CN104445190A - Method for preparation of activated carbon with high specific surface area by using asparagus lettuce leaf as carbon source - Google Patents
Method for preparation of activated carbon with high specific surface area by using asparagus lettuce leaf as carbon source Download PDFInfo
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Abstract
The invention discloses a method for preparation of activated carbon with high specific surface area by using asparagus lettuce leaf as a carbon source. The method provided by the invention adopts asparagus lettuce leaf as raw material, and comprises the steps of: carbonizing the material to obtain a carbonized product, mixing the carbonized product with an alkaline medium, activating the mixture in argon, and finally washing and drying to obtain activated carbon with superhigh specific surface area. The prepared activated carbon has specific surface area of about 1000-3500 m<2> / g, pore volume of 1-2 cm<3> / g and average pore diameter of 0.5-3 nm, and can be widely used as a novel porous carbon material in the fields of batteries, super capacitors and gas adsorption.
Description
Technical field
The present invention relates to the technology of preparing of absorbent charcoal material, be specially the method for the gac preparing high-specific surface area with biomass waste resource and asparagus lettuce leaf.
Background technology
Gac is a kind of contenting carbon material, has specific surface area large, and internal voids structure is flourishing, and high adsorption capacity, acid and alkali-resistance, the advantage such as renewable, can be widely used in the fields such as chemical industry, metallurgy, military protection, battery, environment protection.Around one of the basic and applied research important topic remaining scientific research of gac.
The selection of activated carbon raw material is the hot issue that people pay close attention to always, because this is directly connected to quality and the subsequent applications of material.The raw material type preparing gac is various, current commercial applications and scientific research more mainly contain coal (A. G. Pandolfo, A. F. Hollenkamp,
journal of Power Sources,
2006, 157,11-27), refinery coke (J. Wang, M. M. Chen, C. Y. Wang, J. Z. Wang, J. M. Zheng,
journal of Power Sources,
2011, 196,550-558), high molecular polymer (J. Yan, Tong, Wei, W. M. Qiao, Z. J. Fan, L. J. Zhang, T. Y. Li, Q. K. Zhao,
electrochemistry Communications,
2010, 12,1279-1282), biomass material (timber (F. C. Wu, R. L. Tseng, C. C. Hu, C. C. Wang,
journal of Power Sources,
2004, 138,351-359), apricot shell (B. Xu, Y. F. Chen, G. Wei, G. P. Cao, H. Zhang, Y. S. Yang,
materials Chemistry and Physics,
2010, 124,504-509), husk (M.S Balathanigaimani, W. G. Shin, M. J. Lee, C. Kim, J. W. Lee, H. Moon,
electrochemistry Communications,
2008, 10,868-871), coconut husk (Li Yanfang, Liang great Ming, Liu Chunlan,
clean coal technology,
2009, 15,5-13) etc.).These carbon sources, after charing and activation, can obtain the absorbent charcoal material of certain specific surface area.Comparatively speaking, biomass material shows good application prospect, has that abundance, cost are low, the advantage such as can to accomplish scale production.But utilize absorbent charcoal material prepared by the above-mentioned biomass material mentioned at present, specific surface area is still lower, which limits its potential using value.
Summary of the invention
The object of the invention is to propose one utilizes biomass carbon source-asparagus lettuce leaf to prepare the approach of the active material of high-ratio surface, method has cost low (recycling of waste biomass material), flow process is simple, the advantage such as can to prepare in a large number, therefore can be used as a kind of Perfected process being suitable for preparing the gac of high-specific surface area.
Technical scheme of the present invention is:
The invention provides a kind of method utilizing biomass carbon source to prepare the gac of high-ratio surface, the method adopts asparagus lettuce leaf to be raw material, and first charing obtains carbide, is mixed by carbide with alkaline medium, activate in argon gas, then washing obtains the gac of superhigh specific surface area.
Take asparagus lettuce leaf as the method that carbon source prepares active carbon with high specific surface area, it is characterized in that, the method step is:
A, asparagus lettuce leaf carbonize: by asparagus lettuce leaf seasoning, dehydration, under argon shield, adopt progressively temperature-rising method to carbonize asparagus lettuce leaf, heat-up rate is 1 ~ 20 DEG C/min, and carbonization temperature is 100 ~ 1000 DEG C, and soaking time is 1 ~ 10 h, form carbide A;
B, KOH activate: ground by carbide A; and mix with potassium hydroxide and water; after seasoning, under argon shield, progressively temperature-rising method is adopted to activate carbide A; wherein the mass ratio of KOH and carbide A is 1:1 ~ 10:1; heat-up rate is 1 ~ 20 DEG C/min, and activation temperature is 500 ~ 1000 DEG C, and soaking time is 1 ~ 10 h; obtain the gac B of high-specific surface area, gac B cooling, washing are obtained product to neutrality, drying.
The present invention adopts progressively temperature-rising method to carbonize asparagus lettuce leaf, and heat-up rate is preferably 4 ~ 10 DEG C/min, and carbonization temperature is preferably 400 ~ 800 DEG C, and soaking time is preferably 1 ~ 3 h.
The present invention adopts progressively temperature-rising method to activate carbide A, and wherein the mass ratio of KOH and carbide A is preferably 2:1 ~ 8:1, and heat-up rate is preferably 2 ~ 10 DEG C/min, and activation temperature is preferably 700 ~ 900 DEG C, and soaking time is preferably 0.5 ~ 3 h.
The present invention adopts Micromeritics ASAP 2020 to test the specific surface area of this serial absorbent charcoal material, and the specific surface area of the gac of preparation is 1000 ~ 3500 m
2/ g, pore volume 1 ~ 2 cm
3/ g, mean pore size is 0.5 ~ 3 nm.
Feature of the present invention and beneficial effect are:
Realize biomass energy refuse reclamation, integrated artistic is simple, and controllability is strong, the low in raw material price selected, and is applicable to low cost, large-scale production.The gac of preparation has superhigh specific surface area, and pore volume is higher, the equal first-class advantage in aperture.
The inventive method is simple and easy to control, and preparation cycle is short, and product particle size is even, duct is abundant, pore volume is high, constant product quality, cost performance advantages of higher.Be expected to be used widely in fields such as battery, ultracapacitor, adsorbents as a kind of novel porous active Carbon Materials.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph of embodiment gac.
Fig. 2 is the transmission electron microscope photo of embodiment gac.
Fig. 3 is the adsorption desorption curve of embodiment gac.
Fig. 4 is the adsorption desorption curve of embodiment gac.
Embodiment
Embodiment 1
By asparagus lettuce leaf seasoning, get 5g and put in the middle of tube furnace, pass into argon gas (40 sccm), with 5 DEG C/min heat-up rate to 600 DEG C, be incubated two hours, be then down to room temperature, obtain carbonizing asparagus lettuce leaf.Take three parts of charing lettuce leaves 2 g, add 6 g KOH and a small amount of water respectively, mix rear drying.Sample number into spectrum is that 600-CL-3(wherein 600 represents the temperature carbonizing bamboo shoot leaves, and 3 represent the mass ratio that KOH/ carbonizes bamboo shoot leaf).Pass into argon gas (40 sccm), with 5 DEG C/min heat-up rate to 800 DEG C, be incubated one hour, be then down to room temperature, take out activation products, first use hydrochloric acid cleaning, then wash unnecessary impurity and by product with water.Activated carbon with high specific surface area can be obtained after drying.As shown in Figure 3, the adsorption desorption curve of prepared above-mentioned sample is IV type curve, and the hole of the gac prepared by displaying is meso-hole structure.The specific surface area of sample 600-CL-3 is respectively 3330 cm
2/ g.
Embodiment 2
By asparagus lettuce leaf seasoning, get 5 g and put in the middle of tube furnace, pass into argon gas (40 sccm), with 5 DEG C/min heat-up rate to 600 DEG C, be incubated two hours, be then down to room temperature, obtain carbonizing asparagus lettuce leaf.Take three parts of charing lettuce leaves 2 g, add 8 g KOH and a small amount of water respectively, mix rear drying.Sample number into spectrum is that 600-CL-4(wherein 600 represents the temperature carbonizing bamboo shoot leaves, and 4 represent the mass ratio that KOH/ carbonizes bamboo shoot leaf).Pass into argon gas (40 sccm), with 5 DEG C/min heat-up rate to 800 DEG C, be incubated one hour, be then down to room temperature, take out activation products, first use hydrochloric acid cleaning, then wash unnecessary impurity and by product with water.Activated carbon with high specific surface area (as illustrated in fig. 1 and 2) can be obtained after drying.As shown in Figure 3, the adsorption desorption curve of prepared above-mentioned sample is IV type curve, and the hole of the gac prepared by displaying is meso-hole structure.The specific surface area of sample 600-CL-4 is respectively 3289 cm
2/ g.
Embodiment 3
By asparagus lettuce leaf seasoning, get 5 g and put in the middle of tube furnace, pass into argon gas (40 sccm), with 5 DEG C/min heat-up rate to 600 DEG C, be incubated two hours, be then down to room temperature, obtain carbonizing asparagus lettuce leaf.Take three parts of charing lettuce leaves 2 g, add 10 g KOH and a small amount of water respectively, mix rear drying.Sample number into spectrum is that 600-CL-4(wherein 600 represents the temperature carbonizing bamboo shoot leaves, and 4 represent the mass ratio that KOH/ carbonizes bamboo shoot leaf).Pass into argon gas (40 sccm), with 5 DEG C/min heat-up rate to 800 DEG C, be incubated one hour, be then down to room temperature, take out activation products, first use hydrochloric acid cleaning, then wash unnecessary impurity and by product with water.Activated carbon with high specific surface area can be obtained after drying.As shown in Figure 3, the adsorption desorption curve of prepared above-mentioned sample is IV type curve, and the hole of the gac prepared by displaying is meso-hole structure.The specific surface area of sample 600-CL-4 is respectively 2657 cm
2/ g.
Embodiment 5
By asparagus lettuce leaf seasoning, get 5 g and put in the middle of tube furnace, pass into argon gas (40 sccm), be warming up to heat-up rate to 400 DEG C respectively with 5 DEG C/min, be incubated two hours, be then down to room temperature, obtain carbonizing asparagus lettuce leaf.Take three parts of charing lettuce leaves 2 g, add 8 g KOH and a small amount of water, mix rear drying.Sample number into spectrum is that 400-CL-4(wherein 400 represents the temperature carbonizing bamboo shoot leaves, and 4 mass ratios representing KOH/ charing bamboo shoot leaf are 4).Pass into argon gas (40 sccm), with 5 DEG C/min heat-up rate to 800 DEG C, be incubated one hour, be then down to room temperature, take out activation products, first use hydrochloric acid cleaning, then wash unnecessary impurity and by product with water.Activated carbon with high specific surface area can be obtained after drying.As shown in Figure 4, sample 400-CL-4 smoking desorption curve is IV type curve, and the hole of the gac prepared by displaying is meso-hole structure.The specific surface area of sample 400-CL-4 is respectively 1788 cm
2/ g.
Embodiment 6
By asparagus lettuce leaf seasoning, get 5 g and put in the middle of tube furnace, pass into argon gas (40 sccm), be warming up to heat-up rate to 500 DEG C respectively with 5 DEG C/min, be incubated two hours, be then down to room temperature, obtain carbonizing asparagus lettuce leaf.Take three parts of charing lettuce leaves 2 g, add 8 g KOH and a small amount of water, mix rear drying.Sample number into spectrum is that 500-CL-4(wherein 500 represents the temperature carbonizing bamboo shoot leaves, and 4 mass ratios representing KOH/ charing bamboo shoot leaf are 4).Pass into argon gas (40 sccm), with 5 DEG C/min heat-up rate to 800 DEG C, be incubated one hour, be then down to room temperature, take out activation products, first use hydrochloric acid cleaning, then wash unnecessary impurity and by product with water.Activated carbon with high specific surface area can be obtained after drying.As shown in Figure 4, sample 500-CL-4 smoking desorption curve is IV type curve, and the hole of the gac prepared by displaying is meso-hole structure.The specific surface area of sample 500-CL-4 is respectively 2549 cm
2/ g.
Embodiment 7
By asparagus lettuce leaf seasoning, get 5 g and put in the middle of tube furnace, pass into argon gas (40 sccm), be warming up to heat-up rate to 600 DEG C respectively with 5 DEG C/min, be incubated two hours, be then down to room temperature, obtain carbonizing asparagus lettuce leaf.Take three parts of charing lettuce leaves 2 g, add 8 g KOH and a small amount of water, mix rear drying.Sample number into spectrum is that 600-CL-4(wherein 600 represents the temperature carbonizing bamboo shoot leaves, and 4 mass ratios representing KOH/ charing bamboo shoot leaf are 4).Pass into argon gas (40sccm), with 5 DEG C/min heat-up rate to 800 DEG C, be incubated one hour, be then down to room temperature, take out activation products, first use hydrochloric acid cleaning, then wash unnecessary impurity and by product with water.Activated carbon with high specific surface area can be obtained after drying.As shown in Figure 4, sample
600-CL-4 smoking desorption curve is IV type curve, and the hole of the gac prepared by displaying is meso-hole structure.The specific surface area of sample 600-CL-4 is respectively 3289 cm
2/ g.
Embodiment 8
By asparagus lettuce leaf seasoning, get 5 g and put in the middle of tube furnace, pass into argon gas (40 sccm), be warming up to heat-up rate to 700 DEG C respectively with 5 DEG C/min, be incubated two hours, be then down to room temperature, obtain carbonizing asparagus lettuce leaf.Take three parts of charing lettuce leaves 2 g, add 8 g KOH and a small amount of water, mix rear drying.Sample number into spectrum is that 700-CL-4(wherein 700 represents the temperature carbonizing bamboo shoot leaves, and 4 mass ratios representing KOH/ charing bamboo shoot leaf are 4).Pass into argon gas (40 sccm), with 5 DEG C/min heat-up rate to 800 DEG C, be incubated one hour, be then down to room temperature, take out activation products, first use hydrochloric acid cleaning, then wash unnecessary impurity and by product with water.Activated carbon with high specific surface area can be obtained after drying.As shown in Figure 4, sample 700-CL-4 smoking desorption curve is IV type curve, and the hole of the gac prepared by displaying is meso-hole structure.The specific surface area of sample 700-CL-4 is respectively 2890 cm
2/ g.
Embodiment 9
By asparagus lettuce leaf seasoning, get 5 g and put in the middle of tube furnace, pass into argon gas (40 sccm), be warming up to heat-up rate to 800 DEG C respectively with 5 DEG C/min, be incubated two hours, be then down to room temperature, obtain carbonizing asparagus lettuce leaf.Take three parts of charing lettuce leaves 2 g, add 8 g KOH and a small amount of water, mix rear drying.Sample number into spectrum is that 800-CL-4(wherein 800 represents the temperature carbonizing bamboo shoot leaves, and 4 mass ratios representing KOH/ charing bamboo shoot leaf are 4).Pass into argon gas (40 sccm), with 5 DEG C/min heat-up rate to 800 DEG C, be incubated one hour, be then down to room temperature, take out activation products, first use hydrochloric acid cleaning, then wash unnecessary impurity and by product with water.Activated carbon with high specific surface area can be obtained after drying.As shown in Figure 4, sample 800-CL-4 smoking desorption curve is IV type curve, and the hole of the gac prepared by displaying is meso-hole structure.The specific surface area of sample 800-CL-4 is respectively 1315 cm
2/ g.
Pattern and structural characterization result show, this absorbent charcoal material possesses the meso-hole structure of three-dimensional UNICOM.
As shown in Figure 1, the absorbent charcoal material homogeneous grain diameter prepared by the method, there is a large amount of mesoporous existence on surface, illustrates that the method can obtain high-quality porous active Carbon Materials.
As shown in Figure 2, the meso-hole structure that the absorbent charcoal material prepared by the method is connected by three-dimensional forms, and surface has a large amount of micropores, illustrates that the method can obtain the abundant porous active Carbon Materials in duct.
As shown in Figure 3, the gac prepared by the method has IV type curvilinear characteristic, shows to utilize the method, by regulating and controlling the addition of activator, can obtain dissimilar high-specific surface area absorbent charcoal material.
As shown in Figure 4, the gac prepared by the method has IV and I type curvilinear characteristic, shows Application way, by regulation and control carbonization temperature, can obtain the absorbent charcoal material of different meso-hole structure.
Claims (3)
1. be the method that carbon source prepares active carbon with high specific surface area with asparagus lettuce leaf, it is characterized in that, the method step is:
A, asparagus lettuce leaf carbonize: by asparagus lettuce leaf seasoning, dehydration, under argon shield, adopt progressively temperature-rising method to carbonize asparagus lettuce leaf, heat-up rate is 1 ~ 20 DEG C/min, and carbonization temperature is 100 ~ 1000 DEG C, and soaking time is 1 ~ 10 h, form carbide A;
B, KOH activate: ground by carbide A; and mix with potassium hydroxide and water; after seasoning, under argon shield, progressively temperature-rising method is adopted to activate carbide A; wherein the mass ratio of KOH and carbide A is 1:1 ~ 10:1; heat-up rate is 1 ~ 20 DEG C/min, and activation temperature is 500 ~ 1000 DEG C, and soaking time is 1 ~ 10 h; obtain the gac B of high-specific surface area, gac B cooling, washing are obtained product to neutrality, drying.
2. the method for claim 1, is characterized in that, adopts progressively temperature-rising method to carbonize asparagus lettuce leaf, and heat-up rate is 4 ~ 10 DEG C/min, and carbonization temperature is 400 ~ 800 DEG C, and soaking time is 1 ~ 3 h.
3. the method for claim 1, is characterized in that, adopts progressively temperature-rising method to activate carbide A, wherein the mass ratio of KOH and carbide A is 2:1 ~ 8:1, heat-up rate is 2 ~ 10 DEG C/min, and activation temperature is 700 ~ 900 DEG C, and soaking time is 0.5 ~ 3 h.
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CN108314591A (en) * | 2018-05-08 | 2018-07-24 | 湖南农业大学 | A kind of biology charcoal slow-release fertilizer and preparation method thereof |
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CN109133049A (en) * | 2018-08-03 | 2019-01-04 | 太原工业学院 | A kind of preparation method and application with multi-pore channel, the biomass-based active carbon of level pore structure |
CN111180220A (en) * | 2020-01-18 | 2020-05-19 | 温州大学 | Preparation method of supercapacitor electrode material based on citrus peel biomass charcoal |
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