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WO2013006409A1 - Polyéthylène doté d'une résistance élevée à l'état fondu pour une utilisation en revêtement par extrusion - Google Patents

Polyéthylène doté d'une résistance élevée à l'état fondu pour une utilisation en revêtement par extrusion Download PDF

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Publication number
WO2013006409A1
WO2013006409A1 PCT/US2012/044844 US2012044844W WO2013006409A1 WO 2013006409 A1 WO2013006409 A1 WO 2013006409A1 US 2012044844 W US2012044844 W US 2012044844W WO 2013006409 A1 WO2013006409 A1 WO 2013006409A1
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WO
WIPO (PCT)
Prior art keywords
target
resin
polyethylene
polyethylene resin
amine derivative
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Application number
PCT/US2012/044844
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English (en)
Inventor
Jian Wang
Mehmet Demirors
Nicolas Cardoso MAZZOLA
Jorge Caminero GOMES
Original Assignee
Dow Global Technologies Llc
Dow Brasil S.A.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Application filed by Dow Global Technologies Llc, Dow Brasil S.A. filed Critical Dow Global Technologies Llc
Publication of WO2013006409A1 publication Critical patent/WO2013006409A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/34—Heterocyclic compounds having nitrogen in the ring
    • C08K5/3412—Heterocyclic compounds having nitrogen in the ring having one nitrogen atom in the ring
    • C08K5/3432—Six-membered rings
    • C08K5/3435—Piperidines
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F8/00—Chemical modification by after-treatment
    • C08F8/30—Introducing nitrogen atoms or nitrogen-containing groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/04—Homopolymers or copolymers of ethene
    • C08L23/06—Polyethene
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D123/00—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers
    • C09D123/02—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
    • C09D123/04—Homopolymers or copolymers of ethene
    • C09D123/06—Polyethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2810/00—Chemical modification of a polymer
    • C08F2810/10—Chemical modification of a polymer including a reactive processing step which leads, inter alia, to morphological and/or rheological modifications, e.g. visbreaking
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure

Definitions

  • This invention pertains to polyethylene extrusion compositions.
  • the invention pertains to ethylene polymer extrusion compositions having high drawdown and substantially reduced neck-in.
  • the invention also pertains to a method of making the ethylene polymer extrusion composition and a method for making an extrusion coated article, an article in the form of an extrusion profile and an article in the form of an extrusion cast film.
  • low density polyethylene made by high-pressure polymerization of ethylene with free -radical initiators as well as homogeneous or heterogeneous linear low density polyethylene (LLDPE) and ultra low density polyethylene (ULDPE) made by the copolymerization of ethylene and oc-olefins with metallocene or
  • Ziegler coordination (transition metal) catalysts at low to medium pressures can be used, for example, to extrusion coat substrates such as paper board, paper, and/or polymeric substrates; to prepare extrusion cast film for applications such as disposable diapers and food packaging; and to prepare extrusion profiles such as wire and cable jacketing.
  • LDPE extrusion compositions lack sufficient abuse resistance and toughness for many applications.
  • efforts to improve abuse properties by providing LDPE compositions having high molecular weights are not effective since such compositions inevitably have too much melt strength to be successfully drawn down at high line speeds.
  • LLDPE and ULDPE extrusion compositions offer improved abuse resistance and toughness properties and MDPE (medium density polyethylene) extrusion compositions offer improved barrier resistance (against, for example, moisture and grease permeation), these linear ethylene polymers exhibit unacceptably high neck-in and draw instability; they also exhibit relatively poor extrusion processability compared to pure MDPE (medium density polyethylene)
  • LDPE LDPE
  • One proposal commonly used in the industry is to blend LDPE with LLDPE.
  • LLDPEs currently used large amounts (e.g. more than 60%) of LDPE must be used in order to achieve the required neck-in.
  • the availability of LDPE may be limited, or there may be other reasons for desiring a lower level of LDPE, without unduly increasing neck-in. It has been discovered that if the melt strength of the LLDPE component can be increased without a significant decrease in melt index, the neck-in of its blend with LDPE can be reduced while still maintaining similar extrusion processability.
  • the neck-in is less than approximately two and a half inches (1.25" per side) at a haul-off rate of approximately 440 feet/minute.
  • the neck-in generally decreases with increasing haul-off rates, making neck-in particularly problematic when using older equipment which is limited in the haul off rates obtainable.
  • the practical range of melt index is from about 3 to about 30 g/10 min in most coating applications, and the compositions of the present invention can cover this entire range.
  • the maximum operating speed of the extrusion coating equipment not be limited by the properties of the resin being used.
  • resin which exhibits neither draw instability nor breaking before the maximum line speed is reached.
  • the resins provided in this invention exhibit low neck-in and excellent draw stability while the drawdown capability required is obtained by selecting the correct melt index.
  • the melt index of the overall blend is in the range of 5-15 g/ 10 min. It is a further feature of this invention that it provides a resin composition at for example 8 MI that will be suitable for extrusion on both older equipment having slow take-off and modern high speed equipment. In both situations the neck-in can be less than 2.5 inches.
  • Melt Strength can be enhanced by using resins with higher molecular weight, but such resins will generally require more robust equipment and more energy use because they tend to generate higher extrusion pressure during the extrusion process. Therefore, properties must be balanced to provide an acceptable combination of physical properties and processability.
  • the ethylene/alpha-olefin interpolymer of the present invention provides good neck- in properties.
  • the present invention is a new process for increasing the melt strength of polyethylene involving reacting molten polyethylene with an alkoxyamine derivative through regular extrusion processing.
  • one aspect of the invention is a method for increasing the melt strength of a polyethylene resin comprising first selecting a polyethylene resin having a density, as determined according to ASTM D792, in the range of from 0.90 g/cm 3 to 0.955 g/cm 3 , and a melt index, as determined according to ASTM D1238 (2.16 kg, 190°C), in the range of from 3 g/lOmin to 30 g/10 min and then reacting an alkoxy amine derivative with the polyethylene resin in an amount and under conditions sufficient to increase the melt strength of the polyethylene resin.
  • the present invention may also increase the Viscosity Ratio of the resin, indicating good processability.
  • the present invention is a method for producing improved extrusion coatings in which the method involves increasing the melt strength of a target polyethylene resin.
  • Polyethylene resin includes all polymers or polymer blends which are derived at least 50% by weight from ethylene monomer units. This includes materials known in the art as high density polyethylene (HDPE), linear low density polyethylene (LLDPE), and low density polyethylene made using high pressure reactors (LDPE).
  • HDPE high density polyethylene
  • LLDPE linear low density polyethylene
  • LDPE low density polyethylene made using high pressure reactors
  • the target polyethylene resin selected should have a density, as determined according to ASTM D792, in the range of from 0.90 g/cm 3 to 0.955 g/cm 3 and a melt index, as determined according to ASTM D1238 (2.16 kg, 190°C), in the range of from 3 g/lOmin to 30 g/10 min,
  • Suitable polyethylene resins can be produced with conventional Ziegler Natta or Chromium catalysts but also with metallocene or single site catalysts. Such resins may have monomodal or multimodal molecular weight distributions.
  • Preferred target resins are Linear Low Density Resins having a density of from 0.90 to 0.93 g/cm 3 ' more preferably from 0.905 to 0.920 g/cm3, and a melt index of from 4 to 20 g/10 min, more preferably from 6 to 10 g/10 min.
  • alkoxy amine derivatives includes nitroxide derivatives.
  • the alkoxy amine derivative is added in an amount and under conditions sufficient to increase the melt strength of the polyethylene resin.
  • the alkoxy amine derivatives correspond to the formula:
  • Ri and R 2 are each independently of one another, hydrogen, C4-C42 alkyl or C4-C42 aryl or substituted hydrocarbon groups comprising O and/or N, and where Ri and R 2 may form a ring structure together; and where R 3 is hydrogen, a hydrocarbon or a substituted hydrocarbon group comprising O and/or N.
  • R 3 Preferred groups for R 3 include -Ci-Ci 9 alkyl; - C 6 -C 10 aryl; -C 2 -C 19 akenyl; -0-C C 19 alkyl; -O-C 6 -C 10 aryl; -NH-C C 19 alkyl; -NH-C 6 - Cioaryl; -N-(Ci-Ci 9 alkyl) 2. .
  • R 3 most preferably contains an acyl group.
  • the preferred compound may form nitroxyl radical (Rl)(R2)N-0* or amynil radical (R1)(R2)N* after decomposition or thermolysis.
  • alkoxy amine derivative is 9-(acetyloxy)-3,8,10- triethyl-7,8,10-trimethyl-l,5-dioxa-9-azaspiro[5.5]undec-3-yl]methyl octadecanoate which has the followi
  • Examples of some preferred species for use in the present invention include the following:
  • hydroxyl amine esters are more preferred with one particularly favored hydroxyl amine ester being 9-(acetyloxy)-3,8,10-triethyl-7,8,10-trimethyl-l,5-dioxa-9- azaspiro[5.5]undec-3-yl]methyl octadecanoate.
  • the alkoxy amine derivatives are added in an amount sufficient to increase the melt strength and/or increase the elongational viscosity to the desired level.
  • the alkoxy amine derivatives are added in an amount of from 1 to 900 ppm of the total amount of polyethylene polymer by weight (that is from 1 to 900 parts alkoxy amine derivative per million parts (by weight) of target resin plus carrier resin, if any), more preferably from 50 to 500 ppm, more preferably from 75 to 400 ppm and still more preferably from 100 to 300 ppm.
  • the addition to the polyethylene polymer can be carried out in all customary mixing machines in which the polymer is melted and mixed with the additives. Suitable machines are known to those skilled in the art. They are predominantly mixers, kneaders and extruders.
  • the process is preferably carried out in an extruder by introducing the additive during processing.
  • Particularly preferred processing machines are single-screw extruders, contra rotating and co rotating twin-screw extruders, planetary-gear extruders, ring extruders or co-kneaders. It is also possible to use processing machines provided with at least one gas removal compartment to which a vacuum can be applied. Suitable extruders and kneaders are described, for example, in Handbuch der Kunststoffstoftextrusion, Vol 1maschinen, Editors F. Hensen, W. Knappe, H. Potente, 1989, pp.
  • the screw length can be 1-60 times the screw diameter, preferably 35-48 times the screw diameters.
  • the rotational speed of the screw is preferably 10-600 rotations per minute (rpm), more preferably 25-300 rpm. It is also possible to first prepare a concentrated mixture of the additive in a carrier polyethylene resin, preferably at 1,000 to 10,000 ppm, and then introduce this concentrate or "masterbatch" via an extruder into a melted polyethylene using a static mixer to blend the two materials, preferably at 1 to 20 wt of the concentrate in the melted resin.
  • the concentrate could be processed in an extruder, preferably at temperatures from 180 to 220°C.
  • the temperatures in the static mixer could range from 200 to 250°C, with a residence time in the mixer ranging from 1 to 10 minutes.
  • the maximum throughput is dependent on the screw diameter, the rotational speed and the driving force.
  • the process of the present invention can also be carried out at a level lower than maximum throughput by varying the parameters mentioned or employing weighing machines delivering dosage amounts.
  • the polymers need to be subjected to an elevated temperature for a sufficient period of time, so that the desired changes occur.
  • the temperature is generally above the softening point of the polymers.
  • a temperature range lower than 280°C, particularly from about 160°C to 280°C is employed.
  • the temperature range from about 200°C to 270°C is employed.
  • the period of time necessary for reaction can vary as a function of the temperature, the amount of material to be reacted and the type of, for example, extruder used. It is usually from about 10 seconds to 30 minutes, in particular from 20 seconds to 20 minutes.
  • the alkoxy amine derivative can advantageously be added to the mixing device by use of a masterbatch.
  • the carrier resin for the masterbatch should be chosen to be compatible with the resin to be modified.
  • LDPE high pressure low density polyethylene polymers referred to in the industry as "LDPE" were unexpectedly found to be the preferred carrier due to the lower reactivity as evidenced by little variation of the extrusion pressure during masterbatch production.
  • HDPE may be a better carrier as it will react even less because it does not have tertiary carbons and very low vinyls.
  • Another advantage of this invention is the discovery that polypropylene is not a good carrier for this additive, as it tends to degrade at typical processing temperatures.
  • the carrier resin should be substantially free of any antioxidant additives, meaning that the carrier resin should preferably have less than 1,000 ppm of antioxidant additives, preferably less than 500 ppm and more preferably less than 100 ppm by weight, as antioxidants tend to suppress the activity of the additive.
  • the preferred carrier resin should be compatible with the application at hand; it should have similar viscosity with the target polyethylene resin with which it is going to be blended. It should be preferably an LDPE or HDPE resin with minimal trisubstituted unsaturation units, preferably fewer than 70 per 1,000,000 carbon atoms.
  • the preferred carrier resin should have a molecular weight (Mn) that is less than 50,000 so that it is easy to process, as demonstrated by the pressure drop through the extruder.
  • the carrier resin could incorporate other additives for processing aids but it should be substantially free of antioxidant compounds, preferably containing less than 1,000 ppm, more preferably less than 500 ppm and still more preferably less than 100 ppm by weight, of any antioxidant compound.
  • the target polyethylene resin could be a copolymer of ethylene with any alkene monomer containing 3 to 12 carbons.
  • the target polyethylene resin should have a level of trisubstituted unsaturation units per 1,000,000 carbon atoms in the range of from 200 to 450. It should have a molecular weight slightly lower than the carrier resin, as measured by the melt index (g/10 min).
  • the melt index of the polyethylene resin should be higher by 0.2-0.5 units (g/10 min) than the final desired resin.
  • the polyethylene resin should contain minimal or no antioxidant additives, and any additives should be well- dispersed in the resin prior to being blended with the carrier resin.
  • the amount of the alkoxy amine derivative material in the carrier resin should be in the range of 0.1 to 30% by weight, preferably from 0.1 to 5%, and more preferably in the range of 0.2 to 1%.
  • the amount of the masterbatch is added so that the alkoxy amine derivative is added to the target product is in the range of 1 to 900 ppm, more preferably from 50 to 500 ppm, more preferably from 75 to 400 ppm and still more preferably from 100 to 300 ppm. It will be readily understood by one of ordinary skill in the art that the amount of alkoxy amine derivative in the final product will be reduced from the added amounts, as the compound reacts with the target and carrier polyethylene.
  • antioxidant additives it may be desirable to add one or more antioxidant additives, to protect the properties of the modified target resin.
  • One way to accomplish this is to blend the resin after reaction with the alkoxy amine derivative with another resin that is rich in antioxidants.
  • the reacted target polyethylene resin may comprise from 1 to 99 percent by weight of the reacted target polyethylene resin, more preferably from 1 to 90 percent, with the low density polyethylene composition comprising from 1 to 90 percent, preferably 10 to 90 percent. In many applications it may be desirable for the composition to comprise less than 60% of the low density polyethylene composition.
  • Compression molded samples for density measurement are prepared according to
  • Resins were compression-molded into "3 mm thick x 1 inch" circular plaques at 350°F for five minutes, under 1500 psi pressure in air. The sample was then taken out of the press, and placed on the counter to cool.
  • the stress response was analyzed in terms of amplitude and phase, from which the storage modulus (G'), loss modulus (G"), complex modulus (G*), complex viscosity ⁇ *, tan
  • Viscosity Ratio V0.1/V100 were calculated.
  • the G' vs. G" data from dynamic mechanical spectroscopy measurement at 190°C was interpolated using the Akima spline interpolation algorithm with the 3rd order piecewise polynomial fits.
  • Hiroshi Akima "A new method of interpolation and smooth curve fitting based on local procedures", J. ACM, 17(4), 589-602 (1970).
  • the sample was drawn uni-axially to a set of accelerating nips located 100 mm below the die, with an acceleration of 2.4 mm/s 2 .
  • the tensile force was recorded as a function of the take-up speed of the nip rolls. Melt strength was reported as the plateau force (cN) before the strand broke.
  • a Triple Detector Gel Permeation Chromatography (3D-GPC or TDGPC) system was used.
  • This system consists of a Waters (Milford, Mass) model 150C High Temperature Chromatograph (other suitable high temperatures GPC instruments include Polymer Laboratories (Shropshire, UK) Model 210 and Model 220), equipped with a Precision Detectors (Amherst, Mass.) 2-angle laser light scattering (LS) detector Model 2040, an IR4 infra-red detector from Polymer ChAR (Valencia, Spain), and a Viscotek (Houston, Texas) 150R 4-capillary solution viscometer (DP).
  • a GPC with these latter two independent detectors and at least one of the former detectors is sometimes referred to as "3D-GPC” or "TDGPC,” while the term “GPC” alone generally refers to conventional GPC.
  • Data collection is performed using Viscotek TriSEC software, Version 3, and a 4-channel Viscotek Data Manager DM400. The system is also equipped with an on-line solvent degassing device from Polymer Laboratories (Shropshire, United Kingdom).
  • Suitable high temperature GPC columns can be used, such as four 30 cm long Shodex HT803 13 micron columns, or four 30 cm Polymer Labs columns of 20-micron mixed-pore-size packing (MixA LS, Polymer Labs). Here, the MixA LS columns were used.
  • the sample carousel compartment is operated at 140°C, and the column compartment is operated at 150°C.
  • the samples are prepared at a concentration of "0.1 grams of polymer in 50 milliliters of solvent.”
  • the chromatographic solvent and the sample preparation solvent is 1 ,2,4-trichlorobenzene (TCB) containing 200 ppm of 2,6-di-tert-butyl- 4methylphenol (BHT).
  • TAB ,2,4-trichlorobenzene
  • BHT 2,6-di-tert-butyl- 4methylphenol
  • the solvent is sparged with nitrogen.
  • the polymer samples are gently stirred at 160°C for four hours.
  • the injection volume is 200 micro
  • the IR4 detector is used, and the GPC column set is calibrated by running 21 narrow molecular weight distribution polystyrene standards.
  • the molecular weight (MW) of the standards ranges from 580 g/mol to 8,400,000 g/mol, and the standards are contained in 6 "cocktail" mixtures. Each standard mixture has at least a decade of separation between individual molecular weights.
  • the standard mixtures are purchased from Polymer Laboratories.
  • the polystyrene standards are prepared at "0.025 g in 50 mL of solvent" for molecular weights equal to or greater than 1,000,000 g/mol, and at "0.05 g in 50 mL of solvent” for molecular weights less than 1,000,000 g/mol.
  • the polystyrene standards are dissolved at 80°C, with gentle agitation, for 30 minutes.
  • the narrow standards mixtures are run first, and in order of decreasing highest molecular weight component to minimize degradation.
  • the polystyrene standard peak molecular weights are converted to polyethylene molecular weight using Equation (1) (as described in Williams and Ward, J. Polym. Sci., Polym. Letters, 6, 621 (1968)):
  • Mpolyethylene A x (Mpolystyrene) B (Eq. 1), where M is the molecular weight of polyethylene or polystyrene (as marked), and B is equal to 1.0. It is known to those of ordinary skill in the art that A may be in a range of about 0.38 to about 0.44, and is determined at the time of calibration using a broad polyethylene standard. Use of this polyethylene calibration method to obtain molecular weight values, such as the molecular weight distribution (MWD or Mw/Mn), and related statistics, is defined here as the modified method of Williams and Ward. The number average molecular weight, the weight average molecular weight, and the z- average molecular weight are calculated from the following equations.
  • the linear low density polyethylene, LLDPE1, used is produced in a dual reactor configuration using constrained geometry catalysts and has an 8.6 melt index (I 2 or MI), 0.913 g/cm 3 density, without any antioxidant package.
  • Examples were produced from this LLDPE1 and extruded with different concentrations of an alkoxy amine derivative additive.
  • the specific additive used is 9- (acetyloxy)-3,8,10-triethyl-7,8,10-trimethyl-l,5-dioxa-9-azaspiro[5.5]undec-3-yl]methyl octadecanoate, which was added as an LDPE masterbatch having less than 1% of the additive (note that the ppm levels reported below refer to the active ingredient only and not the entire masterbatch).
  • LLDPE1 and the alkoxy amine derivative additive are compounded in a 30mm co- rotating, intermeshing Coperion Werner-Pfleiderer ZSK-30 (ZSK-30) twin screw extruder.
  • ZSK-30 has ten barrel sections with an overall length of 960 mm and a 32 length to diameter ratio (L/D).
  • a two hole strand die is used without a breaker plate or screen pack.
  • the extruder consists of a DC motor, connected to a gear box by V-belts.
  • the 15HP motor is powered by a GE adjustable speed drive located in a control cabinet.
  • the control range of the screw shaft speed is 1: 10.
  • the maximum screw shaft speed is 500 RPM.
  • a pressure transducer was positioned in front of the die to measure die pressure.
  • the extruder has 8 heated/cooled barrel sections along with a 30 mm spacer, which makes up five temperature controlled zones. It has a cooled only feed section and a heated only die section, which is held together by tie-rods and supported on the machine frame. Each section can be heated electrically with angular half-shell heaters and cooled by a special system of cooling channels.
  • the screws consist of continuous shafts on which screw-flighted components and special kneading elements are installed in any required order.
  • the elements are held together radially by keys and keyways and axially by a screwed-in screw tip.
  • the screw shafts are connected to the gear-shafts by couplings and can easily be pulled out of the screw barrel for dismantling.
  • a Conair pelletizer is used to pelletize the blends. It is a 220 volt variable speed, solid cutter unit.
  • the variable speed motor drives a solid machined cutting wheel, which in turn drives a fixed metal roller.
  • a movable rubber roller presses against the fixed roller and helps pull the strands by friction into the cutting wheel. The tension on the movable roller may be adjusted as necessary.
  • the temperatures are set in the feed zone, 4 zones in the extruder, and the die as:
  • the screw shaft speed is set at 325 revolutions per minute (RPM), resulting in an output rate of approximately 40 lb/hr.
  • the amount of neck-in (the difference in actual coating width versus deckle width with a 6" (15 cm) air gap) is measured at 440fpm and 880 fpm resulting in 1 mil and 1 ⁇ 2 mil coatings respectively.
  • Drawdown is the speed at which edge
  • Blends for use in the extrusion coating experiments consisted of 70% by weight of the LLDPE of Comparative Example 1 and Examples 3 and 4 together with a LDPE produced in an autoclave reactor having a melt index of 8.0 g/10 min and a density of 0.918 g/cm 3 .
  • Blends of the various components are produced by weighing out the pellets and then tumble blending samples until a homogenous blend was obtained (approximately 30 minutes for each sample).
  • LLDPE1 with 200 ppm and 300 ppm alkoxy amine derivate additive.
  • Table 2 Neck-in, drawdown and other processing conditions at the extrusion coating trial.

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Abstract

La présente invention concerne un procédé de fabrication résine particulièrement bien appropriée pour des applications de revêtement d'extrusion, ledit procédé comprenant les étapes consistant à choisir une résine polyéthylène cible puis à augmenter la résistance à la fusion de la résine polyéthylène par réaction de la résine polyéthylène avec un dérivé alcoxy amine, puis à former un revêtement par extrusion à partir du polyéthylène cible ayant réagi.
PCT/US2012/044844 2011-07-06 2012-06-29 Polyéthylène doté d'une résistance élevée à l'état fondu pour une utilisation en revêtement par extrusion WO2013006409A1 (fr)

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US61/504,723 2011-07-06

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3099665A4 (fr) * 2014-01-31 2017-10-04 Fina Technology, Inc. Polyéthylène et articles à base de celui-ci
WO2019018023A1 (fr) 2017-07-21 2019-01-24 Exxonmobil Chemical Patents Inc. Matériau stratifié et son procédé de fabrication
US10844210B2 (en) 2016-03-31 2020-11-24 Dow Global Technologies Llc Modified polyethylene resins and method for making the same
US11193009B2 (en) 2017-09-27 2021-12-07 Dow Global Technologies Llc Modified polyethylene compositions and method for making the same
US11952480B2 (en) * 2018-02-05 2024-04-09 Exxonmobil Chemical Patents Inc. Enhanced processability of LLDPE by addition of ultra-high molecular weight density polyethylene

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050256270A1 (en) * 2002-09-23 2005-11-17 Weeks Ronald J Polymer compositions for extrusion coating
US20060281866A1 (en) * 2003-09-05 2006-12-14 Oswald Thomas T Resin compositions for extrusion coating
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