CN114085482B - 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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- -1 3, 5-di-tert-butyl-4-hydroxyphenyl Chemical group 0.000 claims description 3
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- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
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- WPMYUUITDBHVQZ-UHFFFAOYSA-N 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoic acid Chemical compound CC(C)(C)C1=CC(CCC(O)=O)=CC(C(C)(C)C)=C1O WPMYUUITDBHVQZ-UHFFFAOYSA-N 0.000 description 1
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Classifications
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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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- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
- C08K5/134—Phenols containing ester groups
- C08K5/1345—Carboxylic esters of phenolcarboxylic acids
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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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention discloses an ultraviolet light crosslinking low-voltage ethylene propylene rubber insulating material and a preparation method thereof, and belongs to the technical field of preparation of electrical materials. The invention solves the problem of low crosslinking processing production efficiency of the low-voltage ethylene propylene rubber insulating material for the existing cable. The ultraviolet crosslinking low-voltage ethylene propylene rubber insulating material consists of ethylene propylene diene monomer rubber, nano silicon dioxide, an ultraviolet crosslinking initiator, a multifunctional group crosslinking agent and an antioxidant. The raw materials are uniformly mixed at the temperature of 100-120 ℃ and the rotating speed of 50-60r/min to obtain the ultraviolet crosslinking low-voltage ethylene propylene rubber insulating material, and the ultraviolet crosslinking low-voltage ethylene propylene rubber insulating material is obtained by irradiation crosslinking in a molten state.
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 has a high saturation structure, has the advantages of flexible molecular chains, good elasticity and the like, and is widely used for insulating medium-voltage cable by virtue of excellent insulativity, mechanical property, heat resistance and corrosion resistance. Ethylene propylene diene monomer rubber insulated cables are mostly used for power supply occasions such as ships, mines, underground, rolling stock and the like which often bear moving, rolling and torsion conditions. At present, the cable has been developed into a plurality of products such as medium-low voltage cables, marine cables, motor connecting wires and the like. Meanwhile, ethylene propylene diene monomer is also one of the commonly used insulating materials for cable accessories.
At present, the cross-linking method of 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 monomer rubber product prepared by the chemical crosslinking method has the defects of low production efficiency, complex process flow and high energy consumption, and the sulfur vulcanized ethylene propylene diene monomer rubber has safe operation process and good physical and mechanical properties, but is easy to generate a frosting phenomenon, and the ethylene propylene diene monomer rubber has low reaction activity, difficult sulfur vulcanization, large compression set and poor heat aging resistance; the peroxide vulcanized rubber has better heat stability and compression set resistance, but has poorer tear resistance, and when peroxide is used for crosslinking, the reaction temperature must be strictly controlled, otherwise, problems such as pre-crosslinking, excessive crosslinking and the like are easy to occur; silane crosslinking involves hydrolysis reaction, and the product has poor stability, voltage resistance and temperature resistance; high-energy radiation crosslinking equipment investment is high, operation and maintenance are complex, protection requirements are severe, and additional cost in the production process is high.
The ultraviolet crosslinking technology is used as a preparation technology of a newly developed wire and cable insulating material, and 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 to cause the photoinitiator to be excited to a triplet excited state, the photoinitiator in the triplet excited state takes hydrogen in high polymer molecules to form macromolecular free radicals, and the macromolecular free radicals are combined with each other to form a three-dimensional network structure. Compared with other crosslinking technologies, the ultraviolet crosslinking technology has the advantages of non-thermosensitive material, 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 ethylene propylene diene monomer containing a large amount of inorganic filler is difficult to cross-link by transmitting ultraviolet light, so that the ultraviolet light cross-linking technology is not applied to ethylene propylene diene monomer cable insulation manufacture at present, and the difficulty is how to realize the formulation design of the ethylene propylene diene monomer insulation material with low solid filler and high ultraviolet light cross-linking sensitivity at present.
Disclosure of Invention
The invention provides an ultraviolet crosslinking low-voltage ethylene propylene rubber insulating material and a preparation method thereof, which aim to solve the problems that the existing ethylene propylene rubber insulating material crosslinking process is low in production efficiency and high in energy consumption and cannot be suitable for an efficient ultraviolet crosslinking production process.
The technical scheme of the invention is as follows:
the ultraviolet cross-linking low-voltage ethylene propylene rubber insulating material uses ethylene propylene diene monomer rubber as base material, and nano silicon dioxide 3.8-4.2 parts, ultraviolet cross-linking initiator 1.8-2.2 parts, multifunctional cross-linking agent 0.8-1.2 parts and antioxidant 0.4-0.6 parts are added according to the total weight of 100 parts of the base material.
Further defined, the nanosilica is hydrophobic fumed nanosilica.
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 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 the ethylene propylene diene monomer is completely melted, continuously mixing for 8-12 min, adding an ultraviolet crosslinking initiator, a multifunctional crosslinking agent and an antioxidant, and continuously mixing for 3-5 min to obtain an ethylene propylene rubber insulating material;
step 2, processing and forming and ultraviolet crosslinking reaction: and (2) molding the ethylene propylene rubber insulating material obtained in the step (1) at the temperature of 100-120 ℃ by adopting a molding method or an extrusion molding method, maintaining the molten state of the molded product, and placing the molded product under an ultraviolet irradiation lamp for ultraviolet crosslinking to obtain the ultraviolet crosslinked low-voltage ethylene propylene rubber insulating material.
Further defined, the ultraviolet radiation lamp has a wavelength of 365nm.
Further limited, the ultraviolet irradiation time in the ultraviolet crosslinking process is 11-13 s.
The invention has the beneficial effects that:
(1) The invention adopts low-content nano silicon dioxide particles as the reinforcing agent of ethylene propylene diene monomer rubber to improve the mechanical properties of ethylene propylene rubber such as tensile strength, elongation at break and the like. In the process of processing and mixing the ethylene propylene rubber, physical adsorption and covalent bonding actions are generated between the nano silicon dioxide particles and the ethylene propylene rubber to form an interface bonding layer, and filler particles with high modulus are used as physical adsorption points and stress concentration areas, so that stress is redistributed, and the stress of materials around the nano particles is reduced, thereby effectively improving the tensile capacity and mechanical strength of the materials and improving the mechanical property of the ethylene propylene rubber.
(2) The addition amount of the nano silicon dioxide particles provided by the invention can ensure that the material has enough mechanical properties, can keep transparent, and ensures the transmittance of ultraviolet light, so 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 crosslinked low-voltage ethylene propylene rubber insulating material with better heat aging resistance, can pass a heat aging test at 135 ℃ for 168 hours, and can further enhance the mechanical property of the ultraviolet crosslinked low-voltage ethylene propylene rubber insulating material.
(4) The ultraviolet crosslinking low-voltage ethylene propylene rubber insulating material provided by the invention can obtain enough crosslinking degree in a shorter ultraviolet irradiation time, and the production efficiency of the low-voltage ethylene propylene rubber insulating cable is greatly improved.
Drawings
FIG. 1 is a graph showing the tensile strength contrast of an ultraviolet crosslinked low-voltage ethylene propylene rubber insulating material obtained at different irradiation times with the addition of different antioxidants;
FIG. 2 is a graph showing the comparison of elongation at break of UV crosslinked low pressure ethylene propylene rubber insulation obtained at different irradiation times with the addition of different antioxidants;
FIG. 3 is a graph showing the tensile strength comparison of the ultraviolet light crosslinked low-voltage ethylene propylene rubber insulating material before and after heat aging, wherein the ultraviolet light crosslinked low-voltage ethylene propylene rubber insulating material is obtained by adding different antioxidants and has irradiation time of 12 s;
FIG. 4 is a graph showing the comparison of elongation at break before and after heat aging of an ultraviolet light crosslinked low-voltage ethylene propylene rubber insulating material obtained by adding different antioxidants and irradiating for 12 s;
FIG. 5 is a photograph of a sample of an ultraviolet light crosslinked low pressure ethylene propylene rubber insulating material obtained by adding different antioxidants and irradiating for 12s after heat aging.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The experimental methods used in the following examples are conventional methods unless otherwise specified. The materials, reagents, methods and apparatus used, without any particular description, are those conventional in the art and are commercially available to those skilled in the art.
Example 1:
1. adding 40g of ethylene propylene diene monomer into an internal mixer, melting at 110 ℃, rotating at 60r/min, adding 1.6g of nano silicon dioxide after melting, mixing for 10min at the same temperature and rotating speed, adding 0.8g of benzophenone and 0.4g of triallyl isocyanurate, continuously mixing for 3min at the same temperature and rotating speed, adding 0.2g of antioxidant 1010, mixing for 3min at the same temperature and rotating speed, obtaining an ethylene propylene rubber insulating material, respectively placing the ethylene propylene rubber insulating material into moulds (0.1 mm and 1 mm) with different thickness specifications, performing hot press molding in a flat vulcanizing machine at 110 ℃ and 15MPa, rapidly taking out, irradiating for 12s under an ultraviolet LED lamp array, and obtaining the ultraviolet crosslinked low-voltage ethylene propylene rubber insulating material.
2. The ultraviolet crosslinking low-voltage ethylene propylene rubber insulating material obtained in the embodiment is subjected to performance test, and the test process and the result are as follows:
(1) The tensile strength and elongation at break were measured at a tensile rate of 250mm/min using dumbbell-shaped test specimens of 1mm thickness, respectively 18.55MPa and 642.05%.
(2) And (3) applying linearly-raised alternating-current high voltage to a round sample with the thickness of 0.1mm and the diameter of 80mm of the insulating material at normal temperature until the sample breaks down to respectively obtain alternating-current breakdown field strengths of 15 samples, and obtaining characteristic breakdown field strengths by adopting two-parameter Weibull distribution statistics, wherein the result is 89.19kV/mm.
(3) A dumbbell-shaped test specimen with a thickness of 1mm is adopted, the test is carried out under the stress of 0.2MPa, the test temperature is 200 ℃, the test result is expressed as the average value of 3 times of results, and the thermal elongation rate is 35%.
(4) A dumbbell specimen with a thickness of 1mm is adopted for heat aging test, the heat aging test temperature is 135 ℃, the aging time is 168 hours, the tensile strength and the elongation at break are tested after aging, the tensile rate is 250mm/min, and the results are 19.16MPa and 666.64 percent respectively.
Example 2:
this embodiment differs from embodiment 1 in that: the irradiation time under the ultraviolet LED lamp array is 4s without adding antioxidant, and the rest operation steps and parameter settings are the same as those of the embodiment 1.
Example 3:
this embodiment differs from embodiment 1 in that: the irradiation time under the ultraviolet LED lamp array was 8s without adding an antioxidant, and the rest of the operation steps and parameter settings were the same as in example 1.
Example 4:
this embodiment differs from embodiment 1 in that: the procedure and parameter settings were the same as in example 1, except that no antioxidant was added.
The ultraviolet light crosslinking low-voltage ethylene propylene rubber insulating materials obtained in examples 2 to 4 were subjected to mechanical property test and thermal elongation test (the specific process is the same as that of example 1), and the test results are shown in the following table.
The thermal elongation of the ethylene propylene rubber at different irradiation times is shown in the table. It can be seen that the thermal elongation decreases rapidly and the degree of crosslinking increases rapidly with increasing irradiation time. At an irradiation time of 4s, the ethylene propylene rubber failed the thermal extension test. When the irradiation time is 12s, the thermal elongation is 30%, which accords with the practical use standard, and the crosslinking time is greatly shortened compared with the traditional crosslinking mode. The tensile strength and elongation at break of the ethylene propylene rubber are rapidly reduced along with the increase of irradiation time, which indicates that the material is degraded under the irradiation of ultraviolet light.
Example 5:
this embodiment differs from embodiment 1 in that: 0.2g of antioxidant 300 was used in place of 0.2g of antioxidant 1010, and the rest of the procedure and parameters were the same as in example 1.
Example 6:
this embodiment differs from embodiment 1 in that: 0.12g of antioxidant 300 was used in place of 0.2g of antioxidant 1010, and the rest of the procedure and parameters were the same as in example 1.
Example 7:
this embodiment differs from embodiment 1 in that: 0.2g of antioxidant 1035 was used in place of 0.2g of antioxidant 1010, and the rest of the procedure and parameters were the same as in example 1.
Example 8:
this embodiment differs from embodiment 1 in that: 0.2g of antioxidant 4020 was used in place of 0.2g of antioxidant 1010, and the rest of the procedure and parameters were the same as in example 1.
Thermal extension test (the specific process is the same as that of example 1) is carried out on the ultraviolet crosslinking low-voltage ethylene propylene rubber insulating materials obtained in examples 1 and 5-8, and the test results are shown in the following table:
as shown in the above table, when the antioxidant is the antioxidant 4020, the insulation material is fused in the thermal extension test, and cannot pass the thermal extension test, because 4020 is black powdery solid, and after 4020 is added, the transparency of the ethylene propylene rubber is damaged, so that the crosslinking degree is reduced, and the requirement of photocrosslinking cannot be met, so 4020 is not suitable for being used as an anti-aging agent of the photocrosslinked ethylene propylene rubber material; in addition, at an antioxidant 300 addition level of 0.5phr, the material thermal elongation is as high as 110% and the material crosslinking degree is low.
Example 9:
this embodiment differs from embodiment 1 in that: 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:
this embodiment differs from embodiment 1 in that: 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:
this embodiment differs from embodiment 6 in that: 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:
this embodiment differs from embodiment 6 in that: 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:
this embodiment differs from embodiment 7 in that: 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 7.
Example 14:
this embodiment differs from embodiment 7 in that: 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.
Mechanical property tests (the specific process is the same as that of example 1) are carried out on the ultraviolet light crosslinking low-voltage ethylene propylene rubber insulating materials obtained in examples 1-4, 6 and 7 and examples 9-14, and the test results are shown in fig. 1 and 2, wherein fig. 1 is tensile strength comparison, and fig. 2 is elongation at break comparison. As can be seen from fig. 1 and fig. 2, the tensile strength of the three antioxidants is not significantly reduced at different irradiation times, which proves that the antioxidants can inhibit the degradation of the ethylene propylene rubber caused by the increase of the irradiation time to a certain extent, wherein the inhibition effect of the antioxidant 300 is better.
The ultraviolet light crosslinking low-voltage ethylene propylene rubber insulating materials obtained in examples 1, 4, 6 and 7 were subjected to thermal aging for 168 hours in a thermal aging oven at 135 ℃ to obtain the test results shown in fig. 3 and 4, wherein fig. 3 shows tensile strength comparison before and after aging, and fig. 4 shows elongation at break comparison before and after aging. As shown in figures 3 and 4, after aging, the mechanical properties of the antioxidant-added samples are slightly increased, while the ethylene propylene rubber insulating materials without the antioxidant cannot maintain the morphology after aging, and the mechanical properties are completely lost. After comparing the colors of samples of the ethylene propylene rubber insulating materials added with different types of antioxidants after aging, the ethylene propylene rubber samples added with the antioxidant 300 are found to be serious in yellowing, and the ethylene propylene rubber samples added with the antioxidants 1010 and 1035 are only slightly yellowing, as shown in fig. 5.
Example 15:
this embodiment differs from embodiment 1 in that: the mass of the added nano silica was 0.8g, and the rest of the operation steps and parameter settings were the same as in example 1.
Example 16:
this embodiment differs from embodiment 1 in that: the mass of the added nanosilica was 2.4g, and the rest of the procedure and parameter settings were the same as in example 1.
Example 17:
this embodiment differs from embodiment 1 in that: the procedure and parameter settings were the same as in example 1 without the addition of nanosilica.
The ultraviolet crosslinking 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:
compared with the prior art, the ultraviolet crosslinking low-voltage ethylene propylene rubber insulating material has the advantages that the performance of the ultraviolet crosslinking low-voltage ethylene propylene rubber insulating material is obviously improved, but the thermal elongation is slightly increased, because the ultraviolet shielding effect can be formed by adding the nano silicon dioxide into rubber, the ultraviolet irradiation absorption degree of the photoinitiator is weakened, the free radical generating 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. Example 1 has substantially unchanged ac breakdown strength compared to examples 15-17. With the increase of the content of the nano silicon dioxide, the mechanical property of the material is firstly increased and then decreased, wherein the mechanical property is optimal when the content of the silicon dioxide is 4 phr.
The above description is merely a preferred embodiment of the present invention, and since the person skilled in the art can make appropriate changes and modifications to the above-described embodiment, the present invention is not limited to the above-described embodiment, and some modifications and changes of the present invention should fall within the scope of the claims of the present invention.
Claims (5)
1. The ultraviolet light crosslinking low-voltage ethylene propylene rubber insulating material is characterized in that the insulating material takes ethylene propylene diene monomer rubber 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;
the ultraviolet crosslinking initiator is diphenyl ketone;
the multifunctional crosslinking agent is triallyl isocyanurate;
the antioxidant is pentaerythritol tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ].
2. The ultraviolet light crosslinking low-voltage ethylene propylene rubber insulating material according to claim 1, wherein the nano silicon dioxide is hydrophobic gas phase method nano silicon dioxide.
3. A method for preparing the ultraviolet light crosslinking low-voltage ethylene propylene rubber insulating material as claimed in claim 1, which is 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 the ethylene propylene diene monomer is completely melted, continuously mixing for 8-12 min, adding an ultraviolet crosslinking initiator, a multifunctional crosslinking agent and an antioxidant, and continuously mixing for 3-5 min to obtain an ethylene propylene rubber 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) at the temperature of 100-120 ℃ by adopting a molding method or an extrusion molding method, maintaining the molten state of the molded product, and placing the molded product under an ultraviolet irradiation lamp for ultraviolet crosslinking to obtain the ultraviolet crosslinked low-voltage ethylene propylene rubber insulating material.
4. The method for preparing the ultraviolet crosslinking low-voltage ethylene propylene rubber insulating material according to claim 3, wherein the wavelength of the ultraviolet irradiation lamp is 365nm.
5. The method for preparing the ultraviolet light crosslinking low-voltage ethylene propylene rubber insulating material according to claim 3, wherein the ultraviolet light irradiation time in the ultraviolet light crosslinking process is 11-13 s.
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