1. October 8-9 Trabzon, Turkey
obtention of cellulose nanofiber from almond shell using Different chemical treatments
Eduardo Robles, Iñaki Urruzola, Rodrigo Llano-Ponte, Rodrigo Llano-Ponte, Jalel Labidi
Biorefinery Process Group
Department of Chemical and Environmental Engineering
University of Basque Country
Pza. Europa 1, 20018, San Sebastian, SPAIN
Correspondence to:

2. COST Action FP1105 October 8-9 Trabzon, Turkey
Objectives
Determining the best chemical treatment to remove lignin content in almond shell (Prunus dulcis)
Determining the best crystallinity achieved with the different mercerizations.
Analysis:
FTIR
TGA
X-Ray
Obtention Of Cellulose Nanofibers From Almond Shell Using Different Chemical Treatments. Eduardo Robles, Iñaki Urruzola, Rodrigo Llano-Ponte, Jalel Labidi.

3. COST Action FP1105 October 8-9 Trabzon, Turkey
Procedure
Pretreatment
NaOH (1%) w/w alkaline solution
T = 20 ºC
t = 24 h
NaOH 7.5% w/w
T = 60 ºC
Formic acid/water 90/10 v/v
T = 130 ºC
t = 90 min
Ethanol/water 60/40 v/v
KOH 7.5% w/w
NaOH 15% w/w
T = 120 ºC
FTIR and TGA analysis
Bleaching
NaClO2 (25 % w/w)
T = 75 ºC
t = 120 min
NaOH + H2O2 + DTPA + MgSO4
T = 70 ºC
t = 150 min
Acetylation
HNO3 (1/3) w/w
Acetic Acid (1/20) w/w
T= boiling
t = 30 min
Hydrolysis
H2SO4 (8..5 mL /g)
T = 45 ºC
t = 60 min
AFM and X-Ray analysis
Obtention Of Cellulose Nanofibers From Almond Shell Using Different Chemical Treatments. Eduardo Robles, Iñaki Urruzola, Rodrigo Llano-Ponte, Jalel Labidi.

4. Results Crystallinity Content
COST Action FP1105 October 8-9 Trabzon, Turkey
Results
Content
Method
Extracts %
Moisture
Lignin
Almond shell
0.72 ± 0.02
10.76 ± 0.06
52.59 ± 0.14
Organosolv
5.28 ± 0.02
30.55 ± 0.06
43.21 ± 0.06
NaOH 15%
3.28 ± 0.02
19.03 ± 0.06
42.76 ± 0.06
KOH 7.5%
1.06 ± 0.02
0.435 ± 0.06
39.92 ± 0.06
NaOH 7.5%
1.35 ± 0.02
0.432 ± 0.06
35.34 ± 0.06
Formic acid
4.21 ± 0.02
2.16 ± 0.06
30.72 ± 0.06
Crystallinity
Pulp
(%)
Acetylated + Hydrolyzed + Homogenized
72.29 -
75.73
80.57
69.35
76.95
62.51
78.23
69.13
79.79
56.77
78.69
Obtention Of Cellulose Nanofibers From Almond Shell Using Different Chemical Treatments. Eduardo Robles, Iñaki Urruzola, Rodrigo Llano-Ponte, Jalel Labidi.

5. COST Action FP1105 October 8-9 Trabzon, Turkey
Results
FT-IR spectra of the a) Almond shell, b) Organosolv, c) NaOH 15%, d) KOH, e) NaOH 7.5%, f) Formic acid.
3345 cm-1
OH stretching vibrations
2920 cm-1
CH3 group stretching vibrations
2860 cm-1
CH2 group stretching vibrations
1645 cm-1
absorbed water (bending)
1420 cm-1
CH2 bending
1215 cm-1
OH in plane-bending cellulose
1150 cm1
C-O antisymetric bridge stretching
890 cm-1
β-glycosidic linkages
Obtention Of Cellulose Nanofibers From Almond Shell Using Different Chemical Treatments. Eduardo Robles, Iñaki Urruzola, Rodrigo Llano-Ponte, Jalel Labidi.

6. COST Action FP1105 October 8-9 Trabzon, Turkey
Conclusions
Different lignin elimination methods were performed to determine their effectiveness in almond shell. Sodium hydroxide at 7.5% v/v and formic acid treatments were the best in eliminating lignin as the amount of lignin present in almond shell was reduced 17 and 22 % respectively.
The different nature of the methods and their reactives influence in the properties of the final fiber, as change in crystallinity, lignin content and affinity to different compounds can be reached with these methods, then depending of the final use of the fiber, it can be chosen the most suitable method.
Obtention Of Cellulose Nanofibers From Almond Shell Using Different Chemical Treatments. Eduardo Robles, Iñaki Urruzola, Rodrigo Llano-Ponte, Jalel Labidi.

7. COST Action FP1105 October 8-9 Trabzon, Turkey
THANK YOU!
Author would also like to thank to CONACyT, Mexico for support provided through Scholarship
Obtention Of Cellulose Nanofibers From Almond Shell Using Different Chemical Treatments. Eduardo Robles, Iñaki Urruzola, Rodrigo Llano-Ponte, Jalel Labidi.