Pan 1

PRESENTATION APPROACH
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Carbon
Fiber
Polyme
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PAN
• Polyacrylonitrile (PAN), also known as Creslan 61,
is a synthetic, semicrystalline organic polymer
resin, with the linear formula (C3H3N)n.
• Though it is thermoplastic, it does not melt under
normal conditions.
• It degrades before melting. It melts above 300 °C
if the heating rates are 50 degrees per minute or
above.
PAN
• Almost all polyacrylonitrile resins are copolymers made
from mixtures of monomers with acrylonitrile as the
main component.
• It is a versatile polymer used to produce large variety
of products including ultra filtration membranes,
hollow fibers for reverse osmosis, fibers for textiles,
oxidized PAN fibers.
•
PAN
• PAN fibers are the chemical precursor of high-quality carbon fiber.
• PAN is first thermally oxidized in air at 230 degrees to form an
oxidized PAN fiber and then carbonized above 1000 degrees in
inert atmosphere to make carbon fibers found in a variety of both
high-tech and common daily applications
• such as civil and military aircraft primary and secondary structures,
missiles, solid propellant rocket motors, pressure vessels, fishing
rods, tennis rackets, badminton rackets & high-tech bicycles.
• It is a component repeat unit in several important copolymers,
such as styrene-acrylonitrile (SAN) and acrylonitrile
butadiene styrene (ABS) plastic.
PAN
• Polyacrylonitrile (PAN), a synthetic resin prepared by
the polymerization of acrylonitrile.
• A member of the important family of acrylic resins, it
is a hard, rigid thermoplastic material that is resistant
to most solvents and chemicals, slow to burn, and of
low permeability to gases.
• Most polyacrylonitrile is produced as acrylic and
modacrylic fibre, a common substitute for wool in
clothing and home furnishings.
PAN
• Acrylonitrile (CH2=CHCN) is obtained by reacting propylene
(CH2=CHCH3) with ammonia (NH3) and oxygen in the presence of
catalysts.
• It is a flammable liquid that is highly toxic if ingested and is a

known carcinogen; strictly regulated procedures are required for its
handling and disposal.
• Acrylonitrile monomers (single-unit molecules) are suspended,

almost always in combination with other monomers, as fine
droplets in water and are induced to polymerize to PAN through
the action of free-radical initiators.
PAN
• The acrylonitrile repeating unit of the polymer
has the following structure:
PAN
• Owing to the formation of strong chemical bonds
between the nitrile (CN) groups, the polymer
molecules resist most organic solvents and do not
melt without decomposing.
• In most cases the polymer is dissolved in special
solvents and spun into acrylic fibres, which are defined
as fibres that contain 85 percent or more of PAN.
• Because PAN is difficult to dissolve and is highly
resistant to dyeing, very little fibre is produced
containing PAN alone.
PAN
• On the other hand, a copolymer containing 2 to 7 percent
of a vinyl comonomer such as vinyl acetate can be solution-
spun readily to fibres that soften enough to allow
penetration by dyestuffs.
• Acrylic fibres are soft and flexible, producing lightweight,
lofty yarns.
• Such properties closely resemble those of wool; hence, the
most common use of acrylics in apparel and carpets is as a
wool replacement—for example, in knitted wear such as
sweaters and socks.
•
PAN
• Acrylics can be sold at a fraction of the cost of
the natural fibre, and they offer better sunlight
resistance, mildew resistance, and resistance
to attack by moths.
• Acrylic fibres are also used as precursors for
the production of carbon and graphite fibres,
as replacements for asbestos in cement, and
in industrial filters and battery separators.
POLYACRYLONITRILE (PAN)
• In 1893 Acrylonitrile was prepared by
reacting Propylene with Ammonia
(NH3) and oxygen in the presence of
catalysts.
• PAN is a vinyl polymer and a derivative
of the acrylate family of polymers.
• It is made from acrylonitrile monomer
through suspension methods using
free-radical initiators.
POLYACRYLONITRILE (PAN)
PAN LAB SYNTHESIS
• Polymerization of acrylonitrile (AN) by
redox method
• Flask or lab reactor
• Nitrogen atmosphere
• Fitted with a condenser
• Reaction medium (Dimethylsulfoxide
(DMSO) solvent or water)
PAN LAB SYNTHESIS
• Emulsifier ( e.g Sodium bisulfite (SBS) )
• Initiators ( e.g Potassium Persulfate (KPS),
Azodiisobutyronitrile (AIBN), Itaconic acid (IA) )
• Time 1–3.5 hr
• Precipitation
• Filtration
• Washing ( methanol and deionized water etc)
• Drying under vacuum till a constant weight
PAN INDUSTRIAL PRODUCTION
POLYMER SYNTHESIS PILOT PLANT
DEPARTMENT OF POLYMER ENGG. PU LHR
PAN FIBER & CARBON FIBER
IMPORTANCE OF CARBON FIBER
Carbon fiber parts will be lighter and
stronger. Because of such properties
you find this technology used in
• Aviation
• Sports
• High-end racing and
• Snowmobiles
IMPORTANCE OF CARBON FIBER
Yield strength: carbon fiber has a very high
yield strength allowing it to flex under extreme
loading and return to its original shape
Corrosion: carbon fiber/epoxy is extremely
resistant to corrosion
CARBON FIBER
Carbon fibers are derived from one of the three
precursor materials
• PAN (Polyacrylonitrile fiber)
• PITCH
• Rayon
PAN FIBER INDUSTRIAL PRODUCTION
• Melt Spinning
• Dry Spinning
• Wet Spinning
• Wet/Dry Spinning
PAN FIBER FORMATION
Polyacrylonitrile fibers were produced by
wet-spinning.
The coagulation bath is normally
• DMSO/H2O system,
• Bath temperature is 60°C
• Bath concentration is 65% (namely,
DMSO/H2O=65/35(wt/wt))
• Bath minus stretch ratio is –10%
CARBON FIBER FORMATION
Fiber changing color. The white
PAN strands at the bottom pass
through the air heated oven and
begin to darken. Quite quickly
they turn to black
CARBON FIBER INDUSTRIAL PRODUCTION
PAN FIBER INDUSTRIAL FORMATION
• Oxidization
• Stress graphitization of
Polyacrylonitrile based carbon fiber
• Carbonization (graphitization)
PAN FIBER INDUSTRIAL FORMATION
Oxidization
• This produces an oxidized ladder polymer
structure approximately parallel to the fiber
axis which may be regarded as the template
for the formation of the oriented carbon fiber.
• Oxidation involves heating the fibers to around
300 oC in air. This evolves hydrogen from the
fibers and adds less volatile oxygen.
• The polymer changes from a ladder to a stable
ring structure, and the fiber changes color
from white though brown to black.
Stress Graphitization of Polyacrylonitrile

Based Carbon Fiber
• Carbon fiber can be made by the
pyrolysis of organic polymer fiber
precursors. The strength of PAN carbon
fiber declines when heated above
1,200° C.
• Therefore increasing strength with
Young's modulus can be obtained if
stress is applied to the fiber at
graphitizing temperatures.
CARBONIZATION (GRAPHITIZATION)
• Involves heating the fibers up to 3000
o
C in an inert atmosphere.
• Fibers are now nearly 100 % carbon
CARBON FIBER FORMATION CHEMISTRY
When we heat Polyacrylonitrile, the heat causes the cyano repeat units to form
cycles…
At higher temperature, carbon atoms kick off their hydrogen, and the rings become
aromatic. This polymer is a series of fused pyridine rings. This expels hydrogen gas,
and gives us a ribbon-like fused ring polymer.
When the temperature increases from 600 up to 1300 oC, the ribbons will
themselves join together to form even wider ribbons like this:
More nitrogen is
expelled and the
ribbons are really
wide, and most of
the nitrogen is
gone, leaving us
with ribbons that
are almost pure
carbon in the
graphite form.
FIBER CHARACERIZATION
• XRD (X Ray Diffraction)
• SEM (Scanning Electron Microscopy)
• DSC (Differential Scanning Calorimeter)
• TGA (Thermo Gravimetric Analyzer)
• DMA (Dynamic Mechanical Analyzer)
• UTM (Universal Testing Machine)

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PRESENTATION APPROACH

• It is a flammable liquid that is highly toxic if ingested and is a

• Acrylonitrile monomers (single-unit molecules) are suspended,

Stress Graphitization of Polyacrylonitrile

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