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Frontiers of Chemical Science and Engineering

Front. Chem. Sci. Eng.    2020, Vol. 14 Issue (5) : 857-867     https://doi.org/10.1007/s11705-019-1880-6
RESEARCH ARTICLE
Synthesis of micro/meso porous carbon for ultrahigh hydrogen adsorption using cross-linked polyaspartic acid
Jun Wei1, Jianbo Zhao1,2, Di Cai1(), Wenqiang Ren3, Hui Cao1(), Tianwei Tan1
1. National?Energy?Research and Development?Center?for?Biorefinery, Beijing University of Chemical Technology, Beijing 100029, China
2. Engineering Laboratory of Chemical Resources Utilization in South Xinjiang of Xinjiang Production and Construction Corps, College of Life Sciences, Tarim University, Alar 843300, China
3. Research Center for Eco-Environmental Sciences, Chinese Academy of Science, Beijing 100085, China
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Abstract

In addition to the specific surface area, surface topography and characteristics such as the pore size, pore size distribution, and micro/mesopores ratio are factors that determine the performance of porous carbons (PCs) in the fields of energy, catalysis, and adsorption. Based on the mechanism of weight loss of polyaspartic acid at high temperatures, this study provided a new method for adjusting the surface morphology of PCs by changing the cross-linking ratio of the precursor, where cross-linked polyaspartic acid was used as precursor without additional activating agents. N2 adsorption analysis indicated that the specific surface area of the obtained PCs was as high as 1458 m2·g–1, of which 1200 m2·g–1 was the contribution of the microporous area and the highest pore volume was 1.13 cm3·g–1, of which the micropore volume was 0.636 cm3·g–1. The thermogravimetric analysis results of the precursor, and also the scanning electron microscopy and Brunauer–Emmet–Teller analysis results of the carbonization product confirmed that the prepared PCs presented multilevel pore structure, and the diameters of most pores were 0.78 and 3.97 nm; moreover, the pore size distribution was relatively uniform. This conferred the PCs the ultrahigh hydrogen adsorption capacity of up to 4.52 wt-% at 77 K and 1.13 bar, in addition to their great energy storage and catalytic potential.

Keywords porous carbon      multilevel pores      polyaspartic acid      cross-linking      hydrogen adsorption     
Corresponding Author(s): Di Cai,Hui Cao   
Online First Date: 15 January 2020    Issue Date: 25 May 2020
 Cite this article:   
Jun Wei,Jianbo Zhao,Di Cai, et al. Synthesis of micro/meso porous carbon for ultrahigh hydrogen adsorption using cross-linked polyaspartic acid[J]. Front. Chem. Sci. Eng., 2020, 14(5): 857-867.
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http://journal.hep.com.cn/fcse/EN/10.1007/s11705-019-1880-6
http://journal.hep.com.cn/fcse/EN/Y2020/V14/I5/857
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Jun Wei
Jianbo Zhao
Di Cai
Wenqiang Ren
Hui Cao
Tianwei Tan
Fig.1  Flowchart of CroPASP and PCs production.
Fig.2  Swelling of CroPASP with different cross-linking ratios.
Fig.3  TGA of CroPASP samples with different cross-linking ratios.
Fig.4  SEM images of PCs. Here, C-CroPASP40, C-CroPASP30, C-CroPASP20 and C-CroPASP15 are carbonized CroPASP specimens with different cross-linking ratios (40, 30, 20 and 15, respectively); C-PASP is carbonized CroPASP.
Fig.5  HRTEM images of PCs. Here, C-CroPASP40, C-CroPASP30, C-CroPASP20 and C-CroPASP15 are carbonized CoPASP specimens with different cross-linking ratios (40, 30, 20 and 15, respectively).
Fig.6  (a) XRD patterns; (b) Raman spectra; (c) ratio of intensities of D/G peaks (ID/IG) and full width at half maximum (FWHM) of PCs. Here, C-CroPASP40, C-CroPASP30, C-CroPASP20 and C-CroPASP15 are carbonized CroPASP specimens with different cross-linking ratios (40, 30, 20 and 15, respectively), and C-PASP is carbonized CroPASP.
Fig.7  XPS profiles of PCs. Here, C-CroPASP40, C-CroPASP30, C-CroPASP20 and C-CroPASP15 are carbonized CroPASP specimens with different cross-linking ratios (40, 30, 20 and 15, respectively), and C-PASP is carbonized CroPASP.
Sample SBET b)
/(m2?g?1)
Smicro c)
/(m2?g?1)
VTotal d)
/(cm3?g?1)
Vmicroe)
/(cm3?g?1)
Elemental content/wt-% f) Elemental content/wt-% g)
C O N C O N
C-CroPASP40 662 542 0.468 0.292 90.30 6.32 3.37 88.42 8.12 3.46
C-CroPASP30 1110 899 0.781 0.485 90.52 7.74 1.75 89.11 8.87 2.02
C-CroPASP20 1458 1200 1.130 0.636 89.95 7.58 2.47 86.02 11.29 2.69
C-CroPASP15 1122 955 0.769 0.515 89.69 7.08 3.23 85.38 13.68 2.94
C-PASP 952 787 0.610 0.42 87.23 11.33 1.44 83.77 14.31 1.92
Tab.1  Pore properties and elemental content of PCs a)
Fig.8  (a) N2 adsorption–desorption isotherms, and (b)?(d) pore size distribution curves of PCs. Here C-CroPASP40, C-CroPASP30, C-CroPASP20 and C-CroPASP15 are carbonized CroPASP specimens with different cross-linking ratios (40, 30, 20 and 15, respectively), and C-PASP is carbonized CroPASP.
Fig.9  Hydrogen adsorption curves of PCs at 77.3 K and pressure as high as 1.13 bar. Hydrogen adsorption properties of commercial active carbon samples from Aladdin (China) and Sigma-Aldrich (Germany) were also included for comparison. Here, C-CroPASP40, C-CroPASP30, C-CroPASP20 and C-CroPASP15 are carbonized CroPASP specimens with different cross-linking ratios (40, 30, 20 and 15, respectively), and C-PASP is carbonized CroPASP.
Sample H2 uptake
/wt-%
SBET
/(m2?g?1)
VTotal
/(cm3?g?1)
Adsorption conditions Ref.
C-CroPASP15 4.33 1122 0.769 77 K, 1.13 bar
C-CroPASP20 4.52 1458 1.130
C-CroPASP30 3.73 1110 0.781
C-CroPASP40 2.93 662 0.468
NAC-1.5-600 2.96 1317 0.64 77 K, 1.0 bar [39]
MDC-1 3.25 3174 4.06 77 K, 1.0 bar [13]
CHCPB-K-700 3.25 3101 1.84 77.3 K, 1.13 bar [2]
RFC_C240 3.16 3540 1.99 77 K, 1.0 bar [40]
RFC_C380 3.26 4079 2.56
PFC_C120 3.05 3283 1.48
CAC0 2.42 3148 1.5 77 K, 1.0 bar [41]
CAC1 2.85 2988 1.36
CAC7 2.66 3530 1.95
Ch700/700/3 2.9 3066 1.38 77 K, 1.0 bar [42]
Ch700/800/3 2.95 2481 0.95
CAC1 2.85 3009 1.44 77 K, 1.0 bar [43]
CAC4 3.21 3708 2
Tab.2  H2 adsorption capacity of C-CroPASPs compared with data reported in the literaturea)
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