cellulose microfibrills and nanotechnologybiorefinery.utk.edu/ciber/portugal_nanocellulose.pdf ·...
TRANSCRIPT
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CelluloseMicrofibrills and Nanotechnology
Art J. Ragauskas
Institute of Paper Science and TechnologySchool of Chemistry and Biochemistry
Georgia Institute of Technology
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World Pulp ProductionMillion metric tons
010203040506070
U.S.A. Canada Sweden Finland Brazil Chile N.Z.
1995 2002Source: Pulp & Paper International,
Paperloop.com
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Cellulosics - TrendsNewsprint capacity fell 1.3% in 2003,decline another 2.8% in 2004lowest since 1989.
Bye bye Paper Tickets TICKETLESS travel will become a global reality by the end of 2007- IATA
•Improved Operations
•Fiber Engineering•Fillers
•New Products
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NanoCellulosic Structures
m
10 µm
1 µm
10 nm
1 nm
100 µmmm
OO
HOOH
OO
HOOH
OH
OH
O
HOOH
OO
HOOH
O-Cellulose
OH
OH
O
OO
HOOH
OO
HOOH
OH
OH
O
HOOH
OO
HOOH
O-Cellulose
OH
OH
O
0
20
40
60
80
100
120
140
E-Glas
sHem
p
Flax
Jute
Sisal
CoirCott
on
Nanoc
ellulo
se W
hiske
rsDou
glas F
ir
Pond
erosa
Pine
StiffnessSpecific Stiffness
approx. 100Carbon Nanotubes400 - 700
NanocelluloseWhiskers
approx. 500Fully Exfoliated Clay100 - 400Fumed Silica25 - 300Graphite
4Paper Fibersapprox.1
Surface Area m2/gE-Glass Fibers
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Cellulosics StructureBackground Native
Cellulose Iα and Iβ
Chains are parallel; Differences due to orientation of Cellulose sheets
• I – IV Polymorphs• Amorphous• Paracrystalline
Cellulose II:
anti-parallel
Elementary fibril
Microfibril
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• Acid Hydrolysis Technique
Bleached softwood kraft pulp Cellulose + H2SO4
Stirred at 45 C, 45 min ~ 1 hourDilute with waterCentrifuged, wash and neutralizeRe-disperse with ultrasonicationAllowed to stand over a mixed bed resin for 48 hThe mixture was centrifuged and the supernatant was filter through filter paper. The filtrate was colloidal nanowhisker suspension
NanoCellulosic Structures
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Cellulase from Trichoderma reesei
0 5 10 15 20 253
4
5
6
7
8
Rel
ativ
e in
tens
ity, %
Hydrolysis time, hr
ΙβCellulose: Iβ
0
20
40
60
80
100
0 10 20 30 40 50
Hydrolysis Time, h
Glu
cose
yie
ld, %
Pulpavicel
Cellulose: Iα
0 5 10 15 20 252.5
3.0
3.5
4.0
4.5
5.0
Rel
ativ
e in
tens
ity, %
Hydrolysis time, hr
ΙαCellulose: Iα
Enzymatic Hydrolysis of Cellulosics
• Cellulolytic filamentous fungus
cellobiohyrolasesendoglucanasesβ-glucosidasesNREL
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0
20
40
60
80
100
0 10 20 30 40 50
Hydrolysis Time, h
Post
-hyd
roly
sis p
erce
ntag
e, %
avicelpulp
Enzymatic Hydrolysis of Cellulosics
0 5 10 15 20 25
33
34
35
36
37
Rel
ativ
e in
tens
ity, %
Hydrolysis time, hr
Para-crystallinePara-crystalline
0 5 10 15 20 25
46
48
50
Rel
ativ
e in
tens
ity, %
Hydrolysis time, hr
AmorphousAmorphous
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AFM images of nanowhisker
NanoCellulosic Structures
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Nanocellulose Whisker Composite Films
Polystyrene (average Mw ~280,000 ) solution in THF (5% w/w) Dry nano whiskersPolymer films were prepared by solution casting into molds. 3% nanocellulose whiskers were added into polymer solution, sonificated and then solvent cast into moldsFilms was of a thickness of 50~110 µm
NanoCellulosic Structures
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Nanocellulose Whisker:Polystyrene Composite Film
Polystyrene /whisker film
Mechanical tests were carried out on an Instron 4400R4.5 inch length * 15 mm width
+ 23%+ 11%+70%Polystyrene/NC whisker
46.51.38.9Polystyrene
Modulus (MPa)
Elongation, %
TEA*, J/m2
*: Tensile energy absorption.
Preliminary Physical Properties
NanoCellulosic Structures
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NanoCellulosic StructuresNanocellulose Whisker
Acrylic Acid Composite Film
Experimental Method
• Dow acrylic latex, solids 50%• Add cellulose whiskers or hardwood bleached
kraft pulp• Mixture cured at RT• Initial film dried 50 ˚C for 2 days.
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0
50
100
150
200
250
300
350
0 5 10 15 20Filler,%
Stra
in, %
WhiskerPulp Fiber
NanoCellulosic StructuresNanocellulose Whisker:Acrylic Acid Composite Film
0
2
4
6
8
10
12
14
0 5 10 15 20Cellulose, %
Tensile strength, MPa
WhiskerPulp Fiber
0
1000
2000
3000
4000
0 5 10 15 20
Filler, %
TEA, J/m2
WhiskerPulp Fiber
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Nanocellulose Whisker:Acrylic Acid Composite Film
NanoCellulosic Structures
Latex Film 20% Cellulose Whiskers:Latex Film
20
25
30
35
40
0 5 10 15 20 25
Whisker content, %
Contact angle
5% Cellulose Whiskers:Latex Film
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Nanocellulose Balls
• SW ECF bleached kraft pulp• Refined to 20-mesh • Swell fibers with 5M NaOH followed by DMSO• Sonicate cellulose with HCl – H2SO4 75 oC • Wash with water, purify by centrafugation• Sonicate cellulose with HCl – H2SO4 75 oC• Wash with water, purify by centrafugation
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Nanocellulose Balls
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First nanocellulose procedure able to provide practical control of particle sphere dimensions!!
050
100150200250300350400450500
0 2 4 6 8 10 12
Time (hour)
Siz
e (n
m)
020406080
100120140160180
0 1 2 3 4 5
Time (hour)
Siz
e (n
m)
Nanocellulose Balls
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Nanocellulose Balls – 76 nmAFM Images
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Nanocellulose Balls
S-800 FE SEM
180 nm balls
76 nm balls
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Nanocellulose Crystallinity Results 13C-CP/MAS NMR Analysis
0.7050 – 100 nm Nanocellulose BallsCellulose II
0.65300 – 500 nm Nanocellulose BallsCellulose II
0.61Original pulp – Cellulose 1
Crystallinity index
C-1
C-4
C-2, 3, 5
C-6
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Nanocellulose Whisker-Balls:Acrylic Acid Composite Film
NanoCellulosic Structures
Latex Film
5% Cellulose Balls:Latex Film 5% Cellulose Whiskers:Latex Film
0200400600800
100012001400
TEA
Latex nanoball whisker acacia
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Pathforward• Nanocellulose balls
– Derivatives to be used for superabsorbers – viscosity modifiers– Artificial blood/drug delivery– Cosmetics– Template for Nanospheres
• Nanocellulose whiskers– Composites with plastics– Composites with natural polymers– In-situ polymerization
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Nano-Enhanced Paper and BoardIPST@GT Research Accomplishments:
Nanocellulose Additives for Innovative Composites
1. Disperse Plastic Resin
2. Heat Press – PMMAPolymethyl methacrylate
Fiber 10% 30% PMMA PMMA
ECF SW Kraft
30
35
40
45
50
55
60
65
70
75
80
0% PMMA 10% PMMA 30% PMMA
Con
tact
Ang
le (d
egre
es)
Micro-sized PMMANano-sized PMMA
60 nm PMMA5-100 micron PMMA
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Composite Fabrication
• Fiber and PMMA powder was mixed in a blender.
• Fiber/PMMA mixture was compression molded at 170°C for 10 minutes.
• Composite specimen was 1.24” in diameter and 1mm in thickness.
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ECF Pulp
SEM
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Nano PMMA, 10%Course PMMA, 10%
SEM
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Course PMMA, 30% Nano PMMA, 30%
SEM
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Polystyrene-ECF Kraft Composite
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Nano-Enhanced Paper: CoatingsApplication of Polyelectrolyte Coating TechnologiesLayer-by-Layer Self-Assembly
General Considerations:General Considerations:
•• Assembly via electrostatic and HAssembly via electrostatic and H--bond interactionsbond interactions•• Aqueous ProcessingAqueous Processing•• Process Parameters:Process Parameters:
•• pH; salt concentrationpH; salt concentration•• Polymer charge/DPPolymer charge/DP
•• Wide range of materials can be employedWide range of materials can be employed
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Nano-Enhanced Paper: Coatings
CNH2O
n
n
N+
Cl-
n
NH3+ Cl-
PolymethylAcrylic acid
Polyallylamine hydrochloride
Polysulfonate styrene Polydimethyldiallylammonium chloride
Poly(acrylamide)
Typical Polymers Employed for Self-Assembly
CO- H+O
n
n
SO3- Na+
CO- H+O
n
CH3
Poly(acrylic acid)
Positive Neutral Anionic
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Nano-Enhanced Paper: Coatings
++++++
Current Studies n
NH3+ Cl-
PAH
_ _ _ _ _
n
N+
Cl-
PDDA
Montmorrilonite Kaolin
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Nano-Enhanced Paper: Coatings
n
NH3+ Cl-
PAH
n
N+
Cl-
PDDAMontmorrilonite Kaolin
8 Bilayers PDDA/Montmorrilonite
8 Bilayers of PDDA/Kaolin
0.00
0.10
0.20
0.30
0.40
0.50
0.60
0.70
0.80
0.90
1.00
250 350 450 550 650 750 850Wavelength (nm)
Abs
orba
nce
Number of bilayers87654321
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Nano-Enhanced Paper: CoatingsCurrent Studies
n
NH3+ Cl-
Initial Fibers 8 Bilayers of PAHKaolin
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Nano-Enhanced Paper: Coatings
n
NH3+ Cl-
8 Bilayers of PAHKaolin
0.0
1.0
2.0
3.0
4.0
5.0
6.0
4 bilayers 8 bilayers 12 bilayers 16 bilayers
Wet
Ten
sile
Inde
x (N
m/g
)
0
10
20
30
40
50
60
70
80
90
100
110
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17
Number of Layers
Con
tact
Ang
le (d
egre
es)
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Nano-Enhanced Paper: CoatingsCurrent Studies
n
NH3+ Cl-
n
N+
Cl-
Bilayers of PAH/Kaolin
Ongoing Studies• Alternative L-b-L technologies • Enhance hydrophobic effect• Utilize other nanomaterials• Unique optical properties• Functional barrier properties
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Where Is This All Going?"Give me a lever, a fulcrum, and place to stand and I will move the world."
Archimedes ∼200 BC
Forest Products CommunityInnovative Products“Nano-Inside”
Societal Demand forCarbon Neutral, Environmentally Friendly, Renewable and SustainableManufacturing Technologies
Consumer DemandValue Added
Products &
Materials
More Relevant Today!!!Leveraging: Nano Research and Development
Partnership Industry, Universities,
Government
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AcknowledgmentsGA Research AllianceNational Science FoundationIPST Industry Consortium