CN113978076A - Heat-shrinkable material, preparation method and application thereof, and double-wall heat-shrinkable sleeve - Google Patents
Heat-shrinkable material, preparation method and application thereof, and double-wall heat-shrinkable sleeve Download PDFInfo
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- CN113978076A CN113978076A CN202110854465.3A CN202110854465A CN113978076A CN 113978076 A CN113978076 A CN 113978076A CN 202110854465 A CN202110854465 A CN 202110854465A CN 113978076 A CN113978076 A CN 113978076A
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- 239000002654 heat shrinkable material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
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- 239000003963 antioxidant agent Substances 0.000 claims abstract description 21
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- 239000005038 ethylene vinyl acetate Substances 0.000 claims abstract description 16
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims abstract description 16
- 239000002250 absorbent Substances 0.000 claims abstract description 15
- 230000002745 absorbent Effects 0.000 claims abstract description 15
- 150000003254 radicals Chemical class 0.000 claims abstract description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052802 copper Inorganic materials 0.000 claims abstract description 14
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- 239000004698 Polyethylene Substances 0.000 claims abstract description 13
- 229920000573 polyethylene Polymers 0.000 claims abstract description 13
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- 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 7
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- 239000002994 raw material Substances 0.000 claims description 7
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 6
- 235000010354 butylated hydroxytoluene Nutrition 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000000155 melt Substances 0.000 claims description 6
- 238000007493 shaping process Methods 0.000 claims description 6
- DPWFWWRPRPJCFX-UHFFFAOYSA-L zinc pyridine sulfate Chemical compound S(=O)(=O)([O-])[O-].[Zn+2].N1=CC=CC=C1 DPWFWWRPRPJCFX-UHFFFAOYSA-L 0.000 claims description 6
- BJELTSYBAHKXRW-UHFFFAOYSA-N 2,4,6-triallyloxy-1,3,5-triazine Chemical compound C=CCOC1=NC(OCC=C)=NC(OCC=C)=N1 BJELTSYBAHKXRW-UHFFFAOYSA-N 0.000 claims description 5
- 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 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical group C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 claims description 4
- 230000001678 irradiating effect Effects 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 239000004945 silicone rubber Substances 0.000 claims description 4
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 4
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 3
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 3
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- HCILJBJJZALOAL-UHFFFAOYSA-N 3-(3,5-ditert-butyl-4-hydroxyphenyl)-n'-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyl]propanehydrazide Chemical group CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 HCILJBJJZALOAL-UHFFFAOYSA-N 0.000 claims description 2
- VSAWBBYYMBQKIK-UHFFFAOYSA-N 4-[[3,5-bis[(3,5-ditert-butyl-4-hydroxyphenyl)methyl]-2,4,6-trimethylphenyl]methyl]-2,6-ditert-butylphenol Chemical compound CC1=C(CC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)C(C)=C(CC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)C(C)=C1CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 VSAWBBYYMBQKIK-UHFFFAOYSA-N 0.000 claims description 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 2
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- ILWVABLRFKUOOO-UHFFFAOYSA-N [3-[2-(3,5-ditert-butyl-4-hydroxyphenyl)-2-methylpropanoyl]oxy-2,2-bis[[2-(3,5-ditert-butyl-4-hydroxyphenyl)-2-methylpropanoyl]oxymethyl]propyl] 2-(3,5-ditert-butyl-4-hydroxyphenyl)-2-methylpropanoate Chemical compound CC(C(=O)OCC(COC(C(C)(C1=CC(=C(C(=C1)C(C)(C)C)O)C(C)(C)C)C)=O)(COC(C(C)(C1=CC(=C(C(=C1)C(C)(C)C)O)C(C)(C)C)C)=O)COC(C(C)(C1=CC(=C(C(=C1)C(C)(C)C)O)C(C)(C)C)C)=O)(C)C1=CC(=C(C(=C1)C(C)(C)C)O)C(C)(C)C ILWVABLRFKUOOO-UHFFFAOYSA-N 0.000 claims 1
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Images
Classifications
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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
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D23/00—Producing tubular articles
- B29D23/001—Pipes; Pipe joints
-
- 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
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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
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
- B32B27/306—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising vinyl acetate or vinyl alcohol (co)polymers
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
- B32B27/308—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising acrylic (co)polymers
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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
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/34—Layered products comprising a layer of synthetic resin comprising polyamides
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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
- C08L23/06—Polyethene
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B17/00—Insulators or insulating bodies characterised by their form
- H01B17/56—Insulating bodies
- H01B17/58—Tubes, sleeves, beads, or bobbins through which the conductor passes
- H01B17/583—Grommets; Bushings
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- 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
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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
- B32B2307/40—Properties of the layers or laminate having particular optical properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B2597/00—Tubular articles, e.g. hoses, pipes
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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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
- C08L2203/18—Applications used for pipes
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Insulating Bodies (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Laminated Bodies (AREA)
Abstract
The invention is applicable to the technical field of materials, provides a heat shrinkable material, a preparation method and application thereof, and a double-wall heat shrinkable sleeve, and comprises an outer layer master batch and a hot melt adhesive modified master batch; the outer layer master batch comprises: 60-90 parts of polyethylene, 10-40 parts of ethylene-methacrylate copolymer, 4-10 parts of polyethylene octene copolymer elastomer, 0.5-3.0 parts of sensitizer, 0.5-1.5 parts of antioxidant and 0.5-2.0 parts of lubricant; the hot melt adhesive modified master batch comprises: 70-90 parts of ethylene-vinyl acetate copolymer hot melt adhesive, 10-30 parts of polyamide hot melt adhesive, 0.5-1.5 parts of copper inhibitor, 0.2-1.0 part of free radical absorbent and 0.5-1.5 parts of antioxidant. The double-wall heat shrinkable sleeve prepared by the invention has the characteristics of realizing rapid shrinkage at high temperature, no carbonization on the surface and no cracking after high-temperature baking shrinkage, solves the problem of poor transparency of the conventional double-wall pipe, and is suitable for sealing and waterproofing a plurality of strands of wire harnesses.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a heat-shrinkable material, a preparation method and application thereof, and a double-wall heat-shrinkable sleeve.
Background
The outer layer of the double-wall heat shrinkable sleeve is made of irradiation cross-linked polyolefin material and has a heat shrinkage memory function, and the inner layer is made of polyolefin or polyamide hot melt adhesive and provides a bonding and sealing function. The double-wall heat shrinkable tube has wide application in occasions requiring electric protection, friction-resistant protection and stress release. In automotive systems moisture may enter the joint area directly or indirectly through capillary action between the individual wires, causing corrosion of the wiring. One important function of double-walled pipes is to provide a moisture-tight seal for electrical joints in automotive systems.
The double-wall pipe is arranged at the central position of the electric joint area, and when the double-wall pipe is heated, the hot melt adhesive is melted and plays a role in holding and sealing the curled or welded electric wire and the conducting wire through the thermal contraction effect of the sleeve. The installed double-walled pipe provides mechanical protection against bending, abrasion and penetration, and electrical insulation. Conventional double-walled pipe is slow because of the shrink speed, and production efficiency is low, and can't provide sufficient shrink stress, leads to the hot melt adhesive of double-walled pipe inlayer can't fill the gap of stranded pencil through the extrusion. Additionally, if the hot melt adhesive parameters are not properly designed, it is likely that the hot melt adhesive will not fill or spill the plurality of wire strands. Secondly, for the high-power shrinkage double-wall pipe, if the condition that uneven cutting occurs and stress concentration points occur in the cutting process, cracking occurs in the shrinkage process of the sleeve. The sealing failure of the double-wall pipe can be caused by the above conditions, and hidden dangers are buried for the safety of an automobile system.
The prior art can increase the radiation dose to increase the crosslinking degree or increase the shrinkage temperature to accelerate the shrinkage of the sleeve, and the technical scheme has the following defects: 1. the high irradiation dose can cause the cross-linking foaming of the hot melt adhesive, the poor fluidity and the cracking in the shrinkage process, a certain proportion of antioxidant is added to inhibit the cross-linking of the hot melt adhesive in the conventional technical scheme, but the high addition proportion can seriously affect the transparency of the pipe; and additionally, can cause cracking of the jacket tube under high temperature shrinkage conditions. If the irradiation dose is too low, the shrinkage speed is slow, the production efficiency is seriously influenced, and the situation of insufficient shrinkage force exists, so that the hot melt adhesive cannot be extruded and filled into the gaps of the multiple strands of wire harnesses. 2. In the case of a low irradiation dose, if the shrinkage speed is accelerated by raising the temperature, the sleeve is subjected to temperature difference resistance due to low crosslinking degree, and the surface is carbonized.
Therefore, the existing double-wall heat shrinkable sleeve can not simultaneously combine the characteristics of quick shrinkage, high-time shrinkage without cracking, high transparency and excellent filling and sealing performance.
Disclosure of Invention
The embodiment of the invention aims to provide a heat-shrinkable material, and aims to solve the problems that the existing double-wall heat-shrinkable sleeve cannot simultaneously achieve the characteristics of quick shrinkage, high-power shrinkage without cracking, high transparency and excellent filling sealing property.
The embodiment of the invention is realized in such a way that the heat shrinkable material comprises an outer layer master batch and a hot melt adhesive modified master batch;
the outer layer master batch comprises the following raw materials in parts by weight:
60-90 parts of polyethylene, 10-40 parts of ethylene-methacrylate copolymer, 4-10 parts of polyethylene octene copolymer elastomer, 0.5-3.0 parts of sensitizer, 0.5-1.5 parts of antioxidant and 0.5-2.0 parts of lubricant;
the hot melt adhesive modified master batch comprises the following raw materials in parts by weight:
70-90 parts of ethylene-vinyl acetate copolymer hot melt adhesive, 10-30 parts of polyamide hot melt adhesive, 0.5-1.5 parts of copper inhibitor, 0.2-1.0 part of free radical absorbent and 0.5-1.5 parts of antioxidant.
Another object of an embodiment of the present invention is to provide a method for preparing a heat shrinkable material, including:
uniformly mixing 60-90 parts of polyethylene, 10-40 parts of ethylene-methacrylate copolymer, 4-10 parts of polyethylene octene copolymer elastomer, 0.5-3.0 parts of sensitizer, 0.5-1.5 parts of antioxidant and 0.5-2.0 parts of lubricant, and performing extrusion granulation to obtain a skin master batch;
uniformly mixing 70-90 parts of ethylene-vinyl acetate copolymer hot melt adhesive, 10-30 parts of polyamide hot melt adhesive, 0.5-1.5 parts of copper inhibitor, 0.2-1.0 part of free radical absorbent and 0.5-1.5 parts of antioxidant, and carrying out underwater granulation and drying to obtain hot melt adhesive modified master batch;
co-extruding the outer skin master batch and the hot melt adhesive modified master batch by a double-layer extruder, irradiating and crosslinking the obtained semi-finished product, irradiating with the dose of 10-15Mrd, expanding by internal and external pressure difference, cooling and shaping to obtain the product.
Another object of an embodiment of the invention is the use of said heat-shrinkable material for the preparation of double-walled heat-shrinkable sleeves.
It is another object of an embodiment of the present invention to provide a double-walled heat shrinkable sleeve made from the heat shrinkable material.
According to the heat shrinkable material provided by the embodiment of the invention, the outer layer master batch is obtained by compounding the polyethylene octene copolymer elastomer, the sensitizer, the antioxidant and the lubricant with the polyethylene and the ethylene-methacrylate copolymer as main components, and the hot melt adhesive modified master batch is obtained by compounding the ethylene-vinyl acetate copolymer hot melt adhesive, the polyamide hot melt adhesive, the copper resistant agent, the free radical absorbent and the antioxidant; in addition, the invention has good fluidity in the contraction process and is suitable for sealing and waterproofing a plurality of strands of wire harnesses.
Drawings
FIG. 1 is a graph of thermal shrinkage curves provided by an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a heat shrinkable material for solving the problem that the existing double-wall heat shrinkable sleeve can not simultaneously combine the characteristics of quick shrinkage, high-power shrinkage without cracking, high transparency and excellent filling sealing property, the outer layer master batch is obtained by compounding polyethylene, ethylene-methacrylate copolymer as a main component with polyethylene octene copolymer elastomer, sensitizer, antioxidant and lubricant, and ethylene-vinyl acetate copolymer hot melt adhesive, polyamide hot melt adhesive, copper resisting agent, free radical absorbent and antioxidant are compounded to obtain hot melt adhesive modified master batch, the double-wall heat shrinkable sleeve prepared from the outer layer master batch and the hot melt adhesive modified master batch can realize rapid shrinkage at high temperature, the surface is not carbonized, and the high-temperature baking shrinkage is not cracked, so that the problem of poor transparency of the double-wall pipe in the prior art is solved; in addition, the invention has good fluidity in the contraction process and is suitable for sealing and waterproofing a plurality of strands of wire harnesses.
In the embodiment of the invention, the heat shrinkable material comprises an outer layer master batch and a hot melt adhesive modified master batch;
the outer layer master batch comprises the following raw materials in parts by weight:
60-90 parts of polyethylene, 10-40 parts of ethylene-methacrylate copolymer, 4-10 parts of polyethylene octene copolymer elastomer, 0.5-3.0 parts of sensitizer, 0.5-1.5 parts of antioxidant and 0.5-2.0 parts of lubricant;
the hot melt adhesive modified master batch comprises the following raw materials in parts by weight:
70-90 parts of ethylene-vinyl acetate copolymer hot melt adhesive, 10-30 parts of polyamide hot melt adhesive, 0.5-1.5 parts of copper inhibitor, 0.2-1.0 part of free radical absorbent and 0.5-1.5 parts of antioxidant.
In the embodiment of the invention, the polyethylene is one or two of LDPE (low density polyethylene) or LLDPE (linear low density polyethylene) which are compounded in any proportion, the melting point is 105-115 ℃, the melt index (MFR) is 0.2-0.5g/10min, and the density is 0.91-0.94g/cm3。
In the embodiment of the invention, the MMA content of the ethylene-methacrylate copolymer (EMMA) is 5-25%, the melt index (MFR) is 0.2-5g/10min, the melting point is 80-100 ℃, and the environmental stress cracking resistance is more than 300 hr.
In the inventive example, the polyethylene octene copolymer elastomer (POE) has a melt index (MFR) of 0.1-3g/10min and a density of 0.8-0.95g/cm 3.
In the embodiment of the invention, the sensitizer is colorless transparent liquid and is prepared by compounding one or more of trimethylolpropane trimethacrylate (TMPTMA), triallyl isocyanurate (TAIC) and triallyl cyanurate (TAC).
In the embodiment of the invention, the lubricant is one or more of low molecular weight silicon rubber, polyethylene wax, zinc stearate and silicone master batches compounded in any proportion.
In the embodiment of the invention, the low molecular weight silicon rubber is methyl vinyl silicone rubber, the molecular weight is 4.5 multiplied by 105-6.0 multiplied by 105, and the vinyl content is 0.01-0.25%.
In the embodiment of the invention, the EVA (ethylene-vinyl acetate copolymer) hot melt adhesive has a softening point of 90-100 ℃ and a rotational viscosity of 70000-100000 mPa.s (tested at 160 ℃).
In the inventive examples, the PA (polyamide) hotmelt adhesives have a softening point of 130 ℃ to 150 ℃ and a rotational viscosity of 50000mPa.s to 70000mPa.s (measured at 160 ℃).
In the embodiment of the invention, the chemical structure of the copper resisting agent is N, N' -bis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine, and the melting point is 210-250 ℃.
In the embodiment of the invention, the free radical absorbent is one or more of ammonium dihydrogen phosphate, zinc sulfate pyridine and lithium carbonate which are compounded in any proportion.
In the embodiment of the invention, the antioxidant is one or more of 3, 5-di-tert-butyl-4-hydroxyphenyl propionic acid octadecyl ester, tetra [ methyl- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, 2, 6-di-tert-butyl-p-cresol and 1, 3, 5-trimethyl-2, 4, 6-tri (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene which are compounded in any proportion.
The embodiment of the invention also provides a preparation method of the heat shrinkable material (double-wall heat shrinkable sleeve), which comprises the following steps:
uniformly mixing 60-90 parts of polyethylene, 10-40 parts of ethylene-methacrylate copolymer, 4-10 parts of polyethylene octene copolymer elastomer, 0.5-3.0 parts of sensitizer, 0.5-1.5 parts of antioxidant and 0.5-2.0 parts of lubricant, and performing extrusion granulation to obtain a skin master batch;
uniformly mixing 70-90 parts of ethylene-vinyl acetate copolymer hot melt adhesive, 10-30 parts of polyamide hot melt adhesive, 0.5-1.5 parts of copper inhibitor, 0.2-1.0 part of free radical absorbent and 0.5-1.5 parts of antioxidant, and carrying out underwater granulation and drying to obtain hot melt adhesive modified master batch;
co-extruding the outer skin master batch and the hot melt adhesive modified master batch by a double-layer extruder, and performing irradiation crosslinking, heating, expansion by internal and external pressure difference, cooling and shaping on the obtained semi-finished product to obtain the product.
The embodiment of the invention also provides an application of the heat shrinkable material in preparing a double-wall heat shrinkable sleeve.
The embodiment of the invention also provides a double-wall heat-shrinkable sleeve prepared from the heat-shrinkable material.
Examples of certain embodiments of the invention are given below, which are not intended to limit the scope of the invention.
In addition, it should be noted that the numerical values given in the following examples are as precise as possible, but those skilled in the art will understand that each numerical value should be understood as a divisor rather than an absolutely exact numerical value due to measurement errors and experimental operational problems that cannot be avoided. For example, it is understood that the weight values of the respective raw materials for preparing the double-walled heat-shrinkable sleeve of the respective examples may have an error of ± 2% or ± 1% due to an error of a weighing instrument.
Example 1
Weighing the outer layer master batch according to parts by weight: 70 parts of low-density polyethylene (LDPE), 30 parts of ethylene-methacrylate copolymer (EMMA), 5 parts of polyethylene octene copolymer elastomer (POE), 2 parts of trimethylolpropane trimethacrylate (TMPTMA), 0.8 part of 2, 6-di-tert-butyl-p-cresol, 0.5 part of zinc stearate and 1 part of methyl vinyl silicone rubber; taking a hot melt adhesive modified master batch: 80 parts of EVA hot melt adhesive, 20 parts of PA hot melt adhesive, 1 part of copper inhibitor, 1 part of pyridine zinc sulfate and 0.5 part of 2, 6-di-tert-butyl-p-cresol. And uniformly mixing the components of the outer-layer master batch and the hot melt adhesive modified master batch by a high-speed stirrer respectively. And carrying out two-time extrusion granulation on the mixed outer layer master batch by a double screw at the granulation temperature of 180 ℃. And carrying out underwater granulation on the mixed hot melt adhesive modified master batch by a double screw at the granulation temperature of 180 ℃. The granulated hot melt adhesive modified master batch is dried by a drier for 12 hours at the temperature of 60 ℃. And co-extruding the outer layer master batch and the hot melt adhesive modified master batch by using a double-layer extruder to obtain an extruded semi-finished product. Then the mixture is irradiated and crosslinked by an electron accelerator, and the irradiation dose is 12 Mrd. And finally, carrying out oil bath heating on the irradiated semi-finished product, expanding and cooling and shaping through internal and external pressure difference to obtain the double-wall heat-shrinkable sleeve.
Example 2
Weighing the outer layer master batch according to parts by weight: 60 parts of low-density polyethylene (LDPE), 40 parts of ethylene-methacrylate copolymer (EMMA), 8 parts of polyethylene octene copolymer elastomer (POE), 0.5 part of triallyl isocyanurate (TAIC), 1.5 parts of 1, 3, 5-trimethyl-2, 4, 6 tris (3, 5-di-tri-butyl-4-hydroxybenzyl) benzene, 1 part of zinc stearate and 1 part of silicone master batch; taking a hot melt adhesive modified master batch: 70 parts of EVA hot melt adhesive, 30 parts of PA hot melt adhesive, 1 part of copper inhibitor, 0.5 part of ammonium dihydrogen phosphate, 0.5 part of zinc sulfate pyridine and 0.5 part of 2, 6-di-tert-butyl-p-cresol. And uniformly mixing the components of the outer-layer master batch and the hot melt adhesive modified master batch by a high-speed stirrer respectively. And carrying out two-time extrusion granulation on the mixed outer layer master batch by a double screw at the granulation temperature of 180 ℃. And carrying out underwater granulation on the mixed hot melt adhesive modified master batch by a double screw at the granulation temperature of 180 ℃. The granulated hot melt adhesive modified master batch is dried by a drier for 12 hours at the temperature of 60 ℃. And co-extruding the outer layer master batch and the hot melt adhesive modified master batch by using a double-layer extruder to obtain an extruded semi-finished product. Then the mixture is irradiated and crosslinked by an electron accelerator, and the irradiation dose is 15 Mrd. And finally, carrying out oil bath heating on the irradiated semi-finished product, expanding and cooling and shaping through internal and external pressure difference to obtain the double-wall heat-shrinkable sleeve.
Example 3
Weighing the outer layer master batch according to parts by weight: 90 parts of low-density polyethylene (LDPE), 10 parts of ethylene-methacrylate copolymer (EMMA), 10 parts of polyethylene octene copolymer elastomer (POE), 1 part of triallyl isocyanurate (TAIC), 2 parts of triallyl cyanurate (TAC), 0.5 part of 2, 6-di-tert-butyl-p-cresol and 0.5 part of methyl vinyl silicone rubber; taking a hot melt adhesive modified master batch: 90 parts of EVA hot melt adhesive, 10 parts of PA hot melt adhesive, 0.5 part of copper inhibitor, 0.7 part of pyridine zinc sulfate and 1 part of tetra [ methyl- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester. And uniformly mixing the components of the outer-layer master batch and the hot melt adhesive modified master batch by a high-speed stirrer respectively. And carrying out two-time extrusion granulation on the mixed outer layer master batch by a double screw at the granulation temperature of 180 ℃. And carrying out underwater granulation on the mixed hot melt adhesive modified master batch by a double screw at the granulation temperature of 180 ℃. The granulated hot melt adhesive modified master batch is dried by a drier for 12 hours at the temperature of 60 ℃. And co-extruding the outer layer master batch and the hot melt adhesive modified master batch by using a double-layer extruder to obtain an extruded semi-finished product. Then the mixture is irradiated and crosslinked by an electron accelerator, and the irradiation dose is 10 Mrd. And finally, carrying out oil bath heating on the irradiated semi-finished product, expanding and cooling and shaping through internal and external pressure difference to obtain the double-wall heat-shrinkable sleeve.
The double-wall heat shrinkable sleeve prepared in the embodiments 1 to 3 of the present invention was subjected to the related performance tests, the test methods and the test results are shown in table 1 (wherein the leakage test is the sealability test of the double-wall sleeve on the 2-to-2 PVC wire).
TABLE 1
In summary, as can be seen from table 1, in examples 1 to 3 of the present invention, a transparent automotive double-wall heat shrinkable sleeve applicable to multi-strand wire harnesses is prepared by selecting a low density polyethylene with specific parameters, compounding the selected low density polyethylene with an ethylene-methacrylate copolymer, and modifying an inner layer hot melt adhesive, and the double-wall heat shrinkable sleeve overcomes the problems of slow shrinkage speed of the double-wall pipe, easy cracking due to shrinkage under high temperature conditions, easy carbonization of a high-temperature baking surface, poor transparency, etc. in the prior art, and has excellent low temperature resistance, aging resistance, and oil resistance, and the product performance is far higher than the standard requirements.
In addition, in the process of the previous experiment, the invention discovers that the selection of the ethylene-methacrylate copolymer used in the system and the proportion of the ethylene-methacrylate copolymer and the low-density polyethylene have obvious influence on the shrinkage speed and the high-temperature resistant baking cracking condition of the obtained double-wall heat-shrinkable sleeve, and the content of the free radical absorbent used in the system has obvious influence on the leakage current, in particular to the following comparative example 1-.
In addition, in the process of the previous experiment, the invention discovers that the selection of the ethylene-methacrylate copolymer used in the system and the proportion of the ethylene-methacrylate copolymer and the low-density polyethylene have obvious influence on the shrinkage speed and the high-temperature resistant baking cracking condition of the obtained double-wall heat-shrinkable sleeve, and the content of the free radical absorbent used in the system has obvious influence on the leakage current, and particularly, the following comparative examples 1 to 8 are found.
Comparative example 1
On the basis of example 1, only the ethylene-methacrylate copolymer component was changed from 30 parts to 70 parts, and the other components and processes were consistent.
Comparative example 2
On the basis of example 1, only the ethylene-methacrylate copolymer component was changed from 30 parts to 45 parts, and the other components and processes were consistent.
Comparative example 3
On the basis of example 1, only the ethylene-methacrylate copolymer component was changed from 30 parts to 0 part, and the other components and processes were consistent.
Comparative example 4
On the basis of example 1, only the ethylene-methacrylate copolymer component was replaced with an ethylene-vinyl acetate copolymer, and the other components and processes were consistent.
Comparative example 5
On the basis of example 1, the type of the ethylene-methacrylate copolymer used was replaced, that is, the ethylene-methacrylate copolymer used in comparative example 5 had a methyl methacrylate content of 2%, a melt index of 2 to 5g/10min, a melting point of 90 to 105 ℃ and an environmental stress crack resistance of > 200 hr.
Comparative example 6
On the basis of example 1, only the free radical absorbent zinc sulfate pyridine is removed, and other components and processes are consistent.
Comparative example 7
On the basis of example 1, only the irradiation dose was replaced with 7Mrd, and the other components and processes were consistent.
Comparative example 8
On the basis of example 1, only the irradiation dose was replaced with 18Mrd, and the other components and processes were consistent.
The double-wall heat shrinkable sleeve prepared in the example 1 and the comparative example 1 of the invention is subjected to a shrinkage test, and the obtained heat shrinkage curve result is shown in fig. 1; in addition, the double-walled heat shrinkable sleeves prepared according to comparative examples 1 to 8 of the present invention were subjected to the above-mentioned related performance tests, and the test results are shown in table 2 (wherein the leakage test is a sealability test of a double-walled sleeve on a 2-by-2 PVC wire).
TABLE 2
In summary, as can be seen from comparative examples 1 to 3 in table 2, the shrinkage rate of the double-wall pipe is reduced by increasing the content of the ethylene-methacrylate copolymer, and as can also be seen from fig. 1, the temperature of the complete shrinkage of the pipe is obviously increased and the shrinkage rate is reduced by increasing the content of the ethylene-methacrylate copolymer, and the cracking is easily caused in the high-temperature shrinkage process by excessively reducing the content of the ethylene-methacrylate copolymer in the system, thereby causing serious hidden danger to the automobile safety burying; in addition, the radical absorbent in the hot melt adhesive modified master batch is removed in the comparative example 5, so that excessive crosslinking and poor fluidity of the hot melt adhesive under a certain irradiation dose can be caused, and the sealing effect of coating a plurality of wire harnesses is poor; furthermore, in comparative examples 6 to 8, it can be seen that too low irradiation dose can reduce shrinkage stress of the sheath sleeve, which affects shrinkage speed, and even fails to press the hot melt adhesive into gaps of the multiple strands of wire harnesses, which affects sealability, but too high irradiation dose can also cause too high cross-linking of the hot melt adhesive, which affects sealing effect.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
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 and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. The heat shrinkable material is characterized by comprising an outer layer master batch and a hot melt adhesive modified master batch;
the outer layer master batch comprises the following raw materials in parts by weight:
60-90 parts of polyethylene, 10-40 parts of ethylene-methacrylate copolymer, 4-10 parts of polyethylene octene copolymer elastomer, 0.5-3.0 parts of sensitizer, 0.5-1.5 parts of antioxidant and 0.5-2.0 parts of lubricant;
the hot melt adhesive modified master batch comprises the following raw materials in parts by weight:
70-90 parts of ethylene-vinyl acetate copolymer hot melt adhesive, 10-30 parts of polyamide hot melt adhesive, 0.5-1.5 parts of copper inhibitor, 0.2-1.0 part of free radical absorbent and 0.5-1.5 parts of antioxidant.
2. The heat-shrinkable material of claim 1, wherein the ethylene-methacrylate copolymer has a methyl methacrylate content of 5 to 25%, a melt index of 0.2 to 5g/10min, a melting point of 80 to 100 ℃, and an environmental stress crack resistance of > 300 hr.
3. The heat-shrinkable material of claim 1, wherein the polyethylene is one of low density polyethylene and linear low density polyethyleneOne or two of them at any ratio, melting point 105-115 deg.C, melt index 0.2-0.5g/10min, and density 0.91-0.94g/cm3(ii) a The polyethylene octene copolymer elastomer has a melt index of 0.1-3g/10min and a density of 0.8-0.95g/cm3。
4. The heat-shrinkable material of claim 1, wherein the sensitizer is one or more of trimethylolpropane trimethacrylate, triallyl isocyanurate and triallyl cyanurate in any proportion; the lubricant is one or more of low molecular weight silicon rubber, polyethylene wax, zinc stearate and silicone master batch in any proportion; the low molecular weight silicon rubber is methyl vinyl silicone rubber with the molecular weight of 4.5 multiplied by 105-6.0×105The content of vinyl is 0.01-0.25%.
5. The heat-shrinkable material of claim 1, wherein the ethylene-vinyl acetate copolymer hot melt adhesive has a softening point of 90 ℃ to 100 ℃ and a rotational viscosity of 70000mpa.s to 100000 mpa.s; the softening point of the polyamide hot melt adhesive is 130-150 ℃, and the rotational viscosity is 50000-70000 mPa.s.
6. The heat-shrinkable material of claim 1 wherein the copper-resistant agent is N, N' -bis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine, having a melting point of 210 ℃ to 250 ℃; the free radical absorbent is one or more of ammonium dihydrogen phosphate, zinc sulfate pyridine and lithium carbonate in any proportion.
7. The heat-shrinkable material of claim 1, wherein the antioxidant is one or more of octadecyl 3, 5-di-tert-butyl-4-hydroxyphenyl propionate, pentaerythritol tetrakis [ methyl- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], 2, 6-di-tert-butyl-p-cresol, 1, 3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene.
8. A method for preparing a heat shrinkable material, comprising:
uniformly mixing 60-90 parts of polyethylene, 10-40 parts of ethylene-methacrylate copolymer, 4-10 parts of polyethylene octene copolymer elastomer, 0.5-3.0 parts of sensitizer, 0.5-1.5 parts of antioxidant and 0.5-2.0 parts of lubricant, and performing extrusion granulation to obtain a skin master batch;
uniformly mixing 70-90 parts of ethylene-vinyl acetate copolymer hot melt adhesive, 10-30 parts of polyamide hot melt adhesive, 0.5-1.5 parts of copper inhibitor, 0.2-1.0 part of free radical absorbent and 0.5-1.5 parts of antioxidant, and carrying out underwater granulation and drying to obtain hot melt adhesive modified master batch;
co-extruding the outer skin master batch and the hot melt adhesive modified master batch by a double-layer extruder, irradiating and crosslinking the obtained semi-finished product, irradiating with the dose of 10-15Mrd, expanding by internal and external pressure difference, cooling and shaping to obtain the product.
9. Use of a heat shrinkable material according to any of claims 1 to 7 for the preparation of double-walled heat shrinkable sleeves.
10. A double-walled heat shrinkable sleeve, wherein the double-walled heat shrinkable sleeve is prepared from the heat shrinkable material of any one of claims 1 to 7.
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| CN107973972A (en) * | 2017-12-21 | 2018-05-01 | 上海长园电子材料有限公司 | A kind of puncture-resistant thermal contraction double-walled pipe and preparation method thereof |
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| CN107973972A (en) * | 2017-12-21 | 2018-05-01 | 上海长园电子材料有限公司 | A kind of puncture-resistant thermal contraction double-walled pipe and preparation method thereof |
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