CN115160739A - Electrical damage self-repairing epoxy resin composite insulating material and preparation method thereof - Google Patents
Electrical damage self-repairing epoxy resin composite insulating material and preparation method thereof Download PDFInfo
- Publication number
- CN115160739A CN115160739A CN202210955105.7A CN202210955105A CN115160739A CN 115160739 A CN115160739 A CN 115160739A CN 202210955105 A CN202210955105 A CN 202210955105A CN 115160739 A CN115160739 A CN 115160739A
- Authority
- CN
- China
- Prior art keywords
- insulating material
- epoxy resin
- self
- preparation
- electrical damage
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/40—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
-
- 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
- C08K2201/01—Magnetic additives
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Organic Insulating Materials (AREA)
Abstract
The invention discloses a novel electrical damage self-repairing epoxy resin composite insulating material and a preparation method thereof. The method comprises preparing a shell containing TiO 2 And Fe 3 O 4 @SiO 2 The microcapsule and the composite insulating material with the microcapsule doped in the epoxy resin carry out electrical damage self-repairing on the insulating material under the condition of not influencing the basic performance of the insulating material, and compared with a pure epoxy resin material, the microcapsule contains TiO 2 And Fe 3 O 4 @SiO 2 Dielectric of microencapsulated epoxy resin composite insulationThe constant is improved by 1-1.5 times, the dielectric loss of the insulating material is improved by a small degree but is still at a lower level on the whole, the breakdown performance and the insulating performance are not influenced, the insulating material has good self-healing performance, good insulating strength is kept after self-healing, the insulating performance of the insulating material is about 97% of that of the original material, and the insulating material has very important significance for improving the electrical damage resistance and the electrical damage self-healing performance of the insulating material.
Description
Technical Field
The invention belongs to the technical field of insulating material preparation, and particularly relates to a novel electrical damage self-repairing epoxy resin composite insulating material and a preparation method thereof.
Background
Epoxy resin insulating materials have excellent electrical insulating property, heat resistance and mechanical property, and are widely applied to electrical equipment, but in the production, transportation and long-term operation processes of the electrical equipment, the insulating materials are easy to age and damage, electrical damage is the most common aging phenomenon in the insulating materials, and is generally considered as a main cause of insulation property deterioration and breakdown, the service life of the insulating materials is seriously influenced, and even the electrical equipment fails prematurely.
Disclosure of Invention
Based on the problems in the existing technology for repairing electrical damage, the invention provides a novel electrical damage self-repairing epoxy resin composite insulating material, and a preparation method and application thereof. The method comprises preparing shell containing TiO 2 And Fe 3 O 4 @SiO 2 The microcapsule and the composite insulating material doped with the microcapsule in the epoxy resin carry out electrical damage self-repairing on the insulating material under the condition of not influencing the basic performance of the insulating material, and carry out systematic experimental research and theoretical analysis on the dielectric constant, the dielectric loss, the breakdown performance, the self-repairing performance of electrical damage self-repairing epoxy resin composite insulating material and the like. Studies have shown that TiO-containing materials are doped 2 And Fe 3 O 4 @SiO 2 The microcapsule modifies the epoxy resin composite insulating material, can improve the dielectric constant of the insulating material, does not influence the dielectric loss and the breakdown performance of the insulating material, and enables the insulating material to have good self-healing performance, thereby improving the overall performance of the insulating material.
By doping the shell with TiO 2 And Fe 3 O 4 @SiO 2 The microcapsule in the epoxy resin composite insulating material contains TiO compared with pure epoxy resin material 2 And Fe 3 O 4 @SiO 2 The dielectric constant of the epoxy resin composite insulating material of the microcapsule is improved by 1-1.5 times, the dielectric loss of the insulating material is improved in a small degree but the whole insulating material is still at a lower level, the breakdown performance and the insulating performance are not influenced, the insulating material has good self-healing performance, after self-healing is carried out, the good insulating strength is also kept, the insulating performance of the insulating material is about 97 percent of that of the original material, and the method has very important significance for improving the electrical damage resistance and the electrical damage self-healing performance of the insulating material.
The invention provides a novel electrical damage self-repairing epoxy resin composite insulating material, and a preparation method and application thereof.
A preparation method of a novel electrical damage self-repairing epoxy resin composite insulating material comprises the following steps:
s1, magnetic Fe 3 O 4 Preparation of the particles: adding ferric chloride and trisodium citrate into an organic solvent, uniformly stirring, then adding sodium acetate, stirring until the sodium acetate is dissolved to obtain a mixed solution, transferring the mixed solution into a hydrothermal reactor, and heating at 180-220 ℃ for 8-12 hours, then removing supernatant, washing the obtained solid and separating to obtain magnetic Fe 3 O 4 Particles;
S2、Fe 3 O 4 @SiO 2 preparation of the particles: magnetic Fe 3 O 4 Uniformly mixing particles, ethanol, ammonium hydroxide solution and tetraethyl silicate, and then separating to obtain Fe 3 O 4 @SiO 2 Particles;
s3, preparing the aqueous emulsion: mixing deionized water, gum arabic and TiO 2 Mixing the nano particles and carrying out ultrasonic treatment to prepare an aqueous emulsion;
s4, preparation of a healing agent: 3, 4-epoxy cyclohexyl methyl 3, 4-epoxy cyclohexyl formate and biphenyl sulfonium hexafluorophosphate according to the mass ratio of 100: 1-10 to obtain a healing agent;
s5, preparing microcapsules: mixing Fe 3 O 4 @SiO 2 Dispersing nanoparticles in Desmodur L75A/C TDI curing agent by ultrasonic waves, adding the healing agent prepared in the step S4, quickly dripping the mixture into the aqueous emulsion prepared in the step S3 after uniformly mixing, carrying out water bath heating at 50 ℃, then adding butanediol, changing the water bath heating temperature to be 60-80 ℃, uniformly mixing the solution, and cleaning and drying to prepare the microcapsule;
s6, preparing resin base liquid: firstly, uniformly mixing a resin monomer bisphenol A diglycidyl ether, methyl tetrahydrophthalic anhydride and phenol to obtain a resin base solution;
s7, preparing a self-healing composite material: adding microcapsules into the resin base liquid prepared in the step S6, uniformly stirring, then carrying out vacuum degassing on the mixture for 10-20 min, standing at 55-65 ℃ for 10-20 min to enable the mixture to be uniformly distributed, then pouring the mixture into a mold, filling the mold with the mixture, putting the mold filled with the mixture into a drying box, standing at 90-100 ℃ for 1-2 hours to enable the mold to be cured, and after the curing is finished, cooling the temperature to room temperature by adopting a gradient cooling method to prepare the self-healing composite material; the content of the microcapsule in the self-healing composite material is 1 to 10 percent.
The technical scheme of the invention is as follows: fe 3 O 4 @SiO 2 The preparation process of the particles comprises the following steps: magnetic Fe prepared by step S1 3 O 4 Adding absolute ethyl alcohol, ammonium hydroxide solution and tetraethyl silicate into the granules, placing the granules in a water bath at the temperature of 30-40 ℃, uniformly stirring, and washing the obtained solid with absolute ethyl alcohol and deionized water in sequence to obtain Fe 3 O 4 @SiO 2 And (3) granules.
In the technical scheme of the invention: in the S1, the mass of ferric chloride, trisodium citrate and sodium acetate is 1-5: 0.5-1.5: 4 to 8.
In the technical scheme of the invention: magnetic Fe in S2 3 O 4 The mass ratio of the particles, the ethanol, the ammonium hydroxide solution with the concentration of 25-28% and the tetraethyl silicate is 10-30: 10 to 20:2 to 8:20 to 30.
In the technical scheme of the invention: deionized water, GA and TiO in S3 2 The mass ratio of the nano particles is 50-70: 1 to 5:0.5 to 1.5.
In the technical scheme of the invention: fe in S5 3 O 4 @SiO 2 The mass ratio of the nano particles, the curing agent, the healing agent, the aqueous emulsion and the butanediol is 0.05-0.15: 3 to 6:1 to 15: 60-70: 1 to 5.
The technical scheme of the invention is as follows: in S6: the mass ratio of the bisphenol A diglycidyl ether to the methyl tetrahydrophthalic anhydride to the phenol is 1000:700 to 900:10 to 20.
A novel electrical damage self-repairing epoxy resin composite insulating material is prepared by adopting the method.
Further S7, a gradient cooling method is applied to the prepared self-healing composite material to reduce the temperature to room temperature,
preferably, the temperature reduction procedure of the gradient temperature reduction method is as follows:
more preferably, the temperature reduction procedure of the gradient temperature reduction method is as follows:
further, the temperature reduction procedure of the gradient temperature reduction method in S7 is as follows:
the second purpose of the invention is to provide a novel electrical damage self-repairing epoxy resin composite insulating material, which is prepared by adopting the method, and the relative dielectric constant of the insulating material is improved.
Further, the doping weight percentage of the microcapsule in the electrical damage self-repairing epoxy resin composite insulating material is 2.5%; preferably, the doping weight percentage of the microcapsule in the electrical damage self-repairing epoxy resin composite insulating material is 5%; further preferably, the doping weight percentage of the microcapsule in the electrical damage self-repairing epoxy resin composite insulating material is 10%.
The third purpose of the invention is to provide a novel electrical damage self-repairing epoxy resin composite insulating material, which is prepared by adopting the method and does not influence the dielectric loss and the breakdown characteristic of the electrical damage self-repairing epoxy resin composite insulating material.
Further, the doping weight percentage of the microcapsule in the electrical damage self-repairing epoxy resin composite insulating material is 1%; preferably, the doping weight percentage of the microcapsule in the electrical damage self-repairing epoxy resin composite insulating material is 10%; further preferably, the doping weight percentage of the microcapsule in the electrical damage self-repairing epoxy resin composite insulating material is 5%.
The fourth purpose of the invention is to provide a novel electrical damage self-repairing epoxy resin composite insulating material, which is prepared by the method, so that the insulating material has good self-healing performance, and the overall performance of the insulating material is improved.
The invention has the beneficial effects that:
1) The electric damage self-repairing epoxy resin composite insulating material prepared by the invention has the advantages that the shells doped with different concentrations contain TiO 2 And Fe 3 O 4 @SiO 2 Compared with a pure epoxy resin material, the microcapsule enables dipoles of the insulating material to perform self-steering along with frequency under a high-frequency condition, keeps the same frequency with an alternating electric field, improves the relative dielectric constant of the insulating material, the dielectric constant of the pure epoxy resin is 3-4 at normal temperature, the dielectric constant of urea resin of a microcapsule shell is 6-9, the larger the relative dielectric constant is, the stronger the capacity of restraining charges is, the better the insulating property of the material is, and the insulating property of the insulating material is effectively improved.
2) The electric damage self-repairing epoxy resin composite insulating material prepared by the invention has the advantages that the shells doped with different concentrations contain TiO 2 And Fe 3 O 4 @SiO 2 The introduction of the microcapsule can increase the interfaces in the composite material, the interface polarization is gradually enhanced, and the interface polarization causes dielectric loss, but the material prepared by the invention only enables the dielectric loss of the composite material to be increased in a small range and still be at a lower level, and does not influence the dielectric loss and the breakdown characteristic of the insulating material.
3) The electrical damage self-repairing epoxy resin composite insulating material prepared by the invention has good self-healing performance, in pure epoxy resin, the damage of an electrical tree starts from the tip of a needle electrode and is diverged in a tree shape, in a starting stage, the tree grows slowly, the damaged area is small, and the electrical tree composite insulating material is the best time for repairing the electrical tree, when the prepared material is subjected to electrical damage, microcapsules are pushed to a high-fault area to heal the electrical tree, after the self-healing, the good insulating strength is also kept, the insulating performance of the prepared material is about 97 percent of that of the original material, and the electrical damage self-repairing material has very important significance for improving the electrical damage resistance and the electrical damage self-repairing performance of the insulating material.
Drawings
FIG. 1 relative dielectric constant of insulating material
FIG. 2 dielectric loss of insulating material
FIG. 3 development of electric tree
FIG. 4 power frequency test transformer platform
FIG. 5 electric tree branch repair
Figure 6 microcapsule morphology of example 1.
Detailed Description
The sources and purities of the chemical reagents used for sample preparation in the method of the invention are shown in table 1:
table 1 summary of main experimental materials
The model and source of the main experimental apparatus for sample preparation in the method of the invention are shown in Table 2:
table 2 summary of sample preparation main experimental apparatus
The present invention is further illustrated by the following examples so that those skilled in the art may better understand the invention and practice it, but the examples are not intended to limit the invention.
Example 1
S1, magnetic Fe 3 O 4 Preparation of the particles: dissolving 3g ferric chloride and 1g trisodium citrate in 100m ethylene glycol by magnetic stirring for about 1 hr, adding 6g sodium acetate, stirring to dissolve, transferring the mixed solution to hydrothermal reactor, heating at 200 deg.C for 10 hr, removing supernatant, and collecting magnetic Fe 3 O 4 Nanoparticles, followed by the first useWashing with absolute ethyl alcohol, separating, washing with deionized water, and separating to obtain magnetic Fe 3 O 4 A particle;
S2、Fe 3 O 4 @SiO 2 preparation of the particles: in a three-necked flask, 20g of magnetic Fe prepared in step S1 was charged 3 O 4 Adding 20ml of absolute ethyl alcohol into the granules, adding 4ml of 25-28% ammonium hydroxide solution, adding 25ml of tetraethyl silicate, placing the tetraethyl silicate in a water bath at 35 ℃ and stirring uniformly, and then separating Fe in the mixed solution 3 O 4 @ SiO2 particles prepared by successively pairing prepared Fe with absolute ethanol and deionized water 3 O 4 @SiO 2 Washing the particles;
s3, preparing the aqueous emulsion: 60g of deionized water, 2g of gum arabic and 1g of amphiphilic TiO 2 Mixing the nano particles and carrying out ultrasonic treatment to prepare an aqueous emulsion;
s4, preparing a healing agent: 3, 4-epoxy cyclohexyl methyl 3, 4-epoxy cyclohexyl formate and propylene carbonate sulfohexafluorophosphate solution are mixed according to the mass ratio of 100:6, mixing;
s5, preparing the microcapsule: dispersing 0.1g of Fe3O4@ SiO2 nano-particles into 4.5g of Desmodur L75A/C TDI curing agent by ultrasonic waves, adding 13.5g of the healing agent prepared in the step S4, quickly dripping the mixture into 63g of the aqueous emulsion prepared in the step S3 after uniform mixing, heating the mixture in a water bath at 50 ℃, then adding 3g of butanediol, changing the heating temperature of the water bath to 70 ℃, uniformly mixing the solution, and cleaning and drying the mixture to prepare the microcapsule;
s6, preparing resin base liquid: firstly, resin monomer bisphenol A diglycidyl ether, methyl tetrahydrophthalic anhydride and phenol are mixed according to the mass ratio of 1000:800:15, uniformly mixing in a beaker to obtain a resin base solution;
s7, preparing a self-healing composite material: adding a certain amount of microcapsules into 100g of resin base liquid prepared in the step S6 to enable the doping weight percentage of the microcapsules in the electrical damage self-repairing epoxy resin composite insulating material to be 1%, uniformly stirring the mixture, degassing the mixture in vacuum for 15min, standing at 60 ℃ for 15min to enable the mixture to be uniformly distributed, pouring the mixture into a mold, filling the mold with the mixture, placing the mold filled with the mixture into a drying box, standing at 90-100 ℃ for 2 hours to enable the mold to be cured, and cooling to room temperature by adopting a gradient cooling method after curing is finished to prepare the self-healing composite material EDSIM (0 #).
The cooling procedure of the gradient cooling method is as follows:
example 2
In this example, except for S7, the doping weight percentage of the microcapsule in the electrical damage self-repairing epoxy resin composite insulating material was 2.5%, and the rest was the same as in example 1, and the self-healing composite material EDSIM (1 #) was prepared.
Example 3
In this example, the self-healing composite EDSIM (# 2) was prepared in the same manner as in example 1 except that in S7, the doping weight percentage of the microcapsules in the electrical damage self-repairing epoxy resin composite insulating material was 5%.
Example 4
In this example, except for S7, the doping weight percentage of the microcapsule in the electrical damage self-repair epoxy resin composite insulating material was 10%, and the rest was the same as in example 1, and the self-healing composite material EDSIM (3 #) was prepared.
Example 5 relative permittivity of self-repairing epoxy resin composite insulating Material for Electrical Damage
This example examines the effect of the doping weight percentage of the microcapsules in the electrical damage self-repairing epoxy resin composite insulating material on the relative dielectric constant of the insulating material.
The experiment was divided into three groups, the differences of each group being shown in table 3:
TABLE 3 addition ratio
From the experimental results, the relative dielectric constant of the insulating material with different doping concentrations is shown in fig. 1. The test frequency range was 0.1Hz to 1000000Hz. The relative dielectric constant of the pure epoxy resin and the epoxy resin composite material doped with the microcapsule increases along with the reduction of the frequency, and the trend is similar. In a low frequency region, the three materials have higher dielectric constants, and along with the increase of frequency, in the insulating material, some dipoles are difficult to keep the same frequency direction with an alternating electric field, so that the dielectric constant is reduced, but the dielectric constant of the composite material is higher than that of pure epoxy resin, and when the doping concentration of the microcapsules is 10%, the relative dielectric constant is the largest, so that the insulating property of the insulating material is effectively improved.
Example 6 dielectric loss and breakdown characteristics of Electrical Damage self-healing epoxy resin composite insulating Material
This example examines the effect of the doping weight percentage of the microcapsules in the electrical damage self-repairing epoxy resin composite insulating material on the dielectric loss and breakdown characteristics of the insulating material.
The experiment was divided into three groups, the differences of each group being shown in table 3:
TABLE 3 addition ratio
From experimental results, the dielectric loss of the insulating material changes with frequency under different doping concentrations as shown in fig. 2, the introduction of the microcapsule also increases the number of interfaces in the composite material, the interface polarization is gradually enhanced, the interface polarization causes the dielectric loss, so that the dielectric loss of the prepared electrical damage self-repairing epoxy resin insulating material is slightly increased, but still at a lower level, wherein when the doping concentration of the microcapsule is 10%, the dielectric loss of the insulating material fluctuates slightly, but when the doping concentration of the microcapsule is 5%, the influence on the dielectric loss of the insulating material is in a very small range, and the relative dielectric constant of the insulating material can be effectively improved.
Example 7 self-healing Properties of Electrical Damage self-healing epoxy resin composite insulating Material
The insulating material is usually absolutely pure to prevent or delay the occurrence of electrical dendrites, but contamination, protrusions and voids of some insulators are difficult to avoid, which cause local electric fields to be too high and thus cause electrical dendrite activation.
An industrial frequency test transformer platform is adopted in the experiment and is shown in figure 4, an alternating current pressurization experiment is carried out on the electrical damage self-repairing epoxy resin insulating material prepared in the previous step, and an electrical tree branch generated at the EDSIM (2 #) needle point is shown in figure 3. As can be seen from fig. 3, after the application of an alternating current, charge injection and partial discharge cause the electrical tree branches to start and propagate, which branch like a tree or a shrub in the insulation material, forming an interconnected structure. The formation of the channels and the generation of carbon substances can further strengthen the local electric field, and micropores are enlarged and continuously damaged under the action of stronger local discharge, so that the polymer breakdown is finally caused, and the insulating material fails.
Compared with the pure epoxy resin sample, the deposition of black carbide in the EDSIM (2 #) electrical dendritic channel in FIG. 5 is obviously reduced, most of the electrical dendritic channels show the color of the microcapsule core material, and air bubbles generated by the core material outflow also appear in the microcapsule. After the wall material is broken through by the electrical branch channel, the repair material in the microcapsule flows out and enters the electrical branch channel, the electrical branch channel is gradually filled, after self-healing, good insulation strength is kept, the insulation performance of the electrical branch channel is about 97% of that of the original material, and the electrical branch channel self-repair material has very important significance in improving the electrical damage resistance and electrical damage self-repair performance of the insulation material.
In conclusion, the doping weight percentage of the microcapsules in the electrical damage self-repairing epoxy resin composite insulating material prepared by the method is optimally 5%, so that the relative dielectric constant of the insulating material is increased, the dielectric loss and the breakdown characteristic of the insulating material are not influenced, and the insulating material has a good self-healing function.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitutions or changes made by the person skilled in the art on the basis of the present invention are all within the protection scope of the present invention. The protection scope of the invention is subject to the claims.
Claims (9)
1. A preparation method of a novel electrical damage self-repairing epoxy resin composite insulating material is characterized by comprising the following steps: the method comprises the following steps:
s1, magnetic Fe 3 O 4 Preparation of the particles: adding ferric chloride and trisodium citrate into an organic solvent, uniformly stirring, then adding sodium acetate, stirring until the sodium acetate is dissolved to obtain a mixed solution, transferring the mixed solution into a hydrothermal reactor, heating at 180-220 ℃ for 8-12 hours, then removing supernatant, washing the obtained solid, and separating to obtain magnetic Fe 3 O 4 Particles;
S2、Fe 3 O 4 @SiO 2 preparation of the particles: magnetic Fe 3 O 4 Uniformly mixing the particles, ethanol, ammonium hydroxide solution and tetraethyl silicate, and then separating to obtain Fe 3 O 4 @SiO 2 A particle;
s3, preparing the aqueous emulsion: mixing deionized water, gum arabic and TiO 2 Mixing the nano particles and carrying out ultrasonic treatment to prepare an aqueous emulsion;
s4, preparation of a healing agent: 3, 4-epoxy cyclohexyl methyl 3, 4-epoxy cyclohexyl formate and biphenyl sulfonium hexafluorophosphate according to the mass ratio of 100: 1-10 to obtain a healing agent;
s5, preparing the microcapsule: mixing Fe 3 O 4 @SiO 2 Dispersing the nano particles in a curing agent by ultrasonic waves, adding the healing agent prepared in the step S4, uniformly mixing, quickly dripping the mixture into the aqueous emulsion prepared in the step S3 after mixing, heating in a water bath at 45-55 ℃, and then adding butanediol to change the situation thatHeating in water bath at 60-80 deg.c, mixing the solution homogeneously, washing and drying to obtain microcapsule;
s6, preparing resin base liquid: firstly, uniformly mixing a resin monomer bisphenol A diglycidyl ether, methyl tetrahydrophthalic anhydride and phenol to obtain a resin base solution;
s7, preparing a self-healing composite material: adding microcapsules into the resin base liquid prepared in the step S6, uniformly stirring, then carrying out vacuum degassing on the mixture for 10-20 min, standing at 55-65 ℃ for 10-20 min to enable the mixture to be uniformly distributed, then pouring the mixture into a mold, filling the mold with the mixture, putting the mold filled with the mixture into a drying box, standing at 90-100 ℃ for 1-2 hours to enable the mold to be cured, and after the curing is finished, cooling the temperature to room temperature by adopting a gradient cooling method to prepare the self-healing composite material; the content of the microcapsule in the self-healing composite material is 1 to 10 percent.
2. The preparation method of the novel electrical damage self-repairing epoxy resin composite insulating material as claimed in claim 1, characterized in that: fe 3 O 4 @SiO 2 The preparation process of the particles comprises the following steps: magnetic Fe prepared by step S1 3 O 4 Adding absolute ethyl alcohol, ammonium hydroxide solution and tetraethyl silicate into the granules, placing the granules in a water bath at the temperature of 30-40 ℃, uniformly stirring, and washing the obtained solid with absolute ethyl alcohol and deionized water in sequence to obtain Fe 3 O 4 @SiO 2 And (3) particles.
3. The preparation method of the novel electrical damage self-repairing epoxy resin composite insulating material as claimed in claim 1 or 2, characterized in that: in the S1, the mass of ferric chloride, trisodium citrate and sodium acetate is 1-5: 0.5 to 1.5:4 to 8.
4. The preparation method of the novel electrical damage self-repairing epoxy resin composite insulating material as claimed in claim 1, characterized in that: magnetic Fe in S2 3 O 4 The mass of the particles, ethanol, 25 to 28 percent ammonium hydroxide solution and tetraethyl silicateThe ratio is 10-30: 10 to 20:2 to 8:20 to 30.
5. The preparation method of the novel electrical damage self-repairing epoxy resin composite insulating material as claimed in claim 1, characterized in that: deionized water, gum powder GA and TiO in S3 2 The mass ratio of the nano particles is 50-70: 1 to 5:0.5 to 1.5.
6. The preparation method of the novel electrical damage self-repairing epoxy resin composite insulating material as claimed in claim 1, characterized in that: fe in S5 3 O 4 @SiO 2 The mass ratio of the nano particles, the curing agent, the healing agent, the aqueous emulsion and the butanediol is 0.05-0.15: 3 to 6:1 to 15: 60-70: 1 to 5.
7. The preparation method of the novel electrical damage self-repairing epoxy resin composite insulating material as claimed in claim 1, characterized in that: in S6: the mass ratio of the bisphenol A diglycidyl ether to the methyl tetrahydrophthalic anhydride to the phenol is 1000:700 to 900:10 to 20.
8. The preparation method of the novel electrical damage self-repairing epoxy resin composite insulating material as claimed in claim 1, characterized in that: the curing agent in S5 is Desmodur L75A/C TDI.
9. The utility model provides a novel electrical damage selfreparing epoxy composite insulating material which characterized in that: the material is made by the method of any one of claims 1 to 7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210955105.7A CN115160739A (en) | 2022-08-10 | 2022-08-10 | Electrical damage self-repairing epoxy resin composite insulating material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210955105.7A CN115160739A (en) | 2022-08-10 | 2022-08-10 | Electrical damage self-repairing epoxy resin composite insulating material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115160739A true CN115160739A (en) | 2022-10-11 |
Family
ID=83479321
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210955105.7A Pending CN115160739A (en) | 2022-08-10 | 2022-08-10 | Electrical damage self-repairing epoxy resin composite insulating material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115160739A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117924883A (en) * | 2024-01-26 | 2024-04-26 | 重庆大学 | Self-detection dielectric composite material and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170158886A1 (en) * | 2015-12-02 | 2017-06-08 | The Board Of Trustees Of The University Of Illinois | Self-healing coating |
| EP3335785A1 (en) * | 2016-12-13 | 2018-06-20 | Fundación Tecnalia Research & Innovation | Self-healing microcapsules, process for the prepartion thereof, polymeric matrix and composite materials comprising the same |
| CN109294166A (en) * | 2018-09-19 | 2019-02-01 | 重庆大学 | Epoxy resin composite insulating material and preparation method thereof |
| CN111154234A (en) * | 2020-01-20 | 2020-05-15 | 清华大学 | Preparation method of medium-high temperature self-repairing insulating material |
| CN113817290A (en) * | 2021-09-28 | 2021-12-21 | 重庆大学 | Anti-shrinkage self-repairing epoxy resin/microcapsule composite material and preparation method thereof |
| CN114874587A (en) * | 2022-06-17 | 2022-08-09 | 重庆大学 | Epoxy resin composite insulating material with mechanical damage targeting self-healing performance |
-
2022
- 2022-08-10 CN CN202210955105.7A patent/CN115160739A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170158886A1 (en) * | 2015-12-02 | 2017-06-08 | The Board Of Trustees Of The University Of Illinois | Self-healing coating |
| EP3335785A1 (en) * | 2016-12-13 | 2018-06-20 | Fundación Tecnalia Research & Innovation | Self-healing microcapsules, process for the prepartion thereof, polymeric matrix and composite materials comprising the same |
| CN109294166A (en) * | 2018-09-19 | 2019-02-01 | 重庆大学 | Epoxy resin composite insulating material and preparation method thereof |
| CN111154234A (en) * | 2020-01-20 | 2020-05-15 | 清华大学 | Preparation method of medium-high temperature self-repairing insulating material |
| CN113817290A (en) * | 2021-09-28 | 2021-12-21 | 重庆大学 | Anti-shrinkage self-repairing epoxy resin/microcapsule composite material and preparation method thereof |
| CN114874587A (en) * | 2022-06-17 | 2022-08-09 | 重庆大学 | Epoxy resin composite insulating material with mechanical damage targeting self-healing performance |
Non-Patent Citations (1)
| Title |
|---|
| WENXIA SIMA等: "Novel Smart Insulating Materials Achieving Targeting Self-Healing of Electrical Trees: High Performance, Low Cost, and Eco-Friendliness", ACS APPLIED MATERIALS & INTERFACES, vol. 13, no. 28, pages 33485 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117924883A (en) * | 2024-01-26 | 2024-04-26 | 重庆大学 | Self-detection dielectric composite material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107266863B (en) | Nonlinear conductivity epoxy resin composite insulating material and preparation method thereof | |
| CN109942793B (en) | Organic fluorine modified epoxy resin for improving surface flashover voltage and preparation method and application thereof | |
| CN109370127B (en) | Two-dimensional layered material-polyvinyl alcohol hydrogel and preparation method thereof | |
| CN115160739A (en) | Electrical damage self-repairing epoxy resin composite insulating material and preparation method thereof | |
| CN113336978B (en) | Preparation method of epoxy micro-nano co-doped composite material | |
| DE102010032555A1 (en) | Insulation for rotating electrical machines | |
| CN101650994B (en) | Suspension insulator | |
| CN103012697A (en) | VPI (vacuum pressure impregnation) resin | |
| CN111171515A (en) | Resin-based composite material bus duct pouring process | |
| CN106920592A (en) | A kind of power cable | |
| CN105462434B (en) | Epoxy casting insulating element coated material and surface modifying method | |
| CN110615877A (en) | Graft modified alumina, preparation method thereof, epoxy composite material and application thereof | |
| KR101072139B1 (en) | Method for preparing epoxy/silica multicomposite for high voltage insulation and product thereby | |
| CN113831247A (en) | Maleic anhydride modified voltage stabilizer and preparation method and application thereof | |
| CN105255017A (en) | Ethylene-propylene rubber insulating material for medium voltage power cable and preparation method thereof | |
| CN112375255A (en) | Nano-filler and epoxy composite insulating material, preparation method thereof and epoxy composite insulating part | |
| EP3438200A1 (en) | Curable composition, cured object obtained therefrom, and rotary device | |
| CN112143172A (en) | Insulator sheath material with low water absorption rate and preparation method thereof | |
| CN109575595A (en) | A kind of preparation method of polyetherimide/barium titanate/graphene dielectric composite material | |
| CN114790324B (en) | Method for improving breakdown strength of aluminum oxide/epoxy resin composite material | |
| CN108484954B (en) | GIL insulator design method with surface conductance two-dimensional U-shaped gradient distribution | |
| CN115232439A (en) | Method for improving surface flashover voltage of epoxy insulating material by nano doping | |
| CN108456588A (en) | A kind of vegetable insulating oil and preparation method thereof | |
| CN110628183B (en) | Epoxy glass fiber nanocomposite for high-voltage switch insulating pull rod and preparation method thereof | |
| CN104201424B (en) | For the Superhydrophilic silicon rubber master batch and preparation method thereof of colloidal electrolyte of lead acid accumulator |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |