WO2020157379A1 - Procédé de production de charbon actif - Google Patents

Procédé de production de charbon actif Download PDF

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Publication number
WO2020157379A1
WO2020157379A1 PCT/FI2020/050040 FI2020050040W WO2020157379A1 WO 2020157379 A1 WO2020157379 A1 WO 2020157379A1 FI 2020050040 W FI2020050040 W FI 2020050040W WO 2020157379 A1 WO2020157379 A1 WO 2020157379A1
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alkali metal
hydroxide
weight
lignin
chloride
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PCT/FI2020/050040
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English (en)
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Nikolai PONOMAREV
Mika SILLANPÄÄ
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Lappeenrannan-Lahden Teknillinen Yliopisto Lut
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Priority to EP20704064.3A priority Critical patent/EP3917880A1/fr
Publication of WO2020157379A1 publication Critical patent/WO2020157379A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • C01B32/342—Preparation characterised by non-gaseous activating agents
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/312—Preparation

Definitions

  • the present invention relates to methods for producing activated carbon, in particular to methods comprising pyrolyzing carbonaceous materials with a mixture of alkali metal hydroxide and alkali metal chloride wherein the alkali metal is selected from sodium and potassium.
  • Activated carbon is carbon produced from carbonaceous source materials such as bamboo, coconut husk, willow peat, wood, coir, lignite, coal, petroleum pitch, cellulose and lignin.
  • Activated carbon is typically produced by physical activation or by chemical activation.
  • Drawbacks of physical activation are preliminary carbonization and a high temperature of activation.
  • preliminary pyrolysis usually is not needed.
  • hazardous properties of some chemicals and high chemical consumption make this method challenging.
  • CN106185921 A disclosed a method for preparing porous carbon material using NaCI as a template and kraft lignin as a starting material.
  • the lignin was mixed with NaCI with a lignin to NaCI ratio of 1 :10 by weight.
  • the mixture was then dried at 60- 100 °C and preliminary carbonized at temperature 400-600 °C.
  • the obtained composite was washed using distilled water and dried.
  • the material was mixed with KOH with a mass ratio of 1 :4. Then, the mixture was pyrolyzed at 850 °C and after cooling the obtained carbide was washed using 1 -12 mol/L of HCI.
  • an inorganic part comprising alkali metal carbonate (M 2 CO3) and alkali metal chloride (MCI), and
  • step c) treating the inorganic part of step c) with calcium hydroxide to produce an admixture comprising calcium carbonate, alkali metal hydroxide (MOH), and alkali metal chloride (MCI),
  • step f recycling the admixture comprising the alkali metal hydroxide (MOH) and the alkali metal chloride (MCI) to step a).
  • MOH alkali metal hydroxide
  • MCI alkali metal chloride
  • MOH alkali metal hydroxide
  • MCI alkali metal chloride
  • figure 1 shows an exemplary non-limiting embodiment for producing activated carbon, and recycling sodium hydroxide and sodium chloride using the method of the present invention
  • figure 2 shows an exemplary non-limiting embodiment for producing activated carbon, and recycling potassium hydroxide and potassium chloride using the method of the present invention
  • figure 3A shows N2 adsorption-desorption isotherms of activated carbon prepared according to the method of the present invention and according to prior art
  • figure 3B shows NLDFT pore size distribution and SEM images of activated carbons prepared using the method of the present invention and according to prior art
  • figure 4A shows XRD spectra of samples prepared using NaCI, NaOH or
  • figure 4B shows SEM micrographs of samples prepared using NaCI, NaOH or NaOH/NaCI before leaching
  • figure 5A shows FTIR spectra of carbons prepared using NaCI, NaOH and
  • figure 5B shows TGA/DTG curves of carbons prepared using NaCI, NaOH and NaOH/NaCI
  • figure 6A shows N2 adsorption-desorption isotherms of prepared carbons using various NaOH/NaCI ratio
  • figure 6B shows BET and yields prepared carbons using various NaOH/NaCI ratio
  • figure 7A shows the FTIR spectra of raw lignin (a), dried mixtures of lignin-NaCI and lignin-NaOH; guaiacyl propane unit (b); reactions of destruction (c); condensation (d) of lignin in alkaline media
  • figure 7B shows SEM images of lignin-NaOH (e) and SEM images of lignin-NaCI (f) mixtures.
  • the present invention concerns a method for producing activated carbon using a mixture of NaOH and NaCI as the activation agent.
  • the method comprises the following steps:
  • an inorganic part comprising sodium carbonate and sodium chloride, and c) separating the activated carbon and the inorganic part.
  • lignin is used as an exemplary non limiting carbonaceous material.
  • lignin is admixed 1 with a mixture of aqueous sodium hydroxide and sodium chloride to form an admixture as a slurry.
  • the slurry is extruded 2 and transferred to a pyrolysis furnace.
  • the method comprises one or more of: swelling, extruding and drying the admixture of step a) prior to step b).
  • Pyrolysis 3 is performed preferably under inert or at least low O2 content atmosphere.
  • the pyrolysis produces activated carbon together with sodium carbonate and carbon dioxide.
  • the inorganic part comprising the sodium carbonate produced, and the remaining sodium chloride is removed by leaching 4, and the isolated activated carbon is dried 5.
  • the method of the present invention is also suitable for recycling the sodium hydroxide and the sodium chloride used as the activating agent in the process.
  • the recycling comprises
  • step c) treating the inorganic part of step c) with calcium hydroxide to produce an admixture comprising calcium carbonate, sodium hydroxide, and sodium chloride,
  • the recycling comprises treating 6 the inorganic part comprising sodium carbonate and sodium chloride with calcium hydroxide to form an admixture comprising precipitated calcium carbonate.
  • the precipitate is then separated 7, and the remaining mixture of sodium hydroxide and sodium chloride is recycled to the admixing 1.
  • the activating agent comprises sodium hydroxide and sodium chloride.
  • the NaOH/NaCI ratio is typically from 1/9 by weight to 3/2 by weight, preferably from 1/4 by weight to 1/1 by weight, most preferably 2/3 by weight.
  • the NaOH/NaCI ratio is 2/3 by weight and the ratio (mixture of NaOH and NaCI)/(carbonaceous material) is 2/3 by weight.
  • a particular carbonaceous material is lignin, preferably hydrolytic lignin.
  • the carbonaceous material such as lignin is mixed with a solution of NaOH and NaCI in deionised water.
  • the obtained admixture is preferably allowed to swell e.g. at room temperature.
  • An exemplary swelling time is 1 h.
  • After swelling the admixture is preferably extruded and also dried.
  • An exemplary drying temperature is 130 °C, and an exemplary drying time is 16 h.
  • the dried material is grinded to produce granules.
  • a typical size of granules is 1 -2 mm.
  • the method comprises pyrolysis of the admixture comprising the carbonaceous material, sodium hydroxide and sodium chloride, preferably pyrolysis of a granulized admixture obtained as described above.
  • the pyrolysis is performed in a tubular furnace.
  • the pyrolysis is performed preferably in inert atmosphere at temperature from 600 °C to 1000 °C, preferably from 700 °C to 900 °C, more preferably from 850 °C to 900 °C.
  • Typical time for pyrolysis is 30-120 min.
  • a particular temperature is 868 °C
  • a particular time for pyrolysis is 47 min when lignin is the carbonaceous material.
  • the inorganic part is leached from the activated carbon preferably with water or with aqueous acid, such as aqueous mineral acid.
  • aqueous mineral acid is hydrochloric acid, such as 0.1 M HCI.
  • the activated carbon is isolated from the solution using a Biichner funnel and washing several times with water until neutral pH.
  • the activated carbon isolated is preferably dried. An exemplary drying is at 130 °C for 16 h.
  • the present invention concerns a method for producing activated carbon using a mixture of KOH and KCI as the activation agent.
  • the method comprises the following steps:
  • lignin is used as an exemplary non limiting carbonaceous material.
  • lignin is admixed 1 with a mixture of aqueous potassium hydroxide and potassium chloride to form an admixture as a slurry.
  • the slurry is extruded 2 and transferred to a pyrolysis furnace.
  • the method comprises one or more of: swelling, extruding and drying the admixture of step a) prior to step b).
  • Pyrolysis 3 is performed preferably under inert or at least low O2 content atmosphere.
  • the pyrolysis produces activated carbon together with potassium carbonate and carbon dioxide.
  • the inorganic part comprising the potassium carbonate produced, and the remaining potassium chloride is removed by leaching 4, and the isolated activated carbon is dried 5.
  • the method is also suitable for recycling the potassium hydroxide and the potassium chloride used as the activating agent in the process. According to this embodiment, the recycling comprises
  • step c) treating the inorganic part of step c) with calcium hydroxide to produce an admixture comprising calcium carbonate, potassium hydroxide, and potassium chloride,
  • the recycling comprises treating 6 the inorganic part comprising potassium carbonate and potassium chloride with calcium hydroxide to form an admixture comprising precipitated calcium carbonate.
  • the precipitate is then separated 7, and the remaining mixture of potassium hydroxide and potassium chloride is recycled to the admixing 1.
  • the present invention concerns a method for producing activated carbon using a mixture of KOH and NaCI as the activation agent.
  • the method comprises the following steps:
  • an inorganic part comprising potassium carbonate and sodium chloride, and c) separating the activated carbon and the inorganic part.
  • the method is also suitable for recycling the potassium hydroxide and the sodium chloride used as the activating agent in the process.
  • the recycling comprises
  • step c) treating the inorganic part of step c) with calcium hydroxide to produce an admixture comprising calcium carbonate, potassium hydroxide, and sodium chloride,
  • the present invention concerns a method for producing activated carbon using a mixture of NaOH and KCI as the activation agent.
  • the method comprises the following steps:
  • an inorganic part comprising sodium carbonate and potassium chloride, and c) separating the activated carbon and the inorganic part.
  • the method is also suitable for recycling the sodium hydroxide and the potassium chloride used as the activating agent in the process.
  • the recycling comprises
  • step c) treating the inorganic part of step c) with calcium hydroxide to produce an admixture comprising calcium carbonate, sodium hydroxide, and potassium chloride,
  • the calcium carbonate formed is isolated and decomposed thermally 8 to produce calcium oxide and carbon dioxide.
  • Treatment of calcium oxide with water 9 produces calcium hydroxide, which is then recycled to the treating step 6.
  • the method thus further comprises
  • chemical reactions related recycling calcium hydroxide comprises the following chemical reactions:
  • Exemplary carbonaceous materials suitable for the method are bamboo, coconut husk, willow peat, wood, coir, lignite, coal, petroleum pitch, cellulose and lignin.
  • a particular carbonaceous material is lignin such as hydrolytic lignin and kraft lignin.
  • An exemplary kraft lignin is BioPiva 100 of UPM.
  • Still another exemplary kraft lignin is precipitated kraft lignin from black liquor.
  • Another particular carbonaceous material is cellulose, preferably microcrystalline cellulose.
  • An exemplary microcrystalline cellulose is AaltoCellTM. Preparation of microcrystalline cellulose has been disclosed in EP 2576629.
  • Still another particular carbonaceous material is sewage sludge of pulp and/or paper.
  • the carbonaceous material is may be powdered, ground of milled prior to use in the method. Also, mixtures of two or more carbonaceous materials can be used.
  • the activating agent comprises alkali metal hydroxide (MOH) and alkali metal chloride (MCI).
  • MOH/MCI ratio is typically from 1/9 by weight to 3/2 by weight, preferably from 1/4 by weight to 1/1 by weight, most preferably 2/3 by weight.
  • biomass of the carbonaceous material is preferably from 1/1 by weight to 0.5/1 by weight, more preferably 0.6/1 by weight.
  • the alkali metal is sodium and NaOH/NaCI ratio is 2/3 by weight and the ratio (mixture of NaOH and NaCI)/(carbonaceous material) is 2/3 by weight.
  • a particular carbonaceous material is lignin, preferably hydrolytic lignin.
  • the alkali metal is potassium and KOH/KCI ratio is 2/3 by weight and the ratio (mixture of KOH and KCI)/(carbonaceous material) is 2/3 by weight.
  • a particular carbonaceous material is lignin, preferably hydrolytic lignin.
  • the alkali metal hydroxide is potassium hydroxide and the alkali metal chloride is sodium chloride KOH/NaCI ratio is 2/3 by weight and the ratio (mixture of KOH and NaCI)/(carbonaceous material) is 2/3 by weight.
  • a particular carbonaceous material is lignin, preferably hydrolytic lignin.
  • the alkali metal hydroxide is sodium hydroxide and the alkali metal chloride is potassium chloride NaOH/KCI ratio is 2/3 by weight and the ratio (mixture of NaOH and KCI)/(carbonaceous material) is 2/3 by weight.
  • a particular carbonaceous material is lignin, preferably hydrolytic lignin.
  • the carbonaceous material such as lignin is mixed with a solution of alkali metal hydroxide (MOH) and alkali metal chloride (MCI) wherein the alkali metal is sodium or potassium in deionised water.
  • MOH alkali metal hydroxide
  • MCI alkali metal chloride
  • the obtained admixture is preferably allowed to swell e.g. at room temperature.
  • An exemplary swelling time is 1 h.
  • After swelling the admixture is preferably extruded and also dried.
  • An exemplary drying temperature is 130 °C, and an exemplary drying time is 16 h.
  • the raw materials for the preparation of activated carbon were hydrolytic lignin, microcrystalline cellulose (MCC)-AaltoCellTM and precipitated kraft lignin from black liquor.
  • the industrial acid hydrolytic lignin from coniferous wood was used (200 pm with 8.5 % moisture content).
  • Microcrystalline cellulose was prepared according to EP 2576629.
  • the kraft lignin was obtained from the black liquor by the following procedure. 500 ml_ of black liquor was mixed with 250 ml_ of 10% w/w HCI and vigorously stirred. The obtained precipitate was isolated from the solution using a Buchner funnel and washed several times with water. The obtained kraft lignin was dried at 130 °C for 16 h.
  • the functional groups of the material were studied using Fourier transform infrared spectroscopy (FTIR) on a Bruker Vertex 70.
  • FTIR Fourier transform infrared spectroscopy
  • the crystalline structure of the material was evaluated using X-ray powder diffraction (XRD) on a high-resolution PANalytical diffractometer. The scans were recorded employing Co Ka radiation at a voltage of 40 kV from 10 ° to 100 ° 20 angles.
  • the crystalline size was calculated using XRD data applying Williamson-Flall (W-FI) method.
  • W-FI Williamson-Flall
  • the structure of the material was studied employing scanning electron microscopy (SEM) on a Hitachi S-4800. Thermogravimetric analyses (TGA) was performed on NETZSCFI TG thermal analyser at a heating rate 10 °C/min from 23 °C to 1000 °C. The yield was calculated using values of raw material and final product masses, respectively.
  • the process variables such as target temperature A (°C), residence time B (min) and lignin to NaOH/NaCI ratio C (g/g) were considered as factors. Three levels of factors, including zero level, were ascribed for each parameter. The minimum, zero and maximum levels are temperature 600, 700 and 800 °C; time 30, 60 and 90 min; lignin to NaOH/NaCI ratio 0.5, 1 .0 and 1 .5 g/g.
  • the BET surface area Y1 (m 2 /g) and yield Y2 (%) were selected as responses for process optimization. To evaluate the reproducibility and validity of experimental findings three repetitions were performed on a zero level. The design of experiments is demonstrated in Table 1 . Experimental data were analysed by RSM using Design Expert 1 1 software and ANOVA analysis was performed to evaluate the adequacy of the models.
  • a. g/g mass ratio (NaOH/NaCI)/lignin
  • the regression coefficients of BET model are increased with increasing of factor values.
  • the yield is decreasing while factors are increasing that can be concluded from the negative values of regression coefficients.
  • the factor of lignin to NaOH/NaCI ratio (C) is the most essential factor since the regression coefficients values are the highest.
  • the influence of temperature (A) on responses is also significant, while time (B) demonstrates the weakest effect.
  • the maximum cannot be achieved for both responses because with increasing of one response another is decreasing. More specifically, the maximum BET surface area appears at 800 °C and 1.5 g/g, while the maximum yield is observed at the minimum temperature 600 °C and 0.5 g/g of ratio.
  • increasing of factors has a positive effect on BET surface whereas the influence on yield is negative.
  • the increasing of ratio, temperature and time lead to the enlarged surface area since the formation of porous texture is occurred in the same manner. Meanwhile, the yield is decreased due to the transformation of micropores to meso- and macropores with the further void formation.
  • the optimal values of factors can be predicted.
  • desirability function has been employed.
  • Table 4 shows predicted and obtained responses at optimal factors.
  • Activated carbons prepared at optimal factors in three repetitions to evaluate reproducibility and difference of predicted and obtained values are negligible indicating additionally validity of the model.
  • the BET surface area of the obtained activated carbons is relatively the same while lignin to activation agent ratio is remarkably lower. Moreover, the NaOH consumption is five times lower compared to the previously reported methods. The discrepancies of yield can be explained by reduced consumption of N2 flow using in experiments.
  • Figure 3A shows adsorption isotherms of carbons prepared after use of NaOH, NaCI and NaOH/NaCI.
  • Adsorption isotherms are described according to the lUPAC report (Tanss, M. et al. (2015) Physisorption of gases, with special reference to the evaluation of surface area and pore size distribution (lUPAC Technical Report), Pure and Applied Chemistry, 87(9-10), pp. 1051-1069. doi: 10.1515/pac-2014- 1 1 17).
  • Isotherm curvature of carbon prepared from the mixture of lignin-NaCI exhibits to composite type I, II assigned to micro- macroporous materials.
  • Activated carbons produced of hydrolytic lignin using NaOH or KOH activation are associated with microporous materials.
  • the isotherm of carbon prepared using a mixture of NaOH and NaCI is also coincided with combined isotherm type I, II, since enhanced N2 uptake is observed at pressures below 0.1 p/p° associated with micropore filling, while ascended curvature of the plateau is inherent for macropores.
  • the adsorption hysteresis of carbons prepared using NaOH is attributed to H4 type and accompanied with isotherms I or composite type I, II indicating micropore filling.
  • the hysteresis loop of carbon prepared using only NaCI is associated with isotherm type II of macropores materials. Adsorption capacities of carbons prepared using only NaCI or NaOH are similar whereas N2 uptake of carbons prepared using NaOH/NaCI mixture is more pronounced.
  • the texture properties of carbons prepared using various mixtures are summarized in Table 6.
  • the samples prepared using only NaOH or NaCI has a relatively similar total volume of pores and BET surface area, while carbon prepared using a mixture of NaOH/NaCI demonstrated significantly higher values.
  • the BET surface area and micropore volume of carbon prepared using NaOH/NaCI are larger compared to NaOH or NaCI activated carbons.
  • the total pore volume of carbon prepared using NaCI is caused by micro and macropore formation, while in case of NaOH micro porosity mainly deals with its origin.
  • Table 6 Texture properties and yield of carbons prepared using a various amount of NaOH and/or NaCI.
  • the product of assumed chemical reaction (1 ) is sodium carbonate that can be detected by analytical methods.
  • the characteristic peaks of Na 2 C0 3 are found in XRD spectra of samples prepared using NaOH (Fig. 4A).
  • the corresponding peaks of Na 2 C0 3 are indexed to reference number ICSD98-008-0985 of standard XRD pattern of sodium carbonate.
  • the SEM micrograph of the sample prepared using NaOH before leaching shows different structure compare to NaCI contained samples.
  • the formed crystals shapes are inherent for sodium carbonate.
  • the peaks at 1423, 1426 cm -1 and 832, 876 cm -1 attributed to carbonates are found on FTIR spectra (Fig.
  • Adsorption isotherms of carbons prepared using different NaOFI to NaCI ratio are presented in Figure 6A. Starting from 1/9 ratio to 3/7 ratio adsorption isotherms exhibit Type I of microporous materials. With increasing of NaOFI presence from 4/6 to 6/4 isotherms demonstrated ascended curvature and pronounced hysteresis H4 that more intrinsic for composite isotherm I, II indicating the development of the porous structure. In particular, the slope of isotherm pointing to macropores formation, while hysteresis H4 type is attributed to micropores. The micropore volume and total volume is significantly increased starting from 4/6 ratio lead to enlarged BET surface area (Table 8). Carbons prepared using NaOFI to NaCI ratio from 1/9 to 3/7 are assigned to microporous materials, while samples prepared using 4/6 to 6/4 ratio are also significantly meso- macroporous.
  • a Micropore volume is calculated by DR equation.
  • b Mesopore volume is calculated as a difference between Vtotai and Vmicro.
  • the strong peaks located at 3341 cm -1 and 2934 cm -1 are assigned to stretching vibrations of OH- and C-H in -CH3 or -CH2-, respectively.
  • the significant changes are observed for the following peaks: 1706 cm -1 - aromatic C-H n stretching; 1270 cm -1 - C-O-C stretching of aryl- alkyl ether bond; 1210 cm 1 -C-0 stretching of guaiacyl ring; 1154 cm -1 and 1110 cm -1 - stretching vibrations in guaiacyl propane unit.
  • the mentioned changes are assigned to linkages, which take part in the reaction of destruction (Fig. 7A, c) and condensation (Fig. 7A, d).
  • the peaks at 1420 cm -1 , 884 cm -1 and 776 cm -1 could be indexed to formed carbonate by captured CO2 from the air.
  • FTIR peaks of lignin are not observed for pyrolyzed carbons (Fig.4A) whatever NaOFI or NaCI was used indicating essential degradation of lignin and formation of carbon like structure.
  • Table 10 summarizes the properties of activated carbons prepared by the method of the present invention, namely hydrolytic lignin, kraft lignin and microcrystalline cellulose and optimized process parameters.
  • the method of the present invention has the following advantages
  • the carbonaceous material is directly mixed with MOFI/MCI, wherein M is Na or K, and pyrolyzed in one single step. This led to reduction of operation steps, energy and water consumption.
  • the optimized carbonaceous material such as lignin to NaOFI/NaCI ratio is 1 :0.6 (1 :0.24 of only NaOFI) w/w.
  • the material is micro- macroporous. There is the accessibility of micropores through the macropores.
  • the material can be easily granulated/extruded without additional binder because of chemical interaction between lignin and NaOH.

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Abstract

La présente invention concerne des procédés de production de charbon actif, en particulier des procédés consistant à traiter des matières carbonées, en particulier de la lignine avec le mélange constitué d'un hydroxyde de métal alcalin et d'un chlorure de métal alcalin, le métal alcalin étant choisi parmi le sodium et le potassium. L'invention concerne également un procédé de recyclage de l'hydroxyde de métal alcalin et du chlorure de métal alcalin dans le procédé.
PCT/FI2020/050040 2019-01-28 2020-01-27 Procédé de production de charbon actif WO2020157379A1 (fr)

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EP20704064.3A EP3917880A1 (fr) 2019-01-28 2020-01-27 Procédé de production de charbon actif

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FI20195047A FI128625B (en) 2019-01-28 2019-01-28 METHOD FOR THE PRODUCTION OF ACTIVATED CARBON
FI20195047 2019-01-28

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CN112279245A (zh) * 2020-10-29 2021-01-29 安徽工业大学 一种制备超级电容器用分级多孔碳的方法
CN112774632A (zh) * 2021-01-12 2021-05-11 河南省高新技术实业有限公司 一种炭基吸附材料的制备方法和应用
CN113289581A (zh) * 2021-06-16 2021-08-24 华南理工大学 一种用于快速净化染料废水的木质素基分级多孔碳及其制备方法
WO2024037175A1 (fr) * 2022-08-15 2024-02-22 东南大学 Matériau composite de carbone poreux à base de biomasse, sa préparation et son utilisation dans l'adsorption de co2
CN115231570A (zh) * 2022-09-01 2022-10-25 江苏海洋大学 一种吸附剂活性炭颗粒及其制备方法
CN115231570B (zh) * 2022-09-01 2023-08-15 江苏海洋大学 一种吸附剂活性炭颗粒及其制备方法
CN116239100A (zh) * 2023-03-27 2023-06-09 四川大学 一种基于松香的氮掺杂多孔硬碳材料及其制备方法和应用
CN116239100B (zh) * 2023-03-27 2023-10-27 四川大学 一种基于松香的氮掺杂多孔硬碳材料及其制备方法和应用

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