CN109337188B - Irradiation crosslinking high-temperature-resistant heat-shrinkable sleeve and production method thereof - Google Patents
Irradiation crosslinking high-temperature-resistant heat-shrinkable sleeve and production method thereof Download PDFInfo
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- CN109337188B CN109337188B CN201811169214.6A CN201811169214A CN109337188B CN 109337188 B CN109337188 B CN 109337188B CN 201811169214 A CN201811169214 A CN 201811169214A CN 109337188 B CN109337188 B CN 109337188B
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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
- C08L23/0892—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms containing monomers with other atoms than carbon, hydrogen or oxygen atoms
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- 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
- C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
- C08K2003/2213—Oxides; Hydroxides of metals of rare earth metal of cerium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- 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
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- 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
- C08L2203/00—Applications
- C08L2203/18—Applications used for 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
- C08L2312/00—Crosslinking
- C08L2312/06—Crosslinking by radiation
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Abstract
The invention discloses an irradiation crosslinking high-temperature-resistant heat-shrinkable tubing, which comprises the following materials in parts by weight: 100 parts of ethylene-tetrafluoroethylene copolymer, wherein the molar ratio of C-F groups to C-H groups of the crosslinked ethylene-tetrafluoroethylene copolymer is 1: 2-9; 0.3-3 parts of a crosslinking agent; 0.3-8 parts of a heat-resistant agent; 0.3-3 parts of an antioxidant; 1-10 parts of antimony trioxide; 0.1-3 parts of pentaerythritol stearate; 0.1-2 parts of N' N-ethylene bis stearamide; 0.1-3 parts of white oil. The irradiation crosslinking high-temperature-resistant heat-shrinkable tubing can be processed at the temperature of 200-238 ℃, has low processing temperature and good crosslinking effect and stability, can effectively improve the heat resistance of the material, and has no obvious smoke or small smoke generation amount in the production process.
Description
Technical Field
The invention relates to a material for preparing a high-temperature-resistant heat-shrinkable sleeve and a preparation method thereof.
Background
The temperature resistance level of the existing heat-shrinkable tubing is generally 150 ℃, and the heat-shrinkable tubing is lack of high temperature resistance. Ethylene-tetrafluoroethylene copolymer (ETFE), also known as F40, used in cables, is the toughest and lightest fluoroplastic. The ETFE has excellent dielectric property, insulating property and mechanical property, and has the advantages of irradiation resistance, cracking resistance, aging resistance, various chemical solvents resistance, high and low temperature resistance and long-term working temperature of between 65 ℃ below zero and 150 ℃. After the ETFE resin is subjected to crosslinking irradiation, the radiation resistance, the tensile strength and the ageing resistance are greatly improved.
However, the cross-linking agent of the prior X-ETFE material is easy to self-polymerize in the production process, has strict requirements on the processing temperature, needs to reach 280-300 ℃, has poor thermal stability in the processing process, is easy to yellow, and further deepens the color after irradiation. Chinese patent publication No. 105061876A discloses a performance-adjustable irradiation crosslinking ethylene-tetrafluoroethylene copolymer insulating material, and the problems of large smoke generation, poor thermal stability and yellowing of a crosslinking agent in the production process are improved and solved by introducing a technology of a composite crosslinking agent containing a crosslinking agent prepolymer.
Therefore, a heat-shrinkable tube which can be processed at a lower temperature and can achieve a high-temperature resistant effect is urgently needed in the technical field of heat-shrinkable tubes.
Disclosure of Invention
The invention aims to solve the problems and provides an irradiation crosslinking high-temperature-resistant heat-shrinkable tubing which can be processed at a lower temperature and can achieve a high-temperature-resistant effect.
In order to achieve the purpose, the invention provides an irradiation crosslinking high-temperature-resistant heat-shrinkable tubing, which is prepared from the following materials in parts by weight: 100 parts of ethylene-tetrafluoroethylene copolymer (ETFE for short), wherein the molar ratio of C-F groups to C-H groups of the crosslinked ethylene-tetrafluoroethylene copolymer is 1: 2-9; 0.3-3 parts of a crosslinking agent; 0.3-8 parts of a heat-resistant agent; 0.3-3 parts of an antioxidant; 1-10 parts of antimony trioxide; 0.1-3 parts of pentaerythritol stearate; 0.1-2 parts of N' N-ethylene bis stearamide; 0.1-3 parts of white oil.
Preferably, the cross-linking agent is a compound of trihydroxymethyl propane trimethacrylate (abbreviated as TMPTMA) and triallyl isocyanurate (abbreviated as TAIC).
Preferably, the heat-resistant agent is cerium oxide or a compound of cerium oxide and titanium dioxide;
preferably, the antioxidant is a complex of 1, 3, 5-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) 2, 4, 6-trimethylbenzene and N, N' -bis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propane ] hydrazine.
Preferably, the weight ratio of the 1, 3, 5-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) 2, 4, 6-trimethylbenzene to the N, N' -bis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propane ] hydrazine in the antioxidant is 1: 0.2.
The invention also provides a production method of the irradiation crosslinking high-temperature-resistant heat-shrinkable tubing, which is prepared from the preparation material of the irradiation crosslinking high-temperature-resistant heat-shrinkable tubing, and the preparation method comprises the following steps:
firstly, 100 parts of ethylene-tetrafluoroethylene copolymer (ETFE for short) in a radiation crosslinking high-temperature-resistant heat-shrinkable sleeve, wherein the molar ratio of C-F groups to C-H groups of the crosslinked ethylene-tetrafluoroethylene copolymer is 1: 2-9; 0.3-3 parts of a crosslinking agent; 0.3-8 parts of a heat-resistant agent; 0.3-3 parts of an antioxidant; 1-10 parts of antimony trioxide; 0.1-3 parts of pentaerythritol stearate; 0.1-2 parts of N' N-ethylene bis stearamide; adding 0.1-3 parts of white oil into a high-speed stirrer, and stirring at a high speed for 5-10 minutes, wherein the temperature of the materials is controlled within the range of 20-80 ℃;
then extruding, drawing wire and air-cooling and granulating the mixture at the temperature of 200-238 ℃ by using a double-screw extruder;
extruding the granulated granules through a single screw at the temperature of 200-238 ℃ to form a sleeve;
then irradiating the material by an electron accelerator or a cobalt source with the irradiation dose of 10-20Mrad, and expanding the irradiated sleeve by 1-3 times by using expansion equipment at the temperature of 230-;
and finally, cooling and shaping to obtain the irradiation crosslinking high-temperature-resistant heat-shrinkable tubing capable of being processed at low temperature.
Compared with the prior art, the invention has the following beneficial technical effects:
the preparation material of the irradiation crosslinking high temperature resistant heat-shrinkable sleeve adjusts the molar ratio of the C-F group and the C-H group of the crosslinked ethylene-tetrafluoroethylene copolymer to 1: 2-9, simultaneously adds the heat-resistant agent, can reach the temperature resistance of 200 ℃ by using the common crosslinking agent, has low processing temperature, can process at the temperature of 200-238 ℃, can ensure that the crosslinking agent is not easy to volatilize and self-polymerize, improves the crosslinking effect and the stability of the material, has higher elongation at break of the crosslinked material, and can keep the elongation at break above 200 percent.
Detailed Description
In order to explain the technical contents, formulation ratios, and objects and effects of the present invention in detail, the following description will be given in conjunction with the embodiments.
The radiation crosslinking high-temperature resistant heat-shrinkable tubing comprises the following preparation materials in parts by weight: 100 parts of ethylene-tetrafluoroethylene copolymer (ETFE for short), wherein the molar ratio of C-F groups to C-H groups of the crosslinked ethylene-tetrafluoroethylene copolymer is 1: 2-9; 0.3-3 parts of a crosslinking agent; 0.3-8 parts of a heat-resistant agent; 0.3-3 parts of an antioxidant; 1-10 parts of antimony trioxide; 0.1-3 parts of pentaerythritol stearate; 0.1-2 parts of N' N-ethylene bis stearamide; 0.1-3 parts of white oil.
Preferably, the cross-linking agent is a compound of trihydroxymethyl propane trimethacrylate (abbreviated as TMPTMA) and triallyl isocyanurate (abbreviated as TAIC).
Preferably, the heat-resistant agent is cerium oxide or a compound of cerium oxide and titanium dioxide;
preferably, the antioxidant is a complex of 1, 3, 5-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) 2, 4, 6-trimethylbenzene and N, N' -bis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propane ] hydrazine.
Preferably, the weight ratio of the 1, 3, 5-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) 2, 4, 6-trimethylbenzene to the N, N' -bis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propane ] hydrazine in the antioxidant is 1: 0.2.
The invention also provides a production method of the irradiation crosslinking high-temperature-resistant heat-shrinkable tubing, which is prepared from the preparation material of the irradiation crosslinking high-temperature-resistant heat-shrinkable tubing, and the preparation method comprises the following steps:
firstly, 100 parts of ethylene-tetrafluoroethylene copolymer (ETFE for short) in a radiation crosslinking high-temperature-resistant heat-shrinkable sleeve, wherein the molar ratio of C-F groups to C-H groups of the crosslinked ethylene-tetrafluoroethylene copolymer is 1- (2-9); 0.3-3 parts of a crosslinking agent; 0.3-8 parts of a heat-resistant agent; 0.3-3 parts of an antioxidant; 1-10 parts of antimony trioxide; 0.1-3 parts of pentaerythritol stearate; 0.1-2 parts of N' N-ethylene bis stearamide; adding 0.1-3 parts of white oil into a high-speed stirrer, and stirring at a high speed for 5-10 minutes, wherein the temperature of the materials is controlled within the range of 20-80 ℃;
then extruding, drawing wire and air-cooling and granulating the mixture at the temperature of 200-238 ℃ by using a double-screw extruder;
extruding the granulated granules through a single screw at the temperature of 200-238 ℃ to form a sleeve;
then irradiating the material by an electron accelerator or a cobalt source with the irradiation dose of 10-20Mrad, and expanding the irradiated sleeve by 1-3 times by using expansion equipment at the temperature of 230-;
and finally, cooling and shaping to obtain the irradiation crosslinking high-temperature-resistant heat-shrinkable tubing capable of being processed at low temperature.
The preparation material of the irradiation crosslinking high temperature resistant heat-shrinkable sleeve adjusts the molar ratio of the C-F group and the C-H group of the crosslinked ethylene-tetrafluoroethylene copolymer to 1: 2-9, simultaneously adds the heat-resistant agent, can reach the temperature resistance of 200 ℃ by using the common crosslinking agent, has low processing temperature, can process at the temperature of 200-238 ℃, can ensure that the crosslinking agent is not easy to volatilize and self-polymerize, improves the crosslinking effect and the stability of the material, has higher elongation at break of the crosslinked material, and can keep the elongation at break above 200 percent.
Several specific examples of this embodiment of the invention are set forth below, all parts being by weight unless otherwise indicated:
example 1
The material composition of example 1 was: 100 parts of ETFE, wherein the molar ratio of C-F groups to C-H groups is 1: 2, 0.5 part of TMPTMA, 1 part of TAIC, 1 part of cerium oxide, 1 part of titanium dioxide, 13302 parts of antioxidant, 10240.4 parts of antioxidant, 5 parts of antimony trioxide, 1 part of pentaerythritol stearate, 0.5 part of N' N-ethylene bis stearamide and 1.5 parts of white oil.
Example 2
The preparation material of the embodiment 2 comprises the following components: 100 parts of ETFE, wherein the molar ratio of C-F groups to C-H groups is 1: 4, 1 part of TMPTMA, 1 part of TAIC, 1 part of cerium oxide, 2 parts of titanium dioxide, 13302 parts of antioxidant, 10240.4 parts of antioxidant, 5 parts of antimony trioxide, 1 part of pentaerythritol stearate, 0.5 part of N' N-ethylene bis stearamide and 1.5 parts of white oil.
Example 3
The preparation material of example 3 comprises the following components: 100 parts of ETFE, wherein the molar ratio of C-F groups to C-H groups is 1: 5, 1.5 parts of TMPTMA, 1 part of TAIC, 2 parts of cerium oxide, 2 parts of titanium dioxide, 13302 parts of antioxidant, 10240.4 parts of antioxidant, 5 parts of antimony trioxide, 1 part of pentaerythritol stearate, 0.5 part of N' N-ethylene bis stearamide and 1.5 parts of white oil.
Example 4
The preparation material of example 4 comprises the following components: 100 parts of ETFE, wherein the molar ratio of C-F groups to C-H groups is 1: 8, 2 parts of TMPTMA, 0.5 part of TAIC, 3 parts of cerium oxide, 13302 parts of antioxidant, 10240.4 parts of antioxidant, 5 parts of antimony trioxide, 1 part of pentaerythritol stearate, 0.5 part of N' N-ethylene bis stearamide and 1.5 parts of white oil.
The materials prepared in the above examples 1 to 4 were used to produce heat shrinkable tubing according to the production method of the radiation crosslinking high temperature resistant heat shrinkable tubing.
The comparative results of the tests on the samples produced in the above examples 1 to 4 according to the above method are as follows:
the test results in the table show that the invention can effectively improve the elongation at break before the insulation aging, the absolute value of the elongation at break after the aging test is carried out for 10 days at 200 ℃ is more than 150%, and the invention can be processed at the temperature of 200-238 ℃, the lower processing temperature reduces the requirements of processing equipment, which can lead the cross-linking agent not to be easily volatilized and self-polymerized, and improve the cross-linking effect and the stability of the material, and simultaneously, the irradiation cross-linking high temperature resistant heat-shrinkable sleeve can resist the temperature of 200 ℃. The elongation at break of the cross-linked material is high, and the elongation at break can be kept above 200%.
The present invention is not limited to the above-described embodiments, and various changes may be made by those skilled in the art, which changes are equivalent or similar to the present invention and are intended to be included within the scope of the appended claims.
Claims (3)
1. An irradiation crosslinking high temperature resistant heat-shrinkable tubing, characterized in that: the preparation material comprises the following components by weight: 100 parts of ethylene-tetrafluoroethylene copolymer, wherein the molar ratio of C-F groups to C-H groups of the ethylene-tetrafluoroethylene copolymer is 1: 2-5; 0.3-3 parts of a crosslinking agent; 0.3-8 parts of a heat-resistant agent; 0.3-3 parts of an antioxidant; 1-10 parts of antimony trioxide; 0.1-3 parts of pentaerythritol stearate; 0.1-2 parts of N' N-ethylene bis stearamide; 0.1-3 parts of white oil; wherein the antioxidant is a compound of 1, 3, 5-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) 2, 4, 6-trimethylbenzene and N, N' -bis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propane ] hydrazine; the cross-linking agent is a compound of trihydroxy methyl propane trimethacrylate and triallyl isocyanurate; the heat-resistant agent is cerium oxide or a compound of cerium oxide and titanium dioxide.
2. The radiation crosslinked, high temperature resistant, heat shrinkable tubing of claim 1, wherein: in the antioxidant, the weight ratio of 1, 3, 5-tri (3, 5-di-tert-butyl-4-hydroxybenzyl) 2, 4, 6-trimethylbenzene to N, N' -bis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propane ] hydrazine is 1: 0.2.
3. An irradiation crosslinking high temperature resistant heat-shrinkable tubing, characterized in that: the heat-shrinkable sleeve is made of the preparation material of the irradiation crosslinking high-temperature-resistant heat-shrinkable sleeve as claimed in any one of claims 1 to 2, and the preparation method comprises the following steps:
firstly, 100 parts of ethylene-tetrafluoroethylene copolymer in a radiation crosslinking high-temperature-resistant heat-shrinkable sleeve, wherein the molar ratio of C-F groups to C-H groups of the ethylene-tetrafluoroethylene copolymer is 1: 2-5; 0.3-3 parts of a crosslinking agent; 0.3-8 parts of a heat-resistant agent; 0.3-3 parts of an antioxidant; 1-10 parts of antimony trioxide; 0.1-3 parts of pentaerythritol stearate; 0.1-2 parts of N' N-ethylene bis stearamide; adding 0.1-3 parts of white oil into a high-speed stirrer, and stirring at a high speed for 5-10 minutes, wherein the temperature of the materials is controlled within the range of 20-80 ℃; wherein the antioxidant is a compound of 1, 3, 5-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) 2, 4, 6-trimethylbenzene and N, N' -bis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propane ] hydrazine;
then extruding, drawing wire and air-cooling and granulating the mixture at the temperature of 200-238 ℃ by using a double-screw extruder;
extruding the granulated granules through a single screw at the temperature of 200-238 ℃ to form a sleeve;
then irradiating the material by an electron accelerator or a cobalt source with the irradiation dose of 10-20Mrad, and expanding the irradiated sleeve by 1-3 times by using expansion equipment at the temperature of 230-;
and finally, cooling and shaping to obtain the irradiation crosslinking high-temperature-resistant heat-shrinkable tubing capable of being processed at low temperature.
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| CN201811169214.6A CN109337188B (en) | 2018-10-08 | 2018-10-08 | Irradiation crosslinking high-temperature-resistant heat-shrinkable sleeve and production method thereof |
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| CN201811169214.6A CN109337188B (en) | 2018-10-08 | 2018-10-08 | Irradiation crosslinking high-temperature-resistant heat-shrinkable sleeve and production method thereof |
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| CN109337188B true CN109337188B (en) | 2022-02-15 |
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| CN112724503A (en) * | 2020-12-31 | 2021-04-30 | 深圳市沃尔核材股份有限公司 | Heat-shrinkable sleeve and manufacturing method thereof |
| US20240106221A1 (en) * | 2021-02-24 | 2024-03-28 | Sumitomo Electric Fine Polymer, Inc. | Heat shrinkable tube, heat shrinkable coupling component, method of manufacturing heat shrinkable tube, and method of manufacturing heat shrinkable coupling component |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104710794A (en) * | 2015-04-09 | 2015-06-17 | 深圳科创新源工业材料有限公司 | Automatic-curing insulation protective material and manufacturing technique thereof |
| CN106317598A (en) * | 2016-08-30 | 2017-01-11 | 上海电缆研究所 | Cross-linked fluoroplastic heat-shrinkable tube and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104710794A (en) * | 2015-04-09 | 2015-06-17 | 深圳科创新源工业材料有限公司 | Automatic-curing insulation protective material and manufacturing technique thereof |
| CN106317598A (en) * | 2016-08-30 | 2017-01-11 | 上海电缆研究所 | Cross-linked fluoroplastic heat-shrinkable tube and preparation method thereof |
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