CN109320832A - EP rubbers semiconductive inner shield material that can be effectively crosslinked and preparation method thereof - Google Patents
EP rubbers semiconductive inner shield material that can be effectively crosslinked and preparation method thereof Download PDFInfo
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- CN109320832A CN109320832A CN201811161292.1A CN201811161292A CN109320832A CN 109320832 A CN109320832 A CN 109320832A CN 201811161292 A CN201811161292 A CN 201811161292A CN 109320832 A CN109320832 A CN 109320832A
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- 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
- C08L23/0846—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
- C08L23/0853—Vinylacetate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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- 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
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
- C08L2312/08—Crosslinking by silane
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Abstract
The invention discloses the EP rubbers semiconductive inner shield material and preparation method thereof that one kind can be effectively crosslinked, and form after expecting and being catalyzed B material mixing by mass ratio for the grafting A of 5~9:1 through warm water crosslinking；Wherein: the grafting A material composition, by weight are as follows: 60~90 parts of EP rubbers, 10~40 parts of ethylene-vinyl acetate copolymer, 1~4 part of silane, 0.2~1 part of initiator, 1~4 part of anti-aging agent, 2~5 parts of promotor, 5~15 parts of softening agent；1~5 part of lubricant；The catalysis B material composition, by weight are as follows: 100 parts of ethylene-vinyl acetate copolymer, 90~125 parts of conductive filler, 10~20 parts of lubricant, 1~5 part of dispersing agent, 0.5~3 part of catalyst, 0.5~2 part of antioxidant.The EP rubbers semiconductive inner shield material that can be effectively crosslinked of the invention has good conductive property, and can especially guarantee that product is effectively crosslinked.
Description
Technical field
The present invention relates to a kind of wire and cable semiconductive modified materials, more particularly to a kind of the third rubber of second that can be effectively crosslinked
Glue semiconductive inner shield material and preparation method thereof.
Background technique
As society and expanding economy, power consumption are continuously increased, high pressure, super-pressure power supply are more and more.High pressure,
In super-pressure service cable, when semiconductive shieldin material essential material, it is radial that main function improves cable internal electric field
Distribution, homogenizing electric field directly or indirectly improve the service life of cable to improve the electrical strength of cable.In shielding material mark
In standard, there are many shielding material of type, but still account for absolute majority both at home and abroad with the shielding material of peroxide crosslinking.In medium voltage electricity
In cable, 10kV chemical crosslinking power cable dosage is very big, and cross-linking type semiconductive inner shield material used is almost all peroxide
Cross-linking type.With the progress of raw material technology of preparing, it is originally used for the organosilane crosslinked polyethylene of low tension wire cable product, is existed
It is applied in 10kV power cable.If inner shield partly can be led using organosilane crosslinked polyethylene and silane-crosslinkable simultaneously
Material produces medium-pressure power cable by the way of steam or warm water crosslinking, with use processes for chemically crosslinked polyethylene, peroxide crosslinking
The mode that shielding material, connection curing tube are crosslinked is compared, and efficiency and cost will be greatly reduced.Therefore, exploitation can be effectively crosslinked
EP rubbers semiconductive inner shield material will become the research and development hot spot in industry.At present about silane-crosslinkable inner shield
The document report or related patents of material are actually rare, and patent CN107868328A is prepared for silane-crosslinkable in such a way that A, B expect
Semiconductive shieldin material.But in the mixed proportion of its A, B material, B expects that proportion is larger, while the content of carbon black in A material is higher, leads
Cause crosslinkable moiety in material less, it is difficult to form the product being effectively crosslinked, it is difficult to guarantee that product is effectively handed over by verifying product
The molten experiment of the leaching of connection.
Summary of the invention
The object of the present invention is to provide a kind of preparations different from silane-crosslinkable semiconductive shieldin material reported at present
Technology provides a kind of EP rubbers semiconductive inner shield material that can be effectively crosslinked and preparation method thereof that can be effectively crosslinked, the material
Material has good conductive property, and can especially guarantee that product is effectively crosslinked, and can be used as the inner shield material of midium voltage cable cable.
The technical solution for realizing the object of the invention is the EP rubbers semiconductive inner shield material that can be effectively crosslinked, described to have
The raw material composition for imitating the EP rubbers semiconductive inner shield material of crosslinking is expected for the grafting A for being 5~9:1 by mass ratio and catalysis B material
It is formed after mixing through warm water crosslinking；Wherein:
The grafting A material composition, by weight are as follows: 60~90 parts of EP rubbers, ethylene-vinyl acetate copolymer 10~
40 parts, 1~4 part of silane, 0.2~1 part of initiator, 1~4 part of anti-aging agent, 2~5 parts of promotor, 5~15 parts of softening agent；Lubricant
1~5 part；
The catalysis B material composition, by weight are as follows: 100 parts of ethylene-vinyl acetate copolymer, conductive filler 90~125
Part, 10~20 parts of lubricant, 1~5 part of dispersing agent, 0.5~3 part of catalyst, 0.5~2 part of antioxidant；
The ethylene-vinyl acetate copolymer being grafted in A material, VA content are 15%~20%, the ethylene-in catalysis B material
Acetate ethylene copolymer, VA content are 25%~30%, the melt flow rate (MFR) under 190 DEG C, the test condition of 2.16kg
For 2.3~7.5g/10min.
Preferably, the mass ratio of the grafting A material and catalysis B material is preferably 6~9:1, it is cross-linking in material to improve
The content of component, guarantees crosslink material validity, and the mass ratio that grafting A material and catalysis B expect is more preferably 8~9:1；The temperature
Water crosslinking is carried out in progress or steam in about 90 DEG C of water.
The conductive filler is one of highly conductive carbon black, carbon nanotube, graphene or a variety of combinations, and synthesis is examined
Consider cost, additive amount, electric conductivity, preferably highly conductive carbon black and carbon nanotube.
The silane is selected from vinyltrimethoxysilane, vinyl-three (2- methoxy ethoxy) silane, vinyl
Triethoxysilane, three tert-butoxy silane of vinyl, vinyl silane tri-butyl peroxy, vinyltriacetoxy silane
One of or a variety of combinations guarantee within the defined warm water crosslinking time real to make material that there is faster crosslinking rate
It is existing full cross-linked, preferably vinyltrimethoxysilane.
The antioxidant is selected from antioxidant 1010, antioxidant 1024, antioxidant 1076, irgasfos 168, antioxidant
One of 300 or a variety of combinations, it is to guarantee that material has good resistant to thermal aging and resistance to metal-catalyzed ageing properties, preferably
For the antioxidant 300 with radical terminator and hydrogen peroxide decomposition agent dual function and there is metallic ion passivation effect
Antioxidant 1024 be used in mixed way.
The initiator is peroxide initiator, is selected from di-tert-butyl peroxide, dibenzoyl peroxide, peroxide
Change diisopropylbenzene (DIPB), new peroxide tert-butyl caprate, peroxide acetic acid butyl ester, peroxidized t-butyl perbenzoate, the tertiary fourth of 1,1- bis-
- 3,3,5 trimethyl-cyclohexane of base peroxidating, 4,4- bis- (tert-butyl hydroperoxide) n-butyl pentanoate, methyl ethyl ketone peroxide, peroxidating
One of hexamethylene or a variety of combinations, it is contemplated that technical maturity, preferably cumyl peroxide.
The anti-aging agent is RD.
The promotor is zinc oxide.
The softening agent is white oil.
The lubricant is stearic acid.
The dispersing agent is selected from for one of TAS-2A, EBS, nanometer calcium carbonate or a variety of combinations, preferably
EBS。
The catalyst is selected from dibutyl tin dilaurate, Bis(lauroyloxy)dioctyltin, stannous octoate, two acetic acid
One of dibutyl tin, two (dodecyl sulphur) dibutyl tins, two mercaptan tin alkyls, dialkyl tin dimaleate are a variety of
Combination, it is contemplated that technical maturity, preferably dibutyl tin dilaurate.
Meanwhile the preparation method for the EP rubbers semiconductive inner shield material that can be effectively crosslinked the present invention also provides one kind, tool
Body step are as follows:
By weight, successively by 60~90 parts of EP rubbers, 10~40 parts of ethylene-vinyl acetate copolymer, silane 1
~4 parts, 0.2~1 part of initiator, 1~4 part of anti-aging agent, 2~5 parts of promotor, 5~15 parts of softening agent；1~5 part of lubricant is by setting
Certainty ratio is added in mixer, starts to be kneaded immediately after, and discharging is sent into taper and is fed when mixing to material temperature is 110 DEG C~120 DEG C
Hopper is granulated, cold cut through twin-screw, and product is made.Wherein, preferably extruder temperature of each section is successively are as follows: extruder temperature of each section
Successively are as follows: 120~145 DEG C of an area, two 155~175 DEG C of areas, three 180~190 DEG C of areas, four 190~200 DEG C of areas, five areas 190~
200 DEG C, six 185~195 DEG C of areas, seven 180~185 DEG C of areas, eight 170~180 DEG C of areas, nine 165~175 DEG C of areas, head temperature 140
~150 DEG C.
By weight, by 100 parts of ethylene-vinyl acetate copolymer, 90~125 parts of conductive filler, lubricant 10~20
Part, it 1~5 part of dispersing agent, 0.5~3 part of catalyst, is squeezed out after 0.5~2 part of antioxidant mixing through reciprocating single-bolt extruder,
It is granulated, preparation catalysis B material；
A material and the respective packaging of catalysis B material are grafted to get finished product.
After above-mentioned technical proposal, the present invention has the effect of below positive:
Semiconductive inner shield material of the invention is realized by using the better conductive black of electric conductivity or conductive powder body
The reduction of the conductive powder body additive amount of common low electric conductivity energy in shielding material；On the basis of the reduction of conductive powder body additive amount,
The further conductive powder body by script addition in A material, addition is in B material；Being used in combination through the above technical solution, greatly improves
The ratio of crosslinkable component in material makes material be easy to get higher crosslinking degree, realizes effectively crosslinking, guarantees by micro-
The decahydronaphthalenes of boiling soaks molten test in 5 hours.
Specific embodiment
The above description is only an overview of the technical scheme of the present invention, in order to better understand the technical means of the present invention,
And it can be implemented in accordance with the contents of the specification, and in order to allow above and other objects of the present invention, feature and advantage can
It is clearer and more comprehensible, the followings are specific embodiments of the present invention.
(embodiment 1)
The present embodiment provides the EP rubbers semiconductive inner shield material that can be effectively crosslinked that one kind can be effectively crosslinked, raw materials
Include:
A material, successively by 65 parts of EP rubbers, 35 parts of ethylene-vinyl acetate copolymers, 1.5 parts of vinyl trimethoxies
Silane, 0.3 part of cumyl peroxide, 3 parts of anti-aging agent RDs, 4.5 parts of promotor zinc oxide, 14 parts of softening agent white oils；4 parts of tristearin
Acid is added in mixer by setting ratio, starts to be kneaded immediately after, and discharging is sent into when mixing to material temperature is 110 DEG C~120 DEG C
Taper feeding hopper is granulated, cold cut through twin-screw, and A material is made.Wherein, preferably extruder temperature of each section is successively are as follows: each section of extruder
Temperature is successively are as follows: 125 DEG C of an area, two 160 DEG C of areas, three 180 DEG C of areas, four 190 DEG C of areas, five 190 DEG C of areas, six 185 DEG C of areas, 7th area
180 DEG C, eight 170 DEG C of areas, nine 165 DEG C of areas, 145 DEG C of head temperature.
B material, by 100 parts of ethylene-vinyl acetate copolymers, 90 parts of conductive fillers (highly conductive carbon black), 10 parts of white oils, 2 parts
EBS, 0.6 part of zinc stearate, 1 part of dibutyl tin dilaurate, 0.8 part of antioxidant 300, by automatic gauge scale device, automatically
Blanking enters extruding pelletization in reciprocating single screw rod, and catalyst B material is made.
Grafting A material and catalysis B material are mixed with mass ratio 6:1, after extrusion molding, handed in about 90 DEG C of water
Connection is to get the silane-crosslinkable EP rubbers semiconductive inner shield material that can be effectively crosslinked.
The performance test results are shown in Table 1.
(embodiment 2)
A material, successively by 75 parts of EP rubbers, 25 parts of ethylene-vinyl acetate copolymers, 2.5 parts of vinyl trimethoxies
Silane, 0.6 part of cumyl peroxide, 2 parts of anti-aging agent RDs, 3.5 parts of promotor zinc oxide, 10 parts of softening agent white oils；3 parts of tristearin
Acid is added in mixer by setting ratio, starts to be kneaded immediately after, and discharging is sent into when mixing to material temperature is 110 DEG C~120 DEG C
Taper feeding hopper is granulated, cold cut through twin-screw, and A material is made.Wherein, preferably extruder temperature of each section is successively are as follows: each section of extruder
Temperature is successively are as follows: 125 DEG C of an area, two 160 DEG C of areas, three 180 DEG C of areas, four 190 DEG C of areas, five 190 DEG C of areas, six 185 DEG C of areas, 7th area
180 DEG C, eight 170 DEG C of areas, nine 165 DEG C of areas, 145 DEG C of head temperature.
B material, by 100 parts of ethylene-vinyl acetate copolymers, 110 parts of conductive filler (groups of carbon nanotube and highly conductive carbon black
Close object), 10 parts of white oils, 3 parts of EBS, 0.8 part of zinc stearate, 1.5 parts of dibutyl tin dilaurates, 1.3 parts of antioxidant 300s pass through
Automatic gauge scale device, automatic blanking enter extruding pelletization in reciprocating single screw rod, and catalyst B material is made.
Grafting A material and catalysis B material are mixed with mass ratio 8:1, after extrusion molding, handed in about 90 DEG C of water
Connection is to get the silane-crosslinkable EP rubbers semiconductive inner shield material that can be effectively crosslinked.
The performance test results are shown in Table 1.
(embodiment 3)
The present embodiment provides the EP rubbers semiconductive inner shield material that can be effectively crosslinked that one kind can be effectively crosslinked, raw materials
Include:
The preparation of A material: successively by 90 parts of EP rubbers, 10 parts of ethylene-vinyl acetate copolymers, 3.5 parts of vinyl three
Methoxy silane, 0.8 part of cumyl peroxide, 1.5 parts of anti-aging agent RDs, 2.5 parts of promotor zinc oxide, 6 parts of softening agent white oils；
2 parts of stearic acid are added in mixer by setting ratio, start to be kneaded immediately after, and mixing to material temperature goes out when being 110 DEG C~120 DEG C
Material is sent into taper feeding hopper, is granulated through twin-screw, cold cut, and A material is made.Wherein, preferably extruder temperature of each section is successively are as follows: squeezes out
Machine temperature of each section is successively are as follows: 125 DEG C of an area, two 160 DEG C of areas, and three 180 DEG C of areas, four 190 DEG C of areas, five 190 DEG C of areas, six 185 DEG C of areas,
Seven 180 DEG C of areas, eight 170 DEG C of areas, nine 165 DEG C of areas, 145 DEG C of head temperature.
The preparation of B material: by 100 parts of ethylene-vinyl acetate copolymers, 125 parts of conductive fillers (graphene), 10 parts of white oils, 4
Part EBS, 1 part of zinc stearate, 2.5 parts of dibutyl tin dilaurates, 1.8 parts of antioxidant 300s, by automatic gauge scale device, certainly
Dynamic blanking enters extruding pelletization in reciprocating single screw rod, and catalyst B material is made.
Grafting A material and catalysis B material are mixed with mass ratio 9:1, after extrusion molding, handed in about 90 DEG C of water
Connection is to get the silane-crosslinkable EP rubbers semiconductive inner shield material that can be effectively crosslinked.
The performance test results are shown in Table 1.
Table 1
In the present invention, by using the better conductive black of some electric conductivities or similar components, carbon black can be reduced
Content improves resin, that is, crosslinkable moiety ratio, while the component that conductive black or similar components are expected as B, is made into simultaneous
Have catalysis and semiconductive masterbatch, then mixed with A material, forms final products, thus crosslinkable component ratio is few in solution material,
It cannot be guaranteed that the problem of product is effectively crosslinked, develops the EP rubbers semiconductive inner shield that can be effectively crosslinked that can be effectively crosslinked
Material.
Particular embodiments described above has carried out further in detail the purpose of the present invention, technical scheme and beneficial effects
It describes in detail bright, it should be understood that the above is only a specific embodiment of the present invention, is not intended to restrict the invention, it is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in guarantor of the invention
Within the scope of shield.
Claims (10)
1. the EP rubbers semiconductive inner shield material that can be effectively crosslinked, it is characterised in that: the EP rubbers that can be effectively crosslinked
It is that the grafting A for being 5~9:1 by mass ratio expects and catalysis B expects after mixing through warm water crosslinking that the raw material of semiconductive inner shield material, which forms,
It forms；Wherein:
The grafting A material composition, by weight are as follows: 60~90 parts of EP rubbers, ethylene-vinyl acetate copolymer 10~40
Part, 1~4 part of silane, 0.2~1 part of initiator, 1~4 part of anti-aging agent, 2~5 parts of promotor, 5~15 parts of softening agent；Lubricant 1
~5 parts；
The catalysis B material composition, by weight are as follows: 100 parts of ethylene-vinyl acetate copolymer, 90~125 parts of conductive filler, profit
10~20 parts of lubrication prescription, 1~5 part of dispersing agent, 0.5~3 part of catalyst, 0.5~2 part of antioxidant；
The ethylene-vinyl acetate copolymer being grafted in A material, VA content are 15%~20%, the ethyl vinyl acetate in catalysis B material
Ethylene copolymer, VA content are 25%~30%, and the melt flow rate (MFR) under 190 DEG C, the test condition of 2.16kg is 2.3
~7.5g/10min.
2. the EP rubbers semiconductive inner shield material according to claim 1 that can be effectively crosslinked, it is characterised in that: described
Conductive filler is one of highly conductive carbon black, carbon nanotube, graphene or a variety of combinations.
3. the EP rubbers semiconductive inner shield material according to claim 1 that can be effectively crosslinked, it is characterised in that: described anti-
Old agent is RD, and the promotor is zinc oxide, and the softening agent is white oil.
4. the EP rubbers semiconductive inner shield material according to claim 1 that can be effectively crosslinked, it is characterised in that: described
Silane is vinyl silanes, is selected from vinyltrimethoxysilane, vinyl-three (2- methoxy ethoxy), three second of vinyl
Oxysilane, three tert-butoxy silane of vinyl, vinyl silane tri-butyl peroxy, in vinyltriacetoxy silane
One or more combinations.
5. the EP rubbers semiconductive inner shield material according to claim 1 that can be effectively crosslinked, it is characterised in that: described
Antioxidant is selected from one of antioxidant 1010, antioxidant 1024, antioxidant 1076, irgasfos 168, antioxidant 300 or more
The combination of kind.
6. the EP rubbers semiconductive inner shield material according to claim 1 that can be effectively crosslinked, it is characterised in that: described to draw
Hair agent is peroxide type initiators, is selected from di-tert-butyl peroxide, dibenzoyl peroxide, cumyl peroxide, mistake
Aoxidize the neodecanoic acid tert-butyl ester, peroxide acetic acid butyl ester, peroxidized t-butyl perbenzoate, 1,1- di-tert-butyl peroxide -3,3,5
One of trimethyl-cyclohexane, 4,4- bis- (tert-butyl hydroperoxide) n-butyl pentanoate, methyl ethyl ketone peroxide, cyclohexane peroxide
Or a variety of combination.
7. the EP rubbers semiconductive inner shield material according to claim 1 that can be effectively crosslinked, it is characterised in that: described
Lubricant is stearic acid.
8. the EP rubbers semiconductive inner shield material according to claim 1 that can be effectively crosslinked, it is characterised in that: described
Dispersing agent is selected from for one of TAS-2A, EBS, nanometer calcium carbonate or a variety of combinations.
9. the EP rubbers semiconductive inner shield material according to claim 1 that can be effectively crosslinked, it is characterised in that: described
Catalyst is selected from dibutyl tin dilaurate, Bis(lauroyloxy)dioctyltin, stannous octoate, dibutyltin diacetate, two (ten
Dialkyl group sulphur) dibutyl tin, two mercaptan tin alkyls, one of dialkyl tin dimaleate or a variety of combinations.
10. the preparation method for the EP rubbers semiconductive inner shield material that can be effectively crosslinked, it is characterised in that: specific steps are as follows:
By weight, successively by 60~90 parts of EP rubbers, 10~40 parts of ethylene-vinyl acetate copolymer, silane 1~4
Part, 0.2~1 part of initiator, 1~4 part of anti-aging agent, 2~5 parts of promotor, 5~15 parts of softening agent；1~5 part of lubricant by setting
Ratio is added in mixer, starts to be kneaded immediately after, and taper feeding is sent into discharging when mixing to material temperature is 110 DEG C~120 DEG C
Bucket is granulated, cold cut through twin-screw, and product is made.Wherein, preferably extruder temperature of each section is successively are as follows: extruder temperature of each section according to
It is secondary are as follows: 120~145 DEG C of an area, two 155~175 DEG C of areas, three 180~190 DEG C of areas, four 190~200 DEG C of areas, five areas 190~200
DEG C, six 185~195 DEG C of areas, seven 180~185 DEG C of areas, eight 170~180 DEG C of areas, nine 165~175 DEG C of areas, head temperature 140~
150℃。
By weight, by 100 parts of ethylene-vinyl acetate copolymer, 90~125 parts of conductive filler, 10~20 parts of lubricant, point
It 1~5 part of powder, 0.5~3 part of catalyst, squeezes out, is granulated through reciprocating single-bolt extruder after 0.5~2 part of antioxidant mixing,
Preparation catalysis B material；
A material and the respective packaging of catalysis B material are grafted to get finished product.
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| CN111825922A (en) * | 2020-06-24 | 2020-10-27 | 苏州通优新材料科技有限公司 | Flame-retardant conductive shielding layer material for automobile engine ECU control system cable and preparation method and application thereof |
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| CN111763374A (en) * | 2020-06-17 | 2020-10-13 | 江阴市海江高分子材料有限公司 | Semiconductive shielding material for polypropylene non-crosslinked cable and preparation method thereof |
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