Ldpe and LLdpe
Transcript of Ldpe and LLdpe
© 2005 NOVA Chemicals Corporation
SPE Polyolefins Conference 2005Low Density and Linear Low Density
Polyethylene Presentation
Presented by J. BayleyNOVA Chemicals Corporation
Note: The content of this presentation is intended for basic learning, the content may not describe or encompass all aspects of materials and processes
© 2005 NOVA Chemicals Corporation
Overview of Presentation Topics• Feedstock for the Manufacture of Polyethylene
• Polyethylene Basics
Unit 1 - LDPE• Manufacturing Processes• Properties• Applications• Future for LDPE
Unit 2 - LLDPE• Molecular Information• Comonomer Information• Properties• Catalyst vs Properties• Manufacturing Processes• Applications• Future of LLDPE
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Natural Gas to Ethane to Ethylene….
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Ethane Supply System
Gas Plant PipelineGas Field
ReprocessingPlant Ethane
PetrochemicalIndustry
Energy MarketsResidueNatural Gas
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Natural Gas Components
Pipeline System ExportPost Gas Plant Post Straddle Plant
C1 Methane 90 – 100% > 98%C2 Ethane 3 – 10% < 2%C3 PropaneC4 Butane < 1% 0C5+ Pentane plusH20 Water 0H2S Sulphur 0CO2 Carbon dioxide 2% < 2%
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Gas Plant - Separate Components
Reinjected underground
Liquids Pipeline
Natural Gas Pipeline
Methane / Ethane / Carbon Dioxide Nitrogen / Propane / B
utane
Pentanes
Butane / Pentanes
Ethane / Propane
Water
Natural Gas Field
Contains many components in varying proportions
MethaneEthane
PropaneButanePentanes Water
NitrogenCarbon Dioxide
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Pentane Plus
Propane
Natural Gas to Fuel Markets
Methane
Deh
ator
Turb
o-ex
pand
er
WaterN
atur
al G
as
Ethane& C02
Confidential
Butane
Pipeline Straddle PlantExtraction andFractionation
ydr
Dem
etha
than
prop
a
utan
nize
r
De-
eiz
er
De-
nize
r
De-
biz
er
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Ethylene Manufacturing from Ethane
Ethane (C2 H6)
H
H C H
H
C HH
H
C H
H
C H
H2 Co-products800° C
then fractionate -160° C Ethylene (C2 H4) hydrogen
• In simple terms Ethane is converted into Ethylene (thermal decomposition) at high temperature in a steam furnace or cracker
• Refrigeration is used to separate the various components, co-products, etc.
• The furnace and auxiliary components are designed to efficientlyproduce as much Ethylene as possible and as few co-products as possible
• Co-Products such as Hydrogen, CO2 etc. can be sold for other uses
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Brief History of Polyethylene• PE synthesis discovered accidentally in 1932 by Imperial Chemical
Company (ICI) Scientists• First High Pressure LDPE plant built in 1939• In 1953, large advancements were made by Scientist Carl Ziegler,
inventor of a new catalyst system. A scientist named Giulio Natta also shares credit for this catalyst development
• Known today as the Ziegler-Natta Catalyst (Z/N), this catalyst facilitated polymer synthesis at lower temperatures and pressures -High Density Polyethylene (HDPE) materials were introduced soon after
• In the late 1970’s LLDPE materials were introduced to the market• Significant Catalyst advances since that time with the advent of
single-site catalysts
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Polyethylene is ...• A polymer of ETHYLENE or a copolymer of ethylene
and a comonomer• ETHYLENE - a gas composed of two carbons and four
hydrogen molecules. Formula: C2H4 The monomer unit for polyethylene forms the backbone of the compound:
H2C=CH2
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Some Basic Definitions
• Monomer - A chemical compound that can undergo polymerization. The basic building block of a polymer
• Comonomer - One of the constituents of a copolymer
• Copolymer - A product of copolymerization
• Copolymerization - Polymerization of two different monomers
• Homopolymer - Manufactured with no comonomer, with ethylene only
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Practical Illustration of Polyethylene Designations
LDPE (0.917 to 0.935 g/cc)
HDPE(0.955 to 0.970 g/cc)
LLDPE(0.905 to 0.955 g/cc)
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Polyethylene DesignationsPolyethylene is classified by density ranges, as defined by ASTM:• LDPE Type I 0.910 - 0.925 g/cc• MDPE Type II 0.926 - 0.940 g/cc• HDPE Type III 0.941 - 0.960 g/cc (Copolymer)• HDPE Type IV >0.961 g/cc (Homopolymer)
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Unit 1
PE Introduction and LDPE Overview
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LDPE• Molecular Structure LDPE - Long Chain Branching (LCB)
results in unique polymer properties
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LDPE Manufacturing Processes
Two main LDPE manufacturing processes in use:
• High Pressure Tubular Reactors• High Pressure Autoclave Reactors
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LDPE Tubular Reactors (Simplified)• A tubular LDPE Reactor is a long heat exchanger• Free Radical polymerization uses Peroxide initiators or Oxygen to
promote polymerization reactions• Ethylene is circulated through a compressor - the main
pressurization of the feed stream is accomplished by a hyper compressor
• Initiators are introduced at various points along the length of the tube - Zone temperatures are accurately controlled
• No backmixing takes place in the tubular system, residence time is limited/short
• The exothermic heat of reaction is removed via water jackets on the outside walls of the tube
• Upon exiting the reactor the material passes through medium pressure and low pressure separators (separates Ethylene from PE), PE moves to the extruder
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Resin ManufacturingHigh Pressure Tubular
PrimaryCompressor
SecondaryCompressor
PREHEATER
TUBULAR REACTOR
Initiator
KnockoutPots
WaxDrum
To Disposal
SEPARATOR
Gear Pump andPelletizer
HOPPER
RAWPRODUCT
SILO
Telogen
Coolers
To Finishing
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LDPE Autoclave Reactors (Simplified)• Free radical type of polymerization uses Peroxide initiators typically• System utilizes a stirred cylindrical vessel• Ethylene feed gas and Peroxide are introduced to a compressor and then
pumped with Peroxide initiator into the stirred autoclave vessel• Proprietary designs baffle or partition the reactor into discreet zones
enabling control of molecular species and amount of LCB of polymer in these zones
• Backmixing does take place in the autoclave system• Walls of the autoclave unit are thick to accommodate high pressure -
Heat of reaction is removed by the introduction of fresh feed• Upon exiting the reactor the material passes through medium pressure
and low pressure separators (separates Ethylene from LDPE polymer)• Polymer enters the pelletization process to be pelletized
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Resin ManufacturingHigh Pressure Autoclave
PrimaryCompressor
SecondaryCompressor
Telogen VAMonomer MA
Monomer
REACTOR SEPARATOR
VoluntaryPurge
DEPROPANIZER
DEMETHANIZER
C2
SPLITTER
HOPPER
Gear Pump andPelletizer
HourlyHold-UpHoppers
RAWPRODUCT
SILO
To Finishing
Ethane toFlare
Solvent/MonomerRemoval
C2
< C3Methaneto Flare
Initiator
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Comparison of High Pressure Autoclave and Tubular LDPE Manufacturing Processes
Information Autoclave Tubular
Length 20 ft Up to 1 mile
Internal Diameter 3 ft 1-3 inches ID
Rx Temperature Range (°F) 350-500 350-600
Pressure within Rx (PSI) 15000-30000 20000-50000
Initiator Types Organic Peroxide Organic Peroxide or Oxygen
Typical Polymer Conversion Ranges per pass
Approx. 22% (varies with product mix)
Approx. 35% (varies with product mix)
Back Mixing Capability Yes No
General Observation More precise tailoring of MW, MWD and Long chain branching (LCB)
Less capable of molecular tailoring and less uniform long
chain branching (LCB)
General Observation Comb-like LCB structure Root-like LCB structure
(Note: This table provides general information. Technology may exist that is not encompassed by or include in this table. The information is intended for basic learning purposes only.)
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Properties of LDPE Materials LDPE Materials
Softness Softer and more pliable than other PE types
Permeability Higher, due to long chain branching and lower % crystallinity
Clarity Available in high clarity for film applications - Improves clarity of LLDPE when blended with LDPE in low amounts
Processing Shear thins in extrusion - processes easily at lower amps and pressures relative to LLDPE or HDPE
Equipment Needs Screw/Die designed for LDPE required if extruding 100% LDPE
Melt Strength Much higher than LLDPE due to presence of long chain side branched molecules - (Important for film blowing, foam etc.)
Other Pros Less prone to melt fracture than LLDPE or HDPE
Suitability as a Blend Resin Good, commonly used, can be detrimental to physical properties-LDPE is generally blended to improve ease of extrusion, increase
melt strength or improve clarity of the end product
Shrink Properties Possesses desirable biaxial shrink properties for shrink film
Limitations Absolute physical properties lowest in class - extensional limitations or drawdown limitations exist - LLDPE and HDPE
can be drawn much thinner in blown or cast film processes
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LDPE Applications• LDPE is still an important PE type• The unique attributes of LDPE due to LCB provide
desirable properties for some specific product applications• LDPE is used at 100% in some applications such as
conventional Shrink Film, Extrusion Coating, Wire and Cable Jacketing, LDPE Foam etc.
• LDPE is used as a property modifier in film and sheeting applications and is often blended with LLDPE (to improve clarity, processability, output rates, etc.)
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2002 APC-LDPE Volume by End Use Process (based on Amercian Plastics Council 2002 Data)
Extrusion Coating16%
Other Extruded Products9%
Injection Molding6%
Blow Molding1%
Other (Resellers, Compounders)
23%
Film (less than 12 mil)44%
Sheet (greater than 12 mil)1%
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LDPE Common Applications• Film Applications - Garment Films, Industrial Liner,
Lamination films, Coextruded Food Packaging, Bakery Films, Film Blends (with LLDPE) for food packaging, Shrink Overwrap, Kitchen Cling Film, etc.
• Extrusion Coating Applications - Paper Board Coating, Package Coating, Coating of other substrates (Examples foil coating, drink box coating, etc.)
• Injection Molding - Lids, Caps and Closures• Other Examples - Wire and Cable applications, PE Foam,
Pipe and Conduit, Non-abrasive films, Blow Molded squeeze bottles, etc.
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The Future of LDPE• Conventional LDPE has existed for many years and was
predicted to be replaced by LLDPE• LDPE future capacity growth is likely to be less than for
LLDPE, though demand continues to be strong for LDPE• LDPE is valued as performance modifier for extrusion
processing or to obtain desired physical properties such as clarity
• Manufacturers can be expected to push the boundaries of their processes and exploit existing technology, but significant advances in resin morphology are not widely expected to occur in this class of materials
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Unit 2
Introduction to LLDPE
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LLDPE - General Information• Linear Low Density Polyethylene (LLDPE) is made by the
copolymerization of ethylene and a comonomer- (Example: Ethylene and Octene copolymerized - can be described as
an Ethylene-Octene Copolymer)
• LLDPE is composed of long linear molecules, the main polymer chain is composed of long strings of repeating Ethylene units - Short side chains (from comonomer) link onto the main polymer chains
• LLDPE typically has no long chain branching (LCB)• LLDPE materials are typically copolymers but terpolymers and
quatropolymers have also been made• LLDPE typically has a narrow distribution of main chain
molecule lengths (LDPE and HDPE tend to be broader)
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LLDPE - Molecular Diagram• LLDPE consists of long linear molecules with short side
chain branches (SCB)• SCB length is a function of comonomer type employed
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Polyethylene Comonomers -Commonly Used
• Butene - A four carbon long moleculeFormula: C4H8
H2C=CH-CH2-CH3
• Hexene - A six carbon long moleculeFormula: C6H12
H2C=CH-CH2-CH2-CH2-CH3
• Octene - An eight carbon long moleculeFormula: C8H16
H2C=CH-CH2-CH2-CH2-CH2-CH2-CH3
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Comonomer Type - Product Properties• Short side chain branching type influences product toughness -
(Example: Butene, Hexene, Octene)• Short side chains, like those made with butene comonomer are less
effective at disrupting chain folding• Longer side chains, like those formed with hexene and octene are
longer and result in superior physical properties• Z/N catalysts tend to have more difficulty than single-site catalysts in
placing comonomer on the longer chain (higher molecular weight) portion of the polymer thus more comonomer ends up on the shorter chains
• Comonomer addition levels are used to control resin density - (Example: Increased comomomer content increases short chain branch content and results in reduced resin density)
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Effect of Comonomer Type on Physical Properties
Melt Index 1.0 1.0 1.0Density 0.919 0.918 0.920Comonomer Type butene hexene octene
Dart Impact (grams/mil) 100 200 335Low Friction Puncture (J/mm) 34 50 56Elmendorf Tear Strength MD (grams/mil 100 300 400Elmendorf Tear Strength TD (grams/mil) 300 650 710Tensile Strength MD (psi) 4800 5300 6800Tensile Strength TD (psi) 3700 4500 6400
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Prone to surface melt fracture in blown film and sheet extrusion-Process Conditions and Process aid additives are used to off-set this problemLimitations of LLDPE
High physical properties possible depending on comonomer used, catalyst used and molecular architecture- Very good elongational ability,
can be drawn down thinner as a film than LDPE, higher strength than LDPE permits downgaging
Strengths of LLDPE
Long linear molecules tend to orient highly in the machine direction-shrinkage as a result is more imbalanced relative to LDPEShrink Properties
Can be blended into LDPE where desired- Eg: Can be blended into shrink film to modify shrinkage propertiesSuitability as a Blend Resin
Much lower than LDPE due to NO long chain side branched molecules, only short chain branching generallyMelt Strength
Screw/Die designed for LLDPE required if extruding-Extruders, Screws, Dies and Air Rings need to be designed for LLDPE Equipment Needs
Stiff in shear during extrusion- Narrow molecular weight distribution, processes at higher amps and head pressures relative to LDPE Processing
Clarity not as good as for LDPE in most cases- LDPE can be blended to improve clarityClarity
Higher % crystallinity relative to LDPE-Barrier Properties dependant on part thickness and resin density to a large degreePermeability
Softer relative to HDPE but not as soft and pliable as LDPESoftness
LLDPE MaterialsProperties of LLDPE
Materials
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Catalyst Information
• Metal based catalysts facilitate the reactions required to polymerize and convert Ethylene to PE
• Z/N catalyst is in common use today though modifications and improvements have been made
• Next generation catalysts known as single-site catalysts and Metallocene catalysts also exist and are used in the production of mLLDPE, sLLDPE and HDPE
*Note: Metallocene catalysts fall into the single-site catalyst family
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Catalyst Influence on LLDPE Properties
• A conventional Z/N catalyst has a variety of active reaction sites producing varied polymer molecules
• The result is a heterogeneous distribution of molecules having:– broader distribution of molecular weight (molecular
lengths) – varied comonomer incorporation levels across the
molecular weight distribution (MWD)
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Catalyst Influence on LLDPE Properties• New advanced Z/N catalysts improve comonomer placement -
comonomer is more uniformly distributed, less bias for the low molecular weight (MW) range
• Improved comonomer placement results in improved physical properties
• MWD of LLDPE is often narrow to maximize finished physical properties
• Narrowing the MWD can make the polymer challenging to process (less shear thinning) therefore MWD is an important consideration in resin design
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Properties for Products Manufactured using Advanced Ziegler-Natta Catalyst
Hexene GasPhase Z/N
Hexene GasPhase
Advanced Z/N
OcteneSolution Z/N
OcteneSolution
Advanced Z/N
Dart Impact *
*These are typical values – advances in technology have significant improvements to product properties.
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Properties for Products Manufactured using Advanced Ziegler-Natta Catalyst
Hexene GasPhase Z/N
Hexene GasPhase
Advanced Z/N
OcteneSolution Z/N
OcteneSolution
Advanced Z/N
MD Elmendorf Tear Stength *
*These are typical values – advances in technology have significant improvements to product properties.
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Properties for Products Manufactured using Advanced Ziegler-Natta Catalyst
Melt Index 1.0 1.0 0.8 0.6Density 0.918 0.920 0.916 0.916Comonomer Type Hexene Octene Super hexene OcteneProcess Gas Phase Solution Gas Phase SolutionCatalyst Type Z/N Z/N Advanced Z/N Advanced Z/NDart Impact (grams/mil) 200 335 500 620Elmendorf Tear Strength MD (grams/mil) 300 400 400 450Elmendorf Tear Strength TD (grams/mil) 650 710 600 750Tensile Strength MD (psi) 5300 6800 6100 7400
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Single-Site Catalyst (SSC) Information
• Every catalyst reaction site is the same, thus the molecules produced are more uniform
• Every polymer molecule contains the same amount of comonomer (can result in improved properties)
• Reduction in low molecular weight polymer component historically resulted in extrusion challenges largely addressed now by resin design and extrusion equipment improvements
• Metallocene catalysts are a subset of the broader single-site family
• Single-site catalyzed materials tend to have reduced low molecular weight grease levels
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0
0.2
0.4
0.6
0.8
1
1.2
1.4
1.6
2 2.5 3 3.5 4 4.5 5 5.5 6 6.5 7
Log(mw)
dW/d
Log(
mw
).
SSC polymer MI=1.9 PD=2.3
Z/N polymer MI=5.0 PD=5.8
Molecular Weight Distribution by GPC Z/N versus SSC
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Physical and Optical Properties for Materials Made Using Single-Site Catalyst
Supplier A Supplier A Supplier B Supplier C Z/NComonomer Type octene octene hexene hexene octeneMelt Index (grams/10 minutes) 0.97 0.94 1.14 1.08 0.95Density 0.9171 0.9172 0.9168 0.9193 0.9203Melt Flow Ratio (I21/I2) 22.3 27.5 16 16.2 27.2
Amps 34 32 39 36.5 31.1Volts 156 144 142 137 143Pressure (psi) 2925 2640 3070 3120 2810Specific Power (lbs/hr./amp) 1.19 1.26 1.04 1.09 1.29Dart Impact (grams) 990 1050 1200 920 180Frictionless Puncture (J/mm) 118 93 114 91 45Elmendorf Tear MD (grams) 255 265 190 235 430Elmendorf Tear TD (grams) 325 370 330 320 730Haze (%) 2 2 3 7 1545 Gloss (%) 88 87 87 57 40Hexane Extractables (%) 0.3 0.4 0.4 0.5 1.1Seal Initiation Temperature (C) 103 103 99 103 111
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Resin Manufacturing Processes• LLDPE Processes:
– Gas Phase– Solvent Based / Solution– Slurry Loop
• Most LLDPE is produced in single reactor systems, but some processes used to manufacture LLDPE do use multiple reactors
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Gas Phase Process (Simplified)
• Feed gases such as Ethylene, Butene or Hexene, Hydrogen etc. areintroduced to the fluidized bed in the base of the gas phase reactor
• Catalyst is introduced to the reactor• The exothermic heat of reaction is controlled by the fresh feed gas
circulation• High Rx throughput rates and low conversion rates per pass are
typically achieved - feed gases recycle through the reactor entering at the base and exiting at the top
• Granular PE product is produced in the reactor and intermittently discharged out of the reactor into a purge bin, hydrocarbons areremoved, granular materials conveyed to pelletization followed by pellet conveying to finishing area
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Example of Gas Phase Process (Simplified)
Reactor
CatalystPreparation
Dryer
ComonomerRecovery Unit
ProductDischarge
System
Degassing and Drying
Cooling Water Exchanger
CompressorFlare
Product
Hexene RailcarDegassing and DryingButene Railcar
NitrogenHydrogenIsopentaneCo-Catalyst
Ethylene
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Solution Polymerization Process (Simplified)
• All aspects of reaction take place in solution• All raw ingredients including, Ethylene feed, Hydrogen, etc. are
dissolved into a solvent resulting in a solution composed of the raw ingredients required
• Catalyst is introduced to the reactor/s• Solution is introduced into one or more stirred autoclave reactors -
temperature, residence time and mixing are controlled• Polymer solution exits the reactor/s, solvent is flashed off in a
separator and returns to distillation• Polymer passes through a low pressure separator into an extruder• A devolatization extuder is used in some cases to remove residual
hydrocarbons while stripping vessels (post-extrusion) may also be used in some processes to accomplish this task
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Low Pressure Solution Process (Simplified)
PelletizedProduct
Vapors
Comonomer
Hydrogen
Ethylene
Recycle Stream
Catalyst Catalyst
12 3
5
4
1. Stirred Autoclave Reactors2. Separator3. Separator
4. Pelletizer5. Compressor
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Slurry Process Description(Simplified)
• Description is simplified but based on the Phillips Slurry loop design that can produce LLDPE, MDPE, HDPE, mLLDPE
• The reactor is a circulation loop, water jacketed to remove heat• A hydocarbon carrier circulates the reactive ingredients around the
loop reactor• The reaction of Ethylene, Comonomer, Hydrogen, etc. results in
polymer particles forming, suspended on the carrier• Polymer settles out and is removed from the reactor into a flash
vessel that separates granular polymer from residual hydrocarbon• Polymer granules exit the flash vessel into a purge vessel where
hydrocarbons are removed• Additives are incorporated, granular material is extruded and
pelletized
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Low Pressure Slurry Process(Simplified)
GranularPolyethylene
Operating Conditions200 - 250 o F500 - 600 psi
CirculatingPump
EthyleneHydrogenComonomer
Flash Tank
Vapors
LOOPREACTOR
DRYER
RECYCLE STREAM
Catalyst
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2002 APC-LLDPE Volume by End Use Process (based on Amercian Plastics Council 2002 Data)
Injection Molding7%
Other Extruded Products3%
Sheet (greater than 12 mil)1% Pipe and Conduit
1%
All Other Uses23%
Film (less than 12 mil)65%
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LLDPE by Market in N.A.• 65% Film (12 mils or less)• 7% Injection Molding• The remainder is spread out over a variety of production
processes such as: – Pipe and Conduit– Sheeting– Blow Molding– Compounding
Source: APC Resin Statistics
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Typical Applications• LLDPE
– Grocery sacks– Garbage bags– Stretch wrap film– Agricultural film and tubing– Milk pouches– Wire and cable coatings– Housewares– Large outdoor toys– Chemical storage tanks– Landfill covers
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Future Development/Outlook• The PE Industry is continuously improving product
performance by:– New Catalyst developments– New reactor configurations and manufacturing
process improvements– Technology Licensing - existing technologies
licensed to operate on new technology platforms=> could result in novel Polyethylene materials
– Polyethylene is evolving Stay Tuned!
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References and Acknowledgements
• NOVA Chemicals Internal Literature• Kirk Othmer Encyclopedia of Chemical Technology• American Plastics Council• Chem Systems (2003)• Commodity Thermoplastics (JP Arlie)• Judy Webb-Barrett (NOVA Chemicals)• Lan Nguyen (NOVA Chemicals)• Chris Foy (NOVA Chemicals)
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Questions?