EP1295301B1 - Cable with recyclable covering - Google Patents
Cable with recyclable covering Download PDFInfo
- Publication number
- EP1295301B1 EP1295301B1 EP01951601A EP01951601A EP1295301B1 EP 1295301 B1 EP1295301 B1 EP 1295301B1 EP 01951601 A EP01951601 A EP 01951601A EP 01951601 A EP01951601 A EP 01951601A EP 1295301 B1 EP1295301 B1 EP 1295301B1
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- EP
- European Patent Office
- Prior art keywords
- cable
- copolymer
- equal
- propylene
- olefin
- Prior art date
- Legal status (The legal status 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 status listed.)
- Expired - Lifetime
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/20—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances liquids, e.g. oils
- H01B3/22—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances liquids, e.g. oils hydrocarbons
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/44—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins
- H01B3/441—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins from alkenes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2913—Rod, strand, filament or fiber
- Y10T428/2933—Coated or with bond, impregnation or core
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2913—Rod, strand, filament or fiber
- Y10T428/2933—Coated or with bond, impregnation or core
- Y10T428/294—Coated or with bond, impregnation or core including metal or compound thereof [excluding glass, ceramic and asbestos]
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2913—Rod, strand, filament or fiber
- Y10T428/2933—Coated or with bond, impregnation or core
- Y10T428/294—Coated or with bond, impregnation or core including metal or compound thereof [excluding glass, ceramic and asbestos]
- Y10T428/2942—Plural coatings
- Y10T428/2947—Synthetic resin or polymer in plural coatings, each of different type
Definitions
- the present invention relates to a cable with recyclable covering.
- the invention relates to a cable for transporting or distributing medium or high voltage electric energy, wherein an extruded covering layer based on a thermoplastic polymer material in admixture with a dielectric liquid with superior mechanical and electrical properties is present, enabling, in particular, the use of high operating temperatures and the transportation of high power energy.
- the various coverings surrounding the conductor commonly consist of polyolefin-based crosslinked polymer, in particular crosslinked polyethylene (XLPE), or elastomeric ethylene/propylene (EPR) or ethylene/propylene/diene (EPDM) copolymers, also crosslinked.
- XLPE crosslinked polyethylene
- EPR elastomeric ethylene/propylene
- EPDM ethylene/propylene/diene
- Electric cables are also known having their insulation consisting of a multi-layer wrapping of a paper or paper/polypropylene laminate impregnated with a large quantity of a dielectric liquid (commonly known as mass impregnated cables or also oil-filled cables). By completely filling the spaces present in the multi-layer wrapping, the dielectric liquid prevents partial discharges arising with consequent perforation of the electrical insulation.
- dielectric liquids products are commonly used such as mineral oils, polybutenes, alkylbenzenes and the like (see for example US-4,543,207, US-4,621,302, EP-A-0987718, WO 98/32137).
- mass impregnated cables have numerous drawbacks compared with extruded insulation cables, so that their use is currently restricted to specific fields of application, in particular to the construction of high and very high voltage direct current transmission lines, both for terrestrial and in particular for underwater installations.
- the production of mass impregnated cables is particularly complex and costly, both for the high cost of the laminates and for the difficulties encountered during the steps of wrapping the laminate and then of impregnating it with the dielectric liquid.
- the dielectric liquid used must have low viscosity under cold conditions to allow rapid and uniform impregnation, while at the same time it must have a low tendency to migrate during installation and operation of the cable to prevent liquid loss from the cable ends or following breakage.
- mass impregnated cables cannot be recycled and their use is limited to an operating temperature of less than 90°C.
- HDPE high density polyethylene
- Thermoplastic low density polyethylene (LDPE) insulating coverings are also used in medium and high voltage cables: again in this case; these coverings are limited by too low an operating temperature (about 70°C).
- LDPE low density polyethylene
- WO 99/13477 describes an insulating material consisting of a thermoplastic polymer forming a continuous phase which incorporates a liquid or easily meltable dielectric forming a mobile interpenetrating phase within the solid polymer structure.
- the weight ratio of thermoplastic polymer to dielectric is between 95:5 and 25:75.
- the insulating material can be produced by mixing the two components while hot either batchwise or continuously (for example by means of an extruder). The resultant mixture is then granulated and used as insulating material for producing a high voltage electric cable by extrusion onto a conductor.
- the material can be used either in thermoplastic or crosslinked form.
- thermoplastic polymers polyolefins, polyacetates, cellulose polymers, polyesters, polyketones, polyacrylates, polyamides and polyamines.
- the use of polymers of low crystallinity is particularly suggested.
- the dielectric is preferably a synthetic or mineral oil of low or high viscosity, in particular a polyisobutene, naphthene, polyaromatic, ⁇ -olefin or silicone oil.
- the Applicant considers as still unsolved the technical problem of producing an electric cable with a covering made from a thermoplastic polymer material having mechanical and electrical properties comparable to those of cables with an insulating covering of crosslinked material.
- the Applicant has considered the problem of producing a cable with a non-crosslinked insulating covering having good flexibilty and high mechanical strength under both hot and cold conditions, while at the same time possessing high dielectric strength, without using products potentially polluting during the life cycle of the cable, i.e. from its production to its disposal.
- the Applicant considers that the addition of dielectric liquids to polymer materials as proposed in the cited WO 99/13477 gives totally unsatisfactory results.
- the Applicant maintains that adding a dielectric liquid to an insulating material should both determine a significant increase in its electrical properties (in particular its dielectric strength), without changing the material characteristics (thermomechanical properties, manageability) and without resulting in exudation of the dielectric liquid.
- the resultant cable should give substantially constant performance with time and hence high reliability, even at high operating temperatures (at least 90°C and beyond).
- the Applicant has now found it possible to solve said technical problem by using, as recyclable polymer base material, a thermoplastic propylene homopolymer or copolymer mixed with a dielectric liquid as hereinafter defined.
- the resultant composition possesses good flexibility even when cold, excellent thermomechanical strength and high electrical performance, such as to make it particularly suitable for forming at least one covering layer, and in particular an electrical insulating layer, of a medium or high voltage cable of high operating temperature, of at least 90°C and beyond.
- the dielectric liquid suitable for implementing the invention has high compatibility with the base polymer and high efficiency in the sense of improving electrical performance, consequently allowing the use of small quantities of additive such as not to impair the thermomechanical characteristics of the insulating layer.
- the dielectric liquid suitable for forming the cable of the invention is free of polar groups, it absorbs water in extremely small quantities, hence preventing formation of insulation defects due to the presence of steam which normally forms during the process of high temperature extrusion.
- the invention therefore relates to a cable (1) comprising at least one electrical conductor (2) and at least one extruded covering layer (3, 4, 5) based on a thermoplastic polymer material in admixture with a dielectric liquid, wherein:
- said extruded covering layer based on said thermoplastic polymer material in admixture with said dielectric liquid is an electrically insulating layer.
- said extruded covering layer based on said thermoplastic polymer material in admixture with said dielectic liquid is a semiconductive layer.
- the propylene homopolymer or copolymer has a melting point of from 145 to 170°C.
- the propylene homopolymer or copolymer has a melting enthalpy of from 30 to 85 J/g.
- the propylene homopolymer or copolymer has a flexural modulus, measured in accordance with ASTM D790, at room temperature, of from30 to 1400 MPa, and more preferably from 60 to 1000 MPa.
- the propylene homopolymer or copolymer has a melt flow index (MFI), measured at 230°C with a load of 21.6 N in accordance with ASTM D1238/L, of from 0.05 to 10.0 dg/min, more preferably from 0.5 to 5.0 dg/min.
- MFI melt flow index
- a copolymer of propylene with an olefin comonomer is used, this latter is preferably present in a quantity of less than or equal to 15 mol%, and more preferably of less than or equal to 10 mol%.
- Propylene/ethylene copolymers are particularly preferred.
- thermoplastic material is selected from:
- the homopolymers or copolymers of class a) show a single-phase microscopic structure, i.e. substantially devoid of heterogeneous phases dispersed as molecular domains of size greater than one micron. These materials do not show in fact the optical phenomena typical of heterophase polymer materials, and in particular are characterised by better transparency and reduced whitening due to local mechanical stresses (commonly known as "stress whitening").
- Particularly preferred of said class a) is a propylene homopolymer or a copolymer of propylene with at least one olefin comonomer selected from ethylene and an ⁇ -olefin other than propylene, said homopolymer or copolymer having:
- the heterophase copolymers of class b) are thermoplastic elastomers obtained by sequential copolymerization of: i) propylene, possibly containing minor quantities of at least one olefin comonomer selected from ethylene and an ⁇ -olefin other than propylene; and then of: ii) a mixture of ethylene with an ⁇ -olefin, in particular propylene, and possibly with minor portions of a diene.
- This class of product is also commonly known by the term "thermoplastic reactor elastomers”.
- the said class b) is a heterophase copolymer in which the elastomeric phase consists of an elastomeric copolymer of ethylene and propylene comprising from 15 to 50 wt% of ethylene and from 50 to 85 wt% of propylene on the weight of the elastomeric phase. Further details of these materials and their use in covering cables are given in European patent application 98830800 filed on 30.12.1998 in the name of the Applicant, incorporated herein for reference.
- thermoplastic base material a propylene homopolymer or copolymer as hereinabove defined can be used in mechanical mixture with a low crystallinity polymer, generally with a melting enthalpy of less than 30 J/g, which mainly acts to increase flexibility of the material.
- the quantity of low crystallinity polymer is generally less than 70 wt%, and preferably of from 20 to 60 wt%, on the total weight of the thermoplastic material.
- the low crystallinity polymer is a copolymer of ethylene with a C 3 -C 12 ⁇ -olefin, and possibly with a diene.
- the ⁇ -olefin is preferably selected from propylene, 1-hexene and 1-octene.
- a diene comonomer is present, this is generally C 4 -C 20 , and is preferably selected from: conjugated or non-conjugated linear diolefins, such as 1,3-butadiene, 1,4-hexadiene, 1,6-octadiene or their mixtures and the like; monocyclic or polycyclic dienes, such as 1,4-cyclohexadiene, 5-ethylidene-2-norbornene, 5-methylene-2-norbornene, 5-vinyl-2-norbornene or their mixtures and the like.
- conjugated or non-conjugated linear diolefins such as 1,3-butadiene, 1,4-hexadiene, 1,6-octadiene or their mixtures and the like
- monocyclic or polycyclic dienes such as 1,4-cyclohexadiene, 5-ethylidene-2-norbornene, 5-methylene-2-norbornene
- Particularly preferred ethylene copolymers are:
- the alkylaryl hydrocarbon of the invention preferably has a dielectric constant, at 25°C, of less than or equal to 3.5 and preferably less than 3 (measured in accordance with IEC 247).
- the alkylaryl hydrocarbon of the invention has a predetermined viscosity such as to prevent fast diffusion of the liquid within the insulating layer and hence its outward migration, while at the same time such as to enable it to be easily fed and mixed into the polymer.
- the dielectric liquid of the invention has a kinematic viscosity, at 20°C, of between 1 and 500 mm 2 /s, preferably between 5 and 100 mm 2 /s (measured in accordance with ISO 3104).
- the alkylaryl hydrocarbon of the invention has a hydrogen absorption capacity greater than or equal to 5 mm 3 /min, preferably greater than or equal to 50 mm 3 /min (measured in accordance with IEC 628-A).
- an epoxy resin can be added to the dielectric liquid suitable for forming the cable of the invention, generally in a quantity of less than or equal to 1 wt% on the weight of the liquid, this being considered to mainly act to reduce the ion migration rate under an electrical field, and hence the dielectric loss of the insulating material.
- the dielectric liquid of the invention comprises at least one alkylaryl hydrocarbon having at least three non-condensed aromatic rings.
- the dielectric liquid of the invention comprises at least one alkylaryl hydrocarbon having at least three non-condensed aromatic rings in a quantity of not less than 10 wt% on the total weight of the dielectric liquid.
- the dielectric liquid of the invention comprises at least one alkylaryl hydrocarbon having the structural formula: wherein:
- the dielectric liquid can also contain minor quantities of at least one triphenylmethane, either unsubstituted or substituted by at least one radical selected from methyl, benzyl and methylbenzyl.
- triphenylmethanes are: ditoluylphenylmethane, dixylylphenylmethane, xylyltoluylphenylmethane and the like, or their mixtures.
- the dielectric liquid of the invention comprises at least one alkylaryl hydrocarbon of the aforegiven formula (I) in which the sum n1+n2 is other than zero.
- Alkylaryl hydrocarbons corresponding to formula (I) in which the sum n1+n2 is equal to zero, and usable advantageously in this invention, are for example: benzyltoluene, benzylxylene, (methylbenzyl)toluene, (methylbenzyl)xylene and the like, or their mixtures.
- Alkylaryl hydrocarbons corresponding to formula (I) in which the sum n1+n2 is other than zero, and usable advantageously in this invention, are for example: dibenzyltoluene, dibenzylxylene, di(methylbenzyl)toluene, di(methylbenzyl)xylene and the like, or their mixtures.
- the alkylaryl hydrocarbons of formula (I) are generally prepared by reacting benzylchloride, methylbenzylchloride or their mixtures, with an aromatic hydrocarbon selected from benzene, toluene, xylene or their mixtures, in the presence of a Friedel-Crafts catalyst (for example FeCl 3 , SbCl 3 , TiCl 4 or AlCl 3 ). Further details regarding the preparation of alkylaryl hydrocarbons of formula (I) are given for example in US-5,192,463, US-5,446,228, US-5,545,355 and US-5,601,755.
- a Friedel-Crafts catalyst for example FeCl 3 , SbCl 3 , TiCl 4 or AlCl 3 .
- the dielectric liquid suitable for implementing the invention has good heat resistance, considerable gas absorption capacity, in particular for hydrogen, and hence high resistance to partial discharges, so that dielectric loss is not high even at high temperature and high electrical gradient.
- the weight ratio of dielectric liquid to base polymer material of the invention is generally between 1:99 and 25:75, preferably between 2:98 and 20:80, and more preferably between 3:97 and 15:85.
- the cable of the invention has at least one extruded covering layer with electrical insulation properties formed from the thermoplastic polymer material in admixture with the aforedescribed dielectric liquid.
- the cable of the invention has at least one extruded covering layer with semiconductive properties formed from the thermoplastic polymer material in admixture with the aforedescribed dielectric liquid.
- a conductive filler is generally added to the polymer material.
- this latter is preferably selected from propylene homopolymers or copolymers comprising at least 40 wt% of amorphous phase, on the total polymer weight.
- the cable of the invention has at least one electrical insulation layer and at least one semiconductive layer formed from a thermoplastic polymer material in admixture with a dielectric liquid as hereinabove described. This prevents the semiconductive layers from absorbing, with time, part of the dielectric liquid present in the insulating layer, so reducing its quantity just at the interface between the insulating layer and semiconductive layer, in particular the inner semiconductive layer where the electrical field is higher.
- the invention relates to a polymer composition
- a polymer composition comprising a thermoplastic polymer material in admixture with a dielectric liquid, in which:
- the invention relates to the use of a polymer composition, as described hereinabove, as the base polymer material for preparing a covering layer (4) with electrical insulation properties, or for preparing a covering layer (3, 5) with semiconductive properties.
- a covering layer for the cable of the invention In forming a covering layer for the cable of the invention, other conventional components can be added to the aforedefined polymer composition, such as antioxidants, processing aids, water tree retardants, and the like.
- antioxidants suitable for the purpose are for example distearyl-thiopropionate and pentaerithryl-tetrakis [3-(3,5-di-tertbutyl-4-hydroxyphenyl)propionate] and the like, or their mixtures.
- Processing aids which can be added to the polymer base include, for example, calcium stearate, zinc stearate, stearic acid, paraffin wax and the like, or mixtures thereof.
- the polymer materials as defined hereinabove can be advantageously used to form an insulating layer.
- these polymer materials show indeed good mechanical characteristics both at ambient temperature and under hot conditions, and also show improved electrical properties.
- they enable high operating temperature to be employed, comparable with or even exceeding that of cables with coverings consisting of crosslinked polymer base materials.
- a conductive filler in particular carbon black, is generally dispersed within the polymer material in a quantity such as to provide the material with semiconductive characteristics (i.e. such as to obtain a resistivity of less than 5 Ohm.m at ambient temperature).
- This quantity is generally between 5 and 80 wt%, and preferably between 10 and 50 wt%, of the total weight of the mixture.
- the possibility to use the same type of polymer composition for both the insulating layer and the semiconductive layers is particularly advantageous in producing cables for medium or high voltage, in that it ensures excellent adhesion between adjacent layers and hence better electrical behaviour, particularly at the interface between the insulating layer and the inner semiconductive layer, where the electrical field and hence the risk of partial discharges are higher.
- compositions of the invention can be prepared by mixing together the base polymer material, the dielectric liquid and any other additives possibly present by methods known in the art. Mixing can be carried out for example by an internal mixer of the type with tangential rotors (Banbury) or with interpenetrating rotors, or, preferably, in a continuous mixer of Ko-Kneader (Buss) type, or of co- or counter-rotating double-screw type.
- the dielectric liquid of the invention can be added to the polymer material during the extrusion step by direct injection into the extruder cylinder.
- the use of the aforedefmed polymer composition in covering cables for medium or high voltage enables recyclable, flexible coverings to be obtained with excellent mechanical and electrical properties.
- the cables of the invention can carry, for the same voltage, a power at least equal to or even greater than that transportable by a traditional cable with XLPE covering.
- the term “medium voltage” generally means a voltage of between 1 and 35 kV, whereas “high voltage” means voltages higher than 35 kV.
- the polymer composition of the invention can be used for covering electrical devices in general and in particular cables of different type, for example low voltage cables, telecommunications cables or combined energy/telecommunications cables, or accessories used in constructing electrical lines, such as terminals or connectors.
- the cable 1 comprises a conductor 2, an inner layer with semiconductive properties 3, an intermediate layer with insulating properties 4, an outer layer with semiconductive properties 5, a metal screen 6, and an outer sheath 7.
- the conductor 2 generally consists of metal wires, preferably of copper or aluminium, stranded together by conventional methods. At least one covering layer selected from the insulating layer 4 and the semiconductive layers 3 and 5 comprises the composition of the invention as heretofore defined.
- a screen 6 generally of electrically conducting wires or strips wound helically. This screen is then covered by a sheath 7 of a thermoplastic material, for example non-crosslinked polyethylene (PE) or preferably a propylene homopolymer or copolymer as heretofore defined.
- PE non-crosslinked polyethylene
- propylene homopolymer or copolymer as heretofore defined.
- the cable can also be provided with an outer protective structure (not shown in Figure 1) the main purpose of which is to mechanically protect the cable against impact or compression.
- This protective structure can be, for example, a metal reinforcement or a layer of expanded polymer as described in WO 98/52197.
- FIG. 1 shows only one possible embodiment of a cable according to the invention. Suitable modifications known in the art can evidently be made to this embodiment, but without departing from the scope of the invention.
- the cable of the invention can be constructed in accordance with known methods for depositing layers of thermoplastic material, for example by extrusion.
- the extrusion is advantageously carried out in a single pass, for example by the tandem method in which individual extruders are arranged in series, or by co-extrusion with a multiple extrusion head.
- the comparison dielectric liquids were:
- the polymer in granular form was preheated to 80°C in a turbomixer.
- the dielectric liquid was added, in the quantities specified for the formulations given in Table 2, to the polymer preheated in the turbomixer under agitation at 80°C over 15 min. After the addition agitation was continued for a further hour at 80°C until the liquid was completely absorbed in the polymer granules.
- the resultant material was kneaded in a laboratory double-screw Brabender Plasticorder PL2000 at a temperature of 185°C to complete homogenization.
- the material left the double-screw mixer in the form of granules.
- the dielectric strength of the polymer compositions obtained was evaluated on test-pieces of insulating material having the geometry proposed by the EFI (Norwegian Electric Power Research Institute) in the publication "The EFI Test Method for Accelerated Growth of Water Trees” (IEEE International Symposium on Electrical insulation, Toronto, Canada, June 3-6 1990).
- the cable is simulated with glass-shaped test pieces of insulating material having their base coated on both sides with a semiconductive material coating.
- the glass-shaped test-pieces were formed by moulding discs of insulating material at 160-170°C from a plate of thickness 10 mm obtained by compressing granules at about 190°C.
- the inner and outer surfaces of the base which had a thickness of about 0.40-0.45 mm, were coated with a semiconductive coating.
- the DS measurement was made by applying to these specimens, immersed in silicone oil at 20°C, an alternating current at 50 Hz starting with a voltage of 25 kV and increasing in steps of 5 kV every 30 minutes until perforation of the test-piece occurred. Each measurement was repeated on 10 test-pieces.
- the values given in Table 2 are the arithmetic mean of the individual measured values.
- the dielectric strength values given in Table 2 highlight the improvement in electrical performance deriving from the dielectric liquids of the invention, compared to that of the base polymer as such or when mixed with the comparison dielectric liquids.
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Description
- said thermoplastic material comprises a propylene homopolymer or a copolymer of propylene with at least an olefin comonomer selected from ethylene and an α-olefin other than propylene, said homopolymer or copolymer having a melting point greater than or equal to 140°C and a melting enthalpy of from 30 to 100 J/g;
- said liquid comprises at least one alkylaryl hydrocarbon having at least two non-condensed aromatic rings and a ratio of number of aryl carbon atoms to total number of carbon atoms greater than or equal to 0.6, and preferably greater than or equal to 0.7.
- a melting point of from 140 to 165°C;
- a melting enthalpy of from 30 to 80 J/g;
- a fraction soluble in boiling diethyl ether in an amount of less than or equal to 12 wt%, preferably from 1 to 10 wt%, having a melting enthalpy of less than or equal to 4 J/g, preferably less than or equal to 2 J/g;
- a fraction soluble in boiling n-heptane in an amount of from 15 to 60 wt%, preferably from 20 to 50 wt%, having a melting enthalpy of from 10 to 40 J/g, preferably from 15 to 30 J/g; and
- a fraction insoluble in boiling n-heptane in an amount of from 40 to 85 wt%, preferably from 50 to 80 wt%, having a melting enthalpy of greater than or equal to 45 J/g, preferably from 50 to 95 J/g.
- said thermoplastic material comprises a propylene homopolymer or a copolymer of propylene with at least one olefin comonomer selected from ethylene and an α-olefin other than propylene, said homopolymer or copolymer having a melting point of greater than or equal to 140°C and a melting enthalpy of from 30 to 100 J/g;
- said liquid comprises at least one alkylaryl hydrocarbon with at least two non-condensed aromatic rings and a ratio of number of aryl carbon atoms to total number of carbon atoms greater than or equal to 0.6, preferably greater than or equal to 0.7.
- Figure 1 is a perspective view of an electric cable, particularly suitable for medium or high voltage, according to the invention.
Dielectric liquid | Dielectric constant | Total carbon atoms | Ratio C(aryl)/C(total) |
JarylecR | 2.8 | MXX = 16 | 0.75 |
| DXX = 24 | ||
JarylecR | 2.7 | 21 | 0.86 |
| |||
BaysiloneR | 2.6 | - | - |
a mixture containing 85 wt% of monoxylylxylene (MXX) and 15 wt% of dixylylxylene (DXX)
dibenzyltoluene (DBT)
polyphenylmethylsiloxane (PPMS), polyaromatic dielectric oil as described in IEEE Transactions on Electrical Insulation Vol. 26, No.4, 1991, having a viscosity of 4 mm2/sec at 25°C;
naphthene-based aromatic oil having a viscosity of 22 mm2/sec at 40°C, consisting of 40 wt% aromatic hydrocarbons, 57 wt% saturated hydrocarbons and 3 wt% polar compounds.
- a flexible propylene homopolymer with melting point 160°C, melting enthalpy 56.7 J/g, MFI 1.8 dg/min and flexural modulus 290 MPa (RexflexRWL105 - commercial product of Huntsman Polymer Corp.) (Examples 1-6)
- a propylene heterophase copolymer with an ethylene/propylene elastomeric phase content of about 65 wt% (propylene 72 wt% in the elastomeric phase), melting enthalpy 32 J/g, melting point 163°C, MFI 0.8 dg/min and flexural modulus of about 70 MPa (HifaxRKSO81 - commercial product of Montell).
Ex. | Polymer | Dielectric liquid | % dielectric liquid by weight | DS (mean) |
1 | RexflexR | -- | -- | 92 |
WL 105 | ||||
2* | RexflexR | BaysiloneR | 5 | 90 |
WL 105 | | |||
3* | RexflexR | FlexonR641 | 5 | 94 |
WL 105 | ||||
4 | RexflexR | JarylecR | 6 | 128 |
WL 105 | | |||
5 | RexflexR | JarylecR | 15 | 150 |
WL 105 | | |||
6 | RexflexR | JarylecR | 4 | 143 |
WL 105 | | |||
7* | HifaxR | -- | -- | 90 |
KS081 | ||||
8 | HifaxR | JarylecR | 15 | 140 |
KS081 | Exp4 |
Days | Composition Example 6 | Composition Example 3 |
0 | 100.00 | 100.00 |
1 | 100.00 | 99.84 |
4 | 99.97 | 99.32 |
5 | 99.97 | 99.14 |
6 | 99.97 | 99.14 |
8 | 99.75 | 98.6 |
12 | 99.45 | 97.91 |
18 | 99.34 | 96.69 |
28 | 99.24 | 94.92 |
39 | 99.14 | 93.54 |
Claims (52)
- A cable (1) comprising at least one electrical conductor (2) and at least one extruded covering layer (3, 4, 5) based on a thermoplastic polymer material in admixture with a dielectric liquid, wherein:said thermoplastic material comprises a propylene homopolymer or a copolymer of propylene with at least an olefin comonomer selected from ethylene and an α-olefin other than propylene, said homopolymer or copolymer having a melting point greater than or equal to 140°C and a melting enthalpy of from 30 to 100 J/g;said liquid comprises at least one alkylaryl hydrocarbon with at least two non-condensed aromatic rings and a ratio of number of aryl carbon atoms to total number of carbon atoms greater than or equal to 0.6.
- A cable as claimed in claim 1, wherein the ratio of number of aryl carbon atoms to total number of carbon atoms is greater than or equal to 0.7.
- A cable as claimed in claim 1 or 2, wherein the propylene homopolymer or copolymer has a melting point of from 145 to 170°C.
- A cable as claimed in any one of the preceding claims, wherein the propylene homopolymer or copolymer has a melting enthalpy of from 30 to 85 J/g.
- A cable as claimed in any one of the preceding claims, wherein the propylene homopolymer or copolymer has a flexural modulus, measured at ambient temperature, of from 30 to 1400 MPa.
- A cable as claimed in any one of the preceding claims, wherein the propylene homopolymer or copolymer has a flexural modulus, measured at ambient temperature, of from 60 to 1000 MPa.
- A cable as claimed in any one of the preceding claims, wherein the propylene homopolymer or copolymer has a melt flow index, measured at 230°C, of from 0.05 to 10.0 dg/min.
- A cable as claimed in any one of the preceding claims, wherein the propylene homopolymer or copolymer has a melt flow index, measured at 230°C, of from 0.5 to 5.0 dg/min.
- A cable as claimed in any one of the preceding claims, wherein the olefin comonomer is present in a quantity of less than or equal to 15 mol%.
- A cable as claimed in any one of the preceding claims, wherein the olefin comonomer is present in a quantity of less than or equal to 10 mol%.
- A cable as claimed in any one of the preceding claims, wherein the olefin comonomer is ethylene or an α-olefin of formula CH2=CH-R, where R is a linear or branched C2-C10 alkyl.
- A cable as claimed in the preceding claim, wherein the α-olefin is selected from 1-butene, 1-pentene, 4-methyl-1-pentene, 1-hexene, 1-octene, 1-decene, 1-dodecene and the like, or combinations thereof.
- A cable as claimed in any one of the preceding claims, wherein the thermoplastic material is selected from:a) a propylene homopolymer or a copolymer of propylene with at least one olefin comonomer selected from ethylene and an α-olefin other than propylene, having a flexural modulus of from 30 to 900 MPa;b) a heterophase copolymer comprising a thermoplastic phase based on propylene and an elastomeric phase based on ethylene copolymerized with an α-olefin, in which the elastomeric phase is present in a quantity of at least 45 wt% on the total weight of the heterophase copolymer.
- A cable as claimed in the preceding claim, wherein the propylene homopolymer or copolymer under a) has a flexural modulus of from 50 to 400 MPa.
- A cable as claimed in claim 13 or 14, wherein the propylene homopolymer or copolymer under a) has:a melting point of from 140 to 165°C;a melting enthalpy of from 30 to 80 J/g;a fraction soluble in boiling diethyl ether in an amount of less than or equal to 12 wt%, having a melting enthalpy of less than or equal to 4 J/g;a fraction soluble in boiling n-heptane in an amount of from 15 to 60 wt%, having a melting enthalpy from 10 to 40 J/g; anda fraction insoluble in boiling n-heptane in an amount of from 40 to 85 wt%, having a melting enthalpy of greater than or equal to 45 J/g.
- A cable as claimed in any one of claims from 13 to 15, wherein the propylene homopolymer or copolymer of a) has:a fraction soluble in boiling diethyl ether in an amount of from 1 to 10 wt%, having a melting enthalpy of less than or equal to 2 J/g;a fraction soluble in boiling n-heptane in an amount of from 20 to 50 wt%, having a melting enthalpy of from 15 to 30 J/g; anda fraction insoluble in boiling n-heptane in an amount of from 50 to 80 wt%, having a melting enthalpy from 50 to 95 J/g.
- A cable as claimed in claim 13, wherein the α-olefin included in the elastomeric phase of the heterophase copolymer under b) is propylene.
- A cable as claimed in the preceding claim, wherein the elastomeric phase consists of an elastomeric copolymer of ethylene and propylene comprising from 15 to 50 wt% of ethylene and from 50 to 85 wt% of propylene on the weight of the elastomeric phase.
- A cable as claimed in any one of the preceding claims, wherein the base thermoplastic material is the propylene homopolymer or copolymer in mechanical mixture with a low crystallinity polymer having a melting enthalpy of less than or equal to 30 J/g, and a quantity of less than or equal to 70 wt% on the total weight of the thermoplastic material.
- A cable as claimed in the preceding claim, wherein the low crystallinity polymer is in a quantity of from 20 to 60 wt% on the total weight of the thermoplastic material.
- A cable as claimed in claims 19 or 20, wherein the low crystallinity polymer is a copolymer of ethylene with a C3-C12 α-olefin.
- A cable as claimed in claim 19 or 20, wherein the low crystallinity polymer is a copolymer of ethylene with an α-olefin and a diene.
- A cable as claimed in claims 21 or 22, wherein the ethylene copolymer is selected fromi) a copolymer having the following monomer composition: 35-90 mol% of ethylene; 10-65 mol% of α-olefin; 0-10 mol% of a diene;ii) a copolymer having the following monomer composition: 75-97 mol% of ethylene; 3-25 mol% of α-olefin; 0-5 mol% of a diene.
- A cable as claimed in the preceding claim, wherein the ethylene copolymer is selected from a copolymer having the following monomer composition: 90-95 mol% of ethylene; 5-10 mol% of α-olefin; 0-2 mol% of a diene.
- A cable as claimed in any one of claims from 21 to 24, wherein the α-olefin is selected from propylene, 1-hexene and 1-octene.
- A cable as claimed in any one of claims from 22 to 25, wherein the diene has from 4 to 20 carbon atoms.
- A cable as claimed in any one of claims from 22 to 26, wherein the diene is selected from a conjugated or non-conjugated linear diolefin, and a monocyclic or polycyclic diene.
- A cable as claimed in any one of claims from 22 to 27, wherein the diene is selected from 1,3-butadiene, 1,4-hexadiene, 1,6-octadiene, 1,4-cyclohexadiene, 5-ethylidene-2-norbornene, 5-methylene-2-norbornene, 5-vinyl-2-norbornene, or their mixtures and the like.
- A cable as claimed in any one of the preceding claims, wherein the alkylaryl hydrocarbon has a dielectric constant at 25°C of less than or equal to 3.5.
- A cable as claimed in any one of the preceding claims, wherein the dielectric constant at 25°C is less than or equal to 3.
- A cable as claimed in any one of the preceding claims, wherein the dielectric liquid has a kinematic viscosity at 20°C of between 1 and 500 mm2/s.
- A cable as claimed in any one of the preceding claims, wherein the dielectric liquid has a kinematic viscosity at 20°C of between 5 and 100 mm2/s.
- A cable as claimed in any one of the preceding claims, wherein the alkylaryl hydrocarbon has a hydrogen absorption capacity of greater than or equal to 5 mm3/min.
- A cable as claimed in the preceding claim, wherein the hydrogen absorption capacity is greater than or equal to 50 mm3/min.
- A cable as claimed in any one of the preceding claims, wherein an epoxy resin is added to the dielectric liquid in a quantity of less than or equal to 1 wt% on the weight of the liquid.
- A cable as claimed in the preceding claim, wherein the alkylaryl hydrocarbon is present in a quantity of greater than or equal to 10 wt% on the total weight of the dielectric liquid.
- A cable as claimed in any one of the preceding claims, wherein the dielectric liquid comprises at least one alkylaryl hydrocarbon having at least three non-condensed aromatic rings.
- A cable as claimed in any one of the preceding claims, wherein the alkylaryl hydrocarbon is selected from benzyltoluene, benzylxylene, (methylbenzyl)toluene, (methylbenzyl)xylene, dibenzyltoluene, dibenzylxylene, di(methylbenzyl)toluene, di(methylbenzyl)xylene and the like, or their mixtures.
- A cable as claimed in any one of the preceding claims, wherein the dielectric liquid comprises at least one triphenylmethane, either unsubstituted or substituted by at least one radical selected from methyl, benzyl and methylbenzyl.
- A cable as claimed in the preceding claim, wherein the triphenylmethane is selected from ditoluylphenylmethane, dixylylphenylmethane, xylyltoluylphenylmethane and the like, or their mixtures.
- A cable as claimed in any one of the preceding claims, wherein the weight ratio of dielectric liquid to base polymer material is from 1:99 to 25:75.
- A cable as claimed in any one of the preceding claims, wherein the weight ratio of dielectric liquid to base polymer material is from 2:98 to 20:80.
- A cable as claimed in any one of the preceding claims, wherein the weight ratio of dielectric liquid to base polymer material is from 3:97 to 15:85.
- A cable as claimed in any one of the preceding claims, wherein the extruded covering layer is a layer (4) with electrical insulation properties.
- A cable as claimed in any one of claims from 1 to 44, wherein the extruded covering layer is a layer (3, 5) with semiconductive properties.
- A cable as claimed in the preceding claim, wherein a conductive filler is dispersed in the layer with semiconductive properties.
- A cable as claimed in any one of the preceding claims, wherein the base polymer material is selected from propylene homopolymers or copolymers comprising at least 40 wt% of amorphous phase, on the total polymer weight.
- A cable as claimed in any one of the preceding claims, wherein at least one layer with electrical insulation properties and at least one layer with semiconductive properties are present.
- A polymer composition comprising a thermoplastic polymer material in admixture with a dielectric liquid in accordance with any one of claims from I to 49.
- Use of a polymer composition as claimed in claim 50, as base polymer material for the preparation of a covering layer (4) with electrical insulation properties.
- Use of a polymer composition as claimed in claim 50, as base polymer material for the preparation of a covering layer (3, 5) with semiconductive properties.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP01951601A EP1295301B1 (en) | 2000-06-28 | 2001-06-15 | Cable with recyclable covering |
Applications Claiming Priority (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP00113661 | 2000-06-28 | ||
EP00113661 | 2000-06-28 | ||
US21603200P | 2000-07-03 | 2000-07-03 | |
US216032P | 2000-07-03 | ||
PCT/EP2001/006820 WO2002003398A1 (en) | 2000-06-28 | 2001-06-15 | Cable with recyclable covering |
EP01951601A EP1295301B1 (en) | 2000-06-28 | 2001-06-15 | Cable with recyclable covering |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1295301A1 EP1295301A1 (en) | 2003-03-26 |
EP1295301B1 true EP1295301B1 (en) | 2004-04-14 |
Family
ID=8169094
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP01951601A Expired - Lifetime EP1295301B1 (en) | 2000-06-28 | 2001-06-15 | Cable with recyclable covering |
Country Status (11)
Country | Link |
---|---|
EP (1) | EP1295301B1 (en) |
CN (1) | CN1249732C (en) |
AR (1) | AR028766A1 (en) |
AT (1) | ATE264539T1 (en) |
AU (2) | AU2001272485B2 (en) |
BR (1) | BR0112004B1 (en) |
CA (1) | CA2412891C (en) |
DE (1) | DE60102817T2 (en) |
ES (1) | ES2219544T3 (en) |
MY (1) | MY123591A (en) |
WO (1) | WO2002003398A1 (en) |
Families Citing this family (34)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6861143B2 (en) * | 1999-11-17 | 2005-03-01 | Pirelli Cavi E Sistemi S.P.A. | Cable with recyclable covering |
WO2002047092A1 (en) | 2000-12-06 | 2002-06-13 | Pirelli S.P.A. | Process for producing a cable with a recyclable coating |
WO2004066317A1 (en) | 2003-01-20 | 2004-08-05 | Gabriele Perego | Cable with recycable covering layer |
NZ547567A (en) * | 2003-12-03 | 2007-12-21 | Prysmian Cavi Sistemi Energia | Impact resistant cable |
ES2346672T3 (en) | 2005-10-25 | 2010-10-19 | Prysmian S.P.A. | POWER CABLE THAT INCLUDES A DIELECTRIC FLUID AND A MIXTURE OF THERMOPLASTIC POLYMERS. |
ES2621851T3 (en) * | 2006-11-15 | 2017-07-05 | Prysmian S.P.A. | Power cable |
US7999188B2 (en) | 2007-06-28 | 2011-08-16 | Prysmian S.P.A. | Energy cable |
WO2011092533A1 (en) | 2010-01-29 | 2011-08-04 | Prysmian S.P.A. | Energy cable |
WO2012069864A1 (en) | 2010-11-25 | 2012-05-31 | Prysmian S.P.A. | Energy cable having a voltage stabilized thermoplastic electrically insulating layer |
KR101831776B1 (en) | 2010-12-23 | 2018-02-23 | 프리즈미안 에스피에이 | Continuous process for manufacturing a high voltage power cable |
WO2012085612A1 (en) | 2010-12-23 | 2012-06-28 | Prysmian S.P.A. | Energy cable having stabilized dielectric resistance |
DE102011075786A1 (en) * | 2011-05-13 | 2012-11-15 | Siemens Aktiengesellschaft | Electrical component |
HUE034073T2 (en) | 2011-08-04 | 2018-01-29 | Prysmian Spa | Energy cable having a thermoplastic electrically insulating layer |
US9697927B2 (en) | 2011-12-23 | 2017-07-04 | Prysmian S.P.A. | Cable comprising an element indicating water infiltration and method using said element |
CN104364853B (en) | 2012-05-18 | 2018-03-16 | 普睿司曼股份公司 | The method of energy cable of the production with thermoplasticity electric insulation layer |
US10297372B2 (en) | 2012-05-18 | 2019-05-21 | Prysmian S.P.A | Process for producing an energy cable having a thermoplastic electrically insulating layer |
CA2881021C (en) * | 2012-09-27 | 2020-09-22 | Dow Global Technologies Llc | Process for reducing peroxide migration in crosslinkable ethylene-based polymer compositions |
JP6092481B2 (en) | 2013-08-12 | 2017-03-08 | エービービー テクノロジー エルティーディー. | Thermoplastic blend composition for cable insulation |
CN103714902A (en) * | 2014-01-14 | 2014-04-09 | 深圳市东佳信电线电缆有限公司 | Special-structure environment-friendly power cable for transformer connection |
WO2016005791A1 (en) | 2014-07-08 | 2016-01-14 | Prysmian S.P.A. | Energy cable having a thermoplastic electrically insulating layer |
US10217544B2 (en) | 2014-12-17 | 2019-02-26 | Prysmian S.P.A | Energy cable having a cold-strippable semiconductive layer |
WO2016150473A1 (en) | 2015-03-20 | 2016-09-29 | Prysmian S.P.A. | Water-tight power cable with metallic screen rods |
BR112018005361B1 (en) * | 2015-09-25 | 2022-07-26 | Prysmian S.P.A. | POWER CORD, AND, PROCESS TO PRODUCE A POWER CORD |
AU2015412459B2 (en) | 2015-10-23 | 2020-08-27 | Prysmian S.P.A. | Joint for electric cables with thermoplastic insulation and method for manufacturing the same |
CN105845226B (en) * | 2016-04-05 | 2019-04-26 | 江苏亨通高压海缆有限公司 | Waterproof submarine cable |
BR112019010814A2 (en) | 2016-11-30 | 2019-10-01 | Prysmian Spa | power cord with an insulation system. |
WO2018122572A1 (en) | 2016-12-27 | 2018-07-05 | Prysmian S.P.A. | Electric cable having a protecting layer |
FR3068038B1 (en) | 2017-06-21 | 2020-09-18 | Nexans | POLYMERIC COMPOSITION INCLUDING A POLAR DIELECTRIC LIQUID |
FR3069799B1 (en) | 2017-08-01 | 2020-09-18 | Nexans | METHOD OF MANUFACTURING AN ELECTRIC CABLE BY EXTRUSION OF A COMPOSITION BASED ON A POLYMER OF PROPYLENE AND A DIELECTRIC LIQUID |
EP3695424B1 (en) | 2017-10-12 | 2022-06-15 | Prysmian S.p.A. | Electric cable with improved thermoplastic insulating layer |
IT201800007853A1 (en) | 2018-08-03 | 2020-02-03 | Prysmian Spa | HIGH VOLTAGE THREE-PHASE CABLE. |
IT202000032015A1 (en) | 2020-12-23 | 2022-06-23 | Prysmian Spa | MEDIUM VOLTAGE ELECTRIC CABLE WITH BETTER FIRE BEHAVIOR |
FR3125354A1 (en) | 2021-07-19 | 2023-01-20 | Nexans | Method for manufacturing an electric cable by extruding a composition based on a propylene polymer and a dielectric liquid with a barrier screw comprising a mixing section |
EP4390976A1 (en) | 2022-12-23 | 2024-06-26 | Nexans | Covering layer obtained from a polymer composition comprising at least one thermoplastic polymer material and at least one compound comprising at least one nitrile group |
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Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB2062671B (en) * | 1979-11-08 | 1983-09-07 | Nissin Electric Co Ltd | Electric device comprising electrical insulating material |
JPH088010B2 (en) * | 1986-09-04 | 1996-01-29 | 日本石油化学株式会社 | Electrical insulating oil composition |
ATE201280T1 (en) * | 1997-01-17 | 2001-06-15 | Nkt Cables As | ELECTRICAL CABLES |
EP1021809A1 (en) * | 1997-09-09 | 2000-07-26 | Nkt Research Center A/S | An electrically insulating material, method for the preparation thereof, and insulated objects comprising said material |
-
2001
- 2001-06-15 BR BRPI0112004-2A patent/BR0112004B1/en not_active IP Right Cessation
- 2001-06-15 CA CA002412891A patent/CA2412891C/en not_active Expired - Lifetime
- 2001-06-15 AU AU2001272485A patent/AU2001272485B2/en not_active Expired
- 2001-06-15 WO PCT/EP2001/006820 patent/WO2002003398A1/en active IP Right Grant
- 2001-06-15 ES ES01951601T patent/ES2219544T3/en not_active Expired - Lifetime
- 2001-06-15 DE DE60102817T patent/DE60102817T2/en not_active Expired - Lifetime
- 2001-06-15 AT AT01951601T patent/ATE264539T1/en active
- 2001-06-15 AU AU7248501A patent/AU7248501A/en active Pending
- 2001-06-15 CN CNB01811959XA patent/CN1249732C/en not_active Expired - Fee Related
- 2001-06-15 EP EP01951601A patent/EP1295301B1/en not_active Expired - Lifetime
- 2001-06-21 MY MYPI20012939 patent/MY123591A/en unknown
- 2001-06-28 AR ARP010103079A patent/AR028766A1/en active IP Right Grant
Also Published As
Publication number | Publication date |
---|---|
CA2412891A1 (en) | 2002-01-10 |
DE60102817T2 (en) | 2004-09-30 |
WO2002003398A1 (en) | 2002-01-10 |
MY123591A (en) | 2006-05-31 |
ATE264539T1 (en) | 2004-04-15 |
CA2412891C (en) | 2009-09-22 |
EP1295301A1 (en) | 2003-03-26 |
CN1503977A (en) | 2004-06-09 |
ES2219544T3 (en) | 2004-12-01 |
DE60102817D1 (en) | 2004-05-19 |
AU7248501A (en) | 2002-01-14 |
BR0112004A (en) | 2003-05-13 |
AR028766A1 (en) | 2003-05-21 |
CN1249732C (en) | 2006-04-05 |
AU2001272485B2 (en) | 2005-04-28 |
BR0112004B1 (en) | 2010-11-16 |
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