CN104888708B - Corn scytoblastema three-dimensional multistage pore structure carbon material and preparation method thereof - Google Patents
Corn scytoblastema three-dimensional multistage pore structure carbon material and preparation method thereof Download PDFInfo
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- CN104888708B CN104888708B CN201510381791.1A CN201510381791A CN104888708B CN 104888708 B CN104888708 B CN 104888708B CN 201510381791 A CN201510381791 A CN 201510381791A CN 104888708 B CN104888708 B CN 104888708B
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Abstract
Corn scytoblastema three-dimensional multistage pore structure carbon material and preparation method thereof, it belongs to three-dimensional multistage pore structure carbon materials.The present invention is using cheap, abundance, renewable biomass maize peel as carbon source, by it is simple, be easy to industrialized template-free method and effectively prepare three-dimensional multistage pore structure new carbon, solve cumbersome, time-consuming template process, high cost, be difficult to industrialized problem.Corn scytoblastema three-dimensional multistage pore structure carbon material of the present invention is to dry maize peel successively through shredding, after washing process, it is subsequently adding in KOH solution, flowed back under water bath condition again, sieved after cooling, then solid is calcined under high pure nitrogen atmosphere, then in turn through hydrochloric acid solution cleaning, centrifugation, washing and drying and processing.Carbon material specific surface area of the present invention is up to 927m2·g‑1, be interconnected macropore, mesoporous and micropore pore structure, pore-size distribution are concentrated, and containing enriched in oxygen functional group, content is 12%~17%.
Description
Technical field
The invention belongs to three-dimensional multistage pore structure carbon material；Specifically related to corn scytoblastema three-dimensional multistage pore structure carbon material and
Its preparation method.
Background technology
Three-dimensional multistage hole carbon (3D-HPCs) causes widely studied as the novel electrode carbon material of a class and sorbing material
Person payes attention to and pays close attention to.3D-HPCs has unique pore structure and topological structure, and many advantages are shown in above-mentioned application field,
Including：(1) interconnected macropore, mesoporous and micropore pore structure；(2) high-ratio surface；(3) continuous electronic transmission path；(4)
Pore-size distribution is narrow.Wherein, the hierarchical porous structure for interconnecting is beneficial to the quick transmission of ion, and high-specific surface area can provide wide
Active interface, with superior chemical property and absorption property.
At present, the preparation method of three-dimensional multistage hole carbon mainly uses hard template method and soft template method, is deposited for die version method
The shortcomings of prepared by template and remove cumbersome, time-consuming process complexity, secondary pollution environment；And for soft template method, there is template
Agent is expensive, carbon source requires the problems such as harsh and generated time is long.The drawbacks described above of the two methods, causes prepared many
The cost performance of level hole carbon material is very low, and industrialized application is hindered to a certain extent.Therefore, explore it is a kind of simple,
The method that the template-free method of environmental protection prepares multi-stage porous carbon, especially with continuable biomass as low price carbon source, with weight
Want realistic meaning, even more one work of challenge.
Maize peel produces 1450 × 10 in China every year as a kind of corn planting accessory substance of abundance4The jade of ton
Rice skin, can prepare advanced multi-stage porous carbon material as cheap biomass carbon source.If successfully exploring maize peel as carbon source
Advanced three-dimensional multistage pore structure carbon material is prepared, the commercial applications of three-dimensional multistage hole carbon material will be promoted, come to agricultural belt
Considerable value and economic benefit.
At present, most of maize peel is all lost or is burnt as agricultural wastes, not only waste of resource but also pollution environment.
So, need the efficient method and technique for utilizing for exploring maize peel badly, make full use of the renewable biomass resources.To being at present
Only, carbon unmanned report in three-dimensional multistage hole is prepared by maize peel using simple, to be easy to industrial applications method.
The content of the invention
Three-dimensional multistage hole carbon material prepared it is an object of the present invention to provide a kind of utilization maize peel and preparation method thereof.This
Invention using cheap, abundance, renewable biomass maize peel as carbon source, by it is simple, be easy to industrialized
Template-free method effectively prepares three-dimensional multistage pore structure new carbon, solves cumbersome, time-consuming template process, high cost, difficulty
To realize industrialized problem.
Corn scytoblastema three-dimensional multistage pore structure carbon material is to dry maize peel successively through shredding, after washing process in the present invention
It is dry, it is subsequently adding in KOH solution, then flowed back under water bath condition, sieved after cooling, then solid is roasted under high pure nitrogen atmosphere
Burn, then in turn through hydrochloric acid solution cleaning, centrifugation, washing and drying and processing.
The preparation method of corn scytoblastema three-dimensional multistage pore structure carbon material is carried out in the steps below in the present invention：
Step one, maize peel is shredded, dried under the conditions of 100 DEG C after washing；
Step 2, the corn that will be processed through step one for 1 ﹕ (10~20) proportionings by the mass ratio of maize peel and KOH solution
During skin adds mass concentration to be 2%~10% KOH solution, the 2h~6h that then flowed back in 60 DEG C~120 DEG C water-baths (obtains brown
Color colloidal liquid), with 200 mesh stainless steel screen filtrations after cooling, leave solid；
It is placed in quartz tube furnace after step 3, the solid drying for obtaining step 2, in high pure nitrogen, (volume fraction is
Purity is that 99.999%) atmosphere, temperature are 1~2h of roasting (gray solid) under the conditions of 600~1000 DEG C；
Then step 4 cleans (purpose is removal sylvite) with hydrochloric acid solution, and centrifugation is dried after washed several times with water；Obtain jade
Rice scytoblastema three-dimensional multistage pore structure carbon material.
In the building-up process of multi-stage porous corn scytoblastema carbon material, KOH plays multiple action to the present invention：(1) KOH is used as pre-
Inorganic agent, the cellulose in maize peel is effectively separated with hemicellulose/lignin；(2) KOH remaining in cellulose is micro-
Crystalline substance plays a part of to manufacture macropore；(3) KOH makes a large amount of micropores as activator, improves the specific surface area of carbon material.
Corn scytoblastema three-dimensional multistage hole of the present invention carbon material has the physicochemical properties of many uniquenesses, and its specific surface area is high
Up to 927m2·g-1, be interconnected macropore, mesoporous and micropore pore structure, and pore-size distribution is concentrated, containing enriched in oxygen functional group,
Content is 12wt%~17wt%.
Brief description of the drawings
Fig. 1 is the SEM photograph of corn scytoblastema three-dimensional multistage pore structure carbon material prepared by specific embodiment tripartite method；Figure
2 is the high magnification SEM photograph of corn scytoblastema three-dimensional multistage pore structure carbon material prepared by specific embodiment tripartite method；Fig. 3 is
The low range TEM photos of corn scytoblastema three-dimensional multistage pore structure carbon material prepared by specific embodiment tripartite method；Fig. 4 is specific
The high magnification TEM photos of corn scytoblastema three-dimensional multistage pore structure carbon material prepared by implementation method tripartite method；Fig. 5 is specific implementation
The nitrogen adsorption desorption curve of corn scytoblastema three-dimensional multistage pore structure carbon material prepared by mode tripartite method；Fig. 6 is specific implementation
The wide-angle XRD spectra of corn scytoblastema three-dimensional multistage pore structure carbon material prepared by mode tripartite method；Fig. 7 is specific embodiment three
The total spectrograms of XPS of corn scytoblastema three-dimensional multistage pore structure carbon material prepared by method.
Specific embodiment
Specific embodiment one：In present embodiment the preparation method of corn scytoblastema three-dimensional multistage pore structure carbon material be by
What following step was carried out：
Step one, maize peel is cut into fractionlet, is dried under the conditions of 100 DEG C after washing；
During step 2, the maize peel that 5g is processed through step one add 100mL mass concentrations to be 5% KOH solution, then
Flow back 4h (obtaining brown colloidal liquid) in 80 DEG C of water-baths, with 200 mesh stainless steel screen filtrations after cooling, leaves solid；
Step 3, the solid for obtaining step 2 are placed in quartz tube furnace after being dried under the conditions of 100 DEG C, in High Purity Nitrogen
Gas (volume fraction is that purity is 99.999%) atmosphere, temperature are roasting 2h (gray solid) under the conditions of 800 DEG C；
Step 4 and then (purpose be removal sylvite) is cleaned with the hydrochloric acid solution that concentration is 2mol/L, centrifugation is washed three times
Afterwards 12h is dried under the conditions of 120 DEG C；Obtain maize peel base three-dimensional multistage pore structure carbon material.
Present embodiment obtains corn scytoblastema three-dimensional multistage pore structure carbon material specific surface area for 928m2·g-1, enriched in oxygen
Function mass contg is 14.6wt%.
Specific embodiment two：In present embodiment the preparation method of corn scytoblastema three-dimensional multistage pore structure carbon material be by
What following step was carried out：
Step one, maize peel is cut into fractionlet, is dried under the conditions of 100 DEG C after washing；
During step 2, the maize peel that 5g is processed through step one add 100mL mass concentrations to be 7% KOH solution, then
Flow back 4h (obtaining brown colloidal liquid) in 80 DEG C of water-baths, with 200 mesh stainless steel screen filtrations after cooling, leaves solid；
Step 3, the solid for obtaining step 2 are placed in quartz tube furnace after being dried under the conditions of 100 DEG C, in High Purity Nitrogen
Gas (volume fraction is that purity is 99.999%) atmosphere, temperature are roasting 2h (gray solid) under the conditions of 800 DEG C；
Step 4 and then (purpose be removal sylvite) is cleaned with the hydrochloric acid solution that concentration is 2mol/L, centrifugation is washed three times
Afterwards 12h is dried under the conditions of 120 DEG C；Obtain maize peel base three-dimensional multistage pore structure carbon material.
Present embodiment obtains corn scytoblastema three-dimensional multistage pore structure carbon material specific surface area for 867m2·g-1, enriched in oxygen
Function mass contg is 12.7wt%.
Specific embodiment three：In present embodiment the preparation method of corn scytoblastema three-dimensional multistage pore structure carbon material be by
What following step was carried out：
Step one, maize peel is cut into fractionlet, is dried under the conditions of 100 DEG C after washing；
During step 2, the maize peel that 5g is processed through step one add 100mL mass concentrations to be 9% KOH solution, then
Flow back 4h (obtaining brown colloidal liquid) in 80 DEG C of water-baths, with 200 mesh stainless steel screen filtrations after cooling, leaves solid；
Step 3, the solid for obtaining step 2 are placed in quartz tube furnace after being dried under the conditions of 100 DEG C, in High Purity Nitrogen
Gas (volume fraction is that purity is 99.999%) atmosphere, temperature are roasting 2h (gray solid) under the conditions of 800 DEG C；
Step 4 and then (purpose be removal sylvite) is cleaned with the hydrochloric acid solution that concentration is 2mol/L, centrifugation is washed three times
Afterwards 12h is dried under the conditions of 120 DEG C；Obtain maize peel base three-dimensional multistage pore structure carbon material.
Present embodiment obtains corn scytoblastema three-dimensional multistage pore structure carbon material specific surface area for 814m2·g-1, enriched in oxygen
Function mass contg is 17.01wt%.
Corn scytoblastema three-dimensional multistage pore structure carbon material prepared by present embodiment is tested, structure such as Fig. 1-7 institutes
Show.
As shown in Figure 1, the porous carbon materials for being prepared by maize peel show three-dimensional frame structure, with interconnected big
Pore structure, the thickness of hole wall is about hundreds of nanometers；From big multiplying power surface sweeping electron microscope 2, hole wall surface is coarse, is by nothing
Several nano particles are piled up and are formed, and the diameter of nano particle is about 10nm.
As seen from Figure 3, the hole wall of three-dimensional multistage hole carbon has porous micron flakes pattern, containing a small amount of macropore,
It is substantial amounts of mesoporous.Be can be seen that by high magnification TEM Fig. 4, big hole wall fills micropore by substantial amounts of crack and turbostratic graphite carbon is constituted, and
And there is unordered graphite lattice fringe in the edge of carbon.
As seen from Figure 5, the nitrogen adsorption desorption isotherm of the material is I/IV compound thermoisopleth, shows that this is porous
Carbon material contains substantial amounts of micropore and structure.Obvious hysteresis loop is appeared above in relative partial pressure 0.4, the hysteresis loop is H3 types
Lag loop, and significant adsorption phenomena has been appeared above for 0.95 in relative partial pressure, illustrate that the carbon material contains substantial amounts of
Crack shape is mesoporous and macropore.
As seen from Figure 6, (002), (101) crystalline substance of graphite is corresponded to respectively in two diffraction maximums that 2 θ are 20 ° and 43.8 °
Face, shows there is graphite microcrystalline structure in the carbon material, but the diffraction maximum of (002) crystal face is relatively wide weaker with peak intensity, says
Unordered degree between bright carbon-coating is larger, is amorphous carbon.
As shown in Figure 7, tri- kinds of elements of C, O and N are mainly contained in the three-dimensional multistage pore structure carbon material of present embodiment.
Claims (7)
1. a kind of preparation method of corn scytoblastema three-dimensional multistage pore structure carbon material, it is characterised in that carry out in the steps below：
Step one, maize peel is shredded, dried under the conditions of 100 DEG C after washing；
Step 2, by maize peel and KOH solution mass ratio for 1 ﹕ (10~20) proportioning the maize peel processed through step one is added
Enter in the KOH solution that mass concentration is 2%~10%, then flow back 2h~6h in 60 DEG C~120 DEG C water-baths, is used after cooling
200 mesh stainless steel screen filtrations, leave solid；
It is placed in quartz tube furnace after step 3, the solid drying for obtaining step 2, is 600 in high pure nitrogen atmosphere, temperature
1~2h is calcined under the conditions of~1000 DEG C；
Step 4, by step 3 obtain product clean with hydrochloric acid solution, be centrifuged, after washed several times with water drying；Obtain maize peel
Base three-dimensional multistage pore structure carbon material.
2. the preparation method of corn scytoblastema three-dimensional multistage pore structure carbon material according to claim 1, it is characterised in that step
KOH solution mass concentration described in two is 5%~9%.
3. the preparation method of corn scytoblastema three-dimensional multistage pore structure carbon material according to claim 1, it is characterised in that step
KOH solution mass concentration described in two is 7%.
4. the preparation method of corn scytoblastema three-dimensional multistage pore structure carbon material according to claim 1, it is characterised in that step
Drying temperature described in three is 100 DEG C.
5. the preparation method of corn scytoblastema three-dimensional multistage pore structure carbon material according to claim 1, it is characterised in that step
Sintering temperature described in three is 800 DEG C, and roasting time is 2 hours.
6. the preparation method of corn scytoblastema three-dimensional multistage pore structure carbon material according to claim 1, it is characterised in that step
The concentration of hydrochloric acid solution described in four is 2mol/L.
7. the preparation method of corn scytoblastema three-dimensional multistage pore structure carbon material according to claim 1, it is characterised in that step
Drying temperature described in four is 120 DEG C, and drying time is 12h.
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| CN106311224A (en) * | 2016-09-10 | 2017-01-11 | 上海大学 | Preparation method of charcoal-based oxygen reduction catalyst |
| CN112403435A (en) * | 2019-08-21 | 2021-02-26 | 天津科技大学 | Preparation method of KOH-microwave activated corncob activated carbon for treating cationic dye-containing wastewater |
| CN112062128B (en) * | 2020-09-10 | 2023-01-24 | 中国矿业大学 | Preparation method and application of nitrogen-doped porous carbon material based on crop straws |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1446748A (en) * | 2003-03-07 | 2003-10-08 | 太原理工大学 | Method for preparing active carbon with height ratio surface area |
| CN104445193A (en) * | 2014-12-03 | 2015-03-25 | 盐城工学院 | Branch and leaf porous carbon with function of removing degradation-resistant organic pollutant effluent 2,4,6-trichlorophenol as well as preparation method and application thereof |
| CN104709906A (en) * | 2013-12-17 | 2015-06-17 | 中国科学院过程工程研究所 | Preparation method of three dimensional graded porous activated carbon material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1446748A (en) * | 2003-03-07 | 2003-10-08 | 太原理工大学 | Method for preparing active carbon with height ratio surface area |
| CN104709906A (en) * | 2013-12-17 | 2015-06-17 | 中国科学院过程工程研究所 | Preparation method of three dimensional graded porous activated carbon material |
| CN104445193A (en) * | 2014-12-03 | 2015-03-25 | 盐城工学院 | Branch and leaf porous carbon with function of removing degradation-resistant organic pollutant effluent 2,4,6-trichlorophenol as well as preparation method and application thereof |
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Inventor after: Ma Fangwei Inventor after: Lei Guangping Inventor after: Wu Guang Inventor after: Wan Jiafeng Inventor after: Song Shijiao Inventor before: Ma Fangwei Inventor before: Wan Jiafeng Inventor before: Wu Guang Inventor before: Song Shijiao |
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