CN111331935A - Double-layer composite cold-shrink sleeve and preparation method thereof - Google Patents
Double-layer composite cold-shrink sleeve and preparation method thereof Download PDFInfo
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- CN111331935A CN111331935A CN202010255898.2A CN202010255898A CN111331935A CN 111331935 A CN111331935 A CN 111331935A CN 202010255898 A CN202010255898 A CN 202010255898A CN 111331935 A CN111331935 A CN 111331935A
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- layer composite
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- 239000002131 composite material Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 53
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 52
- 229920000181 Ethylene propylene rubber Polymers 0.000 claims abstract description 46
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000002994 raw material Substances 0.000 claims abstract description 31
- 239000004945 silicone rubber Substances 0.000 claims abstract description 26
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- 238000001125 extrusion Methods 0.000 claims abstract description 16
- 229920002943 EPDM rubber Polymers 0.000 claims abstract description 15
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000003921 oil Substances 0.000 claims abstract description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 8
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims abstract description 8
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000945 filler Substances 0.000 claims abstract description 7
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 7
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 7
- 238000004073 vulcanization Methods 0.000 claims abstract description 7
- 229920001971 elastomer Polymers 0.000 claims abstract description 5
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 4
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 4
- 229910021485 fumed silica Inorganic materials 0.000 claims abstract description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 4
- 229920002545 silicone oil Polymers 0.000 claims abstract description 4
- 239000008117 stearic acid Substances 0.000 claims abstract description 4
- 239000011787 zinc oxide Substances 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 19
- 238000004898 kneading Methods 0.000 claims description 9
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 9
- 229920002554 vinyl polymer Polymers 0.000 claims description 9
- 238000007599 discharging Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical compound C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 claims description 4
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 4
- OKKRPWIIYQTPQF-UHFFFAOYSA-N Trimethylolpropane trimethacrylate Chemical compound CC(=C)C(=O)OCC(CC)(COC(=O)C(C)=C)COC(=O)C(C)=C OKKRPWIIYQTPQF-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- DMWVYCCGCQPJEA-UHFFFAOYSA-N 2,5-bis(tert-butylperoxy)-2,5-dimethylhexane Chemical compound CC(C)(C)OOC(C)(C)CCC(C)(C)OOC(C)(C)C DMWVYCCGCQPJEA-UHFFFAOYSA-N 0.000 claims description 3
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- 229920002367 Polyisobutene Polymers 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 3
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- 239000000178 monomer Substances 0.000 claims description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 3
- 239000012071 phase Substances 0.000 claims description 3
- 239000004033 plastic Substances 0.000 claims description 3
- 229920003023 plastic Polymers 0.000 claims description 3
- 238000005096 rolling process Methods 0.000 claims description 3
- 238000007493 shaping process Methods 0.000 claims description 3
- 239000000454 talc Substances 0.000 claims description 3
- 229910052623 talc Inorganic materials 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- 239000012808 vapor phase Substances 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- 239000010690 paraffinic oil Substances 0.000 claims description 2
- 239000010959 steel Substances 0.000 claims description 2
- 239000010410 layer Substances 0.000 claims 12
- 239000002355 dual-layer Substances 0.000 claims 4
- 238000012360 testing method Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 7
- 230000007774 longterm Effects 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 230000032683 aging Effects 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 230000035882 stress Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000005662 Paraffin oil Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000010734 process oil Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000004078 waterproofing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B1/00—Layered products having a non-planar shape
- B32B1/08—Tubular products
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/002—Methods
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/001—Combinations of extrusion moulding with other shaping operations
- B29C48/0018—Combinations of extrusion moulding with other shaping operations combined with shaping by orienting, stretching or shrinking, e.g. film blowing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/09—Articles with cross-sections having partially or fully enclosed cavities, e.g. pipes or channels
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/16—Articles comprising two or more components, e.g. co-extruded layers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
- B32B25/16—Layered products comprising a layer of natural or synthetic rubber comprising polydienes homopolymers or poly-halodienes homopolymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
- B32B25/20—Layered products comprising a layer of natural or synthetic rubber comprising silicone rubber
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
-
- 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
- C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- H—ELECTRICITY
- H02—GENERATION; CONVERSION OR DISTRIBUTION OF ELECTRIC POWER
- H02G—INSTALLATION OF ELECTRIC CABLES OR LINES, OR OF COMBINED OPTICAL AND ELECTRIC CABLES OR LINES
- H02G15/00—Cable fittings
- H02G15/08—Cable junctions
- H02G15/18—Cable junctions protected by sleeves, e.g. for communication cable
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2250/00—Layers arrangement
- B32B2250/24—All layers being polymeric
- B32B2250/248—All polymers belonging to those covered by group B32B25/00
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/306—Resistant to heat
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/732—Dimensional properties
- B32B2307/734—Dimensional stability
- B32B2307/736—Shrinkable
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2597/00—Tubular articles, e.g. hoses, pipes
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/18—Applications used for pipes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (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)
Abstract
The invention discloses a double-layer composite cold-shrinkable sleeve and a preparation method thereof, wherein the double-layer composite cold-shrinkable sleeve is prepared by double-layer composite co-extrusion of an outer-layer ethylene propylene rubber master batch and an inner-layer silicon rubber master batch, and the ethylene propylene rubber master batch comprises the following raw materials in parts by weight: 100 parts of ethylene propylene diene monomer, 1-8 parts of zinc oxide, 1-8 parts of stearic acid, 10-50 parts of precipitated silica, 5-30 parts of fumed silica, 20-100 parts of inert filler, 10-100 parts of operating oil and 2-10 parts of vulcanizing agent; the silicone rubber master batch is prepared from the following raw materials in parts by weight: 100 parts of methyl vinyl silicone rubber crude rubber, 0.5-5 parts of dimethyl silicone oil, 20-45 parts of gas phase method silicon dioxide, 5-15 parts of hexamethyldisilazane, 2-8 parts of inorganic metal oxide and 2-10 parts of vulcanizing agent. The invention can realize co-vulcanization, and the prepared double-layer composite cold-shrinkage sleeve is reliable in integral forming and bonding and has excellent comprehensive performances such as high and low temperature resistance, puncture resistance, wear resistance and the like.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the technical field of cold-shrink sleeve preparation, in particular to a double-layer composite cold-shrink sleeve and a preparation method thereof.
[ background of the invention ]
The cold-shrink sleeve is widely applied to the fields of power cables, communication cables and the like as a sealing component, common materials of the cold-shrink sleeve comprise silicon rubber and ethylene propylene rubber, the silicon rubber tube is mainly used domestically, and the ethylene propylene rubber tube is mainly used abroad. The silicone rubber cold-shrinkable tube has the advantages of excellent high and low temperature resistance and good retraction performance, but the price of raw materials is high, the puncture resistance, the acid and alkali resistance and the wear resistance are insufficient, and the holding force generated by shrinkage is low. Compared with silicon rubber, the ethylene propylene diene monomer cold-shrinkable tube is low in price, excellent in puncture resistance and tear resistance, large in stress at definite elongation under the same expansion rate, capable of generating larger radial holding force and capable of ensuring excellent waterproof sealing performance, partial discharge level and operation stability; however, ethylene propylene diene monomer has poor high and low temperature resistance, for example, aging, cracking and the like easily occur in the long-term operation process of a cable at a high temperature of 90 ℃, the shrinkage performance of the ethylene propylene diene monomer is inferior to that of silicon rubber in the low-temperature environment of-20 ℃ and below, and the ethylene propylene diene monomer cannot play a role in sealing, waterproofing and the like. Therefore, the two cold-shrink sleeves of silicon rubber and ethylene propylene rubber have respective irreplaceable positions in the fields of electric power and communication due to the difference of the materials, so that the two materials have great limitation in use and cause inconvenience in use.
At present, the silicon rubber cold shrink tube is widely researched, but the research on the ethylene propylene rubber cold shrink tube is few, and the research on the double-layer compounding of the two is almost not available. Chinese patent CN205791324U places the silicone rubber tube in one end of the ethylene propylene rubber tube by means of expansion, which plays a certain double-layer composite role, but still fails to solve the following problems: (1) because the silicone rubber tube is only arranged at one end inside the ethylene propylene rubber tube, in the practical application of the power cable accessory, the inner silicone rubber tube can not play a role of protecting the outer ethylene propylene rubber tube under the action of long-term high temperature, and the high temperature resistance is poorer; (2) adhesion does not exist between the two cold-shrinkable tubes, only the two cold-shrinkable tubes are compounded in a physical expansion mode, an interface gap exists, and due to material difference, the retraction performance of the silicon rubber and the ethylene propylene rubber is inconsistent, so that the partial discharge level is poor, and the operation reliability is reduced; (3) compared with silicon rubber, the low-temperature retraction performance of the ethylene propylene rubber tube is poor, the retraction performance is poor at minus 20 ℃, and the ethylene propylene rubber cold-shrinkable tube almost loses the retraction performance after the support tube is extracted in the environment of minus 30 ℃ and below, so that the problem of poor retraction performance in the low-temperature environment cannot be solved.
In view of the above, it is necessary to develop a novel double-layer composite cold-shrink sleeve and a method for manufacturing the same, so as to overcome the above-mentioned drawbacks.
[ summary of the invention ]
The invention aims to provide a double-layer composite cold-shrink sleeve and a preparation method thereof, wherein the two layers of sleeves have no gap, high connection reliability, excellent high and low temperature resistance, excellent puncture resistance, excellent wear resistance and other comprehensive properties.
In order to achieve the purpose, the invention provides a double-layer composite cold-shrinkage sleeve which is prepared by carrying out double-layer composite co-extrusion on an outer-layer ethylene propylene rubber master batch and an inner-layer silicon rubber master batch, wherein the ethylene propylene rubber master batch comprises the following raw materials in parts by weight: 100 parts of ethylene propylene diene monomer, 1-8 parts of zinc oxide, 1-8 parts of stearic acid, 10-50 parts of precipitated silica, 5-30 parts of fumed silica, 20-100 parts of inert filler, 10-100 parts of operating oil and 2-10 parts of vulcanizing agent;
the silicone rubber master batch is prepared from the following raw materials in parts by weight: 100 parts of methyl vinyl silicone rubber crude rubber, 0.5-5 parts of dimethyl silicone oil, 20-45 parts of gas phase method silicon dioxide, 5-15 parts of hexamethyldisilazane, 2-8 parts of inorganic metal oxide and 2-10 parts of vulcanizing agent.
In a preferred embodiment, the ethylene-propylene-diene monomer content of the ethylene-propylene-diene monomer rubber is 45 to 55% and the third monomer content is 2 to 10%.
In a preferred embodiment, the precipitated silica has a particle size of 150m2A specific surface area of 200m or less, and a silica produced by the vapor phase method2Specific surface area of/g or more.
In a preferred embodiment, the inert filler is at least one of calcined kaolin, talc, calcium carbonate.
In a preferred embodiment, the process oil is at least one of a paraffinic oil, a naphthenic oil, a liquid polyisobutylene.
In a preferred embodiment, the vulcanizing agent is at least one of 2, 5-dimethyl-2, 5 di (t-butylperoxy) hexane, dicumyl peroxide, 1,3(1,4) -bis (t-butylperoxyisopropyl) benzene, triallyl isocyanurate, trimethylolpropane trimethacrylate.
In a preferred embodiment, the raw methyl vinyl silicone rubber has a vinyl terminated vinyl molar content of 0.03% to 0.2% and a methyl terminated vinyl molar content of 0.8% to 8%.
In a preferred embodiment, the inorganic metal oxide is at least one of titanium dioxide, cerium oxide, and ferroferric oxide.
In order to achieve the above object, the present invention further provides a method for preparing a double-layer composite cold-shrink sleeve, comprising the following steps:
1) preparing a master batch: weighing raw materials of the ethylene propylene rubber master batch according to the weight part ratio, putting the raw materials into an internal mixer for mixing to 150-175 ℃, then rolling the raw materials through an open mill, thinning the raw materials, then discharging the sheets, cooling and placing the sheets for more than 12 hours, adding a vulcanizing agent into the open mill, thinning the sheets, discharging the sheets, and cutting the sheets to obtain the ethylene propylene rubber master batch;
weighing raw materials of the silicone rubber master batch according to the weight proportion, putting the raw materials into a kneading machine, kneading and mixing for 1-3 h, placing the kneading machine at the temperature of 100-150 ℃ for vacuumizing for 0.5-2 h, wherein the vacuum degree ranges from-0.05 to-0.1 MPa, then thinning the mixed materials through an open mill, discharging the thin mixed materials out of a sheet, placing the thin mixed materials in the open mill after cooling and placing for more than 12h, adding a vulcanizing agent, thinning the thin mixed materials out of the sheet, and cutting the thin mixed materials to obtain the silicone rubber master batch;
2) double-layer composite co-extrusion: feeding ethylene propylene rubber master batch and silicon rubber master batch into respective cold feeding extruders respectively, and extruding the ethylene propylene rubber master batch and the silicon rubber master batch into a composite pipe through a combined neck ring mold and a core rod of two machine heads;
3) and (3) a vulcanization step: after the extruded composite molded pipe is put on a disc, the disc is heated, pressurized and vulcanized in inert atmosphere through a vulcanizing tank;
4) an expansion step: and expanding the vulcanized pipe by using expansion equipment, and supporting and shaping the lining by using a spiral plastic supporting pipe to obtain a finished sleeve.
In a preferred embodiment, in the step 2), the extrusion temperature of the outer layer extruder is 80-100 ℃, and the extrusion temperature of the inner layer extruder is 18-30 ℃; in the step 3), the pressure of the vulcanizing tank is 0.3-0.7 MPa, and the temperature of the vulcanizing tank is 150-170 ℃.
The invention has the beneficial effects that: the ethylene propylene rubber master batch and the silicone rubber master batch are respectively prepared according to the formula proportion, and then the cold shrinkage sleeve is prepared by double-layer co-extrusion, so that co-vulcanization can be realized, and the integral forming and bonding are reliable; the prepared double-layer composite cold-shrink sleeve has no interface gap, and has good local discharge level and running reliability; under the action of long-term high temperature, ethylene propylene rubber serves as an outer layer to provide excellent mechanical property, silicon rubber serves as an inner layer to provide high-temperature-resistant protection, and the sleeve has good mechanical property and high-temperature-resistant property through double-layer compounding; in a low-temperature environment, although the ethylene propylene rubber has poor retraction performance, the inner silicone rubber tube has good retraction performance, and the stress generated during retraction of the inner silicone rubber tube has a promoting effect on the retraction of the outer ethylene propylene rubber tube, so that the outer ethylene propylene rubber tube can be driven to retract together, the sleeve is ensured to have good retraction performance in the low-temperature environment, and the sleeve can be applied to cold regions.
[ detailed description ] embodiments
Exemplary embodiments of the present invention will be described in more detail below. While the following text sets forth exemplary embodiments of the invention, it should be understood that the invention can be embodied in various forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
The embodiment of the invention provides a double-layer composite cold-shrink sleeve which is prepared by carrying out double-layer composite co-extrusion on ethylene propylene rubber master batch on an outer layer and silicon rubber master batch on an inner layer. The ethylene propylene rubber master batch is prepared from the following raw materials in parts by weight: 100 parts of Ethylene Propylene Diene Monomer (EPDM), 1-8 parts of zinc oxide, 1-8 parts of stearic acid, 10-50 parts of precipitated silica, 5-30 parts of fumed silica, 20-100 parts of inert filler, 10-100 parts of operating oil and 2-10 parts of vulcanizing agent.
The silicone rubber master batch is prepared from the following raw materials in parts by weight: 100 parts of methyl vinyl silicone rubber crude rubber, 0.5-5 parts of dimethyl silicone oil, 20-45 parts of gas phase method silicon dioxide, 5-15 parts of hexamethyldisilazane, 2-8 parts of inorganic metal oxide and 2-10 parts of vulcanizing agent.
According to some embodiments of the invention, the ethylene-propylene-diene monomer content of the ethylene-propylene-diene rubber is 45-55% and the third monomer content is 2-10%.
According to some embodiments of the invention, the precipitated silica has a particle size of 150m2A specific surface area of 200m or less, and a silica produced by the vapor phase method2Specific surface area of/g or more.
According to some embodiments of the invention, the inert filler is at least one of calcined kaolin, talc, calcium carbonate; the operation oil is at least one of paraffin oil, naphthenic oil and liquid polyisobutene.
According to some embodiments of the invention, the vulcanizing agent is at least one of 2, 5-dimethyl-2, 5 di (t-butylperoxy) hexane (bis-dipenta), dicumyl peroxide (DCP), 1,3(1,4) -bis (t-butylperoxyisopropyl) benzene (BIBP), triallyl isocyanurate (TAIC), trimethylolpropane trimethacrylate (TMPTMA).
According to some embodiments of the invention, the methyl vinyl silicone rubber raw rubber has a vinyl terminated vinyl molar content of 0.03% to 0.2%, and a methyl terminated vinyl molar content of 0.8% to 8%; the inorganic metal oxide is at least one of titanium dioxide, cerium oxide and ferroferric oxide.
The embodiment of the invention also provides a preparation method of the double-layer composite cold-shrink sleeve, which comprises the following steps:
1) preparing a master batch: weighing raw materials of the ethylene propylene rubber master batch according to the weight part ratio, putting the raw materials into an internal mixer for mixing to 150-175 ℃, then rolling the raw materials through an open mill, thinly passing the raw materials, then discharging the raw materials, cooling and placing the raw materials for more than 12 hours, adding a vulcanizing agent into the open mill, thinly passing the raw materials out of the open mill, and cutting the raw materials to obtain the ethylene propylene rubber master batch.
Weighing raw materials of the silicone rubber master batch according to the weight proportion, putting the raw materials into a kneading machine, kneading and mixing for 1-3 h, placing the kneading machine at the temperature of 100-150 ℃ for vacuumizing for 0.5-2 h, wherein the vacuum degree ranges from-0.05 to-0.1 MPa, then thinning the mixed materials through an open mill, discharging the thin mixed materials out of a sheet, placing the thin mixed materials in the open mill after cooling and placing for more than 12h, adding a vulcanizing agent, thinning the thin mixed materials out of the sheet, and cutting the thin mixed materials to obtain the silicone rubber master batch.
2) Double-layer composite co-extrusion: feeding the ethylene propylene rubber master batch and the silicon rubber master batch into respective cold feeding extruders respectively, and extruding the ethylene propylene rubber master batch and the silicon rubber master batch into a composite pipe through a combined neck ring mold and a core rod of two machine heads.
3) And (3) a vulcanization step: and (3) heating, pressurizing and vulcanizing the composite pipe in inert atmosphere through a vulcanizing tank after the composite pipe is hung on the plate.
4) An expansion step: and expanding the vulcanized pipe by air or steel wire expansion equipment, and supporting and shaping the lining by a spiral plastic supporting pipe to obtain a finished sleeve.
Preferably, in the step 2), the extrusion temperature of the outer layer extruder is 80-100 ℃, and the extrusion temperature of the inner layer extruder is 18-30 ℃; in the step 3), the pressure of the vulcanizing tank is 0.3-0.7 MPa, and the temperature of the vulcanizing tank is 150-170 ℃. In the step 3), the operation of the inert atmosphere is to firstly vacuumize and then fill inert gases such as oxygen-free nitrogen and the like.
The invention will now be described with reference to specific examples, which are intended to be illustrative only and not to be limiting in any way (the number of experiments is relatively large, and in many of the examples, the following examples and comparative examples are to be considered as references to demonstrate the feasibility and advantages of the formulations).
TABLE 1 ethylene propylene rubber masterbatch Components of the examples and comparative examples
TABLE 2 Silicone rubber masterbatch Components of the examples and comparative examples
The examples in tables 1-2 are prepared into cold-shrink sleeve finished products by the preparation method; comparative examples 1 and 2 in tables 1-2 are respectively prepared by extrusion molding, vulcanization and expansion of ethylene propylene rubber master batch and silicone rubber master batch to obtain cold-shrink sleeve finished products. Further, the examples and comparative examples were subjected to performance tests in accordance with national standards, and the test results are shown in Table 3.
Note that the test method of the permanent deformation rate of-40 ℃ x2h in Table 3 is as follows: measuring the inner diameter of 10 pipes before the pipe is not expanded, taking the average value of the test as data R0, then expanding the pipe by 4 times, statically storing the pipe in a low-temperature test box at the temperature of-40 ℃ for 2h, extracting the support pipe in the low-temperature test box for 2h, testing the inner diameter data after retraction, taking the average value of the 10 tests as R1, and then setting the permanent deformation rate as (R1-R0)/R0 as 100%.
Test method for percent set after aging at 90 ℃ X168h in Table 3: measuring the inner diameter of 10 pipes before the pipe is not expanded, recording the inner diameter as data R2, then expanding the pipe by 4 times, putting the pipe into an aging test box with the temperature of 90 ℃, statically storing the pipe for 168 hours, taking the pipe out, cooling the pipe for more than 8 hours at room temperature, then extracting a supporting strip at room temperature, standing the pipe for 30 minutes, and then testing the retraction inner diameter data, and recording the average value of 10 tests as R3, wherein the permanent deformation rate is (R3-R2)/R2 x 100%.
Table 3 results of performance testing
Comparing the data in table 3, it can be seen that compared with the comparative example one prepared from the ethylene propylene rubber master batch and the comparative example two prepared from the silicon rubber master batch, the double-layer composite cold-shrinkable sleeve prepared from the examples one to twenty has excellent comprehensive properties such as tear resistance, wear resistance and the like, and particularly has low deformation rate in high-temperature and low-temperature environments, because under the action of long-term high temperature, the ethylene propylene rubber provides excellent mechanical properties as an outer layer, and the silicon rubber provides high-temperature resistance protection as an inner layer, the sleeve has good mechanical properties and high-temperature resistance through double-layer compounding, although the retraction property of the ethylene propylene rubber is poor in the low-temperature environment, because the inner silicon rubber tube has good retraction property, the stress generated during retraction thereof has a promotion effect on the retraction of the outer ethylene propylene rubber tube, and can drive the outer ethylene propylene rubber tube to retract together, the sleeve is ensured to have good retraction performance in a low-temperature environment, and the cost is greatly saved.
According to the embodiment of the invention, the ethylene propylene rubber master batch and the silicon rubber master batch are respectively prepared according to the formula proportion, and then the cold-shrink sleeve is prepared by double-layer co-extrusion, so that co-vulcanization is realized, the integral forming and bonding are reliable, the respective inapplicability situations of the silicon rubber and the ethylene propylene rubber pipe in the actual use process are overcome, the advantages of the silicon rubber cold-shrink pipe and the ethylene propylene rubber cold-shrink pipe in the prior art are complemented, the silicon rubber cold-shrink pipe and the ethylene propylene rubber cold-shrink pipe in the prior art can be completely replaced, and the cold-shrink sleeve.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. The double-layer composite cold-shrinkage sleeve is prepared from an outer-layer ethylene propylene rubber master batch and an inner-layer silicon rubber master batch through double-layer composite co-extrusion, and is characterized in that the ethylene propylene rubber master batch comprises the following raw materials in parts by weight: 100 parts of ethylene propylene diene monomer, 1-8 parts of zinc oxide, 1-8 parts of stearic acid, 10-50 parts of precipitated silica, 5-30 parts of fumed silica, 20-100 parts of inert filler, 10-100 parts of operating oil and 2-10 parts of vulcanizing agent;
the silicone rubber master batch is prepared from the following raw materials in parts by weight: 100 parts of methyl vinyl silicone rubber crude rubber, 0.5-5 parts of dimethyl silicone oil, 20-45 parts of gas phase method silicon dioxide, 5-15 parts of hexamethyldisilazane, 2-8 parts of inorganic metal oxide and 2-10 parts of vulcanizing agent.
2. The two-layer composite cold-shrink sleeve of claim 1, wherein the ethylene-propylene-diene monomer content of the ethylene-propylene-diene monomer is 45-55%, and the third monomer content is 2-10%.
3. The dual layer composite cold shrink sleeve of claim 1, wherein said precipitated silica has a thickness of 150m2A specific surface area of 200m or less, and a silica produced by the vapor phase method2Specific surface area of/g or more.
4. The two-layer composite cold-shrink sleeve of claim 1, wherein the inert filler is at least one of calcined kaolin, talc, and calcium carbonate.
5. The dual-layer composite cold-shrink sleeve of claim 1, wherein the operating oil is at least one of a paraffinic oil, a naphthenic oil, and a liquid polyisobutylene.
6. The dual-layer composite cold-shrink sleeve of claim 1, wherein the vulcanizing agent is at least one of 2, 5-dimethyl-2, 5 di (t-butylperoxy) hexane, dicumyl peroxide, 1,3(1,4) -bis (t-butylperoxyisopropyl) benzene, triallyl isocyanurate, trimethylolpropane trimethacrylate.
7. The two-layer composite cold-shrink sleeve of claim 1, wherein the raw methyl vinyl silicone rubber has a vinyl terminated vinyl molar content of 0.03-0.2% and a methyl terminated vinyl molar content of 0.8-8%.
8. The dual-layer composite cold-shrink sleeve of claim 1, wherein the inorganic metal oxide is at least one of titanium dioxide, cerium oxide, and ferroferric oxide.
9. A method of manufacturing a two-layer composite cold shrink sleeve according to any one of claims 1 to 8, wherein the method of manufacturing comprises the steps of:
1) preparing a master batch: weighing raw materials of the ethylene propylene rubber master batch according to the weight part ratio, putting the raw materials into an internal mixer for mixing to 150-175 ℃, then rolling the raw materials through an open mill, thinning the raw materials, then discharging the sheets, cooling and placing the sheets for more than 12 hours, adding a vulcanizing agent into the open mill, thinning the sheets, discharging the sheets, and cutting the sheets to obtain the ethylene propylene rubber master batch;
weighing raw materials of the silicone rubber master batch according to the weight proportion, putting the raw materials into a kneading machine, kneading and mixing for 1-3 h, placing the kneading machine at the temperature of 100-150 ℃ for vacuumizing for 0.5-2 h, wherein the vacuum degree ranges from-0.05 to-0.1 MPa, then thinning the mixed materials through an open mill, discharging the thin mixed materials out of a sheet, placing the thin mixed materials in the open mill after cooling and placing for more than 12h, adding a vulcanizing agent, thinning the thin mixed materials out of the sheet, and cutting the thin mixed materials to obtain the silicone rubber master batch;
2) double-layer composite co-extrusion: feeding ethylene propylene rubber master batch and silicon rubber master batch into respective cold feeding extruders respectively, and extruding the ethylene propylene rubber master batch and the silicon rubber master batch into a composite pipe through a combined neck ring mold and a core rod of two machine heads;
3) and (3) a vulcanization step: after the extruded composite molded pipe is put on a disc, the disc is heated, pressurized and vulcanized in inert atmosphere through a vulcanizing tank;
4) an expansion step: and expanding the vulcanized pipe by air or steel wire expansion equipment, and supporting and shaping the lining by a spiral plastic supporting pipe to obtain a finished sleeve.
10. The method for preparing the double-layer composite cold-shrink sleeve according to claim 9, wherein in the step 2), the extrusion temperature of the outer layer extruder is 80-100 ℃, and the extrusion temperature of the inner layer extruder is 18-30 ℃; in the step 3), the pressure of the vulcanizing tank is 0.3-0.7 MPa, and the temperature of the vulcanizing tank is 150-170 ℃.
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