WO1996010606A1 - Additif pour le traitement des cires - Google Patents

Additif pour le traitement des cires Download PDF

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Publication number
WO1996010606A1
WO1996010606A1 PCT/EP1995/003909 EP9503909W WO9610606A1 WO 1996010606 A1 WO1996010606 A1 WO 1996010606A1 EP 9503909 W EP9503909 W EP 9503909W WO 9610606 A1 WO9610606 A1 WO 9610606A1
Authority
WO
WIPO (PCT)
Prior art keywords
component
polymer
composition
film
less
Prior art date
Application number
PCT/EP1995/003909
Other languages
English (en)
Inventor
Achiel Josphus Maria Van Loon
Original Assignee
Exxon Chemical Patents Inc.
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.)
Filing date
Publication date
Priority claimed from GB9419946A external-priority patent/GB9419946D0/en
Priority claimed from GBGB9500454.5A external-priority patent/GB9500454D0/en
Application filed by Exxon Chemical Patents Inc. filed Critical Exxon Chemical Patents Inc.
Priority to AU37449/95A priority Critical patent/AU3744995A/en
Publication of WO1996010606A1 publication Critical patent/WO1996010606A1/fr

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Classifications

    • 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
    • C08L23/08—Copolymers of ethene
    • C08L23/0807—Copolymers of ethene with unsaturated hydrocarbons only containing more than three carbon atoms
    • C08L23/0815—Copolymers of ethene with aliphatic 1-olefins
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/04—Homopolymers or copolymers of ethene
    • 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
    • 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
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
    • C08L91/06—Waxes

Definitions

  • the invention relates to polymer compositions, pelletised polymer product, polymer conversion processes and products produced therefrom.
  • the invention relates to polymer compositions having improved melt-processability, particularly in extrusion-type polymer conversion processes such as film extrusion as described in our co-pending application GB 9419946.0.
  • This application relates to a modification and amplification of the above GB application.
  • This application incorporates GB 9419946.0 and GB 9500454.5 for US purposes. Background
  • the background is the same as in GB 9419946.0.
  • Low molecular weight components which may range from waxes to polymers having intermediate levels of molecular weight. Use of intermediate levels of molecular weight is shown in EP 128045, WO 90/03414 and WO 94/12568. Higher and lower density polymer components have been suggested with varying molecular weight and in amounts which range from the very low (2%) to the very high (50%).
  • WO 90/03414 discloses blends in which the higher molecular weight component has the higher density but does not specify an upper limit to the molecular weight of the lower molecular weight component and combined with that, a minimum difference in the molecular weights exists.
  • WO 91/08262 describes a blend of an LLDPE and a wax having silane groups capable of cross linking.
  • the LLDPE has a melt index of from 0.2 to 10 and a density of from 0.90 to 0.94.
  • the wax may be a homopolymer wax having a Brookfield viscosity of from 500 to 20 000 and a density of from 0.88 to 0.96, with a density similar to the LLDPE preferred.
  • the wax may be used in an amount of 2 to 10 wt %.
  • the blends provide a good combination of curing rate and processing rate. There is no suggestion that the higher wax levels may be useful in the film or coating area or that the high wax levels should be specifically employed with waxes having crystallinities above that of the LLDPE used in the composition.
  • the linear polyethylene used has no branches and presumably has a high melting point and density. There is no data or suggestion that such high levels of wax treatment can help processability for heat sealable copolymers of lower density. It has been suggested that waxes can be used in lower amounts as processing aids for linear polyethylenes .
  • Plastics Technology July 1986/73 provides an overview. Intern Polymer Processing II (1988) 3/4 page 220 onwards discuss a variety of waxes at low treatment levels. Modern Plastics International, November 1983, pp 36 to 37 describes 1.5 wt % of Epolene N-34 (Registered Trade Mark), an LDPE wax, produced by Eastman Kodak.
  • Kunststoffe 77 (1987) 5 pp 480 onwards discloses LLDPE/wax blends with 8 to 10 % of wax in the blend. Melting point is not indicated. Page 481 indicates that the waxes are "spezielle Wachse, die mit dem Kunststoff Vietnamese mischbar Sind" (i.e. special waxes, which are not mixable with the synthetic material [LLDPE]). Processing of linear polyethylene with very high molecular weights (see J63-03941A and J63-060708A) and hence intrinsic viscosities of over 5 dl/g is aided by an additive which generally has a lower crystallinity. The additive is likely to affect the surface of the molten and solidified material so as to give the rise to screw slippage at high levels of addition.
  • GB 1 037 183 discloses (p 2 line 30) use of hydrocarbons of intermediate molecular weight and substantially paraffinic nature. The molecular weight is between 250 and 20 000. Side chains may be present. The waxes may be microcrystalline waxes. There is no stated link between the polymer and wax crystallinity. In the Examples a low density wax is combined with a high density polymer. The effect is likely to be similar to those of the "Epolene" waxes described above. GB 849 389 uses a microcrystalline wax in an amount (see page 2 line 47) of from 5 to 15 weight percent. It is suggested that the highest melting point wax be used. The density of the polymer should be above 0.94. In the example a wax which is likely to have a density lower than that of the polymer.
  • US 4680330 discloses a composition in which a liquid cling agent is used in conjunction with a microcrystalline wax.
  • the crystallinity of the waxes can be high but the particular waxes disclosed have a low viscosity which would interfere to a degree with the polymer product properties.
  • Very low viscosity waxes may interfere with product properties causing weakening of the physical properties and poor surface appearance, particularly at higher treat levels.
  • Very low viscosity waxes may lead to screw slippage and other processing difficulties; again particularly at higher treat levels.
  • the maximum level of was disclosed is 20 wt% of the sum of the components.
  • the maximum wax amount expressed on the total composition weight equals 20 wt% times 10 wt%; which results in 2 wt%; too low a level to provide a significant processing influence.
  • the processing aids have varied in molecular weight, density, melting point and proportion. Even with the wide choice described above melt processing may suffer from bottlenecks in extrusion temperature, extrusion capacity (screw-speed), extrusion pressure amongst others.
  • the manner of adding the processing aid can also be critical to avoid screw slippage in a blending step. It is amongst the aims of the invention to provide a polymer composition including LLDPE and a processing aid which reduces the restraints of those bottlenecks, which permits higher outputs and lower energy costs and/or can be incorporated into a blend in a convenient manner without undue screw slippage or reduction in extruder output.
  • the invention involves generally a blend of particular high and low, wax-like, low molecular weight components.
  • the blend contains at least 50 wt% of component (A), component (A) having a density of from 0.88 to 0.94, being prepared from ethylene and a comonomer having from 4 to 12 carbon atoms and having a melt index of less than 100, and from 3 to 30 wt% of a low molecular weight wax component (B), component (B) having a Brookfield viscosity of from 25 mPa.s to less than 15 Pa.s at 190°C and a crystallinity at least equal to that of component A, the weight percent of
  • (B) being determined on the basis of the overall weight of the composition.
  • the crystallinity is determined by DSC.
  • the component (A) has an MI which provides melt strength in melt processing while component (B) has, on its own, insufficient melt strength and serves to assist and influence the overall melt processability of the blend without adding unduly to extractability.
  • the melt index for component (A) indicates a lower molecular weight limit
  • the viscosity for component (B) indicates an upper molecular weight limit.
  • the melt index is determinable according to
  • ASTM-D 1238 190°C condition E 2.16 kg and is expressed in g/10 min.
  • the invention provides specifically for the use of the blend in processes and forms not disclosed or suggested by WO90/0314; WO91/08262 and Polymer Engineering and Science 10, 193-201 (1970).
  • component (B) Because of the levels of crystallinity in component (B) that component will not extract easily and, it is surmised, will be part of or constitute a crystalline phase and does not migrate to the polymer surface. Use of component (B) is thus compatible with the use of other additives which lower surface friction with a die in melt processing.
  • component (A) and component (B) are selected so that at least part of the component (A) crystallizes around at least part of component (B). This may be manifested by the fact that the blend has an equal or slightly higher crystallinity than component (A) alone and/or an equal or slightly higher melting point or in that (B) forms crystals inside the amorphous phase of (A).
  • thermoplastic polymer composition comprising:
  • reactor outputs can be increased when the wax addition helps to increase the extruder capacity while the blend performs equivalent to pure polymers of comparable melt index.
  • virgin polymer refers to polymer emerging from the reactor, such as a gas-phase reactor, which has not undergone a pelletisation step.
  • Virgin polymer may or may not be mixed with stabilizing additives such as anti- oxidants.
  • the virgin polymer may be blended and/or pelletised on the site of the reactor or off-site.
  • the invention provides secondly a pelletised thermoplastic polymer comprising a blend with components (A) and (B) as discussed above or a film containing at least one layer with such a blend.
  • the components (A) and (B) are blended in an extruder of film producing apparatus.
  • the invention also provides a composition, regardless of the physical form of such a blend, substantially devoid of a cross-linking additive so as to permit into flexible and sealable film.
  • component (A) has a melt index of less than 20, preferably less than 5, and/or component (B) has a Brookfield viscosity at 190°C of less than 5 Pa.s, preferably less than 2 Pa.s.
  • the melt index is at least 0.1, preferably at least 0.4 and especially at least 0.8.
  • the process, pellet, film employ a composition in which the difference in crystallinity is at least 10%, preferably at least 20% and a process, pellet, film or composition in which the component (B) has a crystallinity equal to or above that of component (A).
  • a process, pellet, film or composition has a component (A) with an Mw/Mn of less than 8; preferably less than 6 and/or a density of from 0.87 to 0.95, preferably from 0.89 to 0.94 and/or component (B) has a viscosity at 190°C of from 25 to 15000 mPa.s, preferably from 100 to 1000 mPa.s.
  • the melt index is from 0.1 to 6, especially from 0.3 to 3.
  • a predominant amount of the composition is derived from the high molecular weight component and the melt index is generally selected such that the composition as a whole is readily melt processable into a film. Because of the presence of the low molecular weight component, extra and unusually low melt index materials may be used which provide added physical properties.
  • melt index of the polymer without wax is less than 1. Low melt index polymers can be extruded more easily.
  • Polymer having such a melt index and a MWD of less than 8 are normally fairly restricted in melt processing conditions.
  • the range of conditions (speed, temperature, extrusion power, extrusion output, feed pressure) for melt processing can be enlarged; presence of other components (other than LLDPE and wax) may be reduced or eliminated.
  • the viscosity of the low molecular weight component is such that it has at all times a molecular weight below that of the high molecular weight polyethylene and generally with a Brookfield viscosity at 190°C below 15 Pa.s. Within that viscosity range, a person skilled in the art can select those characteristics which, in combination with the high molecular weight material, give the desired processability.
  • the low molecular weight material (herein referred to as a wax) has a molecular weight and a extent of branching (if any) derived from either long chains or short chains from comonomers yielding a crystallinity at least equal to that of the high molecular weight material.
  • the blend components can be selected to give low or no wax migration to the surface by keeping the wax distributed in the matrix of the high molecular weight polymer. Die build up may be low or absent.
  • the amount of the wax should be sufficient to have a significant impact on the overall melt viscosity and so is generally above 5 wt % preferably up to around 10 wt %.
  • the polymer contains other additives, conventionally used for heat sealable films, such as stabilizers, anti-oxidants, slip agents, anti-block and polymer processing aids. It is however preferred for film forming uses that the polymer is free of cross-linking agents such as silane etc., which are incompatible or not conventionally used for a heat sealable flexible film.
  • composition may still contain a migratable additive to reduce surface friction in extrusion such as non- cocrystallisable products or fluorinated materials such as Viton A.
  • such surface friction improving additives are used in amounts of less than 1/2 preferably less than 1/4 of the amount of the wax. Depending on the type of additive, the amount is preferably from 200 - 2000 ppm.
  • the polymer composition may also contain minor amounts, generally less than 30%, especially less than 10 % wt of high molecular weight polymers selected to aid processability such as non-linear LDPE's or EVA's.
  • melt processing Using suitable compositions as described above melt processing, particularly those for melt blowing or cast extrusion of film, can be performed under optimized conditions. These process ranges encompass or overlap with processing ranges which may be used for the plain high molecular weight polyethylene not containing a high crystallinity wax.
  • the invention permits combining a lower extrusion temperature with an acceptable back pressure OR a normal extrusion temperature with a lower back pressure to either reduce the extrusion energy requirement and/or increase the line speed over those conventionally practiced as will be illustrated in the Examples.
  • the high molecular weight components may be a polyethylene such as LDPE but is preferably an LLDPE or VLDPE, material having a density of 0.88 to 0.94 prepared using a comonomer having from 4 to 12 carbon atoms such as butene-1; hexene-1 or octene-1.
  • the low molecular weight component may be a wax prepared by any of the known routes for preparing crystalline polar and non-polar waxes such as fractionation from suitable feedstock; polymerization of ethylene using a Ziegler-Natta catalyst or a metallocene based catalyst system or using free radical initiators; or by thermal decomposition.
  • the wax may contain low levels of polar comonomers containing carbonyl or carboxylic acid groups, preferably less than 5 % by weight.
  • a composition may also contain minor amounts of suitable other polymer components and appropriate amounts of fillers and additives.
  • the composition contains less than 10 wt%; preferably less than 5 wt% of filler material.
  • the wax may be melt blended with the polymer at the end of the polymerization process in the extruder for the reactor in which the monomers of the high molecular weight component are combined to form polymer. It may also be possible to prepare the components as a reactor blend using different catalysts in a single reactor or, optionally with the same catalyst, in a series reactor arrangement.
  • pellets may then be processed conventionally without requiring additional processing steps downstream.
  • component (A) and component (B) may be combined in film extrusion apparatus.
  • the invention is illustrated by the Examples.
  • Figure 1A schematically illustrates a polymerisation reactor 2, having an outlet for removing polymer 4 leading to an extruder 6, powered by a motor 8. Wax is added to the extruder 6 from a storage vessel 10. The extruder output is pelletised at 12. By suitable selection of the wax, the extrusion capacity (output) can be increased as a result of the wax addition.
  • Figure 1B also schematically illustrates a conversion-line with a motor 20, driving an extruder 22, supplying molten polymer to a blow extrusion die 24. Pellets of LLDPE/Wax composition are supplied from container 26 either product produced pelletised at 12 or dry-blended using separate polymer and wax streams. Limits in capacity may occur at 20 (no more power available for extrusion); at 22 (screw slippage); at 24 (melt fracture or limits to the cooling the film upon extrusion or maximum pressure).
  • LL A-1 is obtainable from Exxon Chemical as Escorene (Registered Trade Mark) LL(N) 1001 XV and LL A-2 as Escorene LL 1002 XV.
  • LL A-3 is available as LL(N) 1030 XD;
  • LL A-4 is available as LL(N) 1201 XV from Exxon Chemical.
  • the waxes B-l and B-2 were obtainable from Exxon Chemical as Escomer (Registered Trade Mark) H231 and H311.
  • H311 has a viscosity of 1100 MPa.s at 120°C.
  • the output was approximately the same.
  • the presence of the wax permits a higher extruder screw-speed and output for comparable pressures and loads.
  • the pellets were then extruded into film on a Dolci extruder (60 mm screw diameter and 200 mm die diameter) to determine the maximum output using a narrow die-gap.
  • LL A-1 and LL A-2 were blended and pelletised with 10 wt % of Wax B-2 on a ZSK 58 in screw compounding line.
  • the pellets were introduced to an Alpine extruder to make film.
  • the pellets were then extruded into films on a Alpine extruder (65 mm screw diameter and 225 mm diameter) using a narrow diegap.
  • the screw rotated at 60 rpm; at 30 minutes intervals the screw-speed was increased in steps of 10 rpm until output reached a maximum. Pressure, temperature and output were recorded.
  • the extruder temperature settings for the tests were from 200°C to 220°C for the product blend c-1 and reference polymer LL A-1.
  • Blend C-1 never reached a limiting pressure because further output increases were restricted by cooling limitations.
  • Figure 3 shows the results graphically.
  • Figure 3 also includes some pressure levels and outputs where the extruder temperature setting is lowered by 30°C. This demonstrates that under these conditions the maximum pressure is reached at a higher rpm compared to a conventional temperature profile. This suggests that bottlenecks relating to cooling capacity and/or pressure can be eased by using the flexibility in setting the appropriate extruder temperatures.
  • a blend was compared with a pure polymer in order to achieve a comparable melt index.
  • a lower melt index material blend with wax compares favorably with a higher melt index wax free polymer.
  • composition with the high and low viscosity waxes gives a higher output (10 - 20 %) at equal power consumption and lower pressure (20 %) at equal screw- speed than the LLDPE alone.
  • DSC data shown in Figure 5 illustrate that the compositions have a slightly higher crystallinity than the LLDPE LL A-3 pure and that any peak of the pure wax B-2 is absent or barely detectable. This confirms the crystallinity of the blend is not reduced by the use of the wax.
  • the DSC melting point analysis shows that the blend has a comparable melting point. LL A-3 and wax B-2 have hence co-crystallised at least to some degree.

Abstract

L'invention concerne des compositions polymères, une substance polymère granulée, des procédés de conversion de polymères ainsi que les produits de ceux-ci. L'invention concerne notamment des compositions polymères possédant une meilleure aptitude au traitement à chaud, notamment dans des procédés de conversion de polymères de type extrusion, tels que l'extrusion de films comme cela est décrit dans notre demande de brevet également pendante GB 9419945.0. La demande actuelle se rapporte à une modification de la demande de brevet ci-dessus mentionnée et à un élargissement du champ de celle-ci, et elle incorpore les demandes de brevet GB 9419946.0 et GB 9500454.5 pour les Etats-Unis.
PCT/EP1995/003909 1994-10-04 1995-10-03 Additif pour le traitement des cires WO1996010606A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU37449/95A AU3744995A (en) 1994-10-04 1995-10-03 Wax processing aid

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
GB9419946A GB9419946D0 (en) 1994-10-04 1994-10-04 Wax processing aid
GB9419946.0 1994-10-04
GB9500454.5 1995-01-10
GBGB9500454.5A GB9500454D0 (en) 1995-01-10 1995-01-10 Wax processing aid

Publications (1)

Publication Number Publication Date
WO1996010606A1 true WO1996010606A1 (fr) 1996-04-11

Family

ID=26305733

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP1995/003909 WO1996010606A1 (fr) 1994-10-04 1995-10-03 Additif pour le traitement des cires

Country Status (2)

Country Link
AU (1) AU3744995A (fr)
WO (1) WO1996010606A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2527396A3 (fr) * 2007-08-06 2013-03-27 General Cable Technologies Corporation Compositions isolantes résistant aux arborescences

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1037183A (en) * 1962-05-11 1966-07-27 Celanese Corp Thermoplastic compositions
EP0385599A2 (fr) * 1989-02-13 1990-09-05 Exxon Chemical Patents Inc. Film et composition polymère pour ce film

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1037183A (en) * 1962-05-11 1966-07-27 Celanese Corp Thermoplastic compositions
EP0385599A2 (fr) * 1989-02-13 1990-09-05 Exxon Chemical Patents Inc. Film et composition polymère pour ce film

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2527396A3 (fr) * 2007-08-06 2013-03-27 General Cable Technologies Corporation Compositions isolantes résistant aux arborescences

Also Published As

Publication number Publication date
AU3744995A (en) 1996-04-26

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