CN115477796A - Flame-retardant silane crosslinking material with temperature resistance level of 150 ℃ and preparation method thereof - Google Patents
Flame-retardant silane crosslinking material with temperature resistance level of 150 ℃ and preparation method thereof Download PDFInfo
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- 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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
- C08L2312/08—Crosslinking by silane
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention relates to the field of wire and cable materials, and provides a flame-retardant silane crosslinking material with a temperature resistance level of 150 ℃ and a preparation method thereof aiming at the problem of poor high-temperature resistance and aging resistance of the wire and cable materials, wherein the raw materials comprise a component A and a component B; and (2) component A: 40-60 parts of high-density polyethylene, 20-30 parts of linear low-density polyethylene, 5-10 parts of polyolefin elastomer, 5-20 parts of flame retardant, 1-5 parts of antioxidant, 0.5-1.5 parts of anti-UV master batch, 1-3 parts of silane coupling agent and 0.1-1 part of grafting initiator; and the component B comprises: 70-80 parts of linear low-density polyethylene, 0-5 parts of rheological master batch, 0.5-1.5 parts of silane crosslinking catalyst, 5-10 parts of antioxidant and 5-15 parts of anti-UV master batch. The silane crosslinked polyethylene forms a three-dimensional network crosslinked structure, and has better thermal mechanical property than common thermoplastic materials, high heat resistance grade and aging resistance.
Description
Technical Field
The invention relates to the technical field of wire and cable materials, in particular to a flame-retardant silane crosslinking material with a temperature resistance level of 150 ℃ and a preparation method thereof.
Background
The insulation temperature of the power equipment is increased due to overhigh ambient temperature or heat generated by the power equipment during operation. Under the action of high temperature, the mechanical strength of the insulation is reduced, the structure is deformed, the material loses elasticity due to oxidation and polymerization, or the insulation is broken down due to the cracking of the material, so that the voltage is reduced. The strength of the heat resistance of the insulating material directly or indirectly influences the service life of the cable.
Patent CN109306113A discloses an irradiation crosslinking low-smoke halogen-free flame-retardant polyolefin cable material for an automobile wire, which comprises the following components in parts by weight: 25 to 60 parts of ethylene-vinyl acetate copolymer, 5 to 20 parts of compatilizer, 20 to 70 parts of polyethylene, 100 to 160 parts of halogen-free flame retardant, 5 to 30 parts of barium sulfate, 2 to 8 parts of modified nano-silica, 1.0 to 1.6 parts of coupling agent, 1.5 to 3 parts of crosslinking sensitizer, 1.4 to 2.4 parts of antioxidant, 0.5 to 2.0 parts of zinc sulfide and 2 to 5 parts of silicone master batch. According to the invention, the zinc sulfide is used for replacing the copper resisting agent, so that the precipitation and frosting risk caused by using the copper resisting agent is avoided, and the copper ion catalytic aging inhibiting effect is achieved, thereby achieving the copper-carrying high-temperature aging resistance. However, the polyolefin cable material only improves the short-term copper-containing high-temperature aging performance, the aging time is only 240 hours, and the problem of poor long-term high-temperature copper-containing aging performance is not solved. Accordingly, an ideal solution is needed.
Disclosure of Invention
The invention provides a flame-retardant silane crosslinking material with a temperature resistant level of 150 ℃ for overcoming the problem of poor high-temperature aging resistance of wire and cable materials, wherein the insulation material can resist high-temperature aging at 150 ℃ for a long time by crosslinking polyethylene and silane and adding an antioxidant and an anti-UV master batch, and has better processing performance.
In order to achieve the purpose, the invention adopts the following technical scheme:
the flame-retardant silane cross-linking material with the temperature resistance level of 150 ℃ comprises a component A and a component B; the component A comprises the following raw materials in parts by weight: 40 to 60 parts of high-density polyethylene, 20 to 30 parts of linear low-density polyethylene, 5 to 10 parts of polyolefin elastomer, 5 to 20 parts of flame retardant, 1 to 5 parts of antioxidant, 0.5 to 1.5 parts of anti-UV master batch, 1 to 3 parts of silane coupling agent and 0.1 to 1 part of grafting initiator; the component B comprises the following raw materials in parts by weight: 70-80 parts of linear low-density polyethylene, 0-5 parts of rheological master batch, 0.5-1.5 parts of silane crosslinking catalyst, 5-10 parts of antioxidant and 5-15 parts of anti-UV master batch.
The silane crosslinked polyethylene forms a three-dimensional network crosslinked structure, has better thermal mechanical property than common thermoplastic materials, high heat resistance grade and aging resistance, and has the advantages of excellent processing property, simple equipment, low production cost and the like. The invention also adds antioxidant and anti-UV master batch to further improve the high temperature aging resistance of the material. According to the invention, the flame retardant is added into the raw materials to endow the silane crosslinking material with flame retardant performance, and the three-dimensional reticular crosslinking structure of the silane crosslinking material can also improve the dispersibility of the flame retardant, so that the carbonization effect generated when the silane crosslinking material is combusted is facilitated, and the flame retardant performance is improved.
Preferably, the mass ratio of the component A to the component B is (90-94) to (6-10). As a further preference, the mass ratio of the a component to the B component is 92.
Preferably, the flame retardant is a mixture compounded by decabromodiphenylethane and antimony trioxide. Decabromodiphenylethane belongs to a brominated flame retardant, and mainly reacts in a gas phase to release low-energy bromine free radicals, and the low-energy free radicals replace high-energy free radicals (hydrogen free radicals and hydroxyl free radicals), so that the free radical chain reaction for forming flame is inhibited, and the combustion process is slowed down. Antimony trioxide does not have flame retardancy, but antimony oxychloride (SbOCl) which is an oxyhalide is formed when the antimony trioxide is added into a brominated flame retardant, so that a synergistic effect is generated, the brominated flame retardant is promoted to be decomposed into active molecules, and the flame retardant effect of the brominated flame retardant is enhanced.
Preferably, the flame retardant is subjected to the following coating treatment: dissolving vinyl pyrrolidone in a sodium sulfate aqueous solution, heating to 60-80 ℃, adding eugenol and azodiisobutyronitrile, adding a decabromodiphenylethane-antimony trioxide mixture, tween-80 and 1, 4-dioxane, reacting for 3-7h, filtering, washing and drying to obtain the coated flame retardant.
More preferably, the mass ratio of the mixture of the vinyl pyrrolidone, the divinylbenzene and the decabromodiphenylethane-antimony trioxide is 10 (0.5-2) to 80-160.
The flame retardant decabromodiphenylethane and antimony trioxide used in the invention are mutually matched to improve the flame retardant property, but the decabromodiphenylethane and antimony trioxide are both solid and have poor dispersibility in polyethylene, thereby influencing the synergistic effect of the decabromodiphenylethane and antimony trioxide. In order to improve the dispersibility of the flame retardant, the flame retardant is subjected to a coating treatment. The vinyl pyrrolidone monomer and the eugenol are copolymerized, and a coating layer is formed on the surface of the flame retardant through in-situ polymerization, so that the dispersibility and the fluidity of the flame retardant in the polyvinyl red are improved. The eugenol is chemically named as 4-allyl-2-methoxyphenol, a benzene ring and phenolic hydroxyl are introduced into the coating layer, the benzene ring improves the molecular weight and the thermal stability of the coating layer, and the quality of a carbon layer is improved, so that the flame retardant effect is improved; however, the flame retardant has large smoke due to excessive benzene rings, so the using amount of eugenol needs to be reasonably controlled; the phenolic hydroxyl and the carbonyl of the vinyl pyrrolidone form a hydrogen bond, so that the coating polymer has a three-dimensional crosslinking structure, the release of a flame retardant is facilitated, and the mechanical property of the silane crosslinking material is improved.
Preferably, the antioxidant is a compound mixture of pentaerythritol tetrakis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], tris (2, 4-di-tert-butylphenyl) phosphite and 4,4' -bis (alpha, alpha-dimethylbenzyl) diphenylamine.
Preferably, the anti-UV master batch is UV-531.
Preferably, the silane coupling agent is one or more of vinyltrimethoxysilane, vinyltriethoxysilane and vinyltris (2-methoxyethoxy) silane.
Preferably, the grafting initiator is dicumyl peroxide.
Preferably, the silane crosslinking catalyst is dibutyltin dilaurate and/or benzenesulfonic acid. More preferably, the silane crosslinking catalyst is dibutyltin dilaurate.
The invention also provides a preparation method of the flame-retardant silane crosslinking material with the temperature resistance level of 150 ℃, which comprises the following steps:
(1) Weighing the raw materials of the component A in proportion, mixing uniformly, adding the mixture into a double-screw extruder for extrusion granulation, drawing out strips, cooling the strips by a water tank, granulating, drying and packaging to obtain the component A;
(2) Weighing the raw materials of the component B according to a proportion, then uniformly mixing, adding the mixture into a double-screw extruder for extrusion granulation, drawing out material strips, cooling the material strips by a water tank, granulating, drying and packaging to obtain the component B;
(3) And mixing the component A and the component B according to the mass ratio, extruding and molding, and then crosslinking to obtain the flame-retardant silane crosslinking material with the temperature resistance level of 150 ℃.
Preferably, the crosslinking in step (3) is carried out in water or steam at 90-100 ℃.
Therefore, the invention has the following beneficial effects: (1) The insulating material can resist high-temperature aging at 150 ℃ for a long time and has better processing performance by crosslinking polyethylene and silane and adding the antioxidant and the anti-UV master batch; (2) The vinyl pyrrolidone monomer and the eugenol are copolymerized, a coating layer is formed on the surface of the flame retardant through in-situ polymerization, the dispersity and the fluidity of the flame retardant in polyethylene red are improved, benzene rings and phenolic hydroxyl groups are introduced into the eugenol coating layer, the benzene rings improve the molecular weight and the thermal stability of the coating layer, and the improvement of the quality of a carbon layer is facilitated, so that the flame retardant effect is improved; the phenolic hydroxyl and the carbonyl of the vinyl pyrrolidone form a hydrogen bond, so that the coating polymer has a three-dimensional crosslinking structure, and the release of the flame retardant is facilitated.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
In the present invention, unless otherwise specified, all the raw materials and equipments used are commercially available or commonly used in the art, and the methods in the examples are conventional in the art unless otherwise specified.
General examples
A flame-retardant silane cross-linking material with temperature resistance level of 150 ℃ comprises a component A and a component B in a mass ratio of (90-94) to (6-10); the component A comprises the following raw materials in parts by weight: 40 to 60 parts of high density polyethylene, 20 to 30 parts of linear low density polyethylene, 5 to 10 parts of polyolefin elastomer, 5 to 20 parts of flame retardant, 1 to 5 parts of antioxidant, 0.5 to 1.5 parts of anti-UV master batch, 1 to 3 parts of silane coupling agent and 0.1 to 1 part of grafting initiator; the component B comprises the following raw materials in parts by weight: 70-80 parts of linear low density polyethylene, 0-5 parts of rheological master batch, 0.5-1.5 parts of silane crosslinking catalyst, 5-10 parts of antioxidant and 5-15 parts of anti-UV master batch.
The flame retardant is a mixture compounded by decabromodiphenylethane and antimony trioxide.
The antioxidant is a compound mixture of pentaerythritol tetrakis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], tris (2, 4-di-tert-butylphenyl) phosphite and 4,4' -bis (alpha, alpha-dimethylbenzyl) diphenylamine.
The anti-UV master batch is UV-531.
The silane coupling agent is one or more of vinyl trimethoxy silane, vinyl triethoxy silane and vinyl tri (2-methoxyethoxy) silane.
The grafting initiator is dicumyl peroxide.
The silane crosslinking catalyst is dibutyltin dilaurate and/or benzenesulfonic acid.
The preparation method of the flame-retardant silane crosslinking material with the temperature resistance level of 150 ℃ comprises the following steps:
(1) Weighing the raw materials of the component A in proportion, mixing uniformly, adding the mixture into a double-screw extruder for extrusion granulation, drawing out strips, cooling the strips by a water tank, granulating, drying and packaging to obtain the component A;
(2) Weighing the raw materials of the component B according to a proportion, then uniformly mixing, adding the mixture into a double-screw extruder for extrusion granulation, drawing out material strips, cooling the material strips by a water tank, granulating, drying and packaging to obtain the component B;
(3) And mixing the component A and the component B according to a mass ratio, extruding and molding, and then crosslinking in water or steam at 90-100 ℃ to obtain the flame-retardant silane crosslinking material with the temperature resistance level of 150 ℃.
The temperature of each stage is set as follows: the feed section is 120-140 ℃, the compression section is 150-190 ℃, the plasticizing section is 205-225 ℃, the flange is 170-180 ℃, the neck is 170-180 ℃, the head is 210-230 ℃ and the eye die is 230-240 ℃.
Example 1
The flame-retardant silane cross-linking material with the temperature resistance level of 150 ℃ consists of a component A and a component B in a mass ratio of 92; the component A comprises the following raw materials in parts by weight: 51 parts of high-density polyethylene, 25 parts of linear low-density polyethylene, 8 parts of polyolefin elastomer, 10 parts of flame retardant, 3.15 parts of antioxidant, 1 part of anti-UV master batch, 1.6 parts of silane coupling agent and 0.25 part of grafting initiator; the component B comprises the following raw materials in parts by weight: 76 parts of linear low-density polyethylene, 4 parts of rheological master batch, 1 part of silane crosslinking catalyst, 8 parts of antioxidant and 11 parts of anti-UV master batch.
The flame retardant is a mixture compounded by decabromodiphenylethane and antimony trioxide according to the weight ratio of 2; the antioxidant is a mixture compounded by pentaerythritol tetrakis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], tris (2, 4-di-tert-butylphenyl) phosphite and 4,4' -bis (alpha, alpha-dimethylbenzyl) diphenylamine according to a weight ratio of 1.5; the anti-UV master batch is UV-531; the silane coupling agent is vinyl trimethoxy silane; the grafting initiator is dicumyl peroxide; the silane crosslinking catalyst is dibutyltin dilaurate.
The preparation method of the flame-retardant silane crosslinking material with the temperature resistance level of 150 ℃ comprises the following steps:
(1) Weighing the raw materials of the component A in proportion, mixing uniformly, adding the mixture into a double-screw extruder for extrusion granulation, drawing out strips, cooling the strips by a water tank, granulating, drying and packaging to obtain the component A;
(2) Weighing the raw materials of the component B according to a proportion, then uniformly mixing, adding the mixture into a double-screw extruder for extrusion granulation, drawing out material strips, cooling the material strips by a water tank, granulating, drying and packaging to obtain the component B;
(3) And mixing the component A and the component B according to a mass ratio, extruding and molding, and then crosslinking in water at 90 ℃ to obtain the flame-retardant silane crosslinking material with the temperature resistance level of 150 ℃.
Example 2
The flame-retardant silane cross-linking material with the temperature resistance level of 150 ℃ consists of a component A and a component B in a mass ratio of 92; the component A comprises the following raw materials in parts by weight: 51 parts of high-density polyethylene, 25 parts of linear low-density polyethylene, 8 parts of polyolefin elastomer, 10 parts of flame retardant, 3.66 parts of antioxidant, 0.5 part of anti-UV master batch, 1.6 parts of silane coupling agent and 0.25 part of grafting initiator; the component B comprises the following raw materials in parts by weight: 76 parts of linear low-density polyethylene, 4 parts of rheological master batch, 1 part of silane crosslinking catalyst, 7 parts of antioxidant and 12 parts of anti-UV master batch.
The flame retardant is a mixture compounded by decabromodiphenylethane and antimony trioxide according to the weight ratio of 2; the antioxidant is a mixture compounded by pentaerythritol tetrakis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], tris (2, 4-di-tert-butylphenyl) phosphite and 4,4' -bis (alpha, alpha-dimethylbenzyl) diphenylamine according to a weight ratio of 1.5; the anti-UV master batch is UV-531; the silane coupling agent is vinyl trimethoxy silane; the grafting initiator is dicumyl peroxide; the silane crosslinking catalyst is dibutyltin dilaurate.
The preparation method is the same as example 1.
Example 3
The difference from example 1 is that the mass ratio of the a component to the B component is 90.
Example 4
The difference from example 1 is that the flame retardant is coated as follows: dissolving 10g of vinyl pyrrolidone in 20mL of sodium sulfate aqueous solution, heating to 70 ℃, adding 1g of eugenol and 0.1g of azodiisobutyronitrile, then adding 120g of decabromodiphenylethane-antimony trioxide mixture (weight ratio is 2.
Example 5
The difference from example 4 is that the flame retardant is coated with: 10g of vinyl pyrrolidone is dissolved in 20mL of sodium sulfate aqueous solution, the temperature is raised to 70 ℃, 0.1g of azodiisobutyronitrile is added, and then 120g of decabromodiphenylethane-antimony trioxide mixture (weight ratio is 2.
Example 6
The difference from example 1 is that the flame retardant is coated as follows: 10g of vinyl pyrrolidone is dissolved in 20mL of sodium sulfate aqueous solution, the temperature is raised to 70 ℃, 1g of divinylbenzene and 0.1g of azodiisobutyronitrile are added, and then 120g of decabromodiphenylethane-antimony trioxide mixture (weight ratio is 2.
Comparative example 1
The difference from example 1 is that no antioxidant is used.
The preparation method is the same as example 1.
Comparative example 2
The difference from example 1 is that the antioxidant is pentaerythritol tetrakis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ].
Comparative example 3
The flame-retardant silane cross-linking material with the temperature resistance level of 150 ℃ consists of a component A and a component B in a mass ratio of 92; the component A comprises the following raw materials in parts by weight: 28 parts of high-density polyethylene, 28 parts of linear low-density polyethylene, 28 parts of polyolefin elastomer, 10 parts of flame retardant, 3.15 parts of antioxidant, 1 part of anti-UV master batch, 1.6 parts of silane coupling agent and 0.25 part of grafting initiator; the component B comprises the following raw materials in parts by weight: 76 parts of linear low-density polyethylene, 4 parts of rheological master batch, 1 part of silane crosslinking catalyst, 8 parts of antioxidant and 11 parts of anti-UV master batch.
The flame retardant is a mixture compounded by decabromodiphenylethane and antimony trioxide according to the weight ratio of 2; the antioxidant is a mixture compounded by pentaerythritol tetrakis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], tris (2, 4-di-tert-butylphenyl) phosphite and 4,4' -bis (alpha, alpha-dimethylbenzyl) diphenylamine according to a weight ratio of 1.5; the anti-UV master batch is UV-531; the silane coupling agent is vinyl trimethoxy silane; the grafting initiator is dicumyl peroxide; the silane crosslinking catalyst is dibutyltin dilaurate.
The preparation method is the same as example 1.
Comparative example 4
The flame-retardant silane cross-linking material with the temperature resistance level of 150 ℃ consists of a component A and a component B in a mass ratio of 92; the component A comprises the following raw materials in parts by weight: 56 parts of high-density polyethylene, 28 parts of linear low-density polyethylene, 10 parts of flame retardant, 3.15 parts of antioxidant, 1 part of anti-UV master batch, 1.6 parts of silane coupling agent and 0.25 part of grafting initiator; the component B comprises the following raw materials in parts by weight: 76 parts of linear low-density polyethylene, 4 parts of rheological master batch, 1 part of silane crosslinking catalyst, 8 parts of antioxidant and 11 parts of anti-UV master batch.
The flame retardant is a mixture compounded by decabromodiphenylethane and antimony trioxide according to the weight ratio of 2; the antioxidant is a mixture compounded by pentaerythritol tetrakis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], tris (2, 4-di-tert-butylphenyl) phosphite and 4,4' -bis (alpha, alpha-dimethylbenzyl) diphenylamine according to a weight ratio of 1.5; the anti-UV master batch is UV-531; the silane coupling agent is vinyl trimethoxy silane; the grafting initiator is dicumyl peroxide; the silane crosslinking catalyst is dibutyltin dilaurate.
The preparation method is the same as example 1.
Comparative example 5
The flame-retardant silane cross-linking material with the temperature resistance level of 150 ℃ consists of a component A and a component B in a mass ratio of 92; the component A comprises the following raw materials in parts by weight: 56 parts of high-density polyethylene, 28 parts of polyolefin elastomer, 10 parts of flame retardant, 3.15 parts of antioxidant, 1 part of anti-UV master batch, 1.6 parts of silane coupling agent and 0.25 part of grafting initiator; the component B comprises the following raw materials in parts by weight: 76 parts of linear low-density polyethylene, 4 parts of rheological master batch, 1 part of silane crosslinking catalyst, 8 parts of antioxidant and 11 parts of anti-UV master batch.
The flame retardant is a mixture compounded by decabromodiphenylethane and antimony trioxide according to the weight ratio of 2; the antioxidant is a mixture compounded by pentaerythritol tetrakis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], tris (2, 4-di-tert-butylphenyl) phosphite and 4,4' -bis (alpha, alpha-dimethylbenzyl) diphenylamine according to a weight ratio of 1.5; the anti-UV master batch is UV-531; the silane coupling agent is vinyl trimethoxy silane; the grafting initiator is dicumyl peroxide; the silane crosslinking catalyst is dibutyltin dilaurate.
The preparation method is the same as example 1.
Comparative example 6
The difference from example 1 is that the mass ratio of the a component to the B component is 95.
Performance test
The flame-retardant silane cross-linking material prepared in each example and comparative example is subjected to appearance, mechanical property, aging resistance and flame retardance tests, and the test method and technical requirements are as follows:
appearance: the granules have uniform size and color, the size is not more than 3 x 4mm, and no obvious powder substances are required among the granules. All meet the requirements.
Mechanical properties: GB/T1040.3-2006, the required tensile strength is more than or equal to 13.5MPa, and the elongation at break is more than or equal to 350 percent.
Aging resistance: GB/T2951.12-2008 requires that under the conditions of (1) mechanical properties-air heat aging (175 ℃,240 h), the tensile strength is more than or equal to 10MPa, and the elongation at break is more than or equal to 100 percent; (2) long-term aging resistance-air heat aging (150 ℃ C., 3000 h), no cracks were observed visually after winding.
The flame retardant property is as follows: (1) after the flame retardant rating is subjected to combustion test for 10 seconds twice according to UL94 test-V-0 requirements, the flame is extinguished within 30 seconds, and no combustible can fall off; (2) the limiting oxygen index is tested according to GB/T2406.2-2009.
Specific results are shown in the following table.
Analysis shows that the performances of the flame-retardant silane crosslinking materials prepared by the method of the invention in the examples 1-3 meet the requirements. Compared with the embodiment 1, the antioxidant is not added in the comparative example 1, the antioxidant in the comparative example 2 is not compounded, and the heat aging resistance of the product at 150 ℃ does not reach the standard, which shows that the selection of the antioxidant plays a key role in the heat aging resistance; comparative examples 3 to 5 because the ratio of the amounts of the high density polyethylene, the linear low density polyethylene and the polyolefin elastomer was not within the preferable range, the long-term aging resistance was not satisfied, and the mechanical properties were also significantly decreased. In comparative example 6, the mass ratio of the components A and B is out of the preferable range, the long-term aging resistance is not up to the standard, and the performances are also reduced, because the mass ratio of the components A and B directly influences the structure of the silane crosslinking material.
Compared with the embodiment 1, the embodiment 4 has the advantages that the flame retardant is coated, the limiting oxygen index is obviously improved, and the mechanical property is slightly improved. Compared with the embodiment 4, the eugenol is not added when the flame retardant is coated in the embodiment 5, the eugenol is replaced by divinylbenzene when the flame retardant is coated in the embodiment 6, the limited oxygen index is lower than that in the embodiment 4, and the better flame retardant effect can be achieved under the combined action of the benzene ring and the phenolic hydroxyl group of the eugenol.
Although the present invention has been described with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the present invention.
Claims (10)
1. The flame-retardant silane cross-linking material with the temperature resistance level of 150 ℃ is characterized by comprising a component A and a component B; the component A comprises the following raw materials in parts by weight: 40-60 parts of high-density polyethylene, 20-30 parts of linear low-density polyethylene, 5-10 parts of polyolefin elastomer, 5-20 parts of flame retardant, 1-5 parts of antioxidant, 0.5-1.5 parts of anti-UV master batch, 1-3 parts of silane coupling agent and 0.1-1 part of grafting initiator; the component B comprises the following raw materials in parts by weight: 70-80 parts of linear low-density polyethylene, 0-5 parts of rheological master batch, 0.5-1.5 parts of silane crosslinking catalyst, 5-10 parts of antioxidant and 5-15 parts of anti-UV master batch.
2. The flame-retardant silane cross-linking material with the temperature resistance of 150 ℃ is characterized in that the mass ratio of the component A to the component B is (90-94) to (6-10).
3. The flame-retardant silane cross-linking material with the temperature resistance of 150 ℃ is characterized in that the flame retardant is a mixture of decabromodiphenylethane and antimony trioxide.
4. The flame-retardant silane cross-linking material with the temperature resistance of 150 ℃ is characterized in that the flame retardant is coated by the following components: dissolving vinyl pyrrolidone in a sodium sulfate aqueous solution, heating to 60-80 ℃, adding eugenol and azodiisobutyronitrile, adding a decabromodiphenylethane-antimony trioxide mixture, tween-80 and 1, 4-dioxane, reacting for 3-7h, filtering, washing and drying to obtain the coated flame retardant.
5. The flame-retardant silane cross-linking material with the temperature resistance level of 150 ℃ as claimed in claim 4, wherein the mass ratio of the mixture of vinyl pyrrolidone, divinylbenzene and decabromodiphenylethane-antimony trioxide is 10 (0.5-2) to (80-160).
6. The flame-retardant silane crosslinking material with the temperature resistance level of 150 ℃ as claimed in claim 1, wherein the antioxidant is a compound mixture of pentaerythritol tetrakis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], tris (2, 4-di-tert-butylphenyl) phosphite and 4,4' -bis (alpha, alpha-dimethylbenzyl) diphenylamine.
7. The flame-retardant silane crosslinking material with the temperature resistance grade of 150 ℃ according to claim 1, wherein the silane coupling agent is one or more of vinyltrimethoxysilane, vinyltriethoxysilane and vinyltris (2-methoxyethoxy) silane.
8. The flame-retardant silane crosslinking material with the temperature resistance level of 150 ℃ according to claim 1, 6 or 7, wherein the silane crosslinking catalyst is dibutyltin dilaurate and/or benzenesulfonic acid.
9. The preparation method of the flame-retardant silane cross-linking material with the temperature resistance of 150 ℃ according to any one of claims 1 to 8, is characterized by comprising the following steps: (1) Weighing the raw materials of the component A in proportion, then mixing uniformly, adding the mixture into a double-screw extruder for extrusion granulation, drawing out strips, cooling the strips by a water tank, cutting the strips into granules, drying and packaging to obtain the component A;
(2) Weighing the raw materials of the component B according to a proportion, then uniformly mixing, adding the mixture into a double-screw extruder for extrusion granulation, drawing out material strips, cooling the material strips by a water tank, granulating, drying and packaging to obtain the component B;
(3) And mixing the component A and the component B according to the mass ratio, extruding and molding, and then crosslinking to obtain the flame-retardant silane crosslinking material with the temperature resistance level of 150 ℃.
10. The method for preparing the flame-retardant silane cross-linking material with the temperature resistance of 150 ℃ according to claim 9, wherein the cross-linking in the step (3) is carried out in water or steam at the temperature of 90-100 ℃.
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| CN116589815A (en) * | 2023-05-04 | 2023-08-15 | 江苏上上电缆集团新材料有限公司 | Silane crosslinked polyethylene insulating material resistant to temperature of 150 ℃ and preparation method thereof |
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