processing lignins guozhan jiang. objectives to find a method to convert etek and asian lignins into...
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![Page 1: Processing Lignins Guozhan Jiang. Objectives To find a method to convert Etek and Asian lignins into bio-oils. To characterise the products using PyGC/MS](https://reader035.vdocuments.site/reader035/viewer/2022081503/56649ebc5503460f94bc4c0b/html5/thumbnails/1.jpg)
Processing Lignins
Guozhan Jiang
![Page 2: Processing Lignins Guozhan Jiang. Objectives To find a method to convert Etek and Asian lignins into bio-oils. To characterise the products using PyGC/MS](https://reader035.vdocuments.site/reader035/viewer/2022081503/56649ebc5503460f94bc4c0b/html5/thumbnails/2.jpg)
Objectives
• To find a method to convert Etek and Asian lignins into bio-oils.
• To characterise the products using PyGC/MS and other chromatographic or spectroscopic methods.
• To upgrade the bio-oils to valuable chemicals or transportation oils.
![Page 3: Processing Lignins Guozhan Jiang. Objectives To find a method to convert Etek and Asian lignins into bio-oils. To characterise the products using PyGC/MS](https://reader035.vdocuments.site/reader035/viewer/2022081503/56649ebc5503460f94bc4c0b/html5/thumbnails/3.jpg)
Outline
• Component determination
• PyGC-MS work
• Preliminary work for run on 150g/h rig
• Alternative way to pyrolysis
• Future work
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Component determination: wet chemistry method
Extractives: Extracted using: ethanol/toluene (6hrs)ethanol (4hrs)water (2hrs)
Lignin (Klason): 0.1M NaOH boiling 1hr72% H2SO4 treatment 4hrs
Cellulose: NaClO2 bleaching of holocellulose
Hemicellulose: 17.5% NaOH treatment of cellulose
Biomass
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Results
Etek lignin Asian lignin
Extractive (%) 12.74 39.68
Lignin (%) 29.20 -
Cellulose (%) 45.70 -
Hemicellulose (%)
9.32 -
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Component determination
• The component of Etek lignin can be determined using this method.
• This method is not suitable for Asian lignin since the extractive free samples can be completely dissolved in 0.1M NaOH.
• Asian lignin must have a much less cross-linking density in its molecular structure.
Conclusions
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PyGC-MS work, 06-Sep-2007 + 20:02:03
1.50 11.50 21.50 31.50 41.50 51.50 61.50 71.50 81.50 91.50 101.50Time0
100
%
0
100
%
asian lignin 1 Scan EI+ 78+94
1.51e929.59
41.32
38.9035.14
33.52
41.39
52.4147.3543.66 50.24 60.5652.77
57.11
asian lignin 1 Scan EI+ TIC
2.06e1041.32
30.36
29.59
3.64
17.318.554.29 10.23 26.80
35.13
33.52
31.86
38.90
41.39
43.66
47.35
46.78 60.5650.24 52.41
57.11
53.1263.88
Species containing m/z =94 and 78
Asian lignin @600oC for 15s
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, 06-Sep-2007 + 23:52:10
1.50 11.50 21.50 31.50 41.50 51.50 61.50 71.50 81.50 91.50 101.50Time0
100
%
0
100
%
etek lignin 1 Scan EI+ 78+94
5.68e835.17
29.59
8.886.86
30.37
41.35
38.89
35.66
46.79
42.37
44.68
49.97
52.76
57.2854.42
etek lignin 1 Scan EI+ TIC
1.71e1035.18
30.38
17.36
4.80
3.42
9.86
8.517.28
16.70
14.46
27.9523.02
19.68 25.73 33.34
56.5443.13
41.35
38.89
35.77
46.79
43.36 50.84
54.7757.28
Etek lignin species containing m/z = 94 and 78
Etek lignin@600oC for 15s
![Page 9: Processing Lignins Guozhan Jiang. Objectives To find a method to convert Etek and Asian lignins into bio-oils. To characterise the products using PyGC/MS](https://reader035.vdocuments.site/reader035/viewer/2022081503/56649ebc5503460f94bc4c0b/html5/thumbnails/9.jpg)
, 06-Sep-2007 + 20:02:03
1.50 11.50 21.50 31.50 41.50 51.50 61.50 71.50 81.50 91.50 101.50Time0
100
%
0
100
%
asian lignin 1 Scan EI+ TIC
2.06e1041.32
30.36
29.59
3.64
17.318.554.29 10.23 26.80
35.13
33.52
31.86
38.90
41.39
43.66
47.35
46.78 60.5650.24 52.41
57.11
53.1263.88
asian lignin 400a Scan EI+ TIC
1.73e1041.27
3.68 17.27
30.2326.7438.80
60.49
55.9043.53
47.57 55.0850.75
61.4966.31
Asian lignin @400oC for 15s
Asian lignin@600oC for 15s
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, 06-Sep-2007 + 23:52:10
1.50 11.50 21.50 31.50 41.50 51.50 61.50 71.50 81.50 91.50 101.50Time0
100
%
0
100
%
etek lignin 1 Scan EI+ TIC
1.71e1035.18
30.38
17.36
4.80
3.42
9.86
8.517.28
16.70
14.46
27.9523.02
19.68 25.73 33.34
56.5443.13
41.35
38.89
35.77
46.79
43.36 50.84
54.7757.28
etek 400a Scan EI+ TIC
2.29e93.65
3.42
47.59
3.72
3.76
42.91
17.31
4.89
34.5830.26
19.65
41.2738.82 46.72
87.2756.11
50.4654.71
Etek lignin 400 and 600
Etek lignin@400oC for 15s
Etek lignin @600oC for 15s
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PyGC-MS work
• The two lignins can not be pyrolysed effectively at 400oC.
• Asian lignin is a ‘real’ lignin.
• Etek lignin has similar composition to normal biomass.
Conclusions
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Preliminary work for run lignins on 150g/h rig
• The two lignins are difficult to feed continuously.
• Two approaches to be adopted for feeding properly (1) Modify feeding system, (2) Modify lignins.
• Modification of lignins is chosen in this work by pelitization.
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Pellitization
Alcohol extracted compounds as binders
Asian lignin
Ethanol
SuspensionHeating up
80oC
“Dough” like
Drying
Pellet
Mixing
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Pelletization of Asian lignin
Before pelleting After pelleting
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Pellet
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Alternative to pyrolysis
Method % dissolved
0.1 M NaOH aqueous, 4hrs boiling, 10% 10.2
Ethanol + 0.1 M NaOH, 4hrs boiling, 10% 10.5
Isopropanol + 0.1M NaOH, 4hrs boiling, 10% 21.2
Isopropanol + 0.1M H2SO4 + Phenol (13.5% wt), 10% 28.3
Extracted using ethanol/toluene (6hrs), ethanol (4hrs) and water (2hrs), extractive free samples boiling in 0.1M NaOH, 2%
100
Asian lignin
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Alternative to pyrolysis
Extractive free sample dissolved in 0.1M NaOH,2%
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Future work• Run Asian and Etek lignins on 150 g/h rig for
pyrolysis • Hydrogenation of lignin pyrolytic products to
produce saturated phenol and phenol substitutes, which may be used to produce phenolic resin.
• Quantification of mass balance using Py-GC/MS.• Hydrogen, steam or alcohol assisted pyrolysis to
reduce char formation.
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