CN113185761B - Preparation method of cable insulating material with self-repairing function - Google Patents
Preparation method of cable insulating material with self-repairing function Download PDFInfo
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Abstract
The invention discloses a preparation method of a cable insulating material with a self-repairing function, which belongs to the technical field of cable materials and comprises the following steps: s1: preparation of microcapsules: (1) Mixing urea, formaldehyde, melamine and water to obtain a prepolymer; (2) Mixing phenolic resin, dicyclopentadiene, sodium dodecyl benzene sulfonate and water to form a core material; (3) mixing the prepolymer with the core material; s2: preparation of insulating material: (a) vacuum drying the filler; (b) Mixing ethanol with epoxy resin, and adding methyl acrylate, styrene, acrylic acid, organic silicone oil and azodiisobutyronitrile to obtain modified resin; (c) Mixing filler, modified resin, chlorinated rubber, microcapsule, flame retardant, coupling agent and polyethylene glycol, and extrusion molding. The invention has excellent compression resistance, tensile property, insulation, flame retardant property and the like, reduces the damage degree of the insulating material, can timely rupture and repair the microcapsule, and prolongs the service life of the insulating material.
Description
Technical Field
The invention relates to the technical field of cable materials, in particular to a preparation method of a cable insulating material with a self-repairing function.
Background
With the development of national economy, the life quality of people is improved, the power cable needs to adapt to different use environments and occasions, and has the requirements of tear resistance, high and low temperature resistance, weather resistance, oil resistance, solvent resistance, fire resistance and the like, and the cable insulating material also needs to have high technical requirements. The insulating materials commonly used at present are mainly classified into solid insulating materials and liquid insulating materials. For example, low-density polyethylene is a solid insulating material, which has low cost, excellent electrical properties, low relative dielectric constant, low loss factor, high resistivity, excellent mechanical properties at an ambient temperature of 90 ℃ or below, and is used in a large amount in medium-low voltage cable insulating polymers. With the development of power cables in China to high-voltage, large-capacity and long-distance transmission, special purposes and the like, more and more requirements are put on the quality and reliability of insulating materials.
The patent document with the publication number of CN112430390A discloses an electric wire insulation sheath material with a self-repairing function and a preparation method thereof, specifically, polydimethylsiloxane is added into a solvent, polyisocyanate is added after stirring and heating, polyurethane prepolymer is obtained through heating reaction, polyvinyl chloride and chlorinated rubber are added, and the reaction is continued for 3-5 hours; and sequentially adding a chain extender containing disulfide bonds, heating to 100-120 ℃ for reacting for 5-8 hours, finally adding active calcium carbonate, talcum powder, aluminum oxide and flame retardant, and stirring for 3-5 hours at the temperature of 100-120 ℃ to obtain the wire insulation sheath material.
Patent document publication No. CN111154234A discloses a method for preparing a medium-high temperature self-repairing insulating material. Step 1: uniformly mixing epoxy resin and epoxy resin reactive diluent according to a proportion to prepare repair liquid; step 2: preparing an aqueous solution containing sodium dodecyl benzene sulfonate and polyvinyl alcohol, slowly adding the repairing liquid into the aqueous solution, and stirring to form uniformly dispersed oil-in-water core emulsion; step 3: preparing urea and formaldehyde into a solution according to a certain proportion, stirring to form a prepolymer solution of water-soluble monomethylol urea and dimethylol urea, adding a proper amount of deionized water into the prepolymer, cooling to room temperature, and adding dilute hydrochloric acid to adjust the pH value to 7; step 4: adding the prepolymer solution into the oil-in-water core emulsion, adding a catalyst and a pH value regulator, regulating the pH value of the solution to 3-4, heating to 50-60 ℃ for reaction for 3-5 hours, removing unreacted core materials and wall materials, cooling, washing, sieving, and naturally drying to obtain microcapsules; step 5: mixing epoxy resin and 2-ethyl-4-methylimidazole in proportion, adding a normal temperature curing agent of the epoxy resin and the microcapsules, uniformly mixing, vacuum degassing, and pouring into a mold for curing to obtain the self-repairing epoxy resin insulating material with the self-repairing capability of electric damage.
The two insulating materials and the preparation method can perform a self-repairing function, but the repairing function needs to be improved, the flame retardance is poor, and the technical requirements cannot be met.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing a cable insulation material with a self-repairing function.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a cable insulation material with a self-repairing function comprises the following steps:
s1: preparation of microcapsules:
(1) Mixing urea, formaldehyde, melamine and water, and stirring in a water bath to obtain a prepolymer;
(2) Mixing phenolic resin, dicyclopentadiene, sodium dodecyl benzene sulfonate and water, and stirring in a water bath to form a core material;
(3) Mixing and stirring the prepolymer and the core material to form microcapsules, and filtering;
s2: preparation of insulating material:
(a) Vacuum drying the filler;
(b) Mixing ethanol and epoxy resin, adding methyl acrylate, styrene, acrylic acid, organic silicone oil and azodiisobutyronitrile, heating in water bath, and stirring to obtain modified resin;
(c) Placing the dried filler obtained in the step (a), the modified resin obtained in the step (b), the chlorinated rubber, the microcapsule obtained in the step S1, the flame retardant, the coupling agent and the polyethylene glycol into an internal mixer for banburying, and then extruding and forming.
Further, in the prepolymer, the mass ratio of each component is as follows: urea: formaldehyde: melamine: the water is 4-5:8-10:1:50-55.
Further, in the step S1, the mass of dicyclopentadiene is 4 to 5 times that of urea.
Further, in the core material, the mass ratio of each component is as follows: phenolic resin: dicyclopentadiene: sodium dodecyl benzene sulfonate: water is 7-10:10-12:0.1:80-90.
Further, in the step (1), the water bath temperature is 70-75 ℃, the stirring time is 45-60min, and the stirring speed is 500-600r/min; in the step (2), the water bath temperature is 40-45 ℃, the stirring time is 20-30min, and the stirring speed is 800-1000r/min; in the step (3), the stirring time is 60-90min, and the stirring speed is 400-500r/min.
Further, in the step (b), the mass ratio of the components is as follows: ethanol: epoxy resin: methyl acrylate: styrene: acrylic acid: organic silicone oil: azobisisobutyronitrile is 40-50:12-15:14-18:25-30:5-8:3-5:1-3.
Further, in the step (c), the mass ratio of the components is as follows: the dried filler obtained in step (a): the modified resin obtained in the step (b): chlorinated rubber: microcapsules obtained in step S1: flame retardant: coupling agent: polyethylene glycol is 2-3:12-15:28-32:16-20:3-5:0.5-0.8:10-13.
Further, the filler is one or more of nano aluminum oxide, ferrocene and mica powder.
Further, the flame retardant is magnesium hydroxide or ammonium dihydrogen phosphate.
Further, the coupling agent is silane coupling agent KH-560 or KH-570.
Further, in the step (a), the drying time is 2-3 hours, and the temperature is 90-95 ℃.
Further, the filler is a mixture of nano aluminum oxide, ferrocene and mica powder, and the weight ratio of the nano aluminum oxide to the ferrocene is as follows: ferrocene: mica powder is 1:0.2-0.5:2-3.
The cable insulating material is generally used for insulating and protecting the outer layer of the cable, is directly contacted with the external environment, and can be damaged due to aging, external force damage and the like in the transportation and use processesLeakage and power failure accidents. At present, the repair method for the damage of the cable insulating layer mainly comprises a repair liquid filling repair method, a thermal welding repair method and a thermal shrinkage pipe repair method, but the 3 repair methods have the defects of complex process and poor repair effect, and a fault location technology is also required to find a fault point, so that the repair difficulty is easily increased due to the influence of the detection distance, the wound degree and the like, and therefore, the development of a new technology for repairing the damage of the cable insulating layer is needed. The self-repairing material is an intelligent material with the function of automatically identifying the damage or the structural defect and repairing the damage or the structural defect partially or completely. At present, filled self-repairing materials are commonly used, and the purpose of repairing cracks is achieved mainly through dispersing carriers (such as hollow fibers, microcapsules, micro-vessels and the like) of the repairing agents in a polymer matrix, when the materials are broken, the carriers are broken along with the breakage, the repairing agents in the carriers are released, and the repairing agents diffuse to the cracks and react and crosslink. E.g. Peng Ge, zhang Yanfang, li Yudong, effect of microcapsules on insulation properties of polyethylene material [ J]Insulating material, 2021,54 (2): 80-86, discloses the preparation of pure polyethylene samples and polyethylene composite samples doped with microcapsules of different concentrations (0, 0.5%, 1%, 5%, 10%). Wood pine, peng Lei, fuqiang, qian Yihua, chen Tiansheng, zhang, ma Xiaoqian, preparation and performance of self-repairing insulating material based on host and guest inclusion [ J ]]The university chemistry report, 2018, 11:2572-2580 discloses the preparation of an electrically insulating sheath material capable of self-repair, based on the interaction between host-guest molecules, with beta-cyclodextrin-Al 2 O 3 Nanoparticle (NPs) are taken as a main body, 2-hydroxyethyl-methacrylate and adamantane are taken as objects, the main objects and the objects are mutually identified for assembly, then the assembly is subjected to free radical copolymerization with HEMA, butyl Acrylate (BA) and polyvinylpyrrolidone (PVP), and a novel PVP/p (HEMA-co-BA) self-repairing material is obtained, and self-repairing is realized through the intermolecular interaction force of the polymer. The materials can have certain self-repairing capability, but are used for cable insulation protection, and the insulation performance and mechanical performance of the materials cannot meet the technical requirements. Conventional research by those skilled in the art is to improve the mechanical properties of the microcapsules, but this results in less susceptibility of the microcapsules to breakageAnd the material cannot be repaired in time due to cracking. Therefore, the inventor of the application has long-term research on compounding the microcapsule with the modified resin and other components, so that the insulating material has excellent compression resistance, tensile property, insulating property, flame retardant property and the like, the damage degree of the insulating material is reduced, and meanwhile, the microcapsule can be broken and repaired in time, the service life of the insulating material is prolonged, and the safe operation of a circuit is ensured.
The beneficial effects of the invention are as follows:
the invention adopts urea, formaldehyde and melamine as wall materials, uses phenolic resin and dicyclopentadiene as core materials and uses sodium dodecyl benzene sulfonate as an emulsifier to prepare the microcapsule, has enough strength, can keep intact when the cable is subjected to external force, and can not crack, when the cable is subjected to tiny damages such as cracks, the microcapsule can crack in time, releases a healing agent, prevents crack expansion, plays a certain repairing role, and prolongs the service life of the material.
Mixing ethanol and epoxy resin, adding methyl acrylate, styrene, acrylic acid, organic silicone oil and azodiisobutyronitrile, heating in water bath, and stirring to obtain modified resin; the modified resin obtained by modifying the epoxy resin and the organic silicone oil has the characteristics of excellent adhesiveness, electrical insulation and stability.
Mixing and banburying the modified resin with filler, chlorinated rubber, microcapsule, flame retardant, coupling agent and polyethylene glycol, and extruding to obtain the granule of the insulating material. The filler nano alumina, ferrocene and mica powder improve the mechanical strength and corrosion resistance of the insulating material. The flame retardant magnesium hydroxide or monoammonium phosphate can enhance the flame retardant property of the material and has better flame retardant effect.
The self-repairing insulating material prepared by the microcapsule self-repairing system can repair the damage at the initial stage of the damage, and well solves the problems of micropores, microcracks and the like of the cable insulating layer. The insulating material with excellent comprehensive performance is obtained by compounding the modified resin with filler, chlorinated rubber, microcapsule, flame retardant, coupling agent, polyethylene glycol and the like. Volume resistivity of 9-9.8X10 16 And has excellent electrical insulation performance, wherein the dielectric constant is 1.6-1.8, the dielectric strength is 83-89 kV/mm; the tensile strength is 38.6-39.8Mpa, the elongation is 655-679%, and the oxygen index is 41-43.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention are clearly and completely described below. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which are obtained by a person skilled in the art based on the described embodiments of the invention, fall within the scope of protection of the invention.
Example 1
The embodiment provides a preparation method of a cable insulation material with a self-repairing function, which comprises the following steps:
s1: preparation of microcapsules:
(1) Mixing urea, formaldehyde, melamine and water, and stirring in a water bath to obtain a prepolymer; the mass ratio of each component is as follows: urea: formaldehyde: melamine: water is 4:8:1:50; the water bath temperature is 70 ℃, the stirring time is 60min, and the stirring speed is 500r/min;
(2) Mixing phenolic resin, dicyclopentadiene, sodium dodecyl benzene sulfonate and water, and stirring in a water bath to form a core material; the mass of dicyclopentadiene is 4 times of that of urea; the mass ratio of each component is as follows: phenolic resin: dicyclopentadiene: sodium dodecyl benzene sulfonate: the water is 7:10:0.1:80; the water bath temperature is 40 ℃, the stirring time is 20min, and the stirring speed is 1000r/min;
(3) Mixing and stirring the prepolymer and the core material to form microcapsules, and filtering; stirring time is 60min, and stirring speed is 500r/min;
s2: preparation of insulating material:
(a) Vacuum drying the filler for 3 hours at 90 ℃;
(b) Mixing ethanol and epoxy resin, adding methyl acrylate, styrene, acrylic acid, organic silicone oil and azodiisobutyronitrile, heating in water bath, and stirring to obtain modified resin; the mass ratio of each component is as follows: ethanol: epoxy resin: methyl acrylate: styrene: acrylic acid: organic silicone oil: azobisisobutyronitrile is 40:12:14:25:5:3:1;
(c) Placing the dried filler obtained in the step (a), the modified resin obtained in the step (b), the chlorinated rubber, the microcapsule obtained in the step S1, the flame retardant, the coupling agent and the polyethylene glycol into an internal mixer for banburying, and then extruding and forming; the mass ratio of each component is as follows: the dried filler obtained in step (a): the modified resin obtained in the step (b): chlorinated rubber: microcapsules obtained in step S1: flame retardant: coupling agent: polyethylene glycol is 2:12:28:16:3:0.5:10; the filler is nano alumina; the flame retardant is magnesium hydroxide; the coupling agent is silane coupling agent KH-560.
Example 2
The embodiment provides a preparation method of a cable insulation material with a self-repairing function, which comprises the following steps:
s1: preparation of microcapsules:
(1) Mixing urea, formaldehyde, melamine and water, and stirring in a water bath to obtain a prepolymer; the mass ratio of each component is as follows: urea: formaldehyde: melamine: water 4.2:8.5:1:51; the water bath temperature is 71 ℃, the stirring time is 48min, and the stirring speed is 500r/min;
(2) Mixing phenolic resin, dicyclopentadiene, sodium dodecyl benzene sulfonate and water, and stirring in a water bath to form a core material; the mass of dicyclopentadiene is 4.3 times of that of urea; the mass ratio of each component is as follows: phenolic resin: dicyclopentadiene: sodium dodecyl benzene sulfonate: the water is 8:10.5:0.1:82; the water bath temperature is 42 ℃, the stirring time is 30min, and the stirring speed is 800r/min;
(3) Mixing and stirring the prepolymer and the core material to form microcapsules, and filtering; stirring time is 75min, and stirring speed is 400r/min;
s2: preparation of insulating material:
(a) Vacuum drying the filler for 2 hours at 95 ℃;
(b) Mixing ethanol and epoxy resin, adding methyl acrylate, styrene, acrylic acid, organic silicone oil and azodiisobutyronitrile, heating in water bath, and stirring to obtain modified resin; the mass ratio of each component is as follows: ethanol: epoxy resin: methyl acrylate: styrene: acrylic acid: organic silicone oil: azobisisobutyronitrile is 42:12.5:14.5:26:6:3.5:1.5;
(c) Placing the dried filler obtained in the step (a), the modified resin obtained in the step (b), the chlorinated rubber, the microcapsule obtained in the step S1, the flame retardant, the coupling agent and the polyethylene glycol into an internal mixer for banburying, and then extruding and forming; the mass ratio of each component is as follows: the dried filler obtained in step (a): the modified resin obtained in the step (b): chlorinated rubber: microcapsules obtained in step S1: flame retardant: coupling agent: polyethylene glycol is 2.5:12.5:29:17:3.5:0.6:11; the filler is ferrocene; the flame retardant is monoammonium phosphate; the coupling agent is silane coupling agent KH-570.
Example 3
The embodiment provides a preparation method of a cable insulation material with a self-repairing function, which comprises the following steps:
s1: preparation of microcapsules:
(1) Mixing urea, formaldehyde, melamine and water, and stirring in a water bath to obtain a prepolymer; the mass ratio of each component is as follows: urea: formaldehyde: melamine: water 4.5:9:1:52; the water bath temperature is 72 ℃, the stirring time is 48min, and the stirring speed is 600r/min;
(2) Mixing phenolic resin, dicyclopentadiene, sodium dodecyl benzene sulfonate and water, and stirring in a water bath to form a core material; the mass of dicyclopentadiene is 4-5 times of that of urea; the mass ratio of each component is as follows: phenolic resin: dicyclopentadiene: sodium dodecyl benzene sulfonate: water was 8.5:11:0.1:85; the water bath temperature is 45 ℃, the stirring time is 20min, and the stirring speed is 900r/min;
(3) Mixing and stirring the prepolymer and the core material to form microcapsules, and filtering; stirring time is 90min, and stirring speed is 400r/min;
s2: preparation of insulating material:
(a) Vacuum drying the filler for 3 hours at 90 ℃;
(b) Mixing ethanol and epoxy resin, adding methyl acrylate, styrene, acrylic acid, organic silicone oil and azodiisobutyronitrile, heating in water bath, and stirring to obtain modified resin; the mass ratio of each component is as follows: ethanol: epoxy resin: methyl acrylate: styrene: acrylic acid: organic silicone oil: azobisisobutyronitrile is 45:13:15:26:6:4:2;
(c) Placing the dried filler obtained in the step (a), the modified resin obtained in the step (b), the chlorinated rubber, the microcapsule obtained in the step S1, the flame retardant, the coupling agent and the polyethylene glycol into an internal mixer for banburying, and then extruding and forming; the mass ratio of each component is as follows: the dried filler obtained in step (a): the modified resin obtained in the step (b): chlorinated rubber: microcapsules obtained in step S1: flame retardant: coupling agent: polyethylene glycol is 2.5:13:30:18:3.5:0.7:12; the filler is mica powder; the flame retardant is magnesium hydroxide; the coupling agent is silane coupling agent KH-560.
Example 4
The embodiment provides a preparation method of a cable insulation material with a self-repairing function, which comprises the following steps:
s1: preparation of microcapsules:
(1) Mixing urea, formaldehyde, melamine and water, and stirring in a water bath to obtain a prepolymer; the mass ratio of each component is as follows: urea: formaldehyde: melamine: water 4.8:9:1:53; the water bath temperature is 73 ℃, the stirring time is 55min, and the stirring speed is 600r/min;
(2) Mixing phenolic resin, dicyclopentadiene, sodium dodecyl benzene sulfonate and water, and stirring in a water bath to form a core material; the mass of dicyclopentadiene is 4-5 times of that of urea; the mass ratio of each component is as follows: phenolic resin: dicyclopentadiene: sodium dodecyl benzene sulfonate: the water is 9:11:0.1:85; the water bath temperature is 45 ℃, the stirring time is 25min, and the stirring speed is 900r/min;
(3) Mixing and stirring the prepolymer and the core material to form microcapsules, and filtering; stirring time is 80min, and stirring speed is 500r/min;
s2: preparation of insulating material:
(a) Vacuum drying the filler for 3 hours at 92 ℃;
(b) Mixing ethanol and epoxy resin, adding methyl acrylate, styrene, acrylic acid, organic silicone oil and azodiisobutyronitrile, heating in water bath, and stirring to obtain modified resin; the mass ratio of each component is as follows: ethanol: epoxy resin: methyl acrylate: styrene: acrylic acid: organic silicone oil: azobisisobutyronitrile is 48:13.5:16:27:6:4:2;
(c) Placing the dried filler obtained in the step (a), the modified resin obtained in the step (b), the chlorinated rubber, the microcapsule obtained in the step S1, the flame retardant, the coupling agent and the polyethylene glycol into an internal mixer for banburying, and then extruding and forming; the mass ratio of each component is as follows: the dried filler obtained in step (a): the modified resin obtained in the step (b): chlorinated rubber: microcapsules obtained in step S1: flame retardant: coupling agent: polyethylene glycol is 2.8:14:30:19:4:0.6:12; the filler is a mixture of nano aluminum oxide, ferrocene and mica powder, and the weight ratio of the nano aluminum oxide to the ferrocene is as follows: ferrocene: mica powder is 1:0.2:2; the flame retardant is magnesium hydroxide; the coupling agent is silane coupling agent KH-570.
Example 5
The embodiment provides a preparation method of a cable insulation material with a self-repairing function, which comprises the following steps:
s1: preparation of microcapsules:
(1) Mixing urea, formaldehyde, melamine and water, and stirring in a water bath to obtain a prepolymer; the mass ratio of each component is as follows: urea: formaldehyde: melamine: water 5:9.5:1:53; the water bath temperature is 75 ℃, the stirring time is 55min, and the stirring speed is 600r/min;
(2) Mixing phenolic resin, dicyclopentadiene, sodium dodecyl benzene sulfonate and water, and stirring in a water bath to form a core material; the mass of dicyclopentadiene is 4.8 times of that of urea; the mass ratio of each component is as follows: phenolic resin: dicyclopentadiene: sodium dodecyl benzene sulfonate: water 9.5:11.5:0.1:87; the water bath temperature is 43 ℃, the stirring time is 30min, and the stirring speed is 900r/min;
(3) Mixing and stirring the prepolymer and the core material to form microcapsules, and filtering; the stirring time is 90min, and the stirring speed is 500r/min;
s2: preparation of insulating material:
(a) Vacuum drying the filler for 3 hours at 90 ℃;
(b) Mixing ethanol and epoxy resin, adding methyl acrylate, styrene, acrylic acid, organic silicone oil and azodiisobutyronitrile, heating in water bath, and stirring to obtain modified resin; the mass ratio of each component is as follows: ethanol: epoxy resin: methyl acrylate: styrene: acrylic acid: organic silicone oil: azobisisobutyronitrile is 48:14.5:17:29:7:4.5:2.5;
(c) Placing the dried filler obtained in the step (a), the modified resin obtained in the step (b), the chlorinated rubber, the microcapsule obtained in the step S1, the flame retardant, the coupling agent and the polyethylene glycol into an internal mixer for banburying, and then extruding and forming; the mass ratio of each component is as follows: the dried filler obtained in step (a): the modified resin obtained in the step (b): chlorinated rubber: microcapsules obtained in step S1: flame retardant: coupling agent: polyethylene glycol is 2.8:14.5:31:19:4.5:0.7:12; the filler is a mixture of nano aluminum oxide, ferrocene and mica powder, and the weight ratio of the nano aluminum oxide to the ferrocene is as follows: ferrocene: mica powder is 1:0.3:2.5; the flame retardant is monoammonium phosphate; the coupling agent is silane coupling agent KH-560.
Example 6
The embodiment provides a preparation method of a cable insulation material with a self-repairing function, which comprises the following steps:
s1: preparation of microcapsules:
(1) Mixing urea, formaldehyde, melamine and water, and stirring in a water bath to obtain a prepolymer; the mass ratio of each component is as follows: urea: formaldehyde: melamine: water is 5:10:1:55; the water bath temperature is 75 ℃, the stirring time is 45min, and the stirring speed is 500r/min;
(2) Mixing phenolic resin, dicyclopentadiene, sodium dodecyl benzene sulfonate and water, and stirring in a water bath to form a core material; the mass of dicyclopentadiene is 5 times of that of urea; the mass ratio of each component is as follows: phenolic resin: dicyclopentadiene: sodium dodecyl benzene sulfonate: the water is 10: 12:0.1:90; the water bath temperature is 45 ℃, the stirring time is 20min, and the stirring speed is 800r/min;
(3) Mixing and stirring the prepolymer and the core material to form microcapsules, and filtering; stirring time is 90min, and stirring speed is 400r/min;
s2: preparation of insulating material:
(a) Vacuum drying the filler for 3 hours at 90 ℃;
(b) Mixing ethanol and epoxy resin, adding methyl acrylate, styrene, acrylic acid, organic silicone oil and azodiisobutyronitrile, heating in water bath, and stirring to obtain modified resin; the mass ratio of each component is as follows: ethanol: epoxy resin: methyl acrylate: styrene: acrylic acid: organic silicone oil: azobisisobutyronitrile is 50: 15: 18: 30: 8:5:3;
(c) Placing the dried filler obtained in the step (a), the modified resin obtained in the step (b), the chlorinated rubber, the microcapsule obtained in the step S1, the flame retardant, the coupling agent and the polyethylene glycol into an internal mixer for banburying, and then extruding and forming; the mass ratio of each component is as follows: the dried filler obtained in step (a): the modified resin obtained in the step (b): chlorinated rubber: microcapsules obtained in step S1: flame retardant: coupling agent: polyethylene glycol 3:15:32:20:5:0.8:13; the filler is a mixture of nano aluminum oxide, ferrocene and mica powder, and the weight ratio of the nano aluminum oxide to the ferrocene is as follows: ferrocene: mica powder is 1:0.5: 3, a step of; the flame retardant is magnesium hydroxide; the coupling agent is silane coupling agent KH-570.
Example 7
The embodiment provides a preparation method of a cable insulation material with a self-repairing function, which comprises the following steps:
s1: preparation of microcapsules:
(1) Mixing urea, formaldehyde, melamine and water, and stirring in a water bath to obtain a prepolymer; the mass ratio of each component is as follows: urea: formaldehyde: melamine: water 5:9.5:1:53; the water bath temperature is 75 ℃, the stirring time is 55min, and the stirring speed is 600r/min;
(2) Mixing phenolic resin, dicyclopentadiene, sodium dodecyl benzene sulfonate and water, and stirring in a water bath to form a core material; the mass of dicyclopentadiene is 4.8 times of that of urea; the mass ratio of each component is as follows: phenolic resin: dicyclopentadiene: sodium dodecyl benzene sulfonate: water 9.5:11.5:0.1:87; the water bath temperature is 43 ℃, the stirring time is 30min, and the stirring speed is 900r/min;
(3) Mixing and stirring the prepolymer and the core material to form microcapsules, and filtering; the stirring time is 90min, and the stirring speed is 500r/min;
s2: preparation of insulating material:
(a) Vacuum drying the filler for 3 hours at 90 ℃;
(b) Mixing ethanol and epoxy resin, adding methyl acrylate, styrene, acrylic acid, organic silicone oil, azodiisobutyronitrile and carbon nano tubes, and heating and stirring in a water bath to obtain modified resin; the mass ratio of each component is as follows: ethanol: epoxy resin: methyl acrylate: styrene: acrylic acid: organic silicone oil: azobisisobutyronitrile: the carbon nanotubes were 48:14.5:17:29:7:4.5:2.5:1.5;
(c) Placing the dried filler obtained in the step (a), the modified resin obtained in the step (b), the chlorinated rubber, the microcapsule obtained in the step S1, the flame retardant, the coupling agent and the polyethylene glycol into an internal mixer for banburying, and then extruding and forming; the mass ratio of each component is as follows: the dried filler obtained in step (a): the modified resin obtained in the step (b): chlorinated rubber: microcapsules obtained in step S1: flame retardant: coupling agent: polyethylene glycol is 2.8:14.5:31:19:4.5:0.7:12; the filler is a mixture of nano aluminum oxide, ferrocene and mica powder, and the weight ratio of the nano aluminum oxide to the ferrocene is as follows: ferrocene: mica powder is 1:0.3:2.5; the flame retardant is monoammonium phosphate; the coupling agent is silane coupling agent KH-560.
Example 8
The embodiment provides a preparation method of a cable insulation material with a self-repairing function, which comprises the following steps:
s1: preparation of microcapsules:
(1) Mixing urea, formaldehyde, melamine and water, and stirring in a water bath to obtain a prepolymer; the mass ratio of each component is as follows: urea: formaldehyde: melamine: water 5:9.5:1:53; the water bath temperature is 75 ℃, the stirring time is 55min, and the stirring speed is 600r/min;
(2) Mixing phenolic resin, dicyclopentadiene, sodium dodecyl benzene sulfonate and water, and stirring in a water bath to form a core material; the mass of dicyclopentadiene is 4.8 times of that of urea; the mass ratio of each component is as follows: phenolic resin: dicyclopentadiene: sodium dodecyl benzene sulfonate: water 9.5:11.5:0.1:87; the water bath temperature is 43 ℃, the stirring time is 30min, and the stirring speed is 900r/min;
(3) Mixing the prepolymer and the core material, adding resorcinol with a mass half of that of the prepolymer, stirring to form microcapsules, and filtering; the stirring time is 90min, and the stirring speed is 500r/min;
s2: preparation of insulating material:
(a) Vacuum drying the filler for 3 hours at 90 ℃;
(b) Mixing ethanol and epoxy resin, adding methyl acrylate, styrene, acrylic acid, organic silicone oil, azodiisobutyronitrile and carbon nano tubes, and heating and stirring in a water bath to obtain modified resin; the mass ratio of each component is as follows: ethanol: epoxy resin: methyl acrylate: styrene: acrylic acid: organic silicone oil: azobisisobutyronitrile: the carbon nanotubes were 48:14.5:17:29:7:4.5:2.5:1.6;
(c) Placing the dried filler obtained in the step (a), the modified resin obtained in the step (b), the chlorinated rubber, the microcapsule obtained in the step S1, the flame retardant, the coupling agent and the polyethylene glycol into an internal mixer for banburying, and then extruding and forming; the mass ratio of each component is as follows: the dried filler obtained in step (a): the modified resin obtained in the step (b): chlorinated rubber: microcapsules obtained in step S1: flame retardant: coupling agent: polyethylene glycol is 2.8:14.5:31:19:4.5:0.7:12; the filler is a mixture of nano aluminum oxide, ferrocene and mica powder, and the weight ratio of the nano aluminum oxide to the ferrocene is as follows: ferrocene: mica powder is 1:0.3:2.5; the flame retardant is monoammonium phosphate; the coupling agent is silane coupling agent KH-560.
Comparative example 1
This comparative example provides a method for producing a cable insulation material having a self-repairing function, unlike example 1, this comparative example lacks step S1, i.e., no microcapsules are added.
Comparative example 2
This comparative example provides a method for producing a cable insulation material having a self-repairing function, which is different from example 1 in that this comparative example lacks step (b) and the modified resin in step (c) is replaced with an acrylic resin.
Comparative example 3
This comparative example provides a method for producing a cable insulation material having a self-repairing function, unlike example 1, in which a flame retardant is not contained.
Test method
1. Insulation performance test:
the sample volume was 100 mm ×100 mm ×1mm; measuring the volume resistivity of the sample at room temperature by using an HP4329A high-resistance instrument and a high-resistance resistor; measuring the relative dielectric constant by using a DEA2970 dielectric analyzer; the dielectric strength of the sample was measured at 100HZ using a siemens breakdown voltage apparatus.
2. Mechanical property test:
the tensile strength and elongation of the test pieces were measured at room temperature using a universal tensile tester.
3. Flame retardant performance test:
according to GB/T10707-2008 standard.
TABLE 1 test results for Cable insulation of examples 1-8 and comparative examples 1-3
In connection with table 1, the performance of the cable insulation materials of examples 1 to 8 and comparative examples 1 to 3 according to the present invention were tested, and the cable insulation materials of examples 1 to 8 each showed good combination of performance: volume resistivity of 9-9.8X10 16 And has excellent electrical insulation performance, wherein the dielectric constant is 1.6-1.8, the dielectric strength is 83-89 kV/mm; the tensile strength is 38.6-39.8Mpa, the elongation is 655-679%, and the oxygen index is 41-43. Comparative example 1 lacks step S1, i.e. no microcapsules were added; comparative example 2 lacks step (b), replacing the modified resin in step (c) with an acrylic resin; comparative example 3 does not contain flame retardant, and the performance of the insulating material is reduced, which indicates that the formulation and the process of the invention have good suitability.
Finally, it is noted that the above-mentioned embodiments are merely for illustrating the technical solution of the present invention, and that other modifications and equivalents thereof by those skilled in the art should be included in the scope of the claims of the present invention without departing from the spirit and scope of the technical solution of the present invention.
Claims (3)
1. A preparation method of a cable insulation material with a self-repairing function is characterized by comprising the following steps: comprises the following steps:
s1: preparation of microcapsules:
(1) Mixing urea, formaldehyde, melamine and water, and stirring in a water bath to obtain a prepolymer, wherein the mass ratio of the components is as follows: urea: formaldehyde: melamine: the water is 4-5:8-10:1:50-55;
(2) Mixing phenolic resin, dicyclopentadiene, sodium dodecyl benzene sulfonate and water, and stirring in a water bath to form a core material, wherein the mass ratio of the components is as follows: phenolic resin: dicyclopentadiene: sodium dodecyl benzene sulfonate: water is 7-10:10-12:0.1:80-90;
(3) Mixing and stirring the prepolymer and the core material to form microcapsules, and filtering;
the mass of dicyclopentadiene is 4-5 times of that of urea;
s2: preparation of insulating material:
(a) Vacuum drying the filler;
(b) Mixing ethanol and epoxy resin, adding methyl acrylate, styrene, acrylic acid, organic silicone oil and azodiisobutyronitrile, heating in water bath, and stirring to obtain modified resin;
the mass ratio of each component is as follows: ethanol: epoxy resin: methyl acrylate: styrene: acrylic acid: organic silicone oil: azobisisobutyronitrile is 40-50:12-15:14-18:25-30:5-8:3-5:1-3;
(c) Placing the dried filler obtained in the step (a), the modified resin obtained in the step (b), the chlorinated rubber, the microcapsule obtained in the step S1, the flame retardant, the coupling agent and the polyethylene glycol into an internal mixer for banburying, and then extruding and forming; the filler is one or more of nano aluminum oxide, ferrocene and mica powder; the flame retardant is magnesium hydroxide or ammonium dihydrogen phosphate;
the mass ratio of each component is as follows: the dried filler obtained in step (a): the modified resin obtained in the step (b): chlorinated rubber: microcapsules obtained in step S1: flame retardant: coupling agent: polyethylene glycol is 2-3:12-15:28-32:16-20:3-5:0.5-0.8:10-13.
2. The method for preparing the cable insulation material with the self-repairing function as claimed in claim 1, wherein the method comprises the following steps: in the step (1), the water bath temperature is 70-75 ℃, the stirring time is 45-60min, and the stirring speed is 500-600r/min; in the step (2), the water bath temperature is 40-45 ℃, the stirring time is 20-30min, and the stirring speed is 800-1000r/min; in the step (3), the stirring time is 60-90min, and the stirring speed is 400-500r/min.
3. The method for preparing the cable insulation material with the self-repairing function as claimed in claim 2, wherein the method comprises the following steps: the coupling agent is silane coupling agent KH-560 or KH-570.
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