Warsaw University of Life Sciences SGGW
COST FP 1205 Training School
Pretreatment and dissolution of cellulose
April 07-09, 2015, Jena, Germany
INFLUENCE OF PRETREATMENT METHOD OF
CELLULOSE ON THE MOLAR MASS
DISTRIBUTION
Michał Drożdżek1, Andrzej Antczak1, Jakub Gawron2
1Faculty
Contact information:
[email protected]
of Wood Technology,
2Faculty of Production Engineering
COST FP 1205 Training School. Pretreatment and dissolution of cellulose. April 07-09, 2015, Jena, Germany
CELLULOSE „GREEN POLYMER”
 Application
papers, books
 varnish components, paints
 clothes
 biofuels
 nanotechnology

 Advantages – cheap, easily available, rewenable,
environmental friendly, biodegradable material
Introduction
COST FP 1205 Training School. Pretreatment and dissolution of cellulose. April 07-09, 2015, Jena, Germany
Isolation of cellulose from wood:

Kürschner-Hoffer

Seifert

Cross–Bevan
Introduction
COST FP 1205 Training School. Pretreatment and dissolution of cellulose. April 07-09, 2015, Jena, Germany
Acid hydrolysis of cellulose
Introduction
COST FP 1205 Training School. Pretreatment and dissolution of cellulose. April 07-09, 2015, Jena, Germany
Oxidation of cellulose reactions
H
HO
O
OH
OH
H
O
H
O
HO
O
HH
OH
H
OH
OH
H
O
HH
O
H
H
OH
OH
H
O
HO
O
O
HO
HH
H
H
H H
O
O
OH
H
OH
H
H
H
O
O
O
O
O
O
O
H
O
H
O
H
O
OH
O
HO
H H
Introduction
H
OH
H
H
O
H
O
OH
O
O
H
O
H
OH
O
OH
O
O
H
Methods
Large numbers of cycles
Additional pretreatment before dissolution
1% NaOH
Methods
OR
0.01M NaBH4
and next
1% NaOH
Crystallinity
Isolation of
cellulose
Purity
Small numbers of cycles
Degradation of cellulose
COST FP 1205 Training School. Pretreatment and dissolution of cellulose. April 07-09, 2015, Jena, Germany
COST FP 1205 Training School. Pretreatment and dissolution of cellulose. April 07-09, 2015, Jena, Germany
MOLECULAR MASS ANALYSIS

Size exclusion chromatography (SEC)

Calculation of average molecular mass based
on polystyrene standards
Mps×[η]ps = Mcel×[η]cel


Methods
Mark-Houwink equation: [h] = KMa
necessary factors - K and a
COST FP 1205 Training School. Pretreatment and dissolution of cellulose. April 07-09, 2015, Jena, Germany
EXPERIMENTAL MATERIALS
Materials

Softwood
pine wood (Pinus sylvestris L.),
age - 150 years, sapwood zone

Hardwood
poplar wood (Populus tremula L.),
age - 40 years
COST FP 1205 Training School. Pretreatment and dissolution of cellulose. April 07-09, 2015, Jena, Germany
POPLAR CELLULOSE MASS DISTRIBUTIONS AFTER
2 CYCLES ISOLATED BY KÜRSCHNER-HOFFER METHOD
Kürschner-Hoffer
NaOH
NaBH4+ NaOH
Results
COST FP 1205 Training School. Pretreatment and dissolution of cellulose. April 07-09, 2015, Jena, Germany
PINE CELLULOSE MASS DISTRIBUTIONS AFTER
6 CYCLES ISOLATED BY KÜRSCHNER-HOFFER METHOD
Kürschner-Hoffer
NaOH
NaBH4+NaOH
Results
COST FP 1205 Training School. Pretreatment and dissolution of cellulose. April 07-09, 2015, Jena, Germany
MAIN CONCLUSIONS - 1% NaOH
In the case of significantly contaminated cellulose, 1%
NaOH pretreatment gives lower results of average molar mass.
But in the case of cellulose with a high degree of purity 1%
NaOH pretreatment causes the increase of this parameter. This is
due to a different phenomena of 1% NaOH extraction. In the first
case the predominant effect of 1% NaOH pretreatment is the
degradation of wood polysaccharides complexes, which
facilitates the breakdown of cellulose associates and it’s
dissolution. In the second case 1% NaOH dissolves mainly the
residue fractions having a low molar masses and degradation
products.
Conclusions
COST FP 1205 Training School. Pretreatment and dissolution of cellulose. April 07-09, 2015, Jena, Germany
MAIN CONCLUSIONS - NaBH4 and next 1% NaOH
Both cases, it have proved advantageous to use a reducing
agent (NaBH4), on the one hand actively assisted cleavage
polysaccharides complexes, on the other effectively prevents the
rapid degradation of cellulose oxidation products. It should be
appreciated that the use of pretreatment method with NaBH4 and
next 1% NaOH allows more reproducible and reliable results of SEC
analysis.
Conclusions
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