A Nano Perspective of Cellulose Arthur J. Ragauskas Yunqiao Pu - - PowerPoint PPT Presentation

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A Nano Perspective of Cellulose Arthur J. Ragauskas Yunqiao Pu - - PowerPoint PPT Presentation

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A Nano Perspective of Cellulose Arthur J. Ragauskas Yunqiao Pu Jianguo Zhang School of Chemistry and Biochemistry Institute of Paper Science and Technology Georgia Institute of Technology World Pulp Production Million metric tons 70 60 50

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SLIDE 1

A Nano Perspective of Cellulose

Arthur J. Ragauskas Yunqiao Pu Jianguo Zhang School of Chemistry and Biochemistry Institute of Paper Science and Technology Georgia Institute of Technology

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SLIDE 2

World Pulp Production Million metric tons

10 20 30 40 50 60 70

U.S.A. Canada Sweden Finland Brazil Chile N.Z.

1995 2002

Source: Pulp & Paper International, Paperloop.com

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SLIDE 3

Wood Chemistry/Pulp Paper

Research Trends

1975 1980 1985 1990 1995 2000 2005 Starch Filler 500 1000 1500 2000 2500 3000 3500 4000 4500 5000

Citations

1975 1980 1985 1990 1995 2000 2005

Kraft Bleaching

500 1000 1500 2000 2500

Kraft Bleaching

`

20 40 60 80 100 120 140 160 180

1965-70 1970-75 1975-80 1980-85 1985-90 1990-95 1995-00 2000-05

Brightness Reversion Citations

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SLIDE 4

Pulp and Paper Trends

Paper or plastic? Students prefer the latter when it comes to milk containers so schools switching Smurfit-Stone Container to cut costs, increase revenues, close plants (11/9/05) AF&PA: U.S. paper and paperboard capacity continues to decline (02/27/04)

Bye bye Paper Tickets TICKETLESS travel will become a global reality by the end of 2007- IATA

Newsprint capacity fell 1.3% in 2003, decline another 2.8% in 2004 lowest since 1989.

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SLIDE 5

“The Future Ain’t What It Used To Be”

Yogi Berra New York Yankees

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SLIDE 6

What is The Future Innovation

“A change that creates a new dimension of performance” Drucker

Sony Corporation and TOPPAN Printing Co., announced the successful development of 25GB paper disc, the recording layer on which the data is stored lies under a protective layer.

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SLIDE 7

`

All These Examples And Others Use Fibers in An Unconventional Manner

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SLIDE 8

NanoCellulosic Structures

m 10 µm 1 µm 10 nm 1 nm 100 µm mm

O O HO OH O O HO OH OH OH O HO OH O O HO OH O-Cellulose OH OH O O O HO OH O O HO OH OH OH O HO OH O O HO OH O-Cellulose OH OH O

20 40 60 80 100 120 140

E

  • G

l a s s H e m p F l a x J u t e S i s a l C

  • i

r C

  • t

t

  • n

N a n

  • c

e l l u l

  • s

e W h i s k e r s D

  • u

g l a s F i r P

  • n

d e r

  • s

a P i n e

Stiffness Specific Stiffness

  • approx. 100

Carbon Nanotubes 400 - 700 Nanocellulose Whiskers

  • approx. 500

Fully Exfoliated Clay 100 - 400 Fumed Silica 25 - 300 Graphite 4 Paper Fibers approx.1

Surface Area m2/g

E-Glass Fibers

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SLIDE 9
  • Acid Hydrolysis Technique
  • Bleached softwood kraft pulp
  • 8% Cellulose + 64% H2SO4
  • Stirred at 45 C, 45 min ~ 1 hour
  • Dilute with water
  • Centrifuged, wash and neutralize
  • Re-disperse with ultrasonication
  • Allowed to stand over a mixed bed resin for 48 h
  • The mixture was centrifuged and the supernatant was filter through

filter paper. The filtrate was colloidal nanowhisker suspension Over 60% of yield could be achieved by this method.

NanoCellulosic Structures

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SLIDE 10

AFM images of nanowhisker

NanoCellulosic Structures

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SLIDE 11

Nanocellulose Whisker Composite Films

  • Polystyrene (average Mw ~280,000 ) solution in THF (5% w/w)
  • Dry nano whiskers.
  • Polymer films were prepared by solution casting into molds. The films

were left for 24 hours at ambient conditions to allow for solvent evaporation.

  • 3% nanocellulose whiskers were added into polymer solution,

sonificated and then cast into molds. The films were left for 24 hours at ambient conditions to allow for solvent evaporation.

  • Films was of a thickness of 50~110 µm.

NanoCellulosic Structures

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SLIDE 12

Nanocellulose Whisker:Polystyrene Composite Film

Polystyrene /whisker film

  • Mechanical tests were carried out on an Instron 4400R
  • 4.5 inch length * 15 mm width

+ 23% + 11% +70% Polystyrene/ NC whisker 46.5 1.3 8.9 Polystyrene Modulus (MPa) Elongation, % TEA*, J/m2

*: Tensile energy absorption.

Preliminary Physical Properties

NanoCellulosic Structures

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SLIDE 13

NanoCellulosic Structures

Nanocellulose 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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SLIDE 14

50 100 150 200 250 300 350 5 10 15 20 Filler,% Strain, % W hisker Pulp Fiber

NanoCellulosic Structures

Nanocellulose Whisker:Acrylic Acid Composite Film

2 4 6 8 10 12 14 5 10 15 20 Cellulose, % T ensile strength, M Pa

W hisker Pulp Fiber

1000 2000 3000 4000 5 10 15 20 Filler, % T E A , J / m 2

W hisker Pulp Fiber

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SLIDE 15

Nanocellulose Whisker:Acrylic Acid Composite Film

NanoCellulosic Structures

Latex Film 20% Cellulose Whiskers:Latex Film

5% Cellulose Whiskers:Latex Film

20 25 30 35 40 5 10 15 20 25 W hisker content, % Contact angle

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SLIDE 16

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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First nanocellulose procedure able to provide practical control of particle sphere dimensions!!

50 100 150 200 250 300 350 400 450 500 2 4 6 8 10 12 Time (hour) Size (nm) 20 40 60 80 100 120 140 160 180 1 2 3 4 5 Time (hour) Size (nm)

Nanocellulose Balls

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Nanocellulose Balls – 76 nm AFM Images

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SLIDE 19

Nanocellulose Balls

S-800 FE SEM 180 nm balls 76 nm balls

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Nanocellulose Crystallinity Results 13C-CP/MAS NMR Analysis

0.70 50 – 100 nm Nanocellulose Balls Cellulose II 0.65 300 – 500 nm Nanocellulose Balls Cellulose II 0.61 Original pulp – Cellulose 1 Crystallinity index

C-1 C-4 C-2, 3, 5 C-6

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SLIDE 21

Nanocellulose Whisker-Balls:Acrylic Acid Composite Film

NanoCellulosic Structures

Latex Film

5% Cellulose Whiskers:Latex Film

5% Cellulose Balls:Latex Film

200 400 600 800 1000 1200 1400 TEA

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SLIDE 22

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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SLIDE 23

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 Community Innovative Products

“Nano-Inside”

Societal Demand for Carbon Neutral, Environmentally Friendly, Renewable and Sustainable Manufacturing Technologies

Consumer Demand Value Added Products & Materials

More Relevant Today!!! Leveraging: Research and Development Partnership Industry, Universities, Government

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SLIDE 24

arthur.ragauskas@ipst.gatech.edu ragauskas@hotmail.com

Acknowledgments GA Research Alliance IPST Industry Consortium