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Integrated Process of Coal Pyrolysis with Steam Reforming of Methane for Improving Tar Yield Chan Dong, Lijun Jin, Yang Li, Yang Zhou, Liang Zou, and Haoquan Hu Energy Fuels, Just Accepted Manuscript • DOI: 10.1021/ef501796a • Publication Date (Web): 07 Nov 2014 Downloaded from http://pubs.acs.org on November 10, 2014
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Integrated Process of Coal Pyrolysis with Steam Reforming of Methane for Improving Tar Yield Chan Dong, Lijun Jin, Yang Li, Yang Zhou, Liang Zou, Haoquan Hu* State Key Laboratory of Fine Chemicals, Institute of Coal Chemical Engineering, School of Chemical Engineering, Dalian University of Technology, Dalian 116024, China *Corresponding author:
[email protected]. Tel: 86-411-84986157
ABSTRACT: A novel process of integrated coal pyrolysis with steam reforming of methane (CP-SRM) was put forward for improving tar yield. Two Chinese lignites were used to confirm the validity of the integrated process. At the investigated temperature range of 550 to 750 oC, CP-SRM achieves the highest tar yield, total gas yield and C2+C3 gas volume than coal pyrolysis in N2 (CP-N2) and H2 (CP-H2). Compared with steam reforming of methane, CP-SRM has lower CO and H2 yields. At 650 oC, tar yield from CP-SRM is 1.5 to 1.6 times and 1.3 to 1.4 times as those from CP-N2 and CP-H2, respectively. Meanwhile, the tar from CP-SRM at 650 oC has the highest content of phenol oil, naphthalene oil and wash oil among three atmospheres, and the sum of BTX, PCX and tricresol contents from XL-SRM is 37.5%, which is 1.18 and 1.44 times as that from XL-N2 and CP-H2, respectively. Keyword: coal pyrolysis, steam reforming of methane, tar, lignite
1. INTRODUCTION Lignite and sub-bituminous coal are abundant, accounting for 53% of all coal resources in the world and 46% in China [1]. But nearly 90% low-rank coal was consumed by direct combustion for power generation in China, which is considered as an inefficient utilization of 1
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coal energy and environmental unfriendly way. Lignite pyrolysis, considering its upgrading solid product (char) and high valued liquid product and chemicals (tar), would be a potentially effective method for lignite utilization. As to the pyrolysis mechanism, it is usually thought that coal pyrolysis proceeds in two steps: primary devolatilization reactions by the formation of abundant radicals and secondary gas phase reactions to form gas, liquid and solid products due to the combination of free radicals. Therefore, the key to improve tar yield of coal pyrolysis is to offer abundant small radicals to stabilize coal radicals. Many methods can be used to improve tar yield under relatively mild conditions, such as pyrolysis in reactive gas atmospheres, coal pretreatment and catalytic pyrolysis of coal [2-4]. In our previous studies, several integrated processes of coal pyrolysis with methane conversion, including partial oxidation of methane [5], methane aromatization over Mo/HZSM-5 [6], CO2 reforming of methane [7] has been explored. These integrated processes showed the radicals as ·CHx and ·H formed from methane activation participated in coal pyrolysis [8], resulting in increase of liquid yield. The key to acquire high tar yield in coal pyrolysis is to provide enough radicals to match the speed and amount of radicals formed by coal pyrolysis. Steam reforming of methane (SRM), as an important process for methane activation and conversion, is the main hydrogen production method in industry. During the SRM process, methane could be activated at low temperature as 500 oC [9, 12] and some free radicals such as ·CHx (x H2, while the alkane content is in the order of XL-SRM > H2 > N2. The change of alkene to alkane is related with the results of the activated hydrogen produced during steam reforming of methane and H2 pyrolysis. 4. CONCLUSIONS Integrated process of coal pyrolysis with steam reforming of methane (CP-SRM) has positive effects on coal conversion with high tar yield compared with coal pyrolysis under N2 and H2 at the temperature range from 550 oC to 750 oC. The increase of tar yield is 13
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related with coal samples. At 650 oC, the highest tar yield in XL-SRM is 13.9 wt.%, which is 1.57 and 1.44 times as that in XL-N2 and XL-H2, respectively. While in HL pyrolysis, the integrated process achieves tar yield of 17.8 wt.%, which is 1.46 and 1.31 times higher than that under N2 and H2, respectively. Compared with SRM, the integrated process restrains the formation of H2 and CO, but promotes the release of CH4 and C2+C3 compared with CP-N2 at the investigated temperature range. Results of the analysis of tar from XL pyrolysis at 650 oC under different atmosphere show that XL-SRM process can improve tar quality. Higher phenol oil, naphthalene oil and wash oil and less asphaltene contents than those from XL-N2 were observed. GC and GC-MS analyses show that the XL-SRM process can improve BTX content in tars, which is 1.8 times and 1.2 times as those from XL-N2 and XL-H2 respectively; while the total content of PCX and tricresol in tar from XL-SRM accounts for 34.5 wt.%, which is 1.14 and 1.46 times as those from XL-N2 and XL-H2 respectively. The content of naphthalene homologs in tar from XL-SRM is similar to that from XL-H2, but is higher than that from XL-N2. ACKNOWLEDGEMENTS This work was performed with support of the National Natural Science Foundation of China (21176042), the National Basic Research Program of China (973 Program), the Ministry of Science and Technology, China (No. 2011CB201301), and International Science & Technology Cooperation Program, the Ministry of Science and Technology (2013DFG60060). REFERENCES [1] BP Statistical Review of World Energy. June 2012. 14
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[2] Miura, K., Mild conversion of coal for producing valuable chemicals. Fuel Process Technol 2000, 62, 119-135. [3]Solomon, P.R., Fletcher, T.H., Pugmire, R.J., Process in coal pyrolysis. Fuel 1993;72, 587–597. [4] Tromp, P.J.J., Coal pyrolysis. Ph.D. thesis, University Amsterdam; 1987. [5] Liu, Q. R.; Hu, H. Q.; Zhu, S.W., Integrated process of coal pyrolysis with catalytic partial oxidation of methane. International Conference on Coal Science and Technology, Okinawa, Japan, 2005. [6] Jin, L. J.; Zhou, X.; He X. F.; Hu, H. Q., Integrated coal pyrolysis with methane aromatization over Mo/HZSM-5 for improving tar yield. Fuel 2013, 114, 187-190. [7] Liu, J. H.; Hu, H. Q.; Jin, L. J.; Wang, P. F.; Zhu, S. W., Integrated coal pyrolysis with CO2 reforming of methane over Ni/MgO catalyst for improving tar yield. Fuel Processing Technol 2010, 91, 419-423. [8] Wang, P. F.; Jin, L. J.; Liu, J. H.; Zhu, Sh. W.; Hu, H. Q., Isotope analysis for understanding the tar formation in the integrated process of coal pyrolysis with CO2 reforming of methane. Energy Fuels 2010, 24, 4402–4407. [9] Ross, J. R. H.; Steel, M. C. F., Mechanism of the steam reforming of methane over a coprecipitated nickel-alumina catalyst. J. Chem. Soc., Faraday Trans. 1 1973, 69, 10-21. [10] Ross, J. R. H.; Steel, M. C. F.; Zeini-Isfahani, A., Evidence for the participation of surface nickel aluminate sites in the steam reforming of methane over nickel/alumina catalysts. Journal of Catalysis 1978, 52, 280-290. [11] Hou, K. H.; Hughes, R., The kinetics of methane steam reforming over a Ni/α-Al2O3 15
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catalyst. Chemical Engineering Journal 2001, 82, 311-328. [12] Matsumura, Y.; Nakamori, T., Steam reforming of methane over nickel catalysts at low reaction temperature. Applied Catalysis A: General 2004, 258, 107-114. [13] Xu, W. C.; Tomita, A., The effects of temperature and residence time on the secondary reactions of volatiles from coal pyrolysis. Fuel Processing Technol 1989, 21, 25-37. [14] Cypres, R.; Furfari, S., Low-temperature hydropyrolysis of coal under pressure of H2-CH4 mixtures. Fuel 1982, 61, 721-724. [15] Qin, Z. F.; Maier, W. F., Coal pyrolysis in the presence of methane. Energy Fuels 1994, 8, 1033-1038. [16] Fuentes-Cano, D.; Gómez-Barea, A.; Nilsson, S.; Ollero, P., The influence of temperature and steam on the yields of tar and light hydrocarbon compounds during devolatilization of dried sewage sludge in a fluidized bed. Fuel 2013, 108, 341-350. [17] He X.F., Jin, L.J., Wang, D., Zhao, Y.P., Zhu, S.W., Hu H.Q., Integrated Process of Coal Pyrolysis with CO2 Reforming of Methane by Dielectric Barrier Discharge Plasma. Energy Fuels 2011, 25, 4036–4042.
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Table 1. Proximate and ultimate analyses of coal samples Coal samples
Proximate analysis (wt.%) C
H
N
S
O*
41.24
73.70
4.40
1.06
1.10
19.74
45.93
73.51
4.95
1.37
0.29
19.88
Mad
Ad
Vdaf
XL
7.21
16.26
HL
3.87
11.44
*
Ultimate analysis (wt.%, daf)
By difference
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Table 2. XRF analysis of the catalyst (Ni/Al2O3) Component
Al2O3
NiO
CaO
La2O3
SiO2
Na2O
Fe2O3
Content (wt.%)
60.1
27.4
6.5
4.5
0.7
0.5
0.3
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Table 3. Methane conversion in SRM catalyzed by chara from the integrated process
a
T (oC)
550
600
650
700
750
XCH4 (%)
0
0
0
1
4
char sample is obtained from the integrated process at 550-750 oC
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Table 4. Compounds (No. 1 to 34 marked in Figure 10) detected in tar from XL pyrolysis No.
Compound
No.
Compound
No.
Compound
1
1-Undecene
13
n-heptadecene
25
1-Tricosene
2
Undecane
14
n-heptadecane
26
Tricosane
3
1-Dodecene
15
1-Octadecylen
27
1-Tetracosene
4
Dodecane
16
Octadecane
28
Tetracosane
5
1-Tridecene
17
1-Nonadecene
29
1-Pentacosene
6
Tridecane
18
Nonadecane
30
Pentacosane
7
1-Tetradecene
19
1-Eicosene
31
1-Hexacosene
8
Tetradecane
20
Eicosane
32
Hexacosane
9
1-Pentadecene
21
1-Heneicosene
33
1-Heptacosane
10
Pentadecane
22
Heneicosane
34
Heptacosane
11
1-hexadecene
23
1-Docosene
12
Hexadecane
24
Docosane
20
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Figure captions
Figure 1. Schematic diagram of apparatus for coal pyrolysis Figure 2. Tar, char and gas yields of XL (a,b,c) and HL (d,e,f) pyrolysis at 550-750 oC Figure 3. Conversion of methane in CP-SRM and SRM at 550-750 oC Figure 4. Comparison of gas volume from CP-SRM with SRM at 550-750 oC Figure 5. Gas analysis of XL-SRM compared with SRM and XL-N2 at 550-750 oC Figure 6. Gas analysis of HL-SRM compared with SRM and HL-N2 at 550-750 oC Figure 7. C2+C3 volume from XL (a) and HL (b) pyrolysis under different atmosphere at 550-750 oC Figure 8. Fraction contents of tar samples from XL pyrolysis under different atmospheres Figure 9. Gas chromatogram of tar from XL pyrolysis under different atmospheres Figure 10. Compositions of tar from XL-SRM analyzed by GC and GC-MS Figure 11. Distribution of components in tar from XL pyrolysis under different atmospheres Figure 12. Distribution of benzenes (a), phenols (b), naphthaltenes (c) and aliphatics (d) in tar from XL pyrolysis under different atmospheres
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Figure 1. Schematic diagram of apparatus for coal pyrolysis
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16
XL-SRM XL-H2
14
18 (d)
Ytar (wt. %, daf)
Ytar (wt. %, daf)
(a)
XL-N2
12 10 8 6
550
600
650
o
700
16
HL-SRM HL-H2
14
HL-N2
12 10 550
750
75
75
Ychar (wt. %, daf)
Ychar (wt. %, daf)
70
XL-N2
65 60 55 50
550
600
650
o
650
700
750
Temperature ( C) XL-SRM XL-H2
(b)
600
o
Temperature ( C)
700
HL-N2
65 60 55 50
750
HL-SRM HL-H2
(e)
70
550
600
650
700
750
o
Temperature ( C)
Temperature ( C) 3.0
2.5
(c)
2.0
Ygas (l/gcoal, daf)
Ygas (l/gcoal, daf)
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60
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XL-SRM XL-H2
1.5
XL-N2
1.0 0.5 0.0
550
600
650
700 o
2.5 2.0
HL-SRM HL-H2
1.5
HL-N2
1.0 0.5 0.0
750
Temperature ( C)
(f)
550
600
650
o
700
750
Temperature ( C)
Figure 2. Tar, char and gas yields of XL (a,b,c) and HL (d,e,f) pyrolysis at 550-750 oC (Reaction time: 30 min; total gas flow rate: 500 ml/min; for CP-SRM, steam/CH4 ratio: 1.0, methane flow rate: 110 ml/min)
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SRM XL-SRM HL-SRM
60 40
4
XCH (%)
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60
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20 0
550
600
650
700 o
750
Temperature ( C)
Figure 3. Conversion of methane in CP-SRM and SRM at 550-750 oC (Reaction time: 30 min; total gas flow rate: 500 ml/min; steam/CH4 ratio: 1.0, methane flow rate: 110 ml/min)
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5.0 Vt, XL-SRM-Vt, SRM Vt, HL-SRM-Vt, SRM
2.5
△Vt (l)
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60
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0.0
-2.5 -5.0
550
600
650
700
750
o
Temperature ( C)
Figure 4. Comparison of gas volume from CP-SRM with SRM at 550-750 oC (Reaction time: 30 min; total gas flow rate: 500 ml/min; steam/CH4 ratio: 1.0, methane flow rate: 110 ml/min)
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6
0.4
6
0.6
0.2
5
0.4
4
0.0
4
0.2
3
-0.2
3
0.0
2
△△△△ -0.4
2
△△△△ -0.2
1
-0.6
1
-0.4
-0.8
0
XL-SRM XL-N2
5
550
600
650
700 o
750
550
650
700 o
750
-0.6
Temperature ( C) 4.0
6
2.0
10
3.5
5
1.5
8
3.0
4
6
2.5
4
2.0△△△△
2
1.5
1
1.0
0
550
600
650
700 o
750
H2 (l)
VCO (l)
12
0
CO2 (l)
VCO2 (l)
Temperature ( C)
600
1.0
3
0.5△
2
Temperature ( C)
CO (l)
0
CH4 (l)
VCH4 (l)
SRM
VH2 (l)
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60
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0.0 550
600
650
700 o
750
-0.5
Temperature ( C)
Figure 5. Gas analysis of XL-SRM compared with SRM and XL-N2 at 550-750 oC (Reaction time: 30 min; total gas flow rate: 500 ml/min; for SRM and XL-SRM, steam/CH4 ratio: 1.0, methane flow rate: 110 ml/min)
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6
0.0 HL-SRM HL-N2
5
SRM
-1.0
△△△△
2
VCO2 (l)
CH4 (l)
VCH4 (l)
3
6
0.6
5
0.4
4
0.2
3
0.0
2
-0.2△△△△
1
-0.4
-0.5
4
-1.5 1 550
600
650
700 o
750
0
-2.0
550
Temperature ( C)
600
650
700 o
750
-0.6
Temperature ( C) 6
2.0
10
4.0
5
1.5
8
3.5
4
6
3.0
4
2.5
2
2.0
1
1.5
0
0
△△△△
550
600
650
700 o
750
VCO (l)
4.5
H2 (l)
12
1.0
3 0.5△△△△
2
CO (l)
0
VH2 (l)
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60
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CO2 (l)
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0.0 550
Temperature ( C)
600
650
700 o
750
-0.5
Temperature ( C)
Figure 6. Gas analysis of HL-SRM compared with SRM and HL-N2 at 550-750 oC (Reaction time: 30 min; total gas flow rate: 500 ml/min; for SRM and HL-SRM, steam/CH4 ratio: 1.0, methane flow rate: 110 ml/min)
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A
100 C2H4
Volume (ml)
80
40
1
1 2 3
1
3: XL-N2
C3H8
60
(a)
1: XL-SRM 2: XL-H2
C2H6
1 1 23
2
2 2
3
3
3
20 0
550
600
650
700 o
750
Temperature ( C) A
100 C2H4
80
Volume (ml)
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60
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40
1
1 2 3
1
3: HL-N2
C3H8
60
(b)
1: HL-SRM 2: HL-H2
C2H6
1 1 2
3
2
2 2
3
3
3
20 0
550
600
650
700 o
750
Temperature ( C)
Figure 7. C2+C3 volume from XL (a) and HL (b) pyrolysis under different atmosphere at 550-750 oC (Reaction time: 30 min; total gas flow rate: 500 ml/min; for CP-SRM, steam/CH4 ratio: 1.0, methane flow rate: 110 ml/min)
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100 Asphaltene (>360 oC)
80
Content (wt. %)
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60
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Anthracene oil (300-360 oC)
60
Wash oil (230-300 oC)
40
Naphthalene oil (210-230 oC)
20
Phenol oil (170-210 oC)
0
Light oil (
