance.
The porous carbon material making and conductive agent acetylene black and binding agent polyvinylidene difluoride (PVDF) are dispersed in nitrogen methyl-2-pyrrolidone (NMP) according to mass ratio 80:10:10, fully stir and make to mix.The slurry obtaining is evenly applied in metal collector, and wherein, Al paper tinsel is as plus plate current-collecting body, and Cu paper tinsel is as negative current collector.Be placed in vacuum drying oven, in 120 ℃ of dry 24h, transfer to afterwards and in the glove box that is full of argon gas, be assembled into the symmetrical electrochemical capacitor of button.The symmetrical electrochemical capacitor of this button adopts 1M (C
2h
5)
4nBF
4/ Propylene carbonate solution is electrolytic solution, and polypropylene diaphragm is barrier film.As can be seen from Figure 4, the specific energy of this symmetry electrochemical capacitor and specific power density are respectively 16Wh kg
-1with 3750W kg
-1.
Embodiment 2
In Ma'an Mountain food market, buy common egg, get the egg white solution of two pieces of eggs in beaker, toward pouring 200mL acetone in beaker, separate out albumen, the albumen of separating out is after 60 ℃ of oven dry of vacuum drying oven, get 10g and be placed in quartz boat, speed with 3 ℃/min in being connected with the tube furnace of argon gas is warmed up to 450 ℃, insulation 2h.Then the carbon precursor above-mentioned pre-charing being obtained in mass ratio 1:2 and activator fully mixes, and activator is potassium hydroxide, then under argon gas atmosphere, with the speed of 3 ℃/min, is warmed up to 700 ℃ and activates, and soak time is 2h.By the 0.1mol sulfuric acid scrubbing of above-mentioned activation products, then by washed with de-ionized water to neutrality, be dried, obtain porous charcoal.
The electrochemical test method of porous charcoal is identical with embodiment 1.
Embodiment 3
In Ma'an Mountain food market, buy common egg, get the egg white solution of two pieces of eggs in beaker, in beaker, add sodium chloride solution to separate out albumen, the albumen of separating out is after 60 ℃ of oven dry of vacuum drying oven, get 10g and be placed in quartz boat, speed with 10 ℃/min in being connected with the tube furnace of argon gas is warmed up to 500 ℃, insulation 2h.Then the carbon precursor above-mentioned pre-charing being obtained in mass ratio 1:4 and activator fully mixes, and activator is sodium hydroxide, then under argon gas atmosphere, with the speed of 10 ℃/min, is warmed up to 900 ℃ and activates, and soak time is 5h.By 0.1mol nitric acid washing for above-mentioned activation products, then by washed with de-ionized water to neutrality, be dried, obtain porous charcoal.
The electrochemical test method of porous charcoal is identical with embodiment 1.
Embodiment 4
In Ma'an Mountain food market, buy common egg, get the egg white solution of two pieces of eggs in beaker, in beaker, add metabisulfite solution to separate out albumen, the albumen of separating out is after 60 ℃ of oven dry of vacuum drying oven, get 10g and be placed in quartz boat, speed with 1 ℃/min in being connected with the tube furnace of argon gas is warmed up to 550 ℃, insulation 2h.Then the carbon precursor above-mentioned pre-charing being obtained in mass ratio 1:5 and activator fully mixes, and activator is potassium hydroxide, then under argon gas atmosphere, with the speed of 1 ℃/min, is warmed up to 800 ℃ and activates, and soak time is 3h.By 0.1mol salt acid elution for above-mentioned activation products, then by washed with de-ionized water to neutrality, be dried, obtain porous charcoal.
The electrochemical test method of porous charcoal is identical with embodiment 1.
Embodiment 5
In Ma'an Mountain food market, buy common egg, get the egg white solution of two pieces of eggs in beaker, in beaker, add sodium nitrate solution to separate out albumen, the albumen of separating out is after 60 ℃ of oven dry of vacuum drying oven, get 10g and be placed in quartz boat, speed with 4 ℃/min in being connected with the tube furnace of helium is warmed up to 550 ℃, insulation 2h.Then the carbon precursor above-mentioned pre-charing being obtained in mass ratio 1:3 and activator fully mixes, activator is with potassium hydroxide and sodium hydroxide 1:1 proportioning in mass ratio, then under helium atmosphere, with the speed of 4 ℃/min, be warmed up to 1000 ℃ and activate, soak time is 10h.By 0.1mol salt acid elution for above-mentioned activation products, then by washed with de-ionized water to neutrality, be dried, obtain porous charcoal.
The electrochemical test method of porous charcoal is identical with embodiment 1.
Claims (2)
1. the egg white of take is prepared a method for porous charcoal for electrochemical capacitor as raw material, it is characterized in that, described preparation method comprises the steps:
(1) in egg white liquid, add neutral salt or organic solvent to separate out albumen, the albumen obtaining is placed in vacuum drying oven and is dried;
Described neutral salt is one or more in chlorate, vitriol and nitrate; Described organic solvent is one or both mixing of dehydrated alcohol, acetone;
(2) after the dried protein material of step (1) is ground, put into tube furnace, in rare gas element, with 1～10 ℃/min of speed speed, be warmed up to pre-carbonization temperature, at this temperature, be incubated after 2h, obtain carbon precursor;
Described rare gas element is one or more in nitrogen, argon gas, helium; Described pre-carbonization temperature is 450～600 ℃;
(3) carbon precursor step (2) being obtained evenly mixes by a certain percentage with alkali metal hydroxide, then in rare gas element, with speed, 1～10 ℃/min is warmed up to activation temperature, and be incubated 1～10h, under this activation temperature, carbon precursor is carried out to activation treatment, obtain activation products;
Described carbon precursor and the mass ratio of alkali metal hydroxide are 1:2～5; Described alkali metal hydroxide is the mixture of the one or both in potassium hydroxide, sodium hydroxide; Described rare gas element is one or more in nitrogen, argon gas, helium; Described activation temperature is 700～1000 ℃;
(4) acid neutralization for the activation products that step (3) obtained, then extremely neutral by washed with de-ionized water, dry, after grinding, obtain electrochemical capacitor porous charcoal;
Described acid is one or more in hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid.
2. as claimed in claim 1ly a kind ofly take egg white and prepare the method for porous charcoal for electrochemical capacitor as raw material, it is characterized in that, in described step (1), with organic solvent, separate out albumen, this organic solvent is dehydrated alcohol; In described step (2), rare gas element is nitrogen, and pre-carbonization temperature is 600 ℃; In described step (3), the mass ratio of carbon precursor and alkali metal hydroxide is 1:3, and alkali metal hydroxide is potassium hydroxide, and rare gas element is nitrogen, and activation temperature is 800 ℃; In described step (4), acid is hydrochloric acid.
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| CN104810164A (en) * | 2015-04-23 | 2015-07-29 | 北京理工大学 | Method for preparing high-energy-density supercapacitor on basis of bioprotein-based nitrogen-doped porous carbon materials |
| CN104953121A (en) * | 2015-04-23 | 2015-09-30 | 北京理工大学 | Preparation method for lithium-ion capacitor battery by taking bioprotein-based nitrogen-doped porous carbon material as negative material |
| CN105655154A (en) * | 2016-01-11 | 2016-06-08 | 河南师范大学 | Preparation method for preparing electrode material of super capacitor made of graphene-active carbon compounds |
| WO2017045573A1 (en) * | 2015-09-15 | 2017-03-23 | GM Global Technology Operations LLC | Activated carbon powders for hybrid supercapacitor-battery systems |
| CN107697914A (en) * | 2017-08-22 | 2018-02-16 | 河南师范大学 | A kind of method for preparing nitrogen-doped porous carbon material |
| CN108365184A (en) * | 2018-01-02 | 2018-08-03 | 江苏大学 | A kind of lithium ion battery porous SiOC negative materials of rich carbon and preparation method thereof |
| CN108400363A (en) * | 2018-03-09 | 2018-08-14 | 中国科学技术大学 | A kind of electrode material and its preparation method and application |
| CN108622896A (en) * | 2018-05-21 | 2018-10-09 | 桂林电子科技大学 | A kind of egg white based cellular structures carbon material and its preparation method and application |
| CN110127662A (en) * | 2019-05-26 | 2019-08-16 | 天津大学 | A method of assist charing Small molecule organic solvents to prepare porous charcoal using alkali metal |
| CN110467175A (en) * | 2019-09-19 | 2019-11-19 | 深圳烯创先进材料研究院有限公司 | A kind of graphene enhances the preparation method of biomass porous carbon electromagnetic-wave absorbent |
| CN110482526A (en) * | 2019-09-17 | 2019-11-22 | 哈尔滨工业大学 | It is a kind of using egg white as the preparation method of the biomass porous carbon electromagnetic-wave absorbent of presoma |
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| CN111333069A (en) * | 2020-03-14 | 2020-06-26 | 北京神舟茂华环保科技有限公司 | Method for preparing supercapacitor electrode material by using protein in sludge |
| CN112265991A (en) * | 2020-10-30 | 2021-01-26 | 浙江大学 | Preparation method for preparing mesoporous-rich hierarchical porous carbon by using geminal substances |
| CN113104903A (en) * | 2021-03-01 | 2021-07-13 | 西安理工大学 | Preparation method of biomass-based wave-absorbing material |
| CN116216717A (en) * | 2023-05-09 | 2023-06-06 | 四川大学 | Preparation method of activated carbon and low-temperature SCR denitration catalyst and flue gas denitration method |
| CN116282014A (en) * | 2023-03-13 | 2023-06-23 | 中国矿业大学 | Preparation method and application of coal-based porous carbon material |
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| CN104953121A (en) * | 2015-04-23 | 2015-09-30 | 北京理工大学 | Preparation method for lithium-ion capacitor battery by taking bioprotein-based nitrogen-doped porous carbon material as negative material |
| WO2017045573A1 (en) * | 2015-09-15 | 2017-03-23 | GM Global Technology Operations LLC | Activated carbon powders for hybrid supercapacitor-battery systems |
| CN108352253A (en) * | 2015-09-15 | 2018-07-31 | 通用汽车环球科技运作有限责任公司 | Activated carbon powder for hybrid super capacitor-battery system |
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| CN110127662A (en) * | 2019-05-26 | 2019-08-16 | 天津大学 | A method of assist charing Small molecule organic solvents to prepare porous charcoal using alkali metal |
| CN110482526A (en) * | 2019-09-17 | 2019-11-22 | 哈尔滨工业大学 | It is a kind of using egg white as the preparation method of the biomass porous carbon electromagnetic-wave absorbent of presoma |
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| CN111292966A (en) * | 2020-02-11 | 2020-06-16 | 西安理工大学 | Preparation method of porous biomass-based electrode material |
| CN111333069A (en) * | 2020-03-14 | 2020-06-26 | 北京神舟茂华环保科技有限公司 | Method for preparing supercapacitor electrode material by using protein in sludge |
| CN112265991A (en) * | 2020-10-30 | 2021-01-26 | 浙江大学 | Preparation method for preparing mesoporous-rich hierarchical porous carbon by using geminal substances |
| CN112265991B (en) * | 2020-10-30 | 2022-03-25 | 浙江大学 | Preparation method for preparing mesoporous-rich hierarchical porous carbon by using geminal substances |
| CN113104903A (en) * | 2021-03-01 | 2021-07-13 | 西安理工大学 | Preparation method of biomass-based wave-absorbing material |
| CN113104903B (en) * | 2021-03-01 | 2023-09-22 | 西安理工大学 | Preparation method of biomass-based wave-absorbing material |
| CN116282014A (en) * | 2023-03-13 | 2023-06-23 | 中国矿业大学 | Preparation method and application of coal-based porous carbon material |
| CN116216717A (en) * | 2023-05-09 | 2023-06-06 | 四川大学 | Preparation method of activated carbon and low-temperature SCR denitration catalyst and flue gas denitration method |
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