CN102431993A - Method for preparing mesoporous carbon material for electrochemical capacitor by using rice hulls as raw materials - Google Patents
Method for preparing mesoporous carbon material for electrochemical capacitor by using rice hulls as raw materials Download PDFInfo
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Abstract
The invention discloses a method for preparing a mesoporous carbon material for an electrochemical capacitor by using rice hulls as raw materials, and belongs to the technical field of carbon materials and microwave chemistry. The method comprises the following steps of: activating the hulls serving as a carbon source by using zinc chloride serving as an activating agent through microwave auxiliary heating to obtain the mesoporous carbon material in one step, wherein the specific surface area of the obtained mesoporous carbon material is between 1,409 and 1,738m<2>/g, the total pore volume is between 0.71 and 2.14cm<3>/g, the average pore size is between 1.99 and 6.08nm, the ratio of the volume of a non-micro pore to the total pore volume is between 66.2 and 99.5 percent, and the mesoporous carbon yield is between 30.4 and 37.0 percent. The method for preparing the mesoporous carbon material is simple, efficient and energy-saving; and the prepared mesoporous carbon material has a higher ratio of the volume of the non-micro pore to the total pore volume, and has extremely high quick charging and discharging performance when used as an electrode material of the electrochemical capacitor.
Description
Technical field
The invention belongs to raw material of wood-charcoal material and microwave chemical technical field, be specifically related to a kind of method of feedstock production electrochemical capacitor that be with the rice husk with mesopore raw material of wood-charcoal material.
Background technology
The aperture has high adsorption capacity, chemicalstability is good, physical strength is high and uses the back of losing efficacy to be prone to characteristics such as regeneration between the mesopore raw material of wood-charcoal material of 2-50nm, is widely used in fields such as food, chemical industry, the energy and environmental protection.The raw material of producing the mesopore charcoal mainly contains mineral substance, wooden and other carbon raw material.Mineral substance is mainly various coals and oil and processed products thereof, and mineral substance is disposable resource, and is non-renewable.Woodenly type be mainly wood chip, charcoal, rice husk, straw etc., renewable, and inexpensive, be easy to get.
China is Rice Production big country, and rice husk is the sub product after the paddy processing, accounts for 20% of paddy weight.China's rice husk turnout accounts for more than 1/3 of the whole world, aboundresources, but its utilization ratio is very low.Content of lignin is higher in the rice husk, is difficult for suction, and directly being applied to the field, to make fertilizer not perishable, mostly as the primary fuel burning, and contaminate environment not only during burning, and caused the waste of resource.With the rice husk is that carbon source prepares electrochemical capacitor with mesopore raw material of wood-charcoal material, not only can prepare better performances, cheap mesopore charcoal, is used the problem of environmental pollution that causes as fuel but also solved the depleted crop by-product.
Adopt physically activated and chemical activation method to prepare gac or mesopore charcoal by rice husk.In the chemical activation method mainly with zinc chloride, phosphoric acid, Pottasium Hydroxide or sodium hydroxide etc. as acvator; These method common shortcomings are to heat with traditional tube furnace, and its heating/soak time is longer, and activating process is complicated; Activation temperature is higher, and cost is high.Exploration is significant with the effective ways of mesopore raw material of wood-charcoal material for the feedstock production electrochemical capacitor with the rice husk.
Patent 98114553.1 has been announced the preparation method of activated carbon with high specific surface area.In this method, rice husk after carrying out 3-5 h carbonization under 400-600 ℃, with carbide and Pottasium Hydroxide by weight for 1:3 mixes, 400 ℃ handle 30min down after, being warmed up to 750 ℃ carries out activation 60min, the specific surface area that makes gac is 2850m
2/ g.It is that raw material is produced process of active carbon that patent 200910310025.0 has been announced with rice husk, stalk.Elder generation is with behind rice husk, the stalk pulverize separately in this method; By 1: weight ratio (3-5) with powdered rice hulls mix with straw powder obtain compound after; Under 850-950 ℃, carry out carbonization; The phosphate aqueous solution that adds aqueous hydrochloric acid that mass concentration is 1-3% and 3-5% in the charcoal end after carbonization successively stirs the 1.5-2.5h after-filtration down at 120-130 ℃, at 440-460 ℃ of dry 3.5-4.5h down, obtains acid-treated charcoal end.Adding mass concentration in the charcoal end after s.t. is the sodium hydroxide solution of 3-5%, stirs 1.5-2.5 h after-filtration, dry 3.5-4.5h under 440-460 ℃ down at 120-130 ℃.The iodine sorption value that makes gac is greater than 1000mg/g, and the methylene blue adsorption rate is greater than 135mg/g.
Paper " Production of activated carbon from bagasse and rice husk by a single-stage chemical activation method at low retention times " (Bioresource Technology; 99 (2008) 6809-6816) having proposed with the rice husk is raw material; In carbon dioxide atmosphere; When the mass ratio of zinc chloride and rice husk is 1:1, activation temperature is 700
oDuring C, the specific surface area of obtained gac reaches 750m
2/ g.Paper " Characteristics of microporous/mesoporous carbons prepared from rice husk under base-and acid-treated conditions " (Journal of Hazzardous Material 171 (2009) 693-703) adopts conventional heating method to prepare gac by rice husk; In the paper, rice husk by the sodium hydroxide solution pre-treatment after, when the mass ratio of phosphoric acid or zinc chloride and rice husk is respectively 2:1, behind 500 ℃ of following activation 60min, the specific surface area of gained gac is respectively 1741m
2/ g and 2434m
2/ g, total pore volume is respectively 1.32cm
3/ g and 1.34cm
3/ g.
Can find out from above-mentioned document, be carbon source with the rice husk, adopts conventional heating method to prepare the technology of gac or mesopore charcoal, its complex process, and soak time is long, and energy consumption is high, and cost is high, has increased the production cost of gac or mesopore charcoal.Conventional heating is accomplished according to thermal conduction, radiation, three kinds of heat transfer types of convection current, is that the outside ecto-entad from material heats, and the power of heating is the temperature head on the direction of heat flow.The inner rate of heating of most of granule materials is slow, and the internal and external temperature field of granule materials is inhomogeneous, reaches required chronic of the whole even heating of object, needs could accomplish reactivation process through the long period.And to obtain the high specific surface area gac, after having only the top layer hole of granule materials to be activated to collapse, granule materials central porisity could form.On the whole, conventional activation method length consuming time, power consumption is high.
Summary of the invention
The present invention is directed to the deficiency of prior art, propose a kind of method of feedstock production electrochemical capacitor that be with the rice husk with mesopore raw material of wood-charcoal material.These method concrete steps are following:
(1) pre-treatment of rice husk: after with ortho-water rice husk being cleaned, in 110
oC freeze-day with constant temperature 12h, the air-dried moisture of gained rice husk are 6.92%, and ash content is 17.16%; Volatilization is divided into 60.73%, and fixed carbon is 15.19%, and the 6g rice husk is put into beaker; Add the sodium hydroxide solution 300mL of 0.5M, beaker is heated and stirred 2h on the magnetic force heating stirrer, and using 70-80 ℃ distilled water wash rice husk to pH value of filtrate is 7; Rice husk after the washing obtains pretreated rice husk in 110 ℃ of freeze-day with constant temperature 12h;
(2) preparation of mesopore charcoal: measure 150mL zero(ppm) water and put into beaker, the zinc chloride solid that takes by weighing certain mass is dissolved in the zero(ppm) water in the beaker, obtains liquor zinci chloridi after stirring; Take by weighing the pretreated rice husk of a certain amount of step (1) gained; Put into liquor zinci chloridi; The mass ratio of said zinc chloride and rice husk is (1-5): 1; Take out beaker after beaker is placed in the ultrasonator concussion 30min, soak under the room temperature behind the 12h in loft drier, obtain the rice husk after liquor zinci chloridi is handled in 110 ℃ of freeze-day with constant temperature 24h;
(3) rice husk after the liquor zinci chloridi that obtains step (2) is handled is transferred in the ceramic crucible, places in the microwave reactor, and the setting microwave power is 600W; The microwave activation time is that 20min carries out microwave heating activation; Take out after the activation products that obtain after the activation are cooled to room temperature, in activation products, add the hydrochloric acid soln 100mL of 0.5M, behind the washing 2h that refluxes; Use 70-80 ℃ distilled water wash activation products to pH value of filtrate to be 6-7; Obtain the mesopore charcoal, place loft drier behind 110 ℃ of freeze-day with constant temperature 24h, to be ground to 325 orders the mesopore charcoal after the washing, obtain electrochemical capacitor with mesopore raw material of wood-charcoal material.
This method is carbon source with the rice husk, and zinc chloride is an acvator, through microwave-assisted heating zinc chloride activation rice husk one step preparation mesopore raw material of wood-charcoal material.Prepared mesopore raw material of wood-charcoal material specific surface area is between 1409-1738m
2Between/the g, total pore volume is between 0.71-2.14cm
3Between/the g, mean pore size is between 1.99-6.08nm, and the ratio that non-micropore pore volume accounts for total pore volume is between 66.2-99.5%, and mesopore charcoal productive rate is between 30.4-37.0%.Mesopore charcoal preparation method is simple, efficient, energy-conservation, and the non-micropore pore volume of the mesopore charcoal that makes accounts for the large percentage of total pore volume, with its electrode materials as electrochemical capacitor, has good fast charging and discharging performance.
The present invention has the following advantages:
1, with the rice husk be feedstock production mesopore raw material of wood-charcoal material, carbon source is cheap, be easy to get.
2, utilizing microwave that granule materials is had from molecular level heats and to the selectivity heat characteristic of polar material; Overcome granule materials temperature inside gradient; Help the rising of material internal temperature and improve priming reaction speed (only using the 20min soak time), thereby realize cheapness, the efficient production of mesopore charcoal.
3, liquor zinci chloridi has run-inflation effect to rice husk; Porous is to the inside of rice husk, and local superheating does not take place rice husk quick heating and even during activation; And can reduce the generation of volatilizable thing during by the rice husk activation of liquor zinci chloridi dipping, help to improve the productive rate of mesopore raw material of wood-charcoal material.
4, zinc chloride is liquid state in reactivation process, has flowability, in helping/and the formation of macroporous structure.
Description of drawings
Fig. 1 is the nitrogen absorption and the desorption isotherm of the mesopore raw material of wood-charcoal material of the embodiment of the invention 3,4 and 5 preparations.
Fig. 2 is the main graph of pore diameter distribution of mesopore raw material of wood-charcoal material of the embodiment of the invention 3,4 and 5 preparations.
Fig. 3 is that the middle pore carbon electrode of the embodiment of the invention 5 preparations is swept the cyclic voltammogram under the speed in difference.
Fig. 4 is that the specific volume of middle pore carbon electrode material of the embodiment of the invention 3,4 and 5 preparations is with the variation diagram of discharge current density.
Fig. 5 is energy density and the graph of a relation of average power density of the mesopore charcoal electrical condenser of the embodiment of the invention 3,4 and 5 preparations.
Embodiment
Embodiment 1: mesopore charcoal MC
1-600-20Concrete preparation process is following:
(1) pre-treatment of rice husk: with ortho-water rice husk is cleaned and drying after; Take by weighing rice husk 6g and place beaker; Add the sodium hydroxide solution 300mL of 0.5M, beaker heats 2h on the magnetic force heating stirrer, and being cooled to and using 70-80 ℃ distilled water wash rice husk to pH value of filtrate after the room temperature is 7; Rice husk after the washing is put into loft drier in 110 ℃ of freeze-day with constant temperature 12h, obtain pretreated rice husk.
(2) measure 150mL zero(ppm) water in beaker, take by weighing 13.5g zinc chloride solid and be dissolved in the zero(ppm) water in the beaker, obtain liquor zinci chloridi after stirring; Take by weighing the pretreated rice husk of 13.5g step (1) gained; Add in the gained liquor zinci chloridi; After stirring with glass stick; Concussion is taken out beaker behind the 30min in ultrasonator, soaks under the room temperature behind the 12h in loft drier in 110 ℃ of freeze-day with constant temperature 24h, obtains the rice husk after liquor zinci chloridi is handled.
(3) rice husk after the liquor zinci chloridi that step (2) is obtained is handled moves in the ceramic crucible, and ceramic crucible is placed in the microwave chemical reactor, and nitrogengas cylinder, quartzy protector, ceramic crucible, thermopair, fluid collection vials and tail gas wash bottle are connected; Open nitrogengas cylinder, the air in the ceramic crucible is purged, behind the nitrogen purging 5min with high pure nitrogen; Setting microwave power is that 600W and soak time are 20min; Carry out microwave heating activation and prepare the mesopore charcoal, after microwave heating activation finishes, when temperature indicator shows that the temperature of activation products drops to 200 ℃; Close nitrogengas cylinder, with the activation products that make cool to room temperature under air-proof condition.
(4) activation products to the pH value of filtrate that makes with 0.5M Hydrogen chloride and 70-80 ℃ of zero(ppm) water washing step (3) successively is to obtain the mesopore charcoal behind the 6-7; Mesopore charcoal after the washing is ground to 325 orders behind 110 ℃ of freeze-day with constant temperature 24h; Obtain electrochemical capacitor with mesopore raw material of wood-charcoal material, this mesopore raw material of wood-charcoal material is marked as MC
1-600-20
Embodiment 2: mesopore charcoal MC
2-600-20Concrete preparation process is following:
(1) pre-treatment of rice husk: according to embodiment 1 in the same method of step (1) implement.
(2) according to embodiment 1 in the same method of step (2) implement, it is 18g that difference is to take by weighing zinc chloride solid quality, the quality of rice husk is 9g.
(3) according to embodiment 1 in the same method of step (3) implement.
(4) according to embodiment 1 in the same method of step (4) implement.Difference is that gained mesopore raw material of wood-charcoal material is labeled as MC
2-600-20
Embodiment 3: mesopore charcoal MC
3-600-20Concrete preparation process is following:
(1) pre-treatment of rice husk: according to embodiment 1 in the same method of step (1) implement.
(2) according to embodiment 1 in the same method of step (2) implement, it is 20.25g that difference is to take by weighing zinc chloride solid quality, the quality of rice husk is 6.75g.
(3) according to embodiment 1 in the same method of step (3) implement.
(4) according to embodiment 1 in the same method of step (4) implement.Difference is that gained mesopore raw material of wood-charcoal material is labeled as MC
3-600-20
Instance 4:MC
4-600-20Concrete preparation process is following:
(1) pre-treatment of rice husk: according to embodiment 1 in the same method of step (1) implement.
(2) according to embodiment 1 in the same method of step (2) implement, according to embodiment 1 in the same method of step (2) implement, it is 21.6g that difference is to take by weighing zinc chloride solid quality, the quality of rice husk is 5.4g.
(3) according to embodiment 1 in the same method of step (3) implement.
(4) according to embodiment 1 in the same method of step (4) implement.Difference is that gained mesopore raw material of wood-charcoal material is labeled as MC
4-600-20
Embodiment 5:MC
5-600-20Concrete preparation process is following:
(1) pre-treatment of rice husk: according to embodiment 1 in the same method of step (1) implement.
(2) according to embodiment 1 in the same method of step (2) implement, it is 22.5g that difference is to take by weighing zinc chloride solid quality, the quality of rice husk is 4.5g.
(3) according to embodiment 1 in the same method of step (3) implement.
(4) according to embodiment 1 in the same method of step (4) implement.Difference is that gained mesopore raw material of wood-charcoal material is labeled as MC
5-600-20
Embodiment 1-5 gained mesopore raw material of wood-charcoal material pore structure analysis result is listed in the table 1.
Claims (1)
1. be the method for feedstock production electrochemical capacitor with the rice husk, it is characterized in that these method concrete steps are following with mesopore raw material of wood-charcoal material:
(1) pre-treatment of rice husk: after with ortho-water rice husk being cleaned, in 110
oC freeze-day with constant temperature 12h, the air-dried moisture of gained rice husk are 6.92%, and ash content is 17.16%; Volatilization is divided into 60.73%, and fixed carbon is 15.19%, and the 6g rice husk is put into beaker; Add the sodium hydroxide solution 300mL of 0.5M, beaker heats 2h on the magnetic force heating stirrer, and using 70-80 ℃ distilled water wash rice husk to pH value of filtrate is 7; Rice husk after the washing obtains pretreated rice husk in 110 ℃ of freeze-day with constant temperature 12h;
(2) preparation of mesopore charcoal: measure 150mL zero(ppm) water and put into beaker, the zinc chloride solid that takes by weighing certain mass is dissolved in the zero(ppm) water in the beaker, obtains liquor zinci chloridi after stirring; Take by weighing the pretreated rice husk of a certain amount of step (1) gained; Put into said liquor zinci chloridi; The mass ratio of zinc chloride and rice husk is (1-5): 1; Take out beaker after beaker is placed in the ultrasonator concussion 30min, soak under the room temperature behind the 12h in loft drier, obtain the rice husk after liquor zinci chloridi is handled in 110 ℃ of freeze-day with constant temperature 24h;
(3) rice husk after the liquor zinci chloridi that obtains step (2) is handled is transferred in the ceramic crucible; Place in the microwave reactor; The setting microwave power is 600W, and the microwave activation time is that 20min carries out microwave heating activation, takes out after the activation products that obtain after the activation are cooled to room temperature; After the hydrochloric acid soln 100mL that in activation products, adds 0.5M refluxes and washs 2h; Use 70-80 ℃ distilled water wash activation products to pH value of filtrate to obtain the mesopore charcoal, place loft drier behind 110 ℃ of freeze-day with constant temperature 24h, to be ground to 325 orders the mesopore charcoal after the washing, obtain electrochemical capacitor with mesopore raw material of wood-charcoal material as 6-7.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014165435A (en) * | 2013-02-27 | 2014-09-08 | Akita Univ | Electrochemical capacitor |
| CN104118863A (en) * | 2014-08-04 | 2014-10-29 | 安徽工业大学 | Method for preparing porous carbon material for supercapacitor by activating rice husks through ionic liquid |
| CN104150478A (en) * | 2014-07-17 | 2014-11-19 | 吉林大学 | Green cycle process for preparing activated carbon material for supercapacitors by using rice husks |
| CN105247640A (en) * | 2013-05-27 | 2016-01-13 | 日本贵弥功株式会社 | Electrode, electric double-layer capacitor using said electrode, and method for manufacturing said electrode |
| CN106517195A (en) * | 2016-11-14 | 2017-03-22 | 天津工业大学 | Method for preparing porous carbon from phosphate activated biomass and applying porous carbon to supercapacitors |
| CN107188170A (en) * | 2017-06-01 | 2017-09-22 | 镇江四联机电科技有限公司 | A kind of use mixed base activation prepares the production technology of activated carbon |
| CN110316714A (en) * | 2019-06-17 | 2019-10-11 | 西安交通大学苏州研究院 | Three-dimensional porous class graphene structural carbon material based on rice husk and its preparation method and application |
| CN111153410A (en) * | 2019-12-30 | 2020-05-15 | 南昌大学 | Preparation method of rice hull-based inorganic nano material based on ionic liquid treatment |
| CN111298767A (en) * | 2020-02-17 | 2020-06-19 | 安徽工业大学 | Biomass-based carbon material for adsorbing heavy metal ions, preparation method and application |
| CN111320174A (en) * | 2020-03-26 | 2020-06-23 | 常州大学 | Preparation method and application of mesoporous type juicy peach pit activated carbon |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2014165435A (en) * | 2013-02-27 | 2014-09-08 | Akita Univ | Electrochemical capacitor |
| CN105247640A (en) * | 2013-05-27 | 2016-01-13 | 日本贵弥功株式会社 | Electrode, electric double-layer capacitor using said electrode, and method for manufacturing said electrode |
| CN104150478A (en) * | 2014-07-17 | 2014-11-19 | 吉林大学 | Green cycle process for preparing activated carbon material for supercapacitors by using rice husks |
| CN104150478B (en) * | 2014-07-17 | 2016-06-15 | 吉林大学 | A kind of green circulatory technique of being prepared activated carbon for super capacitors material by rice husk |
| CN104118863A (en) * | 2014-08-04 | 2014-10-29 | 安徽工业大学 | Method for preparing porous carbon material for supercapacitor by activating rice husks through ionic liquid |
| CN104118863B (en) * | 2014-08-04 | 2015-11-04 | 安徽工业大学 | A kind of ionic liquid activation rice husk prepares the method for porous carbon material for supercapacitor |
| CN106517195A (en) * | 2016-11-14 | 2017-03-22 | 天津工业大学 | Method for preparing porous carbon from phosphate activated biomass and applying porous carbon to supercapacitors |
| CN107188170A (en) * | 2017-06-01 | 2017-09-22 | 镇江四联机电科技有限公司 | A kind of use mixed base activation prepares the production technology of activated carbon |
| CN110316714A (en) * | 2019-06-17 | 2019-10-11 | 西安交通大学苏州研究院 | Three-dimensional porous class graphene structural carbon material based on rice husk and its preparation method and application |
| CN111153410A (en) * | 2019-12-30 | 2020-05-15 | 南昌大学 | Preparation method of rice hull-based inorganic nano material based on ionic liquid treatment |
| CN111298767A (en) * | 2020-02-17 | 2020-06-19 | 安徽工业大学 | Biomass-based carbon material for adsorbing heavy metal ions, preparation method and application |
| CN111320174A (en) * | 2020-03-26 | 2020-06-23 | 常州大学 | Preparation method and application of mesoporous type juicy peach pit activated carbon |
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Application publication date: 20120502 |