get induction presentation_21 08 12_1
TRANSCRIPT
RIL – Confidential (for internal sharing only)
RTG Hazira
Overview of Polypropylene & PP Catalyst Technology
Development
RIL – Confidential (for internal sharing only)
Outline of presentation
Overview of polymers – general aspects
Polypropylene - Versatile Polymer
Polypropylene value chain
Monomer
Catalyst technology
Polymerization Technology
Polymer Processing
RTG Hazira overview
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Polymers
Chemical Industry- Products pattern
Polymers constitute 20 % of Mega Chemical Industry
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Polymers
POLYMERS
BIO-POLYMERS
Proteins, Nucleic
acid
NATURAL
POLYMERS
Rubber, Starch,
Cellulose
SYNTHETIC
POLYMERS
Polyethylene
Nylon,PVC
Elastomers &
Plastics
Thermosets &
Thermoplastics
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Polymers
Thermoplastics can be softened or melted by heat
and reformed (molded) into another shape.
Most addition polymers are thermoplastics.
The polymer chains are held together by weak
interactions (noncovalent bonds) such as :
van der Waal’s forces,
London dispersion forces and
Dipole-dipole attractions.
These interactions are disrupted by heating, allowing
the chains to become independent of each other.
Heating and reforming can be repeated indefinitely (if
degradation doesn’t occur). This allows recycling.
Thermoplastic Polymers
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Polymers
Thermoset plastics melt initially, but on further
heating they become permanently hardened.
Once formed, thermoset plastics cannot be
remolded, and they cannot be recycled.
On heating, thermoset plastics become cross-linked
(covalent bonds form between the chains). The
cross-linked chains form a rigid network
cross-linked linear
Thermoset Plastic
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Polymers
HIGH-DENSITY POLYMERS
LOW-DENSITY POLYMERS
Linear polymers with chains that can pack closely
together. These polymers are often quite rigid.
Branched-chain polymers that cannot pack together
as closely.
These polymers are often more flexible than high-
density polymers.
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Polymers
Mode of formation
• Addition Polymerization - Polyethylene,
Polypropylene
• Condensation Polymerization - PET, Nylon 66
Mechanism of formation
• Free radical - LDPE, PVC
• Co-ordination - PP,PBR
• Ionic - Cationic, Anionic- Poly acrylonitrile
Polymers based on formation
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Polymers
CH2 CH2 CH2 CH2polyethylene
CH2 CH
CH3
polypropylene CH2 CH
CH3
polystyrene CH2 CH CH2 CH
CH2 CH
Cl
polyvinyl chloride CH2 CH
Cl
Teflon CF2 CF2 CF2 CF2
(PVC)
most common polymer
bags, wire insulation,
squeeze bottles
fibers, bottles,
indoor-outdoor carpet
styrofoam,
inexpensive molded
objects: household items,
toys
synthetic leather, clear
bottles, floor coverings,
water pipe
Addition Polymers
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Polymers
Addition Polymers
Block
Random
Graft
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Polymers- Finger prints
Catalyst & Process controlled Reflected in
Regioselectivity Melting point
Cis/Trans Isomerism Crystallization temp.
Stereoselectivity Glass Transition
temp.
Mol. Wt distributuion Modulus
Polydispersity Crystallinity
Viscosity
Morpohology
Hardness
Stiffness
Transparency
Catalysts & process dictate the property of polymer
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Polypropylene – Versatile Polymer
13
PE
PP
PS
PEEK
ABS
PC
PET
PES
Biopolymer
High Capacity
TP
Engineering
TP
Specialty
TP
Polypropylene Can Cover Area Of Other Polymers Source : Polyolefin Conf
PVC
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• Global Polymer market – 175 MMT
• Global PP market ~ 42.6 MMT (29 %)
• Global PP Growth ~ 6.4 % (mainly
driven by Asia , Africa and other
developing country)
• Indian PP , PE , PVC Consumption ~ 4.6
MMT
•
• Indian PP market ~ 1.5 MMT (34 %)
• PP Growth in India ~ 15 % (2006-07)
• RIL PP Capacity ~ 2.7 MMT
Global Demand - PO+PVC (2006)
PP 42.6 29%
HDPE 29.3 21%LLDPE 18.6 13%
LDPE 18 13%
PVC 33.5 24%
PP HDPE LLDPE LDPE PVC
India Demand - PO+PVC (2006)
PP 1530 33%
HDPE 990 21%LLDPE 650 14%
LDPE 260 6%
PVC 1220 26%
PP HDPE LLDPE LDPE PVC
Polypropylene occupy largest chunk of Market demand
*Source : A. Report 06-07
Polypropylene – Versatile Polymer
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• Propylene
• Isotactic- CH3 on one side of polymer chain (isolated). Commercial PP is 90% to 95% Isotactic
Polypropylene – Versatile Polymer
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16
•Atactic- CH3 in a random order (A- without; Tactic- order) Rubbery
and of limited commercial value.
•Syndiotactic- CH3 in a alternating order (Syndio- ; Tactic- order)
Polypropylene – Versatile Polymer
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• Differences between PP and PE are
– Density: PP = 0.90; PE = 0.941 to 0.965
– Melt Temperature: PP = 176 C; PE = 110 C
– Service Temperature: PP has higher service
temperature
– Hardness: PP is harder, more rigid, and higher
brittle point
– Stress Cracking: PP is more resistant to
environmental stress cracking
Polypropylene – Versatile Polymer
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Polypropylene Value Chain
18
Monomer
Technology
Catalyst
Technology
Polymerization
Process
Polypropylene
Product
Application
Front End
Back End
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Monomer Technology
Naphtha Cracking
Gas Cracking
FCC – Gas Oil Cracking
Propane Dehydrogenation
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Discovered that a combination of certain transition
metal compounds and organo metallic compounds
polymerize ethylene in 1953
Discovered the synthesis of
stereo regular polymers in
1954
The Nobel Prize in Chemistry 1963
TiCl3 / AlEt2Cl (Natta) 1st Gen
2nd Gen
3rd Gen
4th Gen
5th Gen
TiCl3 / AlCl3 / isoamylether / AlEt2Cl
TiCl4 / MgCl2 / Alkyl Benzoate & Ext. Donors
TiCl4 / MgCl2 / Alkyl Phthalate & External Donors
TiCl4 / MgCl2 / 1,3-diethers as Internal Donors
Low activity, Deashing required
Low activity, Deashing required
Medium activity, Actactic removal not required
High activity, No additional process required
High activity, No External donor required
Karl Ziegler
Giulio Natta
Catalyst Technology
21
Z-N Catalyst System accounts for ~95 % of Polypropylene Production globally
Zr/HfX3
Me
Me
Catalyst Technology
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Support
TiCl4 Solvents
Catalyst
Internal
Donor
Titanation
RCT
Aluminum
Alkyl (Co- Catalyst) Propylene and/or
Ethylene Activation/
Polymerzn.
PP
Product
Catalyst External
Donor
• Multiple & Complex
Chemical , Physical reactions
• Active site incorporation on
support with intenral donor
• Activation of Active Species
by Alkylation
• Monomer polymerization for
polymeric product
Magnesium Aloxide
Alcoholated MgCl2
Magnesium Carboxlate
Ethyl Benzoate
Di-isoalkyl Phthalates
Monoester Catalyst
Diester Catalyst
Ether based Catalyst
O,P,N based Donor
Silane based Donors
COOR1
OR2
X
Y
X
Y
OCH 3SiH3CO
Catalyst Technology
• Catalytic cycle for polymerization of Olefin - Cossee-Arlman mechanism
• Direct insertion of olefin across M-alkyl bond
Catalyst Technology
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1. Replacement of one Cl by alkyl group of Al alkyl
2. Bonding of Propylene to a vacant site
3. Insertion of propylene into Metal-alkyl bond- Initiation
4. Creation of vacant site for propylene adsorption
5. Repetition of steps 2,3 & 4 leading to chain growth/propagation
6. Catalyst configuration decides the configuration of added
propylene
7. Termination of polymer chain with hydrogen- Termination
Catalyst Technology
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Polymerization Technology
• Conventional Slurry Process
• Bulk Processes – Spheripol
– Hypol
– Atofina
• Gas Phase Fluidised Bed Processes – Unipol
– Novolen
– Innovene
– Chisso
– Sumitomo
• New Generation Processes – Borstar
– MZCR (Spherizone)
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• Polymerisation in CSTR / 60-80°C / 5-15 bar
• Hydrocarbon diluent (butane, hexane, heptane or iso-octane)
• Polymer formed as suspension
• Slurry flashed to recover monomer
• Residual catalyst deactivation and atactic removal
• Polymer powder separated in centrifuge, dried, compounded and pelletised
Drawbacks
• Purification and recycle of diluent expensive
• Catalyst deactivation & atactic removal steps involved
• Products range limited
Polymerization Technology
Conventional Slurry Process
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Polymerization Technology
Conventional Slurry Process
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Polymerization Technology
• Similar to Slurry process
• Liquid propylene as reaction medium
• High monomer concentration, hence higher reaction rate
& yield
• Upto 50-60% suspension in liquid monomer
• Impact copolymer in Gas Phase reactor
Bulk process
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Polymerization Technology
• Maximum number of plants worldwide
• High Yield High Stereospecific (HYHS) MgCl2 supported
Z.N. catalyst originally developed by Montedison and Mitsui
• No catalyst removal stage
• Two stage process - single or twin bulk loop configuration
with Gas Phase reactor in series
• Polymerisation at 60-80°C & 30-40 bar
• Very wide MFI range : 0.1 to >1500
• Spherical polymer grains with no pelletisation - Adipol
Bulk process
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Polymerization Technology
Bulk process
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Polymerization Technology
Unipol – Dow (UCC)
Novolen - NTH : ABB Lummus + Equistar (BASF)
Innovene – BP (Amoco)
Chisso
Sumitomo
Gas phase process
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Polymerization Technology
• Combines fluid bed reactor technology of Union Carbide and
supported Z.N., Super High Activity Catalyst (SHAC) of Shell
• No deashing and atactic removal steps
• Polymerisation at 60-80°C & 35 bar
• All types - Homo, Random and Impact Copolymer produced
using identical Gas Phase reactors
• MFI of 0.6 - 30 can be produced in reactor with improvement
in catalyst by Dow
• New grades (IMPPAX) with good high impact/stiffness
balance & rubber contents up to 35%
Gas phase process _ Unipol
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Polymerization Technology
Gas phase process _ Unipol
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Polymerization Technology
• Originally developed by BASF
• Mechanically agitated reactors to maintain fluidised bed for
Homo, Random and Impact Copolymers
• Silica supported Z.N.catalyst originally used
• Polymerisation at 60-105°C & 20-35 bar
• Unique extruder design with catalyst deactivation by
addition of water to extruder
• Stiff and tough Homopolymer grades
• Process can make super high Impact Copolymers
• Wide range of reactor MFI (0.3 to >100)
• Use of Metallocene allows high MFI grades (upto 1200) for
Nonwoven application
Gas phase process _ Novolene
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Polymerization Technology
Gas phase process _ Novolene
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Polymerization Technology
Gas phase process _ BP Innovene
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Polymerization Technology
• Borstar - Borealis
• MZCR - Spherizone - Basell
New Polymerization process
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Polymerization Technology
• Borstar PE technology extended to PP
• Dual reactor system - Slurry loop followed by Gas Phase
reactor
• Liquid Propylene diluent
• MgCl2 supported Z.N.catalyst
• Process operating at 70-80°C
• High ethylene (10%) random copolymers
• High stiffness & improved randomness in copolymer grades
• High MFI reactor grades
• Very narrow to very broad MWD capability
• Better creep resistance, higher melt strength and improved
processability
New Polymerization process _ Borstar PE
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Polymerization Technology
New Polymerization process _ Borstar PE
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Polymerization Technology
Latest process invented by Basell
Process technology derived from catalytic
cracking
Two separate zones within one reactor, separated
by a layer of barrier fluid
High productivity per unit volume of the reactor
Very broad or very narrow MWD possible
Flexural modulus upto 2,500 MPa,
Extremely high melt strength
Low seal initiation temperatures
New Polymerization process _ Spherizone Basell
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Polymerization Technology
New Polymerization process _ Spherizone Basell
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Polymerization Technology
Polymerization process _Distribution (2004)
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Polypropylene
Packaging
Infrastructure
Agriculture
Consumer Goods
Health Care
Conservation of
Resources
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44
Mechanical Properties of PP
Mechanical Properties of PolypropylenePolypropylene LDPE
(For Comparison)
HDPE
(For Comparison)
Density 0.90 0.91- 0.925 0.959-0.965
Crystallinity 30% to 50% 30% to 50% 80% to 91%
Molecular Weight 200K to 600K 10K to 30K 250K to 1.5M
Molecular Weight
Dispersity MWD
(Mw/Mn)
Range of
MWD for
processing
Range of MWD
for processing
Range of MWD
for processing
Tensile Strength,
psi
4,500 – 5,500 600 - 2,300 5,000 – 6,000
Tensile Modulus,
psi
165K – 225K 25K – 41K 150K – 158 K
Tensile
Elongation, %
100% - 600% 100% - 650% 10% - 1300%
Impact Strengthft-lb/in
0.4 – 1.2 No break 0.4 – 4.0
Hardness, Shore R80 - 102 D44 – D50 D66 – D73
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45
Physical Properties of PP
Physical Properties of Polypropylene
Polypropylene LDPE HDPE
Optical Transparent to
opaque
Transparent to
opaque
Transparent to opaque
Tmelt 175 C 98 – 115 C 130 –137 C
Tg -20 C -100 C -100 C
H20
Absorption
0.01 – 0.03 Low < 0.01 Low < 0.01
Oxidation
Resistance
Low, oxides
readily
Low, oxides
readily
Low, oxides readily
UV Resistance Low, Crazes
readily
Low, Crazes
readily
Low, Crazes readily
Solvent
Resistance
Resistant
below 80C
Resistant below
60C
Resistant below 60C
Alkaline
Resistance
Resistant Resistant Resistant
Acid
Resistance
Oxidizing
Acids
Oxidizing Acids Oxidizing Acids
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46
Processing Properties of Polyethylene
Processing Properties
Polypropylene LDPE HDPE
Tmelt 175 C 98 – 115 C 130 –137 C
Recommended Temp
Range
(I:Injection, E:Extrusion)
I: 400F – 550F
E: 400F – 500F
I: 300F – 450F
E: 250F – 450F
I: 350F – 500F
E: 350F – 525F
Molding Pressure 10 -20 psi 5 – 15 psi 12– 15 psi
Mold (linear) shrinkage
(in/in)
0.010 – 0.025 0.015 – 0.050 0.015 – 0.040
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Polymer Processing
EXTRUSION
SINGLE SCREW
EXTRUDER
TWIN SCREW
EXTRUDER
• FILM
• TAPES
• PIPES
• FILAMENTS
• INJECTION MOULDING
• BLOW MOULDING
COMPOUNDING WITH
FILLERS / PIGMENTS.
REGID PVC PIPES
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Polymer Processing
BIAXIALLY ORIENTED PP(BOPP) FILM:
Process : Double bubble (Blown film), Tenter
frame (Cast film).
Two directional stretching.
Applications : Print Paper lamination, Adhesive
tapes, synthetic paper, Confectionery and
Cigarette wrappings.
Tubular Quenched PP(TQPP) film:
Process : Inverse bubble, water quenching
Applications : Textile pkg., Confectionery items
pkg., Auto spare parts pkg. etc.
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Polymer Processing
RAFFIA & MONOFILAMENTS: (Extrusion)
Machine : (Screw Dia, Oven/Hotplate)
DIE Width, Spinneret
Process : Stretch Ratio, Line Speed.
Materials : HDPE & PP
Products:
Raffia : Bags for cement/fertilizer/food
grains, sugar/polymer Pkg. & Tarpaulin
appln.
MF : Mosquito & Fishing nets, Ropes,
Geo- textiles
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Polymer Processing
RAFFIA & MONOFILAMENTS
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INJECTION MOULDING :
Machine (tonnage / shot wt.)
Mould (cavity , punch)
IM process / cycle
Products:
HDPE : Crates, Luggages, caps & closures, Buckets, Household articles, Ice trays etc.
PP/PPCP :Furniture, Crates, Luggage, Automotive components, Tooth brush, Industrial products, Textile components, Household articles etc.
PPRCP : Transparent containers, Medical products.
LD/LLD : Caps & closures.
PVC : Pipe fittings, footwears.
Polymer Processing
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Polymer Processing
– BLOW MOULDING : (Extrusion-Small vol.) • Machine (Volume, Station)
• Die/Punch & Mould
• BM Process / Cycle
– Products :
HDPE : Containers for Lube oil, Vegetable oil, Cosmetics, Pesticides, Pharmaceuticals, Healthcare.
PP : Pharmaceutical & cosmetic bottles.
LD/LLD : Toys, IV bottles, Flexible containers.
PVC : Storage containers.
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RTG Hazira
IN
Technology
& Products
Organometallic/
Inorganic
Chemistry
Organic
Chemistry
Polymer
Science
Polymerization
Science
Catalyst &
Chemical
Process
Catalysis
&
Material
Science Analytical
Science
Patents ,Trademark
Publications &
Classified documents
RTG-Hz: FBIV Process
Out
FOCUS
BRILLIENCE
INNOVATION
VALUE
R&D Facilities
RTG-Hz: Facilities
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(100)
C
O OC2H5
C
O OC2H5
MgCl2 Matrix
~85 mol%
Titanium chloride fragments
~10 mol%
(100)(100)
C
O OC2H5
C
O OC2H5
(100)
C
O OC2H5
C
O OC2H5
MgCl2 Matrix
~85 mol%
Titanium chloride fragments
~10 mol%
(100)
Morphology controlled
Precursor
Precursor
Pro-catalyst
Polyolefin Catalyst Technologies
Procatalyst Cocatalyst External Donor
Morphology controlled
Procatalyst
Mg(s) + Alcohol
Controlled
morphology
Mg(alkoxide)
TiCl4(excess) + Lewis Base
Controlled morphologyActive MgCl2
Supported catalystMg(s) + Alcohol
Controlled
morphology
Mg(alkoxide)
TiCl4(excess) + Lewis Base
Controlled morphologyActive MgCl2
Supported catalyst
Mg(s) + Alcohol
Controlled
morphology
Mg(alkoxide)Mg(s) + Alcohol
Controlled
morphology
Mg(alkoxide)
IP- WO
2009/1300707A2,
IN/916/MUM/2008,
IN/1691/MUM/2009
Advance Donor
Technology
External Donor
HomoRandomICP
COOR1
OR2
X
Y
X
Y
Catalyst Technology Advancement
OCH 3SiH3CO
TiCl3 Technology
Supported Titanium
Technology
Advance Donor Technology
V
a
l
u
e
E
n
h
a
n
c
e
m
e
n
t
Single SiteTechnology
Specialty PP
HomoRandomICP
COOR1
OR2
X
Y
X
Y
Catalyst Technology Advancement
OCH 3SiH3CO
TiCl3 Technology
Supported Titanium
Technology
Advance Donor Technology
V
a
l
u
e
E
n
h
a
n
c
e
m
e
n
t
Single SiteTechnology
Specialty PP
HomoRandomICP
COOR1
OR2
X
Y
X
Y
Catalyst Technology Advancement
OCH 3SiH3CO
TiCl3 Technology
Supported Titanium
Technology
Advance Donor Technology
V
a
l
u
e
E
n
h
a
n
c
e
m
e
n
t
Single SiteTechnology
Specialty PP
HomoRandomICP
COOR1
OR2
X
Y
X
Y
Catalyst Technology Advancement
OCH 3SiH3CO
TiCl3 Technology
Supported Titanium
Technology
Advance Donor Technology
V
a
l
u
e
E
n
h
a
n
c
e
m
e
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t
Single SiteTechnology
Specialty PP
Combination of
ester and
ethers donors
IP - IN/539/MUM/2008
IN/540/MUM/2008
IN/541/MUM/2008
IN/1074/MUM/2008
WO 2009/ 116056 A2, WO
2009/16057A2 ,WO 2009/
141831
In-house Technology Development
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IP
• Indonesia Patent No:
WOO.2002.01688 / 26 Jul 2002
• - Korea Patent No- KR533442 / 26 Jul
2002
• - Philippines Patent No- 1-2002-
000064 / 30 Jan 2002
• - Australia Patent No- AU3221501A /
25 Nov 2000
• - Australia Patent No.
AU2003241147A1
• - EP - 008873482.5
• - European Patent No.
2.283048(A2)/16 Feb 2011
1. 1691/MUM/2009 / 22 July 2009
2. 1981/MUM/2010) / 12 Jul 2010
3. 2844/MUM/2010) / 12 Oct 2010
4. 762/MUM/2011 / 17 Mar 2011
5. 1123/MUMNP/2005
6. 1744/MUMNP/2006 / 24 Jun
2006-
7. 1894/MUM/2009 / 18 Aug 2010
8. 539/MUM/2008 / 18 Mar 2008
9. 541/MUM/2008 / 17 Mar 2008
10. 1074/MUM/2008 / 21 May 2008
11. 540/MUM/2008 / 14 Mar 2008
12. 468/MUM/2011 / 13 May 2011
13. 1706/MUM/2011 - 10 June 2011
14. 1424/MUM/2011 / 09 May 2011
15. 916/MUM/2008 / 25 Apr 2008
16. 1691/MUM/2009 / 22 July 2009
• PCT No WO/2009/116056A2 / 24
Sept 2009
• PCT No WO/2009/1418314 . 25
Aug 2008
• PCT No WO/2009/116057 A2 / 24
Sept 2009
• PCT No. WO 2009/128087/A2 / 22
Oct 2009
• PCT No WO/2009/130707 A2 / 29
Oct 2009
• PCT Application -
PCT/IN2010/000809
• PCT Application -
PCT/IN2010/000809
• PCT : WO 2002/44220 A1 / 06
Jun 2002
• PCT No. WO 2004/089998 A1 /
21 Oct 2004
• PCT No. -WO 2005/077990 A1 /
25 Aug 2005
• PCT/IN2011/000028 / 14 Jan 2011
• PCT/IN2011/000029 / / 14 Jan
2011
• US Patent No 2011/0003952 A1 06 Jan 2011
• US Patent No 2011/0046326 / 24 Feb 2011
• US Patent No 2011/0015355 A1 / 20 Jan
2011
• US Patent No. US6841633 B2 / 11 Jan 2005
• US Patent No. US7265074 B2 / 04 Sept
2007
• US Patent No. - US20070260099 A1 / 08
Nov 2007
• US patent 2011/0054129 A1 / 03 Mar 2011
>51 Patents/Applications
PCT India
Europe/Austalia/Korea/ Indonesia
USA
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Awards & Recognitions
In-house Technology Development
ICC - 2010
Indian Science Congress - 2005 Golden Peacock - 2008 ICC Acharya PC Ray - 2008
Indira Innovation - 2009 FICCI - 2009 R&D Lab of Year, USA - 2009
Arch of Excellence - 2009 FGI - 2009
National Technology Award 2011 Vasvik Research Award - 2011
Rashtriya Rattan - 2009
Special Mention Lab of Year Award
Reliance Technology Group Hazira : Polymer R&D
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Thank You!
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to
developing
technology”
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