CN111138738A - 180-DEG C-resistant irradiation crosslinking low-smoke halogen-free cable material and preparation method thereof - Google Patents
180-DEG C-resistant irradiation crosslinking low-smoke halogen-free cable material and preparation method thereof Download PDFInfo
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- CN111138738A CN111138738A CN201911310535.8A CN201911310535A CN111138738A CN 111138738 A CN111138738 A CN 111138738A CN 201911310535 A CN201911310535 A CN 201911310535A CN 111138738 A CN111138738 A CN 111138738A
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- 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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- 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
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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- 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
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C08L2201/22—Halogen free composition
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- 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
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/04—Polymer mixtures characterised by other features containing interpenetrating networks
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
- C08L2312/06—Crosslinking by radiation
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Abstract
The invention discloses a low-smoke halogen-free cable material capable of resisting 180 ℃ irradiation crosslinking, which comprises the following components in parts by weight: 100 parts of base resin; 5-20 parts of epoxy resin mixture; 0.25-2 parts of a photoinitiator; 0.15-1 part of thermal initiator; 100-120 parts of composite flame retardant; 0.5-0.8 part of antioxidant; 1-1.5 parts of a lubricant; 6-8 parts of a crosslinking sensitizer. The invention also discloses a preparation method of the composition. According to the invention, by introducing the epoxy resin mixture capable of generating photothermal dual curing, the cured mixture not only has the toughness of epoxy resin and excellent tensile strength, but also has higher heat resistance, can resist the temperature of 180 ℃, and can react with the base resin simultaneously during irradiation crosslinking to form an interpenetrating network structure. The cable material is not easy to age and lose efficacy under the use environment with the high temperature of 180 ℃, and the problem of reduced tensile strength caused by adding a large amount of filler to retard flame can be avoided.
Description
Technical Field
The invention relates to the field of preparation of low-smoke halogen-free cable materials, in particular to a low-smoke halogen-free cable material capable of resisting irradiation at 180 ℃ and being crosslinked and a preparation method thereof.
Background
In order to meet the requirements of flame retardance and halogen free, the conventional low-smoke halogen-free flame-retardant cable material adopts polyolefin as a base material and is filled with a large amount of inorganic flame retardant to obtain a flame-retardant effect.
However, the method needs to find a balance point between flame retardance and mechanical properties, and the wire and the cable are easily aged and embrittled and lose the protection performance of the wire and the cable when being at a high temperature of 180 ℃ for a long time. If a large amount of inorganic filler is added in order to increase elongation at break, the cable may sacrifice crosslinking density, resulting in a decrease in temperature resistance.
The existing irradiation crosslinking low-smoke halogen-free cable material is easy to crack under the condition of long-term use or stress because a large amount of filling type inorganic flame retardant is added, and is easy to age and lose efficacy if the cable use environment is as high as 180 ℃.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a low-smoke halogen-free cable material capable of resisting 180 ℃ irradiation crosslinking. The cable material is not easy to age and lose efficacy under the use environment with the high temperature of 180 ℃, and can avoid the problem of tensile strength reduction caused by adding a large amount of filler for achieving the flame retardant effect.
The second purpose of the invention is to provide a preparation method of the irradiation crosslinking low-smoke halogen-free cable material capable of resisting 180 ℃.
In order to realize one of the purposes of the invention, the adopted technical scheme is as follows:
the 180 ℃ resistant irradiation crosslinking low-smoke halogen-free cable material comprises the following components in parts by weight:
100 parts of base resin;
5-20 parts of epoxy resin mixture;
0.25-2 parts of a photoinitiator;
0.15-1 part of thermal initiator;
100-120 parts of composite flame retardant;
0.5-0.8 part of antioxidant;
1-1.5 parts of a lubricant;
6-8 parts of a crosslinking sensitizer.
In a preferred embodiment of the present invention, the base resin is High Density Polyethylene (HDPE); the melt index of the high-density polyethylene (HDPE) is 0.5-1.5 g/10min, and the test conditions are as follows: the temperature was 190 ℃ and the load 2.16 KG.
In a preferred embodiment of the present invention, the epoxy resin mixture is a mixture of 3, 4-epoxymethyl 3, 4-epoxyformate, cyclohexane-1, 2-dicarboxylic acid diglycidyl ester and o-cresol epoxy resin.
In a preferred embodiment of the invention, the mass ratio of the 3, 4-epoxy methyl 3, 4-epoxy formate, the diglycidyl cyclohexane-1, 2-dicarboxylate and the o-cresol epoxy resin is 1-2:1-2: 6-8.
In a preferred embodiment of the invention, the composite flame retardant is a mixture of aluminum hydroxide, magnesium hydroxide and aluminum hypophosphite;
in a preferred embodiment of the present invention, the mixing ratio of the aluminum hydroxide, the magnesium hydroxide and the aluminum hypophosphite is: 40-60 parts of aluminum hydroxide, 10-20 parts of magnesium hydroxide and 5-10 parts of aluminum hypophosphite.
In a preferred embodiment of the present invention, the antioxidant is hexa [ β - (3, 5-di-tert-butyl-4-hydroxy-phenyl) propionamidophenyl ] cyclotriphosphazene (HACP).
In a preferred embodiment of the present invention, the lubricant is any one or more of silicone lubricant masterbatch, silicone powder, zinc stearate or PE wax. The organic silicon lubricating master batch is prepared from raw polydimethylsiloxane rubber and polypropylene according to a mass ratio of 1:1, and mixing the components in a ratio of 1.
In a preferred embodiment of the present invention, the crosslinking sensitizer is trimethylolpropane trimethacrylate (TMPTMA).
In a preferred embodiment of the present invention, the epoxy resin is prepared by the following method:
and crushing the o-cresol epoxy resin, adding the 3, 4-epoxy methyl 3, 4-epoxy formate and the cyclohexane-1, 2-dicarboxylic acid diglycidyl ester, uniformly mixing, and adding a photoinitiator accounting for 5-10% of the total mass of the epoxy resin mixture and a thermal initiator accounting for 3-5% of the total mass of the epoxy resin mixture to obtain a mixture A.
In a preferred embodiment of the present invention, the photoinitiator is [ cyclopentadiene-iron-p-xylene ] hexafluorophosphate.
In a preferred embodiment of the invention, the thermal initiator is a mixture of dibenzoyl peroxide and boron trichloride dimethylbenzylamine complex in a mixing mass ratio of 1: 3.
In a preferred embodiment of the invention, the composite flame retardant is prepared by the following method:
and mixing the aluminum hydroxide, the magnesium hydroxide and the aluminum hypophosphite until the temperature reaches 95 +/-5 ℃, stirring for 10-15 minutes, and discharging to obtain the composite flame retardant.
In order to realize the second purpose of the invention, the adopted technical scheme is as follows:
a preparation method of a 180 ℃ resistant irradiation crosslinking low-smoke halogen-free cable material comprises the following steps:
sequentially adding the base resin, the epoxy resin mixture, the composite flame retardant, the lubricant, the antioxidant and the crosslinking sensitizer into an internal mixer, internally mixing, mixing and discharging:
and extruding and granulating to obtain the cable material.
In a preferred embodiment of the present invention, the four temperature zones obtained by extrusion granulation are: the feeding section is 115-120 ℃, the conveying section is 115-120 ℃, the melting section is 120-130 ℃, and the head is 130-135 ℃.
The invention has the beneficial effects that:
the cable material prepared by the invention is not easy to age and lose efficacy under the use environment with the high temperature of 180 ℃, and can avoid the problem of tensile strength reduction caused by adding a large amount of filler for achieving the flame retardant effect.
Detailed Description
The technical principle of the invention is as follows:
introducing a photocurable and thermocurable epoxy resin mixture into a matrix resin, wherein the o-cresol epoxy resin has high heat-resistant characteristics and can be thermocured; 3, 4-epoxy methyl 3, 4-epoxy formate and cyclohexane-1, 2-dicarboxylic acid diglycidyl ester can be cured by light and heat, boron trichloride dimethylbenzylamine with higher initiation temperature is selected by heat initiation and is assisted by a small amount of dibenzoyl peroxide, and a cation initiator [ cyclopentadiene-iron-p-xylene ] hexafluorophosphate is adopted as a photocuring initiator. Cationic photopolymerization is less dependent on light than is radical polymerization.
Radical polymerization is terminated immediately if there is no irradiation with light, whereas cationic photopolymerization requires irradiation with light only in the initial stage and then polymerization can be continued even without light, which is called "dark polymerization" or "living polymerization". Due to this feature, it is very suitable for curing thick layers.
The epoxy resin mixture is physically mixed to prepare uniform particles in a mode of wrapping liquid with powder, so that the epoxy resin mixture is conveniently added in an extrusion granulation stage.
Compared with the prior art, the invention has the advantages that:
the introduced epoxy resin mixture is subjected to photo-thermal dual curing, so that the cured mixture not only has the toughness of the epoxy resin and excellent tensile strength, but also has higher heat resistance, can resist the temperature of 180 ℃, and can react with the base resin simultaneously during irradiation crosslinking to form an interpenetrating network structure.
In order to make the invention more comprehensible, preferred embodiments are described in detail below.
The present invention will be described in further detail with reference to specific examples.
The processing method of the embodiment comprises the following steps:
1. preparing a composite flame retardant: mixing the flame retardant according to the proportion until the temperature reaches 95 +/-5 ℃, stirring for 10-15 minutes and discharging;
2. crushing o-cresol epoxy resin into 80-mesh powder, wrapping the epoxy resin by the o-cresol epoxy resin of 80 meshes according to a proportion to obtain 3, 4-epoxy methyl 3, 4-epoxy formate and cyclohexane-1, 2-dicarboxylic acid diglycidyl ester, mixing to obtain an epoxy resin mixture, and finally adding a photoinitiator and a thermal initiator to uniformly mix to obtain a mixture A.
3. Sequentially adding the base resin, the mixture A, the composite flame retardant, the lubricant, the antioxidant and the crosslinking sensitizer into an internal mixer according to a formula, internally mixing, mixing and discharging:
4. and extruding and granulating by using a double-screw granulator to obtain the irradiation crosslinking low-smoke halogen-free cable material with the temperature resistance of 180 ℃. The four temperature sections in the extrusion granulation process are: the feeding section is 115-120 ℃, the conveying section is 115-120 ℃, the melting section is 120-130 ℃, and the head is 130-135 ℃.
The amounts of the components added in the examples are shown in Table 1, and the properties are shown in Table 2.
TABLE 1
TABLE 2
| Test items | Example 1 | Example 2 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Resin: filler material | 1.33:1 | 1.33:1 | 1.5:1 | 1.33:1 | 1:1 |
| Tensile strength MPa | 18.0 | 19.0 | 18.0 | 17.5 | 15.0 |
| Oxygen index | 38 | 38 | 35 | 30 | 35 |
| Hardness Shore A | 85 | 82 | 70 | 75 | 76 |
| 5% Heat weight loss temperature | 395 | 405 | 315 | 310 | 305 |
| High temperature resistance | 180 | 180 | 150 | 150 | 150 |
The above data are obtained from laboratory measurements.
The test standards and methods were as follows:
tensile strength: determination of tensile Properties of GBT 1040.2-2006 plastics part II: experimental conditions for molding and extruding plastics ";
oxygen index: GBT 2406.2-2009 plastics part 2 of the test for room temperature by measuring the burning behavior by the oxygen index method;
hardness shore a: the hardness of the vulcanized rubber or thermoplastic rubber is measured by using a Shore hardness tester GB/T6031-2017;
5% thermogravimetric temperature: ASTM E2550-2007 Standard test method for thermal stability by thermogravimetric analysis.
As can be seen from tables 1 and 2:
the comparative examples 1 and 2 are compared with the comparative example 3, the tensile strength is improved by reducing the proportion of the filler, and the composite flame retardant is added in a minimum amount, but can achieve higher oxygen index, and the effect is better than that of singly using the aluminum hydroxide. The flame retardant performance of the comparative example 3 meets the requirement but the tensile strength is low, the crack is easy to occur under stress in use, the tensile strength is improved but the flame retardant performance is not enough when the amount of the filler is reduced in the comparative example 2, the addition amount of the filler is reduced by using the composite flame retardant in the comparative example 1, the flame retardant effect is equivalent to that of the example 3, but the tensile strength is greatly improved.
Examples 1 and 2 an epoxy resin mixture was added to obtain tensile strength comparable to that of comparative example 1 (resin: filler ═ 1.5: 1).
In addition, compared with comparative example 2(1.33:1) in which the proportion of the resin filler was the same, the tensile strength was improved by 0.5 to 1.5MPa, and the oxygen index was also improved by using the composite flame retardant. As the amount of the epoxy resin mixture added increases, example 2 can have higher tensile strength than comparative example 1 because the epoxy resin mixture cured has toughness and a high crosslinking density.
Since the crosslinking density is improved along with the increase of the addition amount of the epoxy resin mixture, it can be seen that the 5% thermal weight loss temperature of the epoxy resin composition added in examples 1 and 2 is obviously improved, and the epoxy resin composition can resist the temperature of 180 ℃ for a long time.
Comparative example description:
comparative examples 1-3 are based on the performance of the low smoke zero halogen cable material on the market, the data was measured in the laboratory under the same conditions.
Comparative example 1: the proportion (1.5:1) of the added filler is reduced by using the composite flame retardant, so that the required tensile strength is 18 Mpa;
comparative example 2: aluminum hydroxide is used as a flame retardant, the addition amount of the filler is increased (1.33:1), the tensile strength is reduced to 17.5Mpa, and the flame retardant property is slightly poor;
comparative example 3: aluminum hydroxide is used as a flame retardant, the filler amount is continuously increased (1:1), the tensile strength is obviously reduced, and the flame retardant performance is improved (the oxygen index is equivalent to that of comparative example 1).
The application improves the heat resistance and the tensile strength by adding the photo-thermal dual-curing epoxy resin, and compared with the comparative example 2, the proportion of the filler is the same, but the tensile strength and the heat resistance (ageing resistance) are improved.
The tensile strength reaches the strength of the comparative example 1, the oxygen index is similar to that of the comparative example using the composite flame retardant, and even is improved. In addition, the cost is lower than that of the comparative example 1 because the filler ratio of the present application is increased.
Claims (10)
1. The low-smoke halogen-free cable material capable of resisting 180 ℃ irradiation crosslinking is characterized by comprising the following components in parts by weight:
100 parts of base resin;
5-20 parts of epoxy resin mixture;
0.25-2 parts of a photoinitiator;
0.15-1 part of thermal initiator;
100-120 parts of composite flame retardant;
0.5-0.8 part of antioxidant;
1-1.5 parts of a lubricant;
6-8 parts of a crosslinking sensitizer.
2. The radiation cross-linked low-smoke halogen-free cable material with the temperature resistance of 180 ℃ as claimed in claim 1, wherein the base resin is High Density Polyethylene (HDPE); the melt index of the high-density polyethylene (HDPE) is 0.5-1.5 g/10min, and the test conditions are as follows: the temperature was 190 ℃ and the load 2.16 KG.
3. The low-smoke halogen-free cable material capable of resisting 180 ℃ radiation crosslinking as claimed in claim 1, wherein the epoxy resin mixture is a mixture of 3, 4-epoxy methyl 3, 4-epoxy formate, cyclohexane-1, 2-dicarboxylic acid diglycidyl ester and o-cresol epoxy resin.
4. The low-smoke halogen-free cable material capable of resisting 180 ℃ radiation crosslinking as claimed in claim 1, wherein the mass ratio of 3, 4-epoxy methyl 3, 4-epoxy formate, cyclohexane-1, 2-dicarboxylic acid diglycidyl ester and o-cresol epoxy resin is 1-2:1-2: 6-8.
5. The radiation cross-linking low-smoke halogen-free cable material with the temperature resistance of 180 ℃ as claimed in claim 1, wherein the composite flame retardant is a mixture of aluminum hydroxide, magnesium hydroxide and aluminum hypophosphite.
6. The low-smoke halogen-free cable material capable of resisting 180 ℃ radiation crosslinking as claimed in claim 1, wherein the mixing ratio of the aluminum hydroxide, the magnesium hydroxide and the aluminum hypophosphite is as follows: 40-60 parts of aluminum hydroxide, 10-20 parts of magnesium hydroxide and 5-10 parts of aluminum hypophosphite.
7. The low-smoke halogen-free cable material capable of resisting 180 ℃ radiation crosslinking as claimed in claim 1, wherein the antioxidant is hexa [ β - (3, 5-di-tert-butyl-4-hydroxy-phenyl) propionamidophenyl ] cyclotriphosphazene (HACP);
the lubricant is any one or more of organic silicon lubricating master batch, silicone powder, zinc stearate or PE wax;
the crosslinking sensitizer is trimethylolpropane trimethacrylate (TMPTMA).
8. The radiation crosslinking low-smoke halogen-free cable material with the temperature resistance of 180 ℃ as claimed in claim 1, wherein the epoxy resin is prepared by the following method:
crushing the o-cresol epoxy resin, adding the 3, 4-epoxy methyl 3, 4-epoxy formate and the cyclohexane-1, 2-dicarboxylic acid diglycidyl ester, uniformly mixing, and adding a photoinitiator accounting for 5-10% of the total mass of the epoxy resin mixture and a thermal initiator accounting for 3-5% of the total mass of the epoxy resin mixture to obtain a mixture A;
the photoinitiator is [ cyclopentadiene-iron-p-xylene ] hexafluorophosphate;
the thermal initiator is a mixture of dibenzoyl peroxide and boron trichloride dimethylbenzylamine complex, and the mixing mass ratio is 1: 3.
9. The method for preparing the radiation crosslinking low-smoke halogen-free cable material with the temperature resistance of 180 ℃ according to any one of claims 1 to 8, characterized by comprising the following steps:
sequentially adding the base resin, the mixture A, the composite flame retardant, the lubricant, the antioxidant and the crosslinking sensitizer into an internal mixer, internally mixing, mixing and discharging:
and extruding and granulating to obtain the cable material.
10. The method for preparing the irradiation crosslinking low-smoke halogen-free cable material with the temperature resistance of 180 ℃ according to claim 9, wherein the four temperature sections obtained by extrusion granulation are as follows: the feeding section is 115-120 ℃, the conveying section is 115-120 ℃, the melting section is 120-130 ℃, and the head is 130-135 ℃.
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| CN112852057A (en) * | 2021-01-19 | 2021-05-28 | 安特普工程塑料（苏州）有限公司 | Anti-aging improved polypropylene composition and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109867852A (en) * | 2017-12-04 | 2019-06-11 | 日立金属株式会社 | The manufacturing method of lining material, cable and cable |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109867852A (en) * | 2017-12-04 | 2019-06-11 | 日立金属株式会社 | The manufacturing method of lining material, cable and cable |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112852057A (en) * | 2021-01-19 | 2021-05-28 | 安特普工程塑料（苏州）有限公司 | Anti-aging improved polypropylene composition and preparation method thereof |
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