CN1114928C - Composition for electric cable - Google Patents

Composition for electric cable Download PDF

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Publication number
CN1114928C
CN1114928C CN98810461A CN98810461A CN1114928C CN 1114928 C CN1114928 C CN 1114928C CN 98810461 A CN98810461 A CN 98810461A CN 98810461 A CN98810461 A CN 98810461A CN 1114928 C CN1114928 C CN 1114928C
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composition
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piperidine compound
tetramethyl piperidine
antioxidant
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CN1276907A (en
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R·达默特
B·古斯塔福森
K·利比格
A·斯麦德伯格
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Borealis AS
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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
    • 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
    • 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
    • C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
    • C08K5/3477—Six-membered rings
    • C08K5/3492—Triazines
    • C08K5/34926—Triazines also containing heterocyclic groups other than triazine groups

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Organic Insulating Materials (AREA)
  • Insulated Conductors (AREA)

Abstract

A peroxide-cross-linkable ethylene polymer composition for an insulating layer of an electric cable is described. The composition is characterised in that the additives of the composition comprise an N-substituted 2,2,6,6-tetramethylpiperidine compound as an antioxidant and light stabilising agent; and that the composition after 21 days at 135 DEG C has a retained ultimate tensile strength of at least 75 % and a retained ultimate elongation of at least 75 % when tested in accordance with IEC 811. This additive acts as a combined light and thermo-oxidative stabilising agent and inhibits the generation of moisture thereby reducing the risk of water tree formation. Preferably, the composition contains no conventional antioxidants, such as phenolic antioxidants, organic phosphite oxidants and sulphur containing anti-oxidants.

Description

Composition for electric
Technical field
The present invention relates to a kind of composition that is used for cable, more particularly, the present invention relates to a kind of ethylene polymer composition that is used for the insulating barrier of cable (preferred or height or very high voltage power cable).Said composition comprises a kind of ethene polymers and additive, and the latter comprises peroxide cross-linking agent and stabilizer.
Background technology
Cable, particularly in voltage (MV, 1-35kV), high voltage (HV, 35-500kV) and very high voltage (EHV,＞500kV) power cable can be made up of many polymeric layers of extruding around electric conductor.In power cable, at first use semiconductor internal layer coated with conductive body usually, coat with insulating barrier then, the back bag is wrapped water barrier if any, and is wrapped restrictive coating in the outside with the semiconductor skin on skin again.In addition, some HV and EHV cable are encapsulated in the pipe made of aluminum usually.Each of this cable is layer based on dissimilar ethene polymerss, and these polymer are normally crosslinked.
Crosslinked ethene polymers is used for cable insulation.Term " ethene polymers " is meant the polymer based on polyethylene or ethylene copolymer usually and in the present invention, and wherein vinyl monomer constitutes its major part in the copolymer.Therefore, ethene polymers can be made up of the homopolymers or the copolymer of ethene, wherein copolymer can be ethene and one or more can with the copolymer or the graft copolymer of the monomer of ethylene copolymerization.LDPE (low density polyethylene (LDPE), the i.e. polyethylene that under high pressure prepares by radical polymerization) is main cable insulation material at present.As mentioned above, ethene polymers can be an ethylene copolymer, and this moment it comprise the about 25wt% of 0-, preferably one or more of about 1-20wt% can with the comonomer of ethylene copolymerization.Such monomer is well-known to those skilled in the art and need not to exemplify in detail, but can mention that as an example ethene belongs to unsaturated monomer, as C 3-C 8Alhpa olefin, propylene for example, butylene; Alkadienes, for example 1,7-octadiene, 1,9-decadinene; The ethene that contains functional group such as hydroxyl, alkoxyl, carbonyl, carboxyl and ester group belongs to unsaturated monomer.This type of monomer for example can comprise (methyl) acrylic acid and Arrcostab thereof, as (methyl) acrylic acid methyl ester, ethyl ester and butyl ester; Ethene belongs to undersaturated hydrolyzable silane compound, as vinyltrimethoxy silane; Vinyl acetate etc.Yet if ethene polymers is an ethylene copolymer, it is lower that the amount of polar comonomers should keep, so that this polar comonomers accounts for this polyvinyl 10wt% at the most, in order that increase loss factor with exceeding.Will be in greater detail except below the additive, the other parts of the present composition are made of above-mentioned ethene polymers.The polyvinyl amount in the said composition of this means should be about 95-99.7% of said composition weight, preferably about 96-99%.
For the physical property of improving cable insulation and increase its resistance to the different condition influence, the additive total amount that ethene polymers contains is generally about 0.3-5wt%, preferably about 1-4wt%.These additives comprise the stable with additive such as antioxidant of degraded that antagonism is caused by oxidation, radiation etc.; Lubricating additive is as stearic acid; The additive that is used for water-fast tree property (water-tree resistance), as polyethylene glycol, polysiloxanes etc.; And crosslinking additives is as decomposing and cause the crosslinked peroxide of vinyl plastics of this insulation composition when being heated, this additive optional with when forming the reagent initiation by free radical, have the unsaturated compound that forms the cross-bond ability and be used in combination.
In the cable of the above-mentioned type, should avoid the existence of water or moisture, particularly in insulating barrier, because they have deleterious effects to the performance of cable.Moisture causes forming the defective of dendroid branching, promptly so-called water tree, and the latter can cause again rupturing and possible fault.The voltage of cable is high more, and the danger that forms the water tree is big more.Therefore, wish strongly that especially the moisture in the power cable (MV, HV and EHV cable) is reduced to minimum and if possible eliminated moisture with cable.
Moisture in the cable may be derived from moisture in the ambient atmosphere that migrates in the cable or because the moisture that chemical reaction forms in cable on the spot.
In the cable of the ethene polymers insulating barrier of polymer with peroxide crosslinking such as peroxide crosslinking, interact and produce moisture owing to the decomposition of peroxide and with additive in this polymer.Peroxide cross-linking agent commonly used is a dicumyl peroxide, and it especially obtains cumyl alcohol in cross-linking process, and the latter is easy to resolve into AMS and water again.This reaction is increased when promptly the polymer composition that is formed on this insulating barrier of this decomposition and water contains acidic materials strongly by the strong catalysis of acid.Antioxidant in the cable polymer composition is generally sulfur-containing compound, and it is owing to oxidation and be decomposed to form acid, and as sulfenic acids, and these acidic materials influence peroxide breakdown formation water and catabolite such as AMS strongly.
Therefore,, reduce to minimum or suppress wherein moisture, must reduce the moisture that produces owing to peroxide breakdown as much as possible as the moisture in the ethene polymers of the peroxide crosslinking of cable insulation for polymer with the peroxide crosslinking of cable.
Summary of the invention
Have now found that by using stable (HALS) agent of some hindered amine light as composite antioxidant with light stabilizer is got rid of any conventional antioxidant simultaneously such as phenol antioxidant, organic phosphite antioxidant and sulphur-containing antioxidant can significantly reduce because the moisture that peroxide breakdown causes produces, keep excellent resistance to ag(e)ing simultaneously.Surprisingly, this HALS compound is not only as effective light stabilizer, and as effective anti-oxidants, thereby make that said composition can be by the strict demand of thermo oxidative stability, although said composition seldom contains or do not contain conventional antioxidant.
More specifically, the invention provides a kind of ethylene polymer composition that is used for the available peroxide crosslinking of cable insulation, said composition contains the additive that about at the most 5wt% comprises peroxide cross-linking agent and stabilizer, it is characterized in that stabilizer comprises 2 of N-replacement, 2,6,6-tetramethyl piperidine compound is as antioxidant and light stabilizer; And when testing according to IEC811, the residual ultimate tensile strength of 135 ℃ of said compositions after following 21 days at least 75% and residual ultimate elongation be at least 75%.
After finishing watching following specification and appended claims, can understand other distinguishing characteristics of the present invention and advantage.
Sulphur-containing antioxidant is easy to form acidic materials in oxidation with when decomposing and quickens peroxide breakdown and form moisture as mentioned above, have now found that and to use some by 2,2,6, the sterically hindered amine stabilizer that the N-that 6-tetramethyl piperidine compound is formed replaces is as antioxidant, they can not form acidic materials and therefore can not cause the generation of moisture, but can give excellent resistance to ag(e)ing simultaneously.This 2,2,6,6-tetramethyl piperidine compound preferably is used alone as antioxidant.Different 2,2,6,6-tetramethyl piperidine compound can separately or mutually combine and use used as stabilizers in the present composition.Preferred said composition comprises conventional antioxidant seldom or does not comprise conventional antioxidant.This means that the binding capacity of conventional antioxidant such as phenol antioxidant, organic phosphite antioxidant and sulphur-containing antioxidant is at most the 0.15wt% of said composition weight, preferably 0.10wt% at the most.Most preferably said composition does not contain the conventional antioxidant of any this class.
Can by with other additive such as peroxide cross-linking agent, lubricating additive, the additive etc. that is used for water-fast tree property compounding and with 2,2,6,6-tetramethyl piperidine compound mixes in the ethylene polymer composition together.As a rule, the total amount of antioxidant should be about 0.1-1.0wt%, preferably about 0.1-0.5wt%.
As mentioned above, of the present invention 2,2,6,6-tetramethyl piperidine compound is not only as effective light stabilizer, and astoundingly also as very effective antioxidant, for said composition provides thermo oxidative stability.2,2,6 of this N-replacement, the thermo oxidative stability that 6-tetramethyl piperidine compound provides is normally enough for the requirement of cable insulation layer composition, thereby need not to use other antioxidant that thermo oxidative stability is provided.In view of the requirement of thermo oxidative stability for this fact in useful life for being strict for the cable of about 30-40, only use this 2,2,6, it is surprised especially that 6-tetramethyl piperidine compound just can provide enough thermo oxidative stabilities.
Measure thermo oxidative stability according to international standard IEC 811.According to IEC 811, make the dumbbell test piece and test its thermal-oxidative ageing by composition to be evaluated.Conventional test temperature is 135 ℃, but this test is also carried out under 150 ℃.Before beginning to test and afterwards with the limit fracture tensile strength and the limit elongation at break of preset time measuring space said composition.The result is expressed as residual limit fracture tensile strength of % (RUTS) and the residual limit elongation at break of % (RUE), and initial value (ageing time is 0 day) is decided to be 100%.According to the requirement of IEC 811 be 135 ℃ of residual limit fracture tensile strengths (RUTS) after following 21 days should be at least 75% and residual limit elongation at break (RUE) should be 75% at least.But more and more common requirement is at least also should remain 75% at 150 ℃ of RUTS after following 10 days and RUE in cable industry.
2,2,6, what 6-tetramethyl piperidine compound was that N-replaces is necessary.Substituting group is preferably C 1-C 8Alkyl, C 6-C 12Cycloalkyl, C 1-C 10Acyl group or acyloxy or C 1-C 8Alkoxyl.In these substituting groups, preferred C 1-C 8Alkyl or C 1-C 8Alkoxyl.Particularly preferably be C 1-C 4Alkyl is as methyl, ethyl, propyl group or butyl, C 1-C 4Alkoxyl is as methoxyl group, ethyoxyl, propoxyl group or butoxy.
As an example, as 2,2,6 of antioxidant, 6-tetramethyl piperidine compound can be selected from following in the present invention:
Structure Trade (brand) name CHIMASSORB 119
Figure C9881046100092
CGL-116R=
Figure C9881046100093
Figure C9881046100094
TINUVIN 622 (MW is 3100-4000)
Figure C9881046100095
TINUVIN 765 also estimates next compound in order to contrast:
Figure C9881046100101
CHIMASSORB 944 (MW 2500-4000)
In above-claimed cpd, preferred especially at present Chimassorb 119 is as antioxidant of the present invention.
Preferred N-replace 2,2,6,6-tetramethyl piperidine compound should with the ethene polymers resin compatible of said composition.Here used " compatible " is meant should homogeneous phase fusion 2,2,6,6-tetramethyl piperidine compound and vinyl polymerization resin and do not have 2,2,6, the migration of 6-tetramethyl piperidine compound or ooze out.Preferably by with other additive compoundings of said composition with N-replace 2,2,6,6-tetramethyl piperidine compound mixes in the ethylene polymer composition.
In order further to help understanding the present invention, provide some illustratives below, but non-restrictive example.All umbers and percentage number average refer to weight, unless otherwise.
Embodiment Embodiment 1
By compounding by low density polyethylene (LDPE) (LDPE) (density: 922kg/m 3, MFR 2: 0.9g/10min) additive preparation shown in vinyl polymerization resin of Zu Chenging and the various table 1 is used for the composition of cable insulation.
Prepare three kinds of compositions of the present invention (A, B and C) and two kinds of Comparative composition (D and E).Under 220 ℃ with additive and ethene polymers resin compounding.The content of polymers compositions A-E is shown in Table 1.
Table 1
Form wt% Component A B C D ELDPE 97.9 97.7 97.7 97.7 97.7Chimassorb 119 0.2 0.4CGL-116 0.4Chimassorb 944 0.4Irganox  1035 0.2Irganox  PS 802 0.2 methyl styrene dimer bodies 0.4 0.4 0.4 0.4 0.4 dicumyl peroxides 1.5 1.5 1.5 1.5 1.5
Estimate the following performance of composition B-E: respond to change the peroxide that records 180 ℃ of GottfertElastograph-values (Nm) after following 10 minutes; Respectively AMS content after following 40 minutes of 220 ℃ and 250 ℃ (it is to come from the tolerance that the moisture of this peroxide breakdown produces), by the HPLC assay determination.These values are listed in the table 2.
Table 2
The performance of composition B-E Test B C D EElastograph, 180 ℃, 10min 0.81 0.81 0.81 0.66 AMS, 220 ℃, 40 minutes, 100 130 90 3500 (ppm) AMS, 250 ℃, 40 minutes, 200 320 190 4100 (ppm)
No matter present composition B-C and the peroxide response that also has composition D are that peroxide response or low water form significantly better than Comparative composition E as can be found from Table 2.
Content for AMS, find to comprise 2 respectively from table 2,2,6,6-tetramethyl piperidine Compound C himassorb 119, the AMS content that all HALS based composition and use thereof in packaging B-D of the sulphur-containing antioxidant additive of CGL-116 and Chimassorb 944 rather than routine provide obviously reduces, so the generation of moisture also obviously reduces. Embodiment 2The thermal-oxidative ageing performance
The also composition A-D in the test implementation example 1 in thermal-oxidative ageing test.
In this embodiment, measure heat aging performance.Stamp out the dumbbell test piece and at 135 ℃ (composition C and D) and 150 ℃ (composition A-D) the following thermal-oxidative ageing of test different time from crosslinked compression moulding sheet material by preparation of compositions.Before beginning to test and subsequently with the limit fracture tensile strength and the limit elongation at break of preset time measuring space composition.Each value representation is residual limit fracture tensile strength of % (RUTS) and the residual limit elongation at break of % (RUE) in table 2.Initial value when ageing time is 0 day is decided to be 100%.Requirement is to be not less than 75% at 135 ℃ of RUTS after following 21 days and RUE.As previously mentioned, emerging requirement may be defined in 150 ℃ of RUTS after following 10 days and RUE does not reduce to below 75%.IEC811 tests according to international standard.The results are shown in the table 3.
Table 3 Composition Ageing time under 135 ℃ (my god) RUTS (%) RUE (%)C 0 100 100
14 97 91
21 92 84 D 0 100 100
14 96 82
21 85 72 Composition Ageing time under 150 ℃ (my god) RUTS (%) RUE (%)
A 0 100 100
6 85 86
14 75 78
B 0 100 100
10 89 93
C 0 100 100
5 86 78
15 84 76
D 0 100 100
6 86 69
10 79 62
From these results as can be seen present composition A-C all satisfied this two requirements, but not-Chimassorb 944 that N-replaces can not give composition D enough RUE. Embodiment 3Coke burning performance
In Brabender Plasticorder PL 2000-6, estimate coke burning performance down in 135 ℃.The oil that use has Walzenkneaders W7646 adds heat kneading machine 350,287cm 3Measure torque in time, the value T10 that is reported is the time when observing torque increase 10Nm, uses this minimum value of 10Nm point in contrast.In scorch test, there is and do not exist test composition B under the situation of methyl styrene dimer body.The incipient scorch carryover effects of methyl styrene dimer body is easy to find out from these tests, because the T10 value that records in the composition that does not contain this methyl styrene dimer body is 33 minutes, and the T10 value that records in the composition that contains this methyl styrene dimer body is 55 minutes.
Also tested another potential incipient scorch additive Irganox HP-136, it substitutes the methyl styrene dimer body in composition A, and other condition among the composition A remains unchanged.It is crosslinked poor slightly and the T10 value is shorter to find, but still can replace the methyl styrene dimer body.

Claims (8)

  1. Separately as the N-of unique antioxidant and light stabilizer replace 2,2,6,6-methyl piperidine compound is in the purposes of the ethylene polymer composition of the available peroxide crosslinking that is used for cable insulation, said composition comprises the additive of 5wt% at the most, described additive comprises peroxide cross-linking agent and stabilizer, when testing according to IEC811, the residual ultimate tensile strength of 135 ℃ of said compositions after following 21 days at least 75% and residual ultimate elongation be at least 75%.
  2. 2. according to the purposes of claim 1, wherein 2,2,6,6-tetramethyl piperidine compound C 1-C 8Alkyl, C 6-C 12Cycloalkyl, C 1-C 10Acyl group or acyloxy or C 1-C 8Alkoxyl N-replaces.
  3. 3. according to the purposes of claim 2, wherein 2,2,6,6-tetramethyl piperidine compound C 1-C 4Alkyl N-replaces.
  4. 4. according to the purposes of claim 1, wherein add comprise be selected from following 2,2,6,6-tetramethyl piperidine compound:
    Figure C9881046100021
    R=
    Figure C9881046100031
    MW is 3100-4000;
  5. 5. according to the purposes of claim 4, wherein 2,2,6,6-tetramethyl piperidine compound is
    Figure C9881046100034
  6. 6. according to each purposes among the claim 1-5, wherein said composition with the amount of 0.1-0.5wt% comprise that N-replaces 2,2,6,6-tetramethyl piperidine compound.
  7. 7. according to each purposes among the claim 1-5, when wherein testing according to IEC811, the residual ultimate tensile strength of 150 ℃ of said compositions after following 10 days at least 75% and residual ultimate elongation be at least 75%.
  8. 8. according to the purposes of claim 6, when wherein testing according to IEC811, the residual ultimate tensile strength of 150 ℃ of said compositions after following 10 days at least 75% and residual ultimate elongation be at least 75%.
CN98810461A 1997-10-22 1998-10-21 Composition for electric cable Expired - Fee Related CN1114928C (en)

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SE9703844A SE9703844D0 (en) 1997-10-22 1997-10-22 Composition for electric cables

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CN1114928C true CN1114928C (en) 2003-07-16

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CN107771197A (en) * 2015-06-17 2018-03-06 陶氏环球技术有限责任公司 Include the cable insulation compositions of phosphorous antioxidant

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US6455616B1 (en) * 2000-03-07 2002-09-24 Union Carbide Chemicals & Plastics Technology Corporation Polyethylene crosslinkable composition
US6858296B1 (en) 2000-10-05 2005-02-22 Union Carbide Chemicals & Plastics Technology Corporation Power cable
US6656986B2 (en) 2001-03-01 2003-12-02 Union Carbide Chemicals & Plastics Technology Corporation Polyethylene crosslinkable composition
CN100347792C (en) * 2005-02-24 2007-11-07 无锡江南电缆有限公司 Flame-proof power cable for track traffic and process for manufacture
BR112013011987A2 (en) * 2010-11-25 2016-08-30 Prysmian Spa cable
ES2539486T3 (en) * 2010-12-23 2015-07-01 Prysmian S.P.A. Power cable with stabilized dielectric resistance
RU2505565C1 (en) * 2012-12-07 2014-01-27 Закрытое акционерное общество "МЕТАКЛЭЙ" (ЗАО "МЕТАКЛЭЙ") Silanol-crosslinkable composition for cable insulation
CA2922839C (en) 2013-09-13 2021-10-26 Dow Global Technologies Llc Peroxide-crosslinkable compositions and processes for their manufacture
PL3192633T3 (en) 2016-01-15 2019-02-28 Buss Ag Installation and method for manufacturing cross-linkable polyethylene compounds
US11236220B2 (en) 2017-04-27 2022-02-01 Dow Global Technologies Llc Polyethylene blend composition
EP3401929A1 (en) * 2017-05-09 2018-11-14 Borealis AG Cable insulation
US11674016B2 (en) * 2017-12-18 2023-06-13 Borealis Ag Crosslinkable composition with antioxidant and methane formation and article

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CN107771197B (en) * 2015-06-17 2020-12-01 陶氏环球技术有限责任公司 Cable insulation composition comprising a phosphorus-containing antioxidant

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WO1999021194A8 (en) 1999-06-24
TW589645B (en) 2004-06-01
BR9812937A (en) 2000-11-21
CN1276907A (en) 2000-12-13
RU2191439C2 (en) 2002-10-20
EP1025568A1 (en) 2000-08-09
WO1999021194A1 (en) 1999-04-29
NO20001913L (en) 2000-04-12
NO20001913D0 (en) 2000-04-12
SE9703844D0 (en) 1997-10-22
PL340078A1 (en) 2001-01-15
JP2001521264A (en) 2001-11-06
AU726326B2 (en) 2000-11-02

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