CN114085482A - Ultraviolet light crosslinked low-voltage ethylene propylene rubber insulating material and preparation method thereof - Google Patents
Ultraviolet light crosslinked low-voltage ethylene propylene rubber insulating material and preparation method thereof Download PDFInfo
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
- C08K5/134—Phenols containing ester groups
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention discloses an ultraviolet light cross-linking low-voltage ethylene propylene rubber insulating material and a preparation method thereof, belonging to the technical field of preparation of electrical materials. The invention solves the problem of low cross-linking processing production efficiency of the existing low-voltage ethylene propylene rubber insulating material for the cable. The ultraviolet light crosslinking low-voltage ethylene propylene rubber insulating material consists of ethylene propylene diene monomer, nano silicon dioxide, an ultraviolet light crosslinking initiator, a polyfunctional group crosslinking agent and an antioxidant. The raw materials are uniformly mixed at the temperature of 100-.
Description
Technical Field
The invention relates to an ultraviolet light crosslinking low-voltage ethylene propylene rubber insulating material and a preparation method thereof, belonging to the technical field of preparation of electrical materials.
Background
The ethylene propylene diene monomer rubber has a highly saturated structure, has the advantages of smooth molecular chains, good elasticity and the like, and is widely used as the insulation of medium and low voltage wires and cables due to excellent insulating property, mechanical property, heat resistance and corrosion resistance. The ethylene propylene diene monomer insulated cable is mostly used in power supply occasions which often bear moving, rolling and twisting conditions, such as ships, mines, underground and rolling stock. The cable is developed into a plurality of categories such as medium and low voltage cables, marine cables, motor connecting leads and the like. Meanwhile, ethylene propylene diene monomer is also one of common insulating materials for cable accessories.
At present, the crosslinking method of the ethylene propylene diene monomer mainly comprises the following steps: chemical crosslinking (sulfur, peroxide cure systems), silane crosslinking, and high energy radiation (electron beam radiation). The ethylene propylene diene rubber product prepared by the chemical crosslinking method has the defects of low production efficiency, complex process flow and high energy consumption, the sulfur-vulcanized ethylene propylene diene rubber has safe operation process and good physical and mechanical properties, but is easy to generate blooming phenomenon, and the ethylene propylene diene rubber has low reaction activity, difficult sulfur vulcanization, large compression permanent deformation and poor heat and aging resistance; peroxide vulcanized rubber has better thermal stability and compression permanent deformation resistance, but has poor tear resistance, and when peroxide is used for crosslinking, the reaction temperature must be strictly controlled, otherwise, the problems of pre-crosslinking, excessive crosslinking and the like are easy to occur; silane crosslinking relates to hydrolysis reaction, and the product has poor stability, voltage resistance and temperature resistance; the high-energy radiation crosslinking equipment has high investment, complex operation and maintenance, strict protection requirements and high additional cost in the production process.
As a newly developed preparation process of an electric wire and cable insulating material, an ultraviolet crosslinking technology is successfully applied to the production of low-voltage XLPE insulated power cables below 10kV and low-smoke halogen-free flame-retardant cable insulating layers. The principle is that ultraviolet light is used for irradiating a high polymer material containing a photoinitiator, the energy of the ultraviolet light is absorbed by the photoinitiator, so that the photoinitiator is excited to a triplet excited state, the photoinitiator in the triplet excited state can capture hydrogen in high polymer molecules to form macromolecular free radicals, and the macromolecular free radicals are mutually combined to form a three-dimensional network structure. Compared with other crosslinking technologies, the ultraviolet crosslinking technology has the advantages of non-thermal sensitivity of materials, simple process, less investment, easy operation, low safety protection requirement, convenient maintenance, high energy utilization rate, small environmental pollution and the like. However, the ethylene propylene diene monomer used as cable insulation generally needs to be added with 50-60 wt% of reinforcing inorganic filler, and the ethylene propylene diene monomer containing a large amount of inorganic filler is difficult to transmit ultraviolet light to generate crosslinking, so that the ultraviolet light crosslinking technology is not applied to the insulation manufacturing of the ethylene propylene diene monomer cable at present, and the difficulty lies in how to realize the formula design of the ethylene propylene diene monomer insulation material with low solid filler and high ultraviolet light crosslinking sensitivity.
Disclosure of Invention
The invention provides an ultraviolet crosslinking low-voltage ethylene propylene rubber insulating material and a preparation method thereof, aiming at solving the problems that the existing ethylene propylene rubber insulating material crosslinking process is low in production efficiency, high in energy consumption and incapable of being applied to an efficient ultraviolet crosslinking production process.
The technical scheme of the invention is as follows:
the ultraviolet light crosslinking low-voltage ethylene propylene rubber insulating material takes ethylene propylene diene monomer as a base material, and 3.8-4.2 parts of nano silicon dioxide, 1.8-2.2 parts of ultraviolet light crosslinking initiator, 0.8-1.2 parts of polyfunctional group crosslinking agent and 0.4-0.6 part of antioxidant are added according to 100 parts of the total weight of the base material.
Further limited, the nano-silica is hydrophobic gas phase nano-silica.
Further defined, the ultraviolet crosslinking initiator is benzophenone.
Further defined, the polyfunctional crosslinking agent is triallyl isocyanurate.
Further defined, the antioxidant is pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ].
The preparation method of the ultraviolet light crosslinking low-voltage ethylene propylene rubber insulating material comprises the following steps:
step 2, processing and forming and ultraviolet crosslinking reaction: and (3) molding the ethylene propylene rubber insulating material obtained in the step (1) by adopting a molding method or an extrusion molding method at the temperature of 100-120 ℃, maintaining the molten state of the molded product, placing the molded product under an ultraviolet radiation lamp, and performing ultraviolet crosslinking to obtain the ultraviolet crosslinking low-voltage ethylene propylene rubber insulating material.
Further defined, the ultraviolet radiation lamp has a wavelength of 365 nm.
Further limiting the ultraviolet irradiation time in the ultraviolet crosslinking process to be 11-13 s.
The invention has the beneficial effects that:
(1) the invention adopts low-content nano silicon dioxide particles as a reinforcing agent of the ethylene propylene diene monomer to improve the mechanical properties of the ethylene propylene rubber, such as tensile strength, elongation at break and the like. In the process of processing and mixing ethylene propylene rubber, the nano silicon dioxide particles and the ethylene propylene rubber are subjected to physical adsorption and covalent binding to form an interface binding layer, the high-modulus filler particles are used as physical adsorption points and stress concentration areas to redistribute stress, more molecular chains share the applied load uniformly, and the stress of the material around the nano particles is reduced, so that the tensile strength and the mechanical strength of the material can be effectively improved, and the mechanical property of the ethylene propylene rubber is improved.
(2) The addition amount of the nano silicon dioxide particles provided by the invention can ensure that the material has enough mechanical property, simultaneously can keep the material transparent, ensures the transmittance of ultraviolet light, and ensures that the material has enough crosslinking degree, thereby being suitable for an ultraviolet light crosslinking process and reducing the energy consumption and the production cost in the production process.
(3) The invention adopts tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester as an antioxidant, can endow the ultraviolet light crosslinked low-voltage ethylene propylene rubber insulating material with better heat-resistant aging performance, can pass a heat aging test at 135 ℃ for 168h, and can further enhance the mechanical property of the ultraviolet light crosslinked low-voltage ethylene propylene rubber insulating material.
(4) The ultraviolet light crosslinking low-voltage ethylene propylene rubber insulating material provided by the invention can obtain enough crosslinking degree in a short ultraviolet irradiation time, and the production efficiency of the low-voltage ethylene propylene rubber insulating cable is greatly improved.
Drawings
FIG. 1 is a comparison curve of tensile strength of ultraviolet light crosslinked low-voltage ethylene propylene rubber insulation materials obtained under different irradiation times by adding different antioxidants;
FIG. 2 is a comparison curve of the elongation at break of the ultraviolet light crosslinked low-voltage ethylene propylene rubber insulation material obtained under different irradiation times with different antioxidants added;
FIG. 3 is a comparison curve of tensile strength of the ultraviolet light crosslinked low-voltage ethylene propylene rubber insulation material before and after thermal aging, which is obtained by adding different antioxidants and with the irradiation time of 12 s;
FIG. 4 is a comparison curve of elongation at break before and after thermal aging of the ultraviolet light crosslinked low-voltage ethylene propylene rubber insulation material obtained by adding different antioxidants and with the irradiation time of 12 s;
FIG. 5 is a photo of a sample obtained after ultraviolet light crosslinked low-voltage ethylene propylene rubber insulation material is thermally aged and added with different antioxidants and the irradiation time is 12 s.
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 experimental procedures used in the following examples are conventional unless otherwise specified. The materials, reagents, methods and apparatus used, unless otherwise specified, are conventional in the art and are commercially available to those skilled in the art.
Example 1:
firstly, 40g of ethylene propylene diene monomer is added into an internal mixer, melting is carried out at 110 ℃, the rotating speed is 60r/min, 1.6g of nano silicon dioxide is added after melting, mixing is carried out for 10min at the same temperature and rotating speed, then 0.8g of benzophenone and 0.4g of triallyl isocyanurate are added, mixing is carried out for 3min at the same temperature and rotating speed, finally 0.2g of antioxidant 1010 is added, mixing is carried out for 3min at the same temperature and rotating speed, ethylene propylene rubber insulating materials are obtained, the ethylene propylene rubber insulating materials are respectively put into moulds (0.1mm and 1mm) with different thickness specifications and hot-pressed in a flat plate vulcanizing machine with 110 ℃ and 15MPa, then the ethylene propylene diene monomer insulating materials are rapidly taken out and put under an ultraviolet LED lamp array to irradiate for 12s, and after cross-linking is completed, the ultraviolet light cross-linked low-pressure ethylene propylene rubber insulating material is obtained.
Secondly, the performance of the ultraviolet light crosslinking low-voltage ethylene propylene rubber insulating material obtained in the embodiment is tested, and the test process and the test result are as follows:
(1) tensile strength and elongation at break were measured at a tensile rate of 250mm/min using a 1mm thick dumbbell specimen and were 18.55MPa and 642.05%, respectively.
(2) The circular sample with the thickness of 0.1mm and the diameter of 80mm of the insulating material is applied with linearly increased alternating-current high voltage at normal temperature until the sample breaks down, alternating-current breakdown field strengths of 15 samples are respectively obtained, and characteristic breakdown field strength is obtained by adopting two-parameter Weibull distribution statistics, and the result is 89.19 kV/mm.
(3) A dumbbell-shaped test specimen with the thickness of 1mm is used for testing under the stress of 0.2MPa, the test temperature is 200 ℃, the test result is expressed by the average value of 3 times of results, and the thermal elongation is 35%.
(4) A dumbbell-shaped test sample with the thickness of 1mm is adopted to carry out a heat aging test, the heat aging test temperature is 135 ℃, the aging time is 168 hours, the test of tensile strength and elongation at break is carried out after aging, the tensile rate is 250mm/min, and the results are respectively 19.16MPa and 666.64%.
Example 2:
the difference between this example and example 1 is: the irradiation time under the ultraviolet LED lamp array was 4s without adding antioxidant, and the rest of the operation steps and parameter settings were the same as in example 1.
Example 3:
the difference between this example and example 1 is: the irradiation time under the ultraviolet LED lamp array was 8s without adding antioxidant, and the rest of the operation steps and parameter settings were the same as in example 1.
Example 4:
the difference between this example and example 1 is: the rest of the operation steps and parameter settings were the same as in example 1 without adding antioxidant.
The uv-crosslinked low-voltage ethylene-propylene rubber insulation materials obtained in examples 2 to 4 were subjected to mechanical property test and thermal elongation test (the specific procedure was the same as in example 1), and the test results are shown in the following table.
The thermal elongation of the ethylene-propylene rubber under different irradiation times is shown in the table. It can be seen that, with the increase of the irradiation time, the thermal elongation rate is rapidly reduced, and the crosslinking degree is rapidly improved. When the irradiation time is 4s, the ethylene propylene rubber cannot pass the thermal elongation test. When the irradiation time is 12s, the thermal elongation is further 30%, the practical use standard is met, and the crosslinking time is greatly shortened compared with the conventional crosslinking mode. The tensile strength and the elongation at break of the ethylene propylene rubber are rapidly reduced along with the increase of the irradiation time, which indicates that the material is degraded under the irradiation of ultraviolet light.
Example 5:
the present embodiment differs from embodiment 1 in that: 0.2g of antioxidant 300 was used instead of 0.2g of antioxidant 1010, and the rest of the operation steps and parameter settings were the same as in example 1.
Example 6:
the difference between this example and example 1 is: 0.12g of antioxidant 300 was used instead of 0.2g of antioxidant 1010, and the rest of the operation steps and parameter settings were the same as in example 1.
Example 7:
the difference between this example and example 1 is: the same procedure and parameter settings as in example 1 were followed except that 0.2g of antioxidant 1035 was used instead of 0.2g of antioxidant 1010.
Example 8:
the difference between this example and example 1 is: 0.2g of antioxidant 4020 was used in place of 0.2g of antioxidant 1010, and the rest of the operation steps and parameter settings were the same as in example 1.
The ultraviolet light cross-linking low-voltage ethylene propylene rubber insulating materials obtained in examples 1, 5 to 8 were subjected to a thermal extension test (the specific process is the same as that of example 1), and the test results are shown in the following table:
as can be seen from the above table, when the antioxidant is antioxidant 4020, the insulating material is fused in the thermal extension test, and cannot pass the thermal extension test, because 4020 is a black powdery solid, and the transparency of ethylene propylene rubber is damaged after adding 4020, which causes a decrease in the degree of crosslinking, and cannot meet the requirement of photocrosslinking, so 4020 is not suitable for being used as an anti-aging agent for photocrosslinked ethylene propylene rubber material; in addition, when the addition amount of the antioxidant 300 is 0.5phr, the thermal elongation of the material is as high as 110%, and the degree of crosslinking of the material is low.
Example 9:
the difference between this example and example 1 is: the irradiation time under the ultraviolet LED lamp array was 4s, and the rest of the operation steps and parameter settings were the same as in example 1.
Example 10:
the difference between this example and example 1 is: the irradiation time under the ultraviolet LED lamp array was 8s, and the rest of the operation steps and parameter settings were the same as in example 1.
Example 11:
the difference between this example and example 6 is: the irradiation time under the ultraviolet LED lamp array was 4s, and the rest of the operation steps and parameter settings were the same as in example 6.
Example 12:
the difference between this example and example 6 is: the irradiation time under the ultraviolet LED lamp array was 8s, and the rest of the operation steps and parameter settings were the same as in example 6.
Example 13:
the difference between this example and example 7 is: the exposure time under the uv LED lamp array was 4s and the rest of the operating steps and parameter settings were the same as in example 7.
Example 14:
the difference between this example and example 7 is: the irradiation time under the ultraviolet LED lamp array was 8s, and the rest of the operation steps and parameter settings were the same as in example 7.
The uv crosslinked low pressure ethylene propylene rubber insulation materials obtained in examples 1-4, 6, 7 and examples 9-14 were subjected to mechanical property test (the specific procedure is the same as in example 1), and the test results are shown in fig. 1 and fig. 2, wherein fig. 1 is a tensile strength comparison, and fig. 2 is an elongation at break comparison. As can be seen from FIGS. 1 and 2, the tensile strength of the three antioxidants does not decrease significantly under different irradiation times, which proves that the antioxidants can inhibit the degradation problem of ethylene propylene rubber caused by the increase of the irradiation time to a certain extent, wherein the antioxidant 300 has a better inhibition effect.
The uv crosslinked low pressure ethylene propylene rubber insulation materials obtained in examples 1, 4, 6 and 7 were subjected to mechanical property test before and after thermal aging, wherein the aging process was carried out for 168 hours in a thermal aging chamber at 135 ℃, and the test results are shown in fig. 3 and 4, wherein fig. 3 is a comparison of tensile strength before and after aging, and fig. 4 is a comparison of elongation at break before and after aging. As shown in fig. 3 and fig. 4, after aging, the mechanical properties of the antioxidant-added sample are slightly increased, while the ethylene propylene rubber insulating material without the antioxidant cannot maintain its form after aging, and completely loses the mechanical properties. After comparing the color of the samples after aging of the ethylene-propylene rubber insulating material added with different types of antioxidants, the ethylene-propylene rubber sample added with the antioxidant 300 is found to be yellow seriously, and the ethylene-propylene rubber samples added with the antioxidants 1010 and 1035 are only slightly yellow, as shown in fig. 5.
Example 15:
the difference between this example and example 1 is: the amount of nanosilica added was 0.8g, and the remaining operation and parameter settings were the same as in example 1.
Example 16:
the difference between this example and example 1 is: the amount of nanosilica added was 2.4g, and the remaining operation and parameter settings were the same as in example 1.
Example 17:
the difference between this example and example 1 is: the rest of the operation steps and parameter settings were the same as in example 1 without adding nano silica.
The ultraviolet light crosslinked low-voltage ethylene propylene rubber insulating materials obtained in examples 1 and 15 to 17 were subjected to mechanical property test, thermal elongation test and alternating current breakdown strength test (the specific process is the same as in example 1), and the test results are as follows:
the comparison shows that the performance of the ultraviolet crosslinking low-pressure ethylene propylene rubber insulating material is obviously improved due to the addition of the nano silicon dioxide, but the thermal elongation is slightly increased, because the nano silicon dioxide is added into the rubber, the ultraviolet shielding effect can be formed, the ultraviolet radiation absorption degree of the photoinitiator is weakened, the free radical generation efficiency of the photoinitiator is reduced, and the crosslinking degree of the ethylene propylene rubber is slightly reduced. Because the addition amount of the silicon dioxide is low, the influence on the crosslinking degree is small, and the crosslinking degree can still meet the use requirement. The ac breakdown strength of example 1 was substantially unchanged from examples 15-17. The mechanical property of the material is firstly increased and then decreased along with the increase of the content of the nano silicon dioxide, wherein the mechanical property is optimal when the content of the silicon dioxide is 4 phr.
The above embodiments are merely preferred embodiments of the present invention, and the present invention is not limited to the above embodiments, and modifications and changes thereof may be made by those skilled in the art within the scope of the claims of the present invention.
Claims (8)
1. The ultraviolet light crosslinking low-voltage ethylene propylene rubber insulating material is characterized in that ethylene propylene diene monomer is used as a base material, and 3.8-4.2 parts of nano silicon dioxide, 1.8-2.2 parts of ultraviolet light crosslinking initiator, 0.8-1.2 parts of polyfunctional group crosslinking agent and 0.4-0.6 part of antioxidant are added according to 100 parts of the total weight of the base material.
2. The ultraviolet crosslinked low-voltage ethylene propylene rubber insulating material as claimed in claim 1, wherein the nano silica is hydrophobic vapor-phase nano silica.
3. The UV-crosslinked low-voltage EPDM material as claimed in claim 1, wherein said UV-crosslinking initiator is benzophenone.
4. The UV-crosslinked EPR rubber insulation material according to claim 1, wherein said polyfunctional crosslinking agent is triallyl isocyanurate.
5. The UV-crosslinked low-voltage EPDM rubber insulating material according to claim 1, wherein said antioxidant is pentaerythritol tetrakis [ β - (3, 5-di-t-butyl-4-hydroxyphenyl) propionate ].
6. The preparation method of the ultraviolet light crosslinking low-voltage ethylene propylene rubber insulating material as claimed in claim 1, characterized by comprising the following steps:
step 1, melt blending: adding ethylene propylene diene monomer particles into an internal mixer, setting the mixing temperature to be 100-120 ℃, adding nano silicon dioxide after ethylene propylene diene monomer is completely melted, continuing mixing for 8-12 min, adding an ultraviolet light crosslinking initiator, a polyfunctional group crosslinking agent and an antioxidant, and continuing mixing for 3-5 min to obtain an ethylene propylene monomer insulating material;
step 2, processing and forming and ultraviolet crosslinking reaction: and (3) molding the ethylene propylene rubber insulating material obtained in the step (1) by adopting a molding method or an extrusion molding method at the temperature of 100-120 ℃, maintaining the molten state of the molded product, placing the molded product under an ultraviolet radiation lamp, and performing ultraviolet crosslinking to obtain the ultraviolet crosslinking low-voltage ethylene propylene rubber insulating material.
7. The method for preparing the ultraviolet crosslinking low-voltage ethylene propylene rubber insulating material as claimed in claim 1, wherein the wavelength of the ultraviolet radiation lamp is 365 nm.
8. The preparation method of the ultraviolet crosslinking low-voltage ethylene propylene rubber insulating material according to claim 1, wherein the ultraviolet irradiation time in the ultraviolet crosslinking process is 11-13 s.
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