Laboratory Experiments on Pyrolysis of Lignin Samples
Investigate the pyrolysis of Z10 and Z5 lignin samples conducted under various conditions with Director Daniele Dondi at the University of Pavia. Analysis includes drying under vacuum and TGA in air to assess carbon content and moisture removal.
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CH4rLiE Associate Professor. Dr. Daniele Dondi Director in Laboratory of Radiation Chemistry and EPR Spectroscopy Department of Chemistry, University of Pavia, 27100, Italy. Thursaday, October 03th, 2024
Experiments Performed 1. Z10 drying 2. Pyrolysis of Z10-Melamine 10% sample 3. Pyrolysis of Z10-Lignin 20% sample 4. Pyrolysis of Z5-Lignin 20% sample (batch 1-10) 5. Pyrolysis of Z10-Lignin 20% sample (batch 1-8)
Z10 drying under vacuum 550 C for 3 Hours !PRIN Z10 drying 550C HV 3Hr 2808 PRIN Z10 drying 550C HV 3Hr 2808, 5.2258 mg Method Name: 25....1000_20 C/min BLANK N2 % 100 Step -3.1574 % -0.1650 mg 96.7986 % 5.0585 mg 3.3% of moisture only remains ? Step -0.1748 % -9.1326e-03 mg 99.9560 % 5.2235 mg Residue 98 Residue Inflect. Pt. 291.00 C Midpoint 242.13 C Inflect. Pt. 28.67 C Midpoint 35.49 C 96 50 100 150 200 250 300 350 400 450 500 550 600 650 700 750 800 850 900 950 C 0 5 10 15 20 25 30 35 40 45 min 1/min 0.000 -0.002 \!PRIN Z10 drying 550C HV 3Hr 2808 PRIN Z10 drying 550C HV 3Hr 2808, 5.2258 mg -0.004 -0.006 50 100 150 200 250 300 350 400 450 500 550 600 650 700 750 800 850 900 950 C 0 5 10 15 20 25 30 35 40 45 min Lab: METTLER Lab: METTLER S STA TAR Re e SW 12.10 SW 12.10
Z10 comparison before and after drying % !PRIN Z10 drying 550C HV 3Hr 2808 PRIN Z10 drying 550C HV 3Hr 2808, 5.2258 mg !Z10 PRIN 2024 CH4 Z10 PRIN 2024 CH4, 13.3130 mg 95 90 50 100 150 200 250 300 350 400 450 500 550 600 650 700 750 800 850 900 950 C 0 5 10 15 20 25 30 35 40 45 min 1/min Moisture removed \!PRIN Z10 drying 550C HV 3Hr 2808 PRIN Z10 drying 550C HV 3Hr 2808, 5.2258 mg -0.005 \!Z10 PRIN 2024 CH4 Z10 PRIN 2024 CH4, 13.3130 mg Moisture removed 50 100 150 200 250 300 350 400 450 500 550 600 650 700 750 800 850 900 950 C 0 5 10 15 20 25 30 35 40 45 min Lab: METTLER Lab: METTLER S STA TAR Re e SW 12.10 SW 12.10
Z10-Kraft lignin 20% after pyrolysis TGA in air Carbon content:8.6% !PRIN Z10-LIGNIN 20% AF Pyro Air 0309 PRIN Z10-LIGNIN 20% AF Pyro Air 0309, 6.3000 mg % Method Name: 25....1000_20 C/min BLANK AIR(Chia LUPI) ? Step -15.9207 % -1.0030 mg 84.1148 % 5.2992 mg Step -8.5909 % -0.5412 mg 75.5238 % 4.7580 mg 90 Residue Residue Inflect. Pt. 189.67 C Midpoint Inflect. Pt. 411.67 C Midpoint 170.65 C 405.83 C 80 50 100 150 200 250 300 350 400 450 500 550 600 650 700 750 800 850 900 950 C 0 5 10 15 20 25 30 35 40 45 min 1/min \!PRIN Z10-LIGNIN 20% AF Pyro Air 0309 PRIN Z10-LIGNIN 20% AF Pyro Air 0309, 6.3000 mg -0.01 50 100 150 200 250 300 350 400 450 500 550 600 650 700 750 800 850 900 950 C -0.02 0 5 10 15 20 25 30 35 40 45 min Lab: METTLER Lab: METTLER S STA TAR Re e SW 12.10 SW 12.10
Z5-Kraft lignin 20% after pyrolysis (1g) TGA in air Carbon content:15.2% Method Name: 25....1000_20 C/min BLANK AIR(Chia LUPI) % !PRIN Z5-Lignin 20% af pyro mixed 1109 PRIN Z5-Lignin 20% af pyro mixed 1109, 5.6339 mg 100 Step -1.9166 % -0.1080 mg 78.7380 % 4.4360 mg Step -12.0665 % -0.6798 mg 80.6546 % 4.5440 mg ? Step -7.4237 % -0.4182 mg 92.7211 % 5.2238 mg Residue Residue Residue 90 Inflect. Pt. 983.33 C Midpoint Inflect. Pt. 398.00 C Midpoint Inflect. Pt. 179.33 C Midpoint 879.27 C 422.14 C 196.25 C 80 50 100 150 200 250 300 350 400 450 500 550 600 650 700 750 800 850 900 950 C 0 5 10 15 20 25 30 35 40 45 min 1/min \!PRIN Z5-Lignin 20% af pyro mixed 1109 PRIN Z5-Lignin 20% af pyro mixed 1109, 5.6339 mg 0.000 -0.005 -0.010 -0.015 50 100 150 200 250 300 350 400 450 500 550 600 650 700 750 800 850 900 950 C 0 5 10 15 20 25 30 35 40 45 min Lab: METTLER Lab: METTLER S STA TAR Re e SW 12.10 SW 12.10
Conclusion Drying of zeolite Z10 was observed same as Z5, 3.3% weight loss for 1stweight loss curve in TGA was achieved. Pyrolysis of Z10-Melamine 10% didn t yield the expected carbon incorporated zeolite material. Z10-Lignin 20% sample yielded carbon incorporated zeolite and gram scale batches are underway. 1g of carbon incorporated zeolite was successfully prepared (Z5-lignin 20%) with 15.2% carbon content. Sample of UCSB-9 zeolite prepared has been submitted for Powder XRD studies. Samples of Z5 and Z10 lignin incorporated Zeolite has been submitted for SEM imaging.
