CN103086368A - Method for preparing magnetic nano graphite carbon by taking waste shaddock peels as carbon source - Google Patents
Method for preparing magnetic nano graphite carbon by taking waste shaddock peels as carbon source Download PDFInfo
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Abstract
The invention provides a method for preparing magnetic nano graphite carbon by taking waste shaddock peels as a carbon source, relates to a method for preparing the magnetic nano graphite carbon, and is used for solving the problems of wasting of resource utilization wastes and high cost, environmental pollution and complicated experiment processes and equipment of the existing preparation method. The method comprises the following steps of pretreating the waste shaddock peels, then adding a catalyst, carrying out carbonizing treatment after the reaction is completed, and finally drying so as to obtain the magnetic nano graphite carbon. According to the method, the active components of the catalyst are successfully embedded into a graphitization carbon structure through the regulation and control of the pretreatment of waste shaddock peels as well as the conditions such as the addition amount of the catalyst, drying temperature, heating rate, carbonization temperature and time, impurity removal temperature, impurity removal reaction time and the like, so that the property, appearance and structure of the magnetic nano graphite carbon can be regulated and controlled. The preparation method is simple and environment-friendly, needs simple experiment equipment, and can be applicable to fields such as adsorption, separation, electrochemistry, catalysis and the like.
Description
Technical field
The present invention relates to a kind of method for preparing the magnetic Nano graphite carbon.
Background technology
Shaddock has another name called pomelo, gas mandarin orange, is a kind of fruit of Rutaceae Citrus.China's shaddock resource is very abundant, is distributed widely in the ground such as Guangdong, Guangxi, Fujian, sells and spreads all over all parts of the country.Shaddock is cold in nature, the sweet acid of distinguishing the flavor of, and has that anti-inflammatory is fungi-proofing, preventing phlegm from forming and stopping coughing, the gut purge of regulating the flow of vital energy, lower gas help digestion, enrich blood the effects such as invigorating the spleen.The fragrance of its uniqueness, salubrious mouthfeel enjoys people's favor.The unique texture of pomelo peel makes it can bear surging force up to thousands of newton, and absorbs a large amount of energy; It mainly is made of two kinds of different biological tissues: contain the exterior skin of sebiferous gland, and the spongy middle mesothelium of most white.Contain the various active composition in the crust of shaddock, as: naringin, pectin, volatile oil, pigment etc., have higher health care and pharmaceutical use, also have the effect of control and kill pests; The organic substances such as the spongy material rich cellulose in the cellular middle mesothelium of shaddock, xylogen.Annual have a large amount of pomelo peels to be thrown away in China and even the whole world, causes the significant wastage of resource, and environment and human lives have been produced detrimentally affect.
The structural analysis of pomelo peel is found that skin portion is a process that gradually changes to its density of middle skin portion outside shaddock, can't clearly distinguish the crust of densification and cellular middle mesothelium.This gradual change organize the sudden change of also just having avoided on structural constituent, structure and mechanical property.Pomelo peel has compact structure of fibrous tissue, and there is a large amount of holes in inside, and arrange closely in some holes, and some arrangements are loose, are cellular.Mierocrystalline cellulose and hemicellulose in the surfaces externally and internally of the abundant hole of pomelo peel are rich in hydroxyl and polyphenol group, can produce powerful gravitation arrives the material absorbing in water wherein, and the coherent element in the pomelo peel hole etc. can produce chemical reaction with Cucumber, and they are adsorbed onto pore surface.
In sum, we can expect, if utilize the character of these groups in pomelo peel, make it carry out coordination by the cation constituent in the modes such as different mechanisms such as electrostatic adhesion, complexing, hydrogen bond and catalyzer, so just can prepare the carbon material that has than the high graphitization degree.And the pore texture of fiber can increase the chance that contacts with the catalyst activity component, utilizes its larger specific surface area, makes pomelo peel to the active ingredient of catalyzer, stronger adsorptive power be arranged.Through after charing, can prepare have abundant than bigger serface, hole, than the magnetic Nano graphite carbon of high graphitization degree, realize the changing waste into resources utilization.
Summary of the invention
The present invention is that resourcebility utilizes the waste of refuse and existing preparation method's cost is high in order to solve, the problem of not environmental protection, experimentation and equipment complexity, prepares the method for magnetic Nano graphite carbon and provide a kind of as carbon source take discarded pomelo peel.
Of the present invention a kind ofly carry out according to the following steps take discarded pomelo peel as the method that carbon source prepares the magnetic Nano graphite carbon:
One, pomelo peel surfaces externally and internally impurity is cleaned out, be cut into the strip that 0.5~2cm is wide, 5~10cm is long, dry 22~26h, obtain dry pomelo peel under 50~100 ℃;
Two, be 1 by the pomelo peel of step 1 and the mass ratio of catalyzer: (0.5~3), the pomelo peel of step 1 is joined in the catalyst solution that mass concentration is 50~300g/L, react at ambient temperature 22~26h, then put into air dry oven, dry 22~26h under 50~80 ℃, obtain presoma, wherein catalyzer is molysite, nickel salt or cobalt salt;
Three, the presoma that step 2 is obtained is placed on N
2Carry out charing in tube furnace under atmosphere, carbonization temperature is 900~1100 ℃, and temperature rise rate is 1~20 ℃/min, and carbonization time is 30~300min, obtains carbide;
Four, it is under the condition of 30~90 ℃ in temperature that the carbide that step 3 is obtained is placed in deionized water, stirs 30~120min, then utilizes foreign field to carry out magnetic and separates, and removal of impurities is completed in repetitive operation 2~4 times;
Five, the carbide after the step 4 removal of impurities being placed in air dry oven, is dry 22~26h under the condition of 50~80 ℃ at drying temperature, obtains the magnetic Nano graphite carbon.
The carbon source that adopt a kind of have the following advantages take discarded pomelo peel as the method that carbon source prepares the magnetic Nano graphite carbon (1) of the present invention exists a large amount of holes and surface to be rich in the discarded pomelo peel of oxygen-containing functional group as having compact structure of fibrous tissue, inside.(2) adopt simple charring process, be the higher carbon material of degree of graphitization with organic matter transformation such as the Mierocrystalline cellulose in pomelo peel, hemicelluloses, by the regulation and control reaction conditions, and utilize interaction between pomelo peel and catalyst activity component group, magnetic nano-particle is embedded among the skeleton structure of graphitized carbon, effectively stop its in use oxidation and leaching of magnetic nano-particle, thereby make the magnetic Nano graphite carbon product of preparation keep for a long time its intrinsic characteristic.(3) by changing experiment condition, can realize the content of the magnetic nano-particle on nano-graphite carbon and the regulation and control of size, utilize the distinctive magnetic of magnetic Nano graphite carbon and catalysis characteristics, can be applied to the fields such as absorption, separation, catalysis and electrochemistry, and can not bring in actual applications secondary pollution, can realize cycling and reutilization.(4) explore the discarded pomelo peel treatment process that is adapted to environmental friendliness and recycling economy development theory, will provide scientific basis for the recycling of similar refuse, be also the biomass energy development practice in the urgent need to.(5) simple, the environmental protection of preparation method, experimental installation are simple, and cost is low.
Description of drawings
Fig. 1 is the Raman spectrogram of the magnetic Nano graphite carbon of embodiment 1 preparation;
Fig. 2 is the X-ray diffraction spectrogram of the magnetic Nano graphite carbon of embodiment 1 preparation;
Fig. 3 is the X-ray diffraction spectrogram of the magnetic Nano graphite carbon of embodiment 2 preparations;
Fig. 4 is the N of the magnetic Nano graphite carbon of embodiment 3 preparations
2The adsorption/desorption graphic representation, wherein curve a is N
2Adsorption curve, curve b are N
2The desorption curve;
Fig. 5 is the BJH mean pore size distribution plan of the magnetic Nano graphite carbon of embodiment 3 preparations;
Fig. 6 is the electron scanning micrograph of the magnetic Nano graphite carbon of embodiment 4 preparations;
Fig. 7 is the high-resolution-ration transmission electric-lens photo of the magnetic Nano graphite carbon of embodiment 4 preparations.
Embodiment
Technical scheme of the present invention is not limited to following embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: a kind of of present embodiment carries out according to the following steps take discarded pomelo peel as the method that carbon source prepares the magnetic Nano graphite carbon:
One, pomelo peel surfaces externally and internally impurity is cleaned out, be cut into the strip that 0.5~2cm is wide, 5~10cm is long, dry 22~26h, obtain dry pomelo peel under 50~100 ℃;
Two, be 1 by the pomelo peel of step 1 and the mass ratio of catalyzer: (0.5~3), the pomelo peel of step 1 is joined in the catalyst solution that mass concentration is 50~300g/L, react at ambient temperature 22~26h, then put into air dry oven, dry 22~26h under 50~80 ℃, obtain presoma, wherein catalyzer is molysite, nickel salt or cobalt salt;
Three, the presoma that step 2 is obtained is placed on N
2Carry out charing in tube furnace under atmosphere, carbonization temperature is 900~1100 ℃, and temperature rise rate is 1~20 ℃/min, and carbonization time is 30~300min, obtains carbide;
Four, it is under the condition of 30~90 ℃ in temperature that the carbide that step 3 is obtained is placed in deionized water, stir 30~120min, then utilize foreign field to carry out magnetic and separate, carbide and the deionized water that has dissolved impurity are separated from each other, removal of impurities is completed in repetitive operation 2~4 times;
Five, the carbide after the step 4 removal of impurities being placed in air dry oven, is dry 22~26h under the condition of 50~80 ℃ at drying temperature, obtains the magnetic Nano graphite carbon.
The carbon source that adopt a kind of have the following advantages take discarded pomelo peel as the method that carbon source prepares the magnetic Nano graphite carbon (1) of present embodiment exists a large amount of holes and surface to be rich in the discarded pomelo peel of oxygen-containing functional group as having compact structure of fibrous tissue, inside.(2) adopt simple charring process, be the higher carbon material of degree of graphitization with organic matter transformation such as the Mierocrystalline cellulose in pomelo peel, hemicelluloses, by the regulation and control reaction conditions, and utilize interaction between pomelo peel and catalyst activity component group, magnetic nano-particle is embedded among the skeleton structure of graphitized carbon, effectively stop its in use oxidation and leaching of magnetic nano-particle, thereby make the magnetic Nano graphite carbon product of preparation keep for a long time its intrinsic characteristic.(3) by changing experiment condition, can realize the content of the magnetic nano-particle on nano graphite carbon and the regulation and control of size, utilize the distinctive magnetic of magnetic Nano graphite carbon and catalysis characteristics, can be applied to the fields such as absorption, separation, catalysis and electrochemistry, and can not bring in actual applications secondary pollution, can realize cycling and reutilization.(4) explore the discarded pomelo peel treatment process that is adapted to environmental friendliness and recycling economy development theory, will provide scientific basis for the recycling of similar refuse, be also the biomass energy development practice in the urgent need to.(5) simple, the environmental protection of preparation method, experimental installation are simple, and cost is low.
Embodiment two: what present embodiment was different from embodiment one is: in step 1, dried pomelo peel is put into silica gel drier and is preserved, and other step is identical with embodiment one with parameter.
Embodiment three: what present embodiment was different from embodiment one or two is: in step 2, catalyzer is one or more the mixture in iron(ic) chloride, iron protochloride, iron nitrate, Iron nitrate, ferric sulfate, ferrous sulfate, nickelous chloride, nickelous nitrate, single nickel salt, cobalt chloride, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and rose vitriol, and other step is identical with embodiment one or two with parameter.
Embodiment four: what present embodiment was different from one of embodiment one to three is: be 24h the time of drying in step 1, step 2 and step 4, other step is identical with embodiment three with parameter.
Embodiment five: what present embodiment was different from one of embodiment one to four is: in step 2, the mass ratio of pomelo peel and catalyzer is 1: 1, and other step is identical with one of parameter and embodiment one to four.
Embodiment six: what present embodiment was different from one of embodiment one to five is: the mass concentration of step 2 catalyst solution is 150~200g/L, and other step is identical with one of parameter and embodiment one to five.
Embodiment seven: what present embodiment was different from one of embodiment one to six is: in step 3, carbonization temperature is 1050 ℃, and other step is identical with one of parameter and embodiment one to six.
Embodiment eight: what present embodiment was different from one of embodiment one to seven is: in step 3 during charing temperature rise rate be 10 ℃/min, other step is identical with one of parameter and embodiment one to seven.
Embodiment nine: what present embodiment was different from one of embodiment one to eight is: in step 3, carbonization time is 90min, and other step is identical with one of parameter and embodiment one to eight.
Embodiment ten: what present embodiment was different from one of embodiment one to nine is: in step 4, the removal of impurities process repeats 3 times, and other step is identical with one of parameter and embodiment one to nine.
With following verification experimental verification beneficial effect of the present invention:
Embodiment 1, prepare the method for magnetic Nano graphite carbon as carbon source take discarded pomelo peel, it is characterized in that the method carries out according to the following steps:
One, pomelo peel surfaces externally and internally impurity is cleaned out, be cut into the strip that 0.5cm is wide, 5cm is long, dry 24h under 80 ℃ obtains dry pomelo peel;
Two, it is 1: 1 by the pomelo peel of step 1 and the mass ratio of iron(ic) chloride, the pomelo peel of step 1 is joined in the catalyst solution that mass concentration is 200g/L, react at ambient temperature 24h, then put into air dry oven, dry 24h, obtain presoma under 80 ℃;
Three, the presoma that step 2 is obtained is placed on N
2Carry out charing, N in tube furnace under atmosphere
2Flow is 100mL/min, and carbonization temperature is 900 ℃, and temperature rise rate is 5 ℃/min, and carbonization time is 60min, obtains carbide;
Four, it is under the condition of 80 ℃ in temperature that the carbide that step 3 is obtained is placed in the 100mL deionized water, stir 60min, then utilize foreign field to carry out magnetic and separate, carbide and the deionized water that has dissolved impurity are separated from each other, removal of impurities is completed in repetitive operation 3 times;
Five, the carbide after the step 4 removal of impurities being placed in air dry oven, is dry 24h under the condition of 50 ℃ at drying temperature, obtains the magnetic Nano graphite carbon.
Embodiment 2, prepare the method for magnetic Nano graphite carbon as carbon source take discarded pomelo peel, the present embodiment as different from Example 1 in step 3 carbonization temperature be 1050 ℃, other steps and parameter are identical with embodiment 1.
Embodiment 3, prepare the method for magnetic Nano graphite carbon as carbon source take discarded pomelo peel, the present embodiment temperature rise rate that charing is in step 3 as different from Example 1 is 10 ℃/min, and other steps and parameter are identical with embodiment 1.
Embodiment 4, prepare the method for magnetic Nano graphite carbon as carbon source take discarded pomelo peel, the present embodiment as different from Example 1 in step 3 carbonization time be 90min, other steps and parameter are identical with embodiment 1.
Test one, be that JYHR800 laser co-focusing micro-Raman spectroscopy detects the magnetic Nano graphite carbon that embodiment 1 obtains with model, obtain Raman spectrogram as shown in Figure 1, as can be seen from the figure, at 1325em
-1(D band) and 1578cm
-1(G band) locates to have occurred two characteristic peaks, and D band is corresponding to the defective of graphite, it and sp
3The vibration of carbon atom is relevant, and the G band is corresponding to the E of graphite
2gPattern, it and sp
2The vibration of carbon atom is relevant, so the peak intensity ratio of G band and D band usually is used for expression sp
2Carbon atom number and sp
3Carbonatoms purpose ratio.In Fig. 1 spectrogram, the strong ratio in peak of G band and D band near 2.0, illustrates to have obtained degree of graphitization magnetic Nano graphite carbon preferably.
Test two, be that magnetic Nano graphite carbon that the X-gamma meter of D/max-IIIB type obtains embodiment 1 carries out X-ray diffraction and tests with model, obtain X-ray diffraction spectrogram as shown in Figure 2, as can be seen from the figure, the Fe of main diffraction peak and face-centred cubic structure
3O
4The peak position of (JCPDS card No.75-1609) is consistent, and magnetic particle Fe
3O
4Being embedded in the graphite carbon structure, the peak position of obvious graphite carbon do not occurred, is because Fe
3O
4The peak covered the diffraction peak of ° graphite carbon of locating in 2 θ=26.
Test three, be that magnetic Nano graphite carbon that the X-gamma meter of D/max-IIIB type obtains embodiment 2 carries out X-ray diffraction and tests with model, obtain X-ray diffraction spectrogram as shown in Figure 3, as can be seen from the figure, in the time of 1050 ℃, ° locate to occur the diffraction peak of obvious graphite carbon in 2 θ=26, illustrate to have obtained the magnetic Nano graphite carbon, simultaneously comparison diagram 2, can draw the rising along with carbonization temperature, degree of graphitization increases.
Test four, be the fully-automatic analyzer of TriStarII 3020 with model, the magnetic Nano graphite carbon that embodiment 3 is obtained is specific surface area and the pore size distribution of specimen under 77K in temperature, obtains the N as shown in Figure 4 and 5
2Adsorption/desorption curve and BJH pore size distribution curve figure, the specific surface area (S of magnetic Nano graphite carbon when drawing temperature rise rate and be 10 ℃/min by Fig. 3 and Fig. 4
BET) be 545.9m
2/ g, pore size distribution is wider, and take mesopore as main, mean pore size is 10.7nm.
Test five, be the scanning electron microscope of Hitachi S-4800 with model, with the transmission electron microscope that model is JEM-2100, embodiment 4 is observed, obtain stereoscan photograph and transmission electron microscope photo as Fig. 6 and Fig. 7, as can be seen from Figure 6, a lot of magnetic particles at the surface inserting of bulk carbon material, arrangement is tight and shape is comparatively regular.The lattice fringe spacing that can measure upper left quarter from Fig. 7 is 0.34nm, this is consistent with graphite (002) spacing, show that product has good degree of crystallinity, the black nahlock of middle and lower part is magnetic particle, due to its katalysis, make the gained carbon products higher degree of graphitization occur.
Claims (10)
1. prepare the method for magnetic Nano graphite carbon as carbon source take discarded pomelo peel, it is characterized in that the method carries out according to the following steps:
One, pomelo peel surfaces externally and internally impurity is cleaned out, be cut into the strip that 0.5~2cm is wide, 5~10cm is long, dry 22~26h, obtain dry pomelo peel under 50~100 ℃;
Two, be 1 by the pomelo peel of step 1 and the mass ratio of catalyzer: (0.5~3), the pomelo peel of step 1 is joined in the catalyst solution that mass concentration is 50~300g/L, react at ambient temperature 22~26h, then put into air dry oven, dry 22~26h under 50~80 ℃, obtain presoma, wherein catalyzer is molysite, nickel salt or cobalt salt;
Three, the presoma that step 2 is obtained is placed on N
2Carry out charing in tube furnace under atmosphere, carbonization temperature is 900~1100 ℃, and temperature rise rate is 1~20 ℃/min, and carbonization time is 30~300min, obtains carbide;
Four, it is under the condition of 30~90 ℃ in temperature that the carbide that step 3 is obtained is placed in deionized water, stirs 30~120min, then utilizes foreign field to carry out magnetic and separates, and removal of impurities is completed in repetitive operation 2~4 times;
Five, the carbide after the step 4 removal of impurities being placed in air dry oven, is dry 22~26h under the condition of 50~80 ℃ at drying temperature, obtains the magnetic Nano graphite carbon.
2. according to claim 1ly prepare the method for magnetic Nano graphite carbon as carbon source take discarded pomelo peel, it is characterized in that in step 1, dried pomelo peel is put into silica gel drier to preserve.
3. according to claim 1 and 2ly prepare the method for magnetic Nano graphite carbon as carbon source take discarded pomelo peel, it is characterized in that catalyzer in step 2 is one or more the mixture in iron(ic) chloride, iron protochloride, iron nitrate, Iron nitrate, ferric sulfate, ferrous sulfate, nickelous chloride, nickelous nitrate, single nickel salt, cobalt chloride, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and rose vitriol.
4. according to claim 3ly prepare the method for magnetic Nano graphite carbon as carbon source take discarded pomelo peel, it is characterized in that being time of drying in step 1, step 2 and step 4 24h.
5. according to claim 3ly prepare the method for magnetic Nano graphite carbon as carbon source take discarded pomelo peel, it is characterized in that in step 2, the mass ratio of pomelo peel and catalyzer is 1: 1.
6. according to claim 3ly prepare the method for magnetic Nano graphite carbon as carbon source take discarded pomelo peel, the mass concentration that it is characterized in that the step 2 catalyst solution is 150~200g/L.
7. according to claim 3ly prepare the method for magnetic Nano graphite carbon as carbon source take discarded pomelo peel, it is characterized in that in step 3, carbonization temperature is 1050 ℃.
8. according to claim 3ly prepare the method for magnetic Nano graphite carbon as carbon source take discarded pomelo peel, when it is characterized in that in step 3 charing, temperature rise rate is 10 ℃/min.
9. according to claim 3ly prepare the method for magnetic Nano graphite carbon as carbon source take discarded pomelo peel, it is characterized in that in step 3, carbonization time is 90min.
10. according to claim 3ly prepare the method for magnetic Nano graphite carbon as carbon source take discarded pomelo peel, it is characterized in that in step 4, the removal of impurities process repeats 3 times.
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CN101445234A (en) * | 2009-01-06 | 2009-06-03 | 黑龙江大学 | A preparation method of graphitized carbon nano material |
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CN109167077B (en) * | 2018-09-13 | 2022-05-17 | 大连海事大学 | Phosphorus-doped porous carbon-oxygen reduction catalyst and preparation method and application thereof |
CN109368632A (en) * | 2018-12-17 | 2019-02-22 | 新奥石墨烯技术有限公司 | Graphitized carbon material and preparation method thereof |
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