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SYNTHESIS AND CHARACTERIZATION OF
POLYACRYLONITRILE (PAN) AND CARBON FIBERS
Department of Polymer Engineering & TechnologyUniversity of the Punjab,
Lahore
Prof. Dr. Tahir JamilChairman
Engr. Shahzad Maqsood KhanPresenter
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Polymer
PANCarbon Fiber
PRESENTATION APPROACH
?? ?
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Polymer
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POLYMERTHE SCIENCE AND ENGINEERING OF LARGE MOLECULES
• Long chain molecules
• long molecule made up by the repetition of
small unit called monomers BUILDIGNG BLOCK
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POLYMER AT PLAY
Find Polymers in figure
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POLYMER CLASSESPolymers
OrganicInorganic
Natural
Proteins, Nucleic acids, Lignins, Polysccharides, Polyisoprene, Melanin
Synthetic
PE, PS, Nylons, PET, PVC, PU, PC, PMMA, PVAC, PP, PTFE
Synthetic
Fibrous glass, Silicon Carbide, Poly(boron nitrid), Poly(sulfur nitride)
Natural
Clays, Sands, Glass, Rock-like, Ceramics, Graphite/Diamond, Silicas
Organic/Inorganic
Siloxane, Polyphosphazenes, Polyphosphate esters, Polysilanes, Sol-gel network
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POLYMER-A-A-A-A-A-A-A-A- Homo Polymer
-A-B-B-A-B-A-A-B- Random Copolymer
-A-B-A-B-A-B-A-B- Alternating Copolymer
-A-A-A-A-B-B-B-B- Block Copolymer
-A-A-A-A-A-A-A-A- Graft Copolymer B-B-B-B-B-B-
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POLYMER
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POLYACRYLONITRILE (PAN)
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IMPORTANCE OF PANHomo polymers of Polyacrylonitrile have been used as
• Fibers in hot gas filtration systems
• Outdoor awnings
• Sails for yachts
• Fiber reinforced concrete
Mostly copolymers containing Polyacrylonitrile are
used as
• Fibers to make knitted clothing, like socks and
sweaters
• Outdoor products like tents
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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.
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POLYACRYLONITRILE (PAN)
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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)
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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
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PAN CHARACTERIZATION• FTIR (Fourier Transform Infrared Spectrophotometer)
• NMR (Neutron Magnetic Resonance)
• GPC (Gel Permeation Chromatograph)
• DSC (Differential Scanning Calorimeter)
• TGA (Thermo Gravimetric Analyzer)
• TMA (Thermo Mechanical Analyzer)
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PAN CHARACTERIZATIONFTIR
R. Setnescu, S. Jipa, T. Setnescu, W. Kappel,S. Kobayashi, Z. Osawa. IR and X-ray characterization of the ferromagnetic phase of
pyrolysed polyacrylonitrile, Carbon 37, (1999) 1–6.
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1H-NMR spectrum of the PAN
precursors
13C-NMR spectrum of the PAN
precursors
PAN CHARACTERIZATIONNMR
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PAN CHARACTERIZATIONDSC
N. Yusof and A. F. Ismail. Preparation and characterization ofpolyacrylonitrile/acrylamide-based activatedcarbon fibers developed using a solvent-free
coagulation process, International Journal of Chemical and Environmental Engineering. 1, (2010) 79-84.
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PAN CHARACTERIZATIONTGA
H. B. Sadeghi, H. A. Panahi, M. Abdouss, B. Esmaiilpour,M. N. Nezhati, E. Moniri, Z. Azizi.
Modification and Characterization of Polyacrylonitrile Fiber by Chelating Ligand for Preconcentration and Determination of Neodymium Ion in Biological and Environmental
Samples. J. APPL. POLYM. SCI. (2013) 1125-1130.
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PAN CHARACTERIZATIONTMA
T. V. Sreekumar, T. Liu, B. G. Min, H. Guo, S. Kumar, R. H. Hauge, R. E. Smalley, Polyacrylonitrile Single Walled Carbon Nanotube Composite Fibres. Adv. Mater. 16, (2004)
58-61.
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PAN CHARACTERIZATIONDMA
Temperature v/s Storage Modulus of PAN
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Temperature v/s Tanδ of PAN
PAN CHARACTERIZATIONDMA
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PAN INDUSTRIAL PRODUCTION
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POLYMER SYNTHESIS PILOT PLANT DEPARTMENT OF POLYMER ENGG. PU LHR
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POLYMER SYNTHESIS PILOT PLANT DEPARTMENT OF POLYMER ENGG. PU LHR
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POLYMER SYNTHESIS PILOT PLANT DEPARTMENT OF POLYMER ENGG. PU LHR
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POLYMER SYNTHESIS PILOT PLANT DEPARTMENT OF POLYMER ENGG. PU LHR
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PAN FIBER & CARBON FIBER
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IMPORTANCE OF PAN FIBERPAN-based fibers eventually supplanted most
rayon-based fibers, and they still dominate the
world market. In addition to high modulus fibers,
researchers have also developed a low modulus
fiber from PAN that had extremely high tensile
strength. Used in
• Sporting goods such as golf clubs, tennis rackets,
fishing rods, and skis
• Military
• Commercial aircrafts
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IMPORTANCE OF CARBON FIBER
Strength: carbon fibers tensile strength is
un-matched by any metal available
(Titanium alloys, Cr Mo, steel or Aluminum
alloys)
Weight: carbon fiber/epoxy weight per
volume is less than half that of aluminum
almost 4 times lighter than titanium
Fatigue resistance of carbon fiber
surpasses that of any other structural
material
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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
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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
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CARBON FIBERCarbon fibers are derived from one of the three
precursor materials
• PAN (Polyacrylonitrile fiber)
• PITCH
• Isotropic
• Mesophase
• Rayon
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• Melt Spinning
• Dry Spinning
• Wet Spinning
• Wet/Dry Spinning
PAN FIBER INDUSTRIAL PRODUCTION
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PAN FIBER FORMATIONPolyacrylonitrile 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%
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PAN FIBER INDUSTRIAL PRODUCTION
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PAN FIBER INDUSTRIAL PRODUCTION
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PAN FIBER INDUSTRIAL PRODUCTION
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PAN FIBER INDUSTRIAL PRODUCTION
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CARBON FIBER FORMATIONFiber 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
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CARBON FIBER INDUSTRIAL PRODUCTION
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• Oxidization
• Stress graphitization of
Polyacrylonitrile based carbon fiber
• Carbonization (graphitization)
PAN FIBER INDUSTRIAL FORMATION
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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.
PAN FIBER INDUSTRIAL FORMATION
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CARBON FIBER INDUSTRIAL PRODUCTION
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.
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CARBONIZATION (GRAPHITIZATION)
• Involves heating the fibers up to 3000 oC in an inert atmosphere.
• Fibers are now nearly 100 % carbon
CARBON FIBER INDUSTRIAL PRODUCTION
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When we heat Polyacrylonitrile, the heat causes the cyano repeat units to form
cycles…
CARBON FIBER FORMATION CHEMISTRY
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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.
CARBON FIBER FORMATION CHEMISTRY
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When the temperature increases from 600 up to 1300 oC, the ribbons will
themselves join together to form even wider ribbons like this:
CARBON FIBER FORMATION CHEMISTRY
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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.
CARBON FIBER FORMATION CHEMISTRY
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FIBER CHARACTERIZATION• 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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PAN TO CARBON FIBER CHARACTERIZATIONXRD
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PAN TO CARBON FIBER CHARACTERIZATIONXRD DATA
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PAN TO CARBON FIBER CHARACTERIZATIONFTIR
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PAN CHARACTERIZATIONYOUNG’S MODULUS & TENSILE STRENGTH
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GASES RELEASED DURING PYROLYSIS OF PAN
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ELEMENTAL ANALYSIS
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PAN FIBER GRADEThe Carbonization temperature will determine the grade of fiber produced:
Carbonization Temperature (oC)
to 1000 1000 - 1500 1500 - 2000 2000 +(Graphitization
)
Grade of Carbon Fiber
Low Modulus
StandardModulus
IntermediateModulus
HighModulus
Modulus of Elasticity (GPa)
to 200 200 - 250 250 - 325 325 +
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CARBON FIBER GROUPINGFINAL HEAT TREATMENT TEMPERATURE
Type-I, high-heat-treatment carbon fibers (HTT)
Final heat treatment temperature > 2000C and can be
associated with high-modulus type fiber.
Type-II, intermediate-heat-treatment carbon fibers (IHT)
Final heat treatment temperature should be > = 1500C
and can be associated with high-strength type fiber.
Type-III, low-heat-treatment carbon fibers
Final heat treatment temperatures not greater than
1000C. These are low modulus and low strength materials.
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CARBON FIBER FORM PAN FIBER
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CARBON FIBER FROM PITCH
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MECHANICAL PROPERTIES OF CARBON FIBER
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OUR RESEARCH PAPER61 Journal of Pakistan Institute of Chemical Engineers Vol. XXXVII
Synthesis And Characterization of Polyacrylonitrile Copolymers
Waqar Ahmad, Shahzad Maqood Khan, Muhammad Arif Butt and Tahir Jamil*
Abstract
Polyacrylonitrile (PAN) and copolymers of PAN with monomers like MMA, BA, VA, AM,
AA, and S of varying compositions and molecular weights were prepared by emulsion
polymerization in a continuous aqueous phase in the presence of sodium lauryl sulfate
as emulsifier and potassium persulfate/ammonium persulfate as initiator. The molecular
weights were determined from the dilute solution viscosity using Mark-Houwink
equation. The chemical compositions of copolymers were characterized by FT-IR
spectroscopy.
Keywords: Polyacrylonitrile (PAN), Polymer, Emulsion polymerization, FT-IR
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CONCLUSIONS OF OUR WORK• The synthesis of homo and copolymers of PAN via emulsion polymerization was
successfully achieved
• Maximum yield of 94.5 % for Polyacrylonitrile (100)
• Maximum yield of 90.2 % for P(AN-co-AM-co- MAA, 96.1:3.2:0.7)
• The highest molecular weight, Mv = 144068, for copolymer P(AN-co-AM-co-
MAA, 96.1:3.2:0.7)
• followed by Mv = 75403.85 for P(AN-MMA, 96:4)
• and Mv = 75403.69 for PAN (100).
• MMA was found to be the best monomer for copolymerization of AN.
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CONCLUSIONS OF OUR WORK• As commercially available PAN precursor for carbon fiber have molecular weight
about 150000 and we have achieved 144068 MW for P(AN-co- AM-co-MAA,
96.1:3.2:0.7), this sample of PAN can be a very suitable precursor for carbon
fiber.
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ACKNOWLEGMENTWe are grateful to
• Prof. Dr. Arshad Chughtai (Chairman, Department of Textile Engineering & Technology University of
the Punjab Lahore
• Miss. Nafisa Gull (Research Officer, Department of Polymer Engineering & Technology University of
the Punjab Lahore)
• Dr. Misbah Sultan (Assistant Professor, Department of Polymer Engineering & Technology
University of the Punjab Lahore)
• Engr. Muhammad Shafiq, Engr. Aneela Sabir (Lecturer, Department of Polymer Engineering &
Technology University of the Punjab Lahore)
• Miss Saba Bahzad Khan (Lab Supervisor, Department of Polymer Engineering & Technology
University of the Punjab Lahore)
• Engr, Adnan Ahmed, Engr. Muhammad Azeem Munawar, Engr. Khurram Javed, Miss Sidra Waheed
(Research Technician, Department of Polymer Engineering & Technology University of the Punjab
Lahore)
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THANKS FOR YOUR ATTENTION !
NO QUESTIONS PLZ
BUT STILL YOU ARE WELCOME FOR
QUESTIONING