CN104211040A - Preparation method of porous carbon nano rod with high specific area - Google Patents
Preparation method of porous carbon nano rod with high specific area Download PDFInfo
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- CN104211040A CN104211040A CN201310567042.9A CN201310567042A CN104211040A CN 104211040 A CN104211040 A CN 104211040A CN 201310567042 A CN201310567042 A CN 201310567042A CN 104211040 A CN104211040 A CN 104211040A
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Abstract
The invention provides a preparation method of a porous carbon nano rod with a high specific area. The preparation method comprises the following steps (1) weighing zinc salts and trimesic acid according to a ratio of amount of substance of 0.5-5:1, dissolving the zinc salts and trimesic acid in an organic solvent, fiercely stirring for 0.5-3 hours at a room temperature, then carrying out a solvent heat treatment for 1 to 4 days at a temperature of 80 to 160 DEG C, filtering, washing, carrying out solvent exchange, and drying the obtained solid in vacuum to obtain white powder, wherein the ratio of amount of substance of the organic solvent to zinc salts is 20-200:1; (2) rapidly heating the white powder obtained in the step (1) to a temperature of 910 DEG C or more at a speed of 2-20 DEG C/min in a nitrogen gas atmosphere, maintaining the temperature for 1 to 12 hours, cooling to the room temperature so as to obtain the porous carbon nano rod with a high specific surface area. The provided preparation method has the advantages of economic route, low cost, simple operation, and mild conditions. The target product has a high specific area and narrow pore size distribution, and has an amorphous carbon structure and a graphite carbon structure at the same time.
Description
Technical field
The present invention relates to a kind of preparation method of high specific surface area porous carbon nano rod, belong to carbon nanomaterial preparation technology field.
Background technology
Porous carbon nano material chemical stability, (water) Heat stability is good, specific surface area is high, is widely used in the numerous areas such as absorption, separation, support of the catalyst, electrochemistry.In multiple carbon nanomaterial, carbon nano rod has very large potential using value because of the chemical property of its excellence in battery anode material.But the specific surface area of carbon nano rod is usually less, and there is no maturation and the simple method for preparing of applicable scale operation, seriously constrain the further application of carbon nano rod.Therefore, the preparation method researching and developing high-specific surface area carbon nano rod is particularly important.
At present, carbon nano rod mainly adopts two kinds of method preparations: the aluminium base controllable growth method of anodic oxidation and mesopore molecular sieve hard template method.The former to hold concurrently catalyzer as template with anodised aluminium (AAO), prepares carbon nano rod array by chemical vapor deposition method.AAO substrate needs to be prepared by electrochemical method, consume a large amount of electric energy, and the existence of AAO, the nanometer rod purity obtained is lower, and this method is also not suitable for large-scale production and application (Chen Leishan, Wang Cunjing, Miao Yu, Chen Gairong. anodic oxidation aluminium formwork is substrate controlled synthesis carbon nano rod, heat processing technique, 2013,42 (14): 80-82).Be that template then can prepare the higher organized carbon nano rod array of purity with ordered mesoporous silicon, this method selects the mesoporous silicon material with special hole as template usually, dipping target material or presoma make it react in the duct of mould material, then carbonization obtain the replica of ordered structural material after removing template.Such as Ryoo seminar successively utilizes SBA-15, HMS, KIT-6 floods sucrose, phenolic aldehyde, sucrose, through carbonization and obtain organized carbon nano rod array CMK-3(Shinae Jun after removing template, Sang Hoon Joo, Ryong Ryoo, Michal Kruk, Mietek Jaroniec, Zheng Liu, Tetsu Ohsuna, Osamu Terasaki.Synthesis of new, nanoporous carbon with hexagonally ordered mesostructure, Journal of the American Chemical Society, 2000, 122 (43): 10712-10713), CMK-8(Freddy Kleitz, Shin Hei Choi, Ryong Ryoo.Cubic Ia3d large mesoporous silica:synthesis and replication to platinum nanowires, carbon nanorods and carbon nanotubes, Chemical Communications, 2003, 9 (17): 2136-2137).Clearly, the preparation of the method experience mesoporous silicon hard template, carbon source dipping, carbonization, hard template such as to remove at multiple step, last grow, cost is high, and the carbon nano rod that hard template method obtains also is solid construction, and specific surface area is very little.These features determine hard template method and are also not suitable for scale operation, and the carbon nano rod application of preparation is also very limited.
Recently, utilize metallic organic framework to contain carbon rich and the low feature be easily removed under the high temperature conditions of metallic zinc boiling point, direct carbonization prepares the porous carbon nano material of high-specific surface area containing metallic organic framework one step of zinc, is proved to be a kind of effective method.Such as at 1000 DEG C, direct carbonization ZIF-8 under inert gas conditions, preparing specific surface area is 1110m
2microporous carbon (the Watcharop Chaikittisilp of/g, Ming Hu, Hongjing Wang, Hou-Sheng Huang, Taketoshi Fujita, Kevin C.-W.Wu, Lin-Chi Chen, Yusuke Yamauchi, Katsuhiko Ariga.Nanoporous carbons through direct carbonization of a zeolitic imidazolate framework for supercapacitor electrodes, Chemical Communications, 2012,48 (58): 7259-7261).Yang etc., at 900 DEG C, direct carbonization IRMOF-1, IRMOF-3 and IRMOF-8 under inert gas conditions, obtain specific surface area and are respectively 3174,1678 and 1978m
2porous carbon (the Seung Jae Yang of/g, Taehoon Kim, Ji Hyuk Im, Yern Seung Kim, Kunsil Lee, Haesol Jung, Chong Rae Park.MOF-derived hierarchically porous carbon with exceptional porosity and hydrogen storage capacity, Chemistry of Materials, 2012,24 (3): 464-470).
But all there is the deficiencies such as complex steps, cost is high, purity is low, specific surface area is little in the preparation method of current carbon nano rod.
Summary of the invention
For solving the problems of the technologies described above, the object of the present invention is to provide a kind of preparation method of carbon nano rod, obtain the bar-shaped zinc-containing metal organic backbone of high stability by synthesis and under high temperature cabonization condition, metallic zinc removed, obtaining the porous carbon nanometer rod of high-specific surface area.
For achieving the above object, the invention provides a kind of preparation method of high specific surface area porous carbon nano rod, it comprises the following steps:
(1) zinc salt and trimesic acid is taken according to the amount of substance ratio of 0.5-5:1, the two is dissolved in organic solvent, at room temperature violent stirring 0.5-3h, then the solvent heat treatment of 1-4 days is carried out at 80-160 DEG C, the solid obtained is filtered, washs, after exchange of solvent and vacuum-drying, obtain white powder (it is trimesic acid zinc metallic organic framework), wherein, described organic solvent is 20-200:1 with the amount of substance ratio of zinc salt;
(2) white powder step (1) obtained with more than the ramp to 910 of 2-20 DEG C/min DEG C and constant temperature keeps 1-12h, is then down to room temperature, is obtained high specific surface area porous carbon nano rod in nitrogen atmosphere.
In the above-mentioned methods, preferably, zinc salt and the amount of substance of trimesic acid are than being 0.8:1.
In the above-mentioned methods, preferably, the zinc salt adopted is one or more the mixture in two water zinc acetates, anhydrous zinc acetate, zinc chloride, four water zinc sulphates, four water zinc nitrates and zinc nitrate hexahydrate etc.
In the above-mentioned methods, preferably, the organic solvent adopted is one or more the mixture in N, N'-dimethyl formamide (DMF), N, N'-diethylformamide (DEF) and N, N'-N,N-DIMETHYLACETAMIDE (DMAC) etc.
In the above-mentioned methods, preferably, in step (2), the temperature after intensification is 910-980 DEG C.
In the above-mentioned methods, preferably, step (2) for: the white powder that step (1) is obtained in nitrogen atmosphere with the ramp to 950 of 5 DEG C/min DEG C and constant temperature keeps 2h, be then down to room temperature, obtain described high specific surface area porous carbon nano rod.
In the above-mentioned methods, preferably, the temperature of solvent heat treatment is 140 DEG C, and the time is 2 days.
Present invention also offers a kind of porous carbon nanometer rod, it is prepared by above-mentioned method.
According to specific embodiment of the invention scheme, preferably, the BET specific surface area of this porous carbon nanometer rod is 6510m
2/ g, langmuir specific surface area is 9163m
2/ g.
According to specific embodiment of the invention scheme, preferably, the aperture of this porous carbon nanometer rod is 4.2nm, and pore volume is 4.44cm
3/ g.
The preparation method of carbon nano rod provided by the invention with zinc salt and trimesic acid for raw material, bar-shaped trimesic acid zinc metallic organic framework can be obtained through stirring at room temperature, solvent heat treatment, exchange of solvent and vacuum-drying, it can be used as carbon source afterwards, direct high temperature cabonization obtains the carbon nano rod with high specific surface area and flourishing pore texture.The present invention does not use template, and when high temperature cabonization bar-shaped trimesic acid zinc metallic organic framework, the metallic zinc (boiling point 908 DEG C) that in-situ reducing is formed is removed, and makes the porous carbon nanometer rod of acquisition have high specific surface area and flourishing porosity.
The present invention adopts the simple and easy method of a kind of direct carbonization bar-shaped trimesic acid zinc metallic organic framework to prepare the porous carbon nanometer rod of high-specific surface area, the method preparation process economy, cost is low, simple and easy and the mild condition of operating process, target product specific surface area is high, pore size distribution is narrow, and there is amorphous and Graphitic carbon structure simultaneously, and maturing temperature realization can be changed to material specific surface area, the modulation in aperture and amorphous and modulation that is graphitized carbon ratio, be applicable to making sorbent material, support of the catalyst, electrode materials and synthesize the hard template etc. of other mesoporous material, there is certain market application foreground.
Accompanying drawing explanation
The XRD spectra of the trimesic acid zinc metallic organic framework of Fig. 1 synthesized by embodiment 1;
The XRD spectra of the carbon nano rod of Fig. 2 synthesized by embodiment 1;
The SEM image of the trimesic acid zinc metallic organic framework of Fig. 3 a-Fig. 3 f synthesized by embodiment 1 and carbon nano rod and EDX result, wherein, Fig. 3 a is the SEM image that trimesic acid zinc metallic organic framework amplifies 10000 times, Fig. 3 b is the SEM image that trimesic acid zinc metallic organic framework amplifies 50000 times, Fig. 3 c is the EDX analytical results of trimesic acid zinc metallic organic framework, Fig. 3 d is the SEM image that carbon nano rod amplifies 50000 times, Fig. 3 e is the SEM image of carbon nano rod cross section, and Fig. 3 f is the EDX analytical results of carbon nano rod;
The N of the carbon nano rod of Fig. 4 a synthesized by embodiment 1
2absorption/desorption isotherm;
The pore size distribution curve of the carbon nano rod of Fig. 4 b synthesized by embodiment 1;
The Raman spectrogram of the carbon nano rod of Fig. 5 synthesized by embodiment 1;
Fig. 6 is the standard working curve of aniline absorption;
The aniline adsorption isothermal line of the carbon nano rod of Fig. 7 a synthesized by embodiment 1;
Fig. 7 b is the aniline absorption result adopting Freundlich model-fitting.
Embodiment
In order to there be understanding clearly to technical characteristic of the present invention, object and beneficial effect, existing following detailed description is carried out to technical scheme of the present invention, but can not be interpreted as to of the present invention can the restriction of practical range.
Embodiment 1
Present embodiments provide a kind of preparation method of high specific surface area porous carbon nano rod, it comprises the following steps:
Take 2.6g bis-water zinc acetate (10mmol) and 2.5g trimesic acid (12mmol), be dissolved among 100mL DMF, at room temperature stir 0.5h, then carry out the solvent heat treatment of 2 days at 140 DEG C, the solid DMF obtained slowly is washed, then uses the CHCl of about 75mL
3exchange 24h, in triplicate, finally at 80 DEG C of vacuum-drying 5h, obtain white powder, i.e. trimesic acid zinc metallic organic framework, its XRD figure spectrum as shown in Figure 1;
White powder is placed in nitrogen atmosphere, with the ramp to 950 DEG C of 5 DEG C/min, then keeps 2h at this temperature, obtain carbon nano rod, as shown in Figure 2, its BET specific surface area is 6510m to its XRD figure spectrum
2/ g, langmuir specific surface area is 9163m
2/ g, aperture is 4.2nm, and pore volume is 4.44cm
3/ g.
Embodiment 2
Present embodiments provide a kind of preparation method of high specific surface area porous carbon nano rod, it comprises the following steps:
Take 10mmol tetra-water zinc nitrate and 12mmol trimesic acid, be dissolved among 100mL DEF, at room temperature stir 0.5h, then carry out the solvent heat treatment of 1 day at 140 DEG C, the solid DEF obtained slowly is washed, then uses the CHCl of about 55mL
3exchange 24h, in triplicate, last 80 DEG C of vacuum-drying 3h, obtain white powder;
White powder is placed in nitrogen atmosphere, with the ramp to 910 DEG C of 2 DEG C/min, then keeps 4h at this temperature, obtain carbon nano rod.
Embodiment 3
Present embodiments provide a kind of preparation method of high specific surface area porous carbon nano rod, it comprises the following steps:
Take 100mmol zinc chloride and 10mmol trimesic acid, be dissolved among 200mL DMAC, at room temperature stir 0.5h, then carry out the solvent heat treatment of 2 days at 100 DEG C, the solid 100-200mL DMAC obtained slowly is washed, then uses the CHCl of about 100mL
3exchange 12h, in triplicate, last 80 DEG C of vacuum-drying 8h, obtain white powder;
White powder is placed in nitrogen atmosphere, with the ramp to 980 DEG C of 15 DEG C/min, then keeps 2h at this temperature, obtain carbon nano rod.
Embodiment 4
Carry out aniline adsorption test to carbon nano rod prepared by embodiment, concrete steps are as follows:
(1) mensuration of typical curve
Be that the aniline solution of 100mg/L is as storing solution with concentration, calculate the primary liquid accumulated amount required for aniline solution of each different concns respectively according to mass conservation law, the primary liquid required for them is long-pending is respectively 0.05mL, 0.1mL, 0.15mL, 0.2mL, 0.25mL; Then a series of aniline standard is configured, pipette aniline stock solutions 5mL, 10mL, 15mL, 20mL, 25mL respectively in the volumetric flask of 5 100mL, adding distil water is diluted to scale, its concentration is followed successively by 5mg/L, 10mg/L, 15mg/L, 20mg/L, 25mg/L, finally, reference is made with distilled water, 5 standardized solution are placed in 1cm quartz colorimetric utensil respectively, measure absorbance corresponding to sample with ultraviolet/visible spectrophotometer respectively at 230nm wavelength place, obtain absorbance data (as shown in table 1).Take concentration C as X-coordinate, absorbance A is ordinate zou, drawing standard graphic representation, as shown in Figure 6.
(2) mensuration of porous carbon nanometer rod aniline adsorptive capacity
Accurately take the carbon nano rod that many parts of 5mg embodiments 1 obtain, add in different 50mL Erlenmeyer flasks, add the aniline solution that 25mL concentration is respectively 10mg/L, 20mg/L, 30mg/L, 40mg/L, 50mg/L, 60mg/L, 70mg/L respectively, vibrate under room temperature condition after mixing 1h, filter, get 3mL filtrate respectively and be placed in 1cm quartz colorimetric utensil, measure absorbance corresponding to sample with ultraviolet/visible spectrophotometer respectively at 230nm wavelength place, obtain absorbance data (as shown in table 2).According to typical curve, calculate the concentration of aniline in filtrate, (V is the volume of the aniline solution for adsorbing test, is 25mL, C to utilize following formulae discovery adsorptive capacity
0, C be absorption before with adsorption equilibrium time aniline solution concentration, W is the quality of porous carbon nanometer rod).
Target product XRD, SEM, N that embodiment 1 is obtained
2the technology such as absorption/desorption, Raman spectrum and aniline absorption characterize, and result is respectively as shown in Fig. 2, Fig. 3 a-Fig. 3 f, Fig. 4 a, Fig. 4 b, Fig. 5, Fig. 7 a and Fig. 7 b.The above results shows, the carbon nano rod adopting the inventive method to prepare has high specific surface area and flourishing pore structure, and the specific surface area of carbon nano rod prepared by embodiment 1 is 6510m
2/ g, aperture is 4.2nm, and space is flourishing, and pore volume is 4.44cm
3/ g; There is decolorizing carbon and Graphitic carbon structure (G/D=0.8/1) simultaneously.The carbon nano rod that these constitutional featuress determine embodiment 1 has good adsorptive power to aniline in sewage, to the maximal absorptive capacity of aniline up to 196mg/g, than MCM-41 (the maximal absorptive capacity 14mg/g containing template reported, Xinxin Yang, Qingxin Guan, Wei Li.Effect of template in MCM-41on the adsorption of aniline from aqueous solution, Journal of Environmental Management, 2011, 92 (11): 2939) and carbon nanotube (maximal absorptive capacity 17mg/g, Geng Chenghuai, Cheng Rongming, Xu Xuecheng, Chen Yiwei. aniline adsorpting characteristic on the carbon nanotubes, chemical research and application, 2004, 16 (5): 680-684) all high.
The absorbance data of table 1 aniline standardized solution
| Concentration (mg/L) | 5 | 10 | 15 | 20 | 25 |
| Absorbance A bs | 0.4651 | 0.9203 | 1.3723 | 1.8774 | 2.3455 |
The absorbance data of table 2 aniline filtrate and adsorptive capacity
| Starting point concentration (mg/L) | 10 | 20 | 30 | 40 | 50 | 60 | 70 |
| Absorbance A bs | 0.1341 | 0.6593 | 1.1564 | 1.8680 | 2.4741 | 2.6395 | 2.8423 |
| Concentration (mg/L) after absorbing | 1.44 | 7.06 | 12.38 | 20.00 | 26.50 | 28.27 | 30.44 |
In sum, the present invention adopts the simple and easy method of the bar-shaped metallic organic framework of direct carbonization to prepare the porous carbon nanometer rod of high-specific surface area, the method preparation process economy, cost are low, operating process is simple and easy and mild condition, target product specific surface area is large, pore size distribution is narrow, and there is amorphous and Graphitic carbon structure simultaneously, and maturing temperature realization can be changed to the modulation in material specific surface area, aperture and modulation that is amorphous and graphitized carbon ratio.
Claims (10)
1. a preparation method for high specific surface area porous carbon nano rod, it comprises the following steps:
(1) zinc salt and trimesic acid is taken according to the amount of substance ratio of 0.5-5:1, the two is dissolved in organic solvent, at room temperature violent stirring 0.5-3h, then the solvent heat treatment of 1-4 days is carried out at 80-160 DEG C, the solid obtained is filtered, washs, after exchange of solvent and vacuum-drying, obtain white powder, wherein, described organic solvent is 20-200:1 with the amount of substance ratio of zinc salt;
(2) white powder step (1) obtained with more than the ramp to 910 of 2-20 DEG C/min DEG C and constant temperature keeps 1-12h, is then down to room temperature, is obtained described high specific surface area porous carbon nano rod in nitrogen atmosphere.
2. method according to claim 1, wherein, described zinc salt is 0.8:1 with the amount of substance ratio of trimesic acid.
3. method according to claim 1, wherein, described zinc salt is one or more the mixture in two water zinc acetates, anhydrous zinc acetate, zinc chloride, four water zinc sulphates, four water zinc nitrates and zinc nitrate hexahydrate.
4. method according to claim 1, wherein, described organic solvent is one or more the mixture in N, N'-dimethyl formamide, N, N'-diethylformamide and N, N'-N,N-DIMETHYLACETAMIDE.
5. method according to claim 1, wherein, in described step (2), the temperature after intensification is 910-980 DEG C.
6. method according to claim 1, wherein, described step (2) for: the white powder that step (1) is obtained in nitrogen atmosphere with the ramp to 950 of 5 DEG C/min DEG C and constant temperature keeps 2h, be then down to room temperature, obtain described high specific surface area porous carbon nano rod.
7. method according to claim 1, wherein, the temperature of described solvent heat treatment is 140 DEG C, and the time is 2 days.
8. a porous carbon nanometer rod, it is prepared by the method described in any one of claim 1-7.
9. porous carbon nanometer rod according to claim 8, wherein, the BET specific surface area of this porous carbon nanometer rod is 6510m
2/ g, langmuir specific surface area is 9163m
2/ g.
10. porous carbon nanometer rod according to claim 8 or claim 9, wherein, the aperture of this porous carbon nanometer rod is 4.2nm, and pore volume is 4.44cm
3/ g.
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| CN111498830A (en) * | 2020-03-30 | 2020-08-07 | 南京航空航天大学 | Undoped one-dimensional porous carbon material and preparation method thereof |
| CN111498830B (en) * | 2020-03-30 | 2023-09-15 | 南京航空航天大学 | Undoped one-dimensional porous carbon material and preparation method thereof |
| CN114308094A (en) * | 2020-10-10 | 2022-04-12 | 中国石油大学(北京) | Cobalt monoatomic/nitrogen-doped mesoporous carbon fiber material and preparation method and application thereof |
| CN114308094B (en) * | 2020-10-10 | 2023-09-29 | 中国石油大学(北京) | Cobalt monoatomic/nitrogen doped mesoporous carbon fiber material, and preparation method and application thereof |
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