CN114958152A - Nano modified high-molecular insulation repair coating and preparation method thereof - Google Patents

Nano modified high-molecular insulation repair coating and preparation method thereof Download PDF

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CN114958152A
CN114958152A CN202210850801.1A CN202210850801A CN114958152A CN 114958152 A CN114958152 A CN 114958152A CN 202210850801 A CN202210850801 A CN 202210850801A CN 114958152 A CN114958152 A CN 114958152A
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nano
zinc oxide
coupling agent
silicon dioxide
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蒋超璐
张中杨
杨国清
王德意
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Xian University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
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    • C08K3/20—Oxides; Hydroxides
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    • C—CHEMISTRY; METALLURGY
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Abstract

The invention discloses a nano modified high-molecular insulation repair coating which comprises the following components: adding 50g of RTV silicon rubber, 15g of normal-temperature curing agent, 6.111-13.750 g of glass fiber, 6.111-13.750 g of nano zinc oxide, 6.111-13.750 g of nano silicon dioxide, 1.222-2.750 g of coupling agent, 28.722-64.625 g of absolute ethyl alcohol and 0.611-1.375 g of purified water into every 100g of epoxy resin; the curing time is shortened while the electrical insulating property of the RTV silicon rubber/epoxy resin is taken into consideration, and the cracking resistance of the RTV silicon rubber/epoxy resin after cold and hot cycles is improved; the invention also discloses a preparation method of the nano modified polymer insulation repair coating.

Description

Nano modified high-molecular insulation repair coating and preparation method thereof
Technical Field
The invention belongs to the technical field of high-voltage composite insulating materials, and relates to a nano modified high-molecular insulating repair coating and a preparation method thereof.
Background
The voltage class of the power system is continuously improved, and the insulation requirement on high-voltage equipment is higher and higher. When the equipment runs for a certain time, the insulating part may have defects, cracks and the like. How to repair the insulating part quickly and ensure the safe and stable operation of the equipment is particularly important.
Epoxy resin is one of the most widely applied insulating materials in current high-voltage equipment, but the cured epoxy resin has the defects of brittle and easy fracture, poor thermal conductivity and the like, and modification research on the epoxy resin is necessary for better popularization and application in a power system.
Disclosure of Invention
The invention aims to provide a nano modified high-molecular insulation repair coating, which not only gives consideration to the electrical insulation performance of RTV (room temperature vulcanized) silicone rubber/epoxy resin, but also accelerates the curing time and improves the cracking resistance of the RTV silicone rubber/epoxy resin after cold and hot cycles.
The invention also aims to provide a preparation method of the nano modified high-molecular insulation repair coating.
The first technical scheme adopted by the invention is that the nano modified high-molecular insulation repair coating specifically comprises the following components in percentage by mass: 50g of RTV silicon rubber, 15g of normal-temperature curing agent, 6.111-13.750 g of glass fiber, 6.111-13.750 g of nano zinc oxide, 6.111-13.750 g of nano silicon dioxide, 1.222-2.750 g of coupling agent, 28.722-64.625 g of absolute ethyl alcohol and 0.611-1.375 g of purified water are added into every 100g of epoxy resin.
The first technical feature of the present invention is also characterized in that:
wherein the epoxy resin is bisphenol A type epoxy resin E-51; the normal temperature curing agent is 593 type epoxy curing agent; the coupling agent is gamma-aminopropyl triethoxysilane KH 550; the glass fiber is 100 meshes, and the purity is more than or equal to 99 percent; the particle size of the nano zinc oxide is 50 +/-5 nm, and the purity is more than or equal to 99 percent; the particle size of the nano silicon dioxide is 50 +/-5 nm, and the purity is more than or equal to 99%.
The second technical scheme adopted by the invention is that the preparation method of the nano modified high-molecular insulation repair coating is implemented according to the following steps:
step 1, weighing the following components in parts by mass: adding 50g of RTV silicon rubber, 15g of normal-temperature curing agent, 6.111-13.750 g of glass fiber, 6.111-13.750 g of nano zinc oxide, 6.111-13.750 g of nano silicon dioxide, 1.222-2.750 g of coupling agent, 28.722-64.625 g of absolute ethyl alcohol and 0.611-1.375 g of purified water into 100g of epoxy resin;
step 2, carrying out surface treatment on the nano zinc oxide powder weighed in the step 1;
step 3, carrying out surface treatment on the nano silicon dioxide powder weighed in the step 1;
step 4, placing the nano zinc oxide subjected to the surface treatment in the step 2, the nano silicon dioxide subjected to the surface treatment in the step 3 and the glass fiber weighed in the step 1 into a constant-temperature drying box for drying;
and 5, diluting the epoxy resin weighed in the step 1, adding the RTV silicone rubber and a normal-temperature curing agent, sequentially adding the glass fiber, the nano zinc oxide and the nano silicon dioxide dried in the step 4, and uniformly mixing to obtain the glass fiber, nano zinc oxide and nano silicon dioxide co-modified RTV silicone rubber/epoxy resin composite repair coating.
The second technical scheme of the invention is also characterized in that:
wherein the step 2 is implemented according to the following steps:
step 2.1, drying the weighed nano zinc oxide;
step 2.2, after the step 2.1, putting the dried nano zinc oxide into absolute ethyl alcohol with the mass 2 times of that of the dried nano zinc oxide, and mechanically and ultrasonically stirring the mixture uniformly under the condition of water bath;
step 2.3, putting a coupling agent with the mass of 0.1 time of that of the nano zinc oxide into a beaker, and adding purified water with the mass of 0.5 time of that of the coupling agent for hydrolysis; then adding absolute ethyl alcohol with the mass 3.5 times of that of the coupling agent to obtain coupling agent hydrolysate;
step 2.4, adding the hydrolysate obtained in the step 2.3 into the nano zinc oxide solution obtained in the step 2.2, and mechanically and ultrasonically stirring the hydrolysate uniformly under the condition of water bath to enable the coupling agent and the nano zinc oxide to fully react; the stirring time is more than or equal to 40min, and the water bath temperature is 25-30 ℃; the mechanical rotating speed is 200-250 r/min; ultrasonic frequency 40 kHz;
2.5, placing the coupling agent modified nano zinc oxide solution obtained in the step 2.4 in a constant-temperature drying oven for drying for 4-6 hours, and grinding for later use after drying;
wherein in the step 2.1, the temperature of the constant-temperature drying oven is set to be 80 ℃, and the drying time is 4-6 hours;
wherein in the step 2.2, the stirring time is more than or equal to 20min, the water bath temperature is 25-30 ℃, the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz;
wherein the step 3 is implemented according to the following steps:
step 3.1, drying the weighed nano silicon dioxide;
step 3.2, adding the dried nano silicon dioxide into absolute ethyl alcohol with the mass 2 times of that of the dried nano silicon dioxide, and mechanically and ultrasonically stirring the mixture uniformly under the condition of water bath to completely dissolve the dried nano silicon dioxide;
step 3.3, putting a coupling agent with the mass of 0.1 time of that of the nano silicon dioxide into a beaker, and adding purified water with the mass of 0.5 time of that of the coupling agent to completely hydrolyze the nano silicon dioxide; adding absolute ethyl alcohol with the mass of 3.5 times of that of the coupling agent to obtain coupling agent hydrolysate;
step 3.4, adding the hydrolysate obtained in the step 3.3 into the nano-silica solution obtained in the step 3.2, and mechanically and ultrasonically stirring the hydrolysate uniformly under the condition of water bath to enable the coupling agent and the nano-silica to fully react; the stirring time is more than or equal to 40min, and the water bath temperature is 25-30 ℃; the mechanical rotating speed is 200-250 r/min; ultrasonic frequency 40 kHz;
step 3.5, placing the coupling agent modified nano-silica solution obtained in the step 3.4 in a constant-temperature drying oven for drying for 4-6 hours, and grinding for later use after drying;
wherein the temperature of the constant-temperature drying oven in the step 3.1 is set to be 80 ℃, and the drying time is 4-6 hours; 3.2, the temperature of the water bath is 25-30 ℃, the stirring time is more than or equal to 20min, the mechanical rotating speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz;
wherein the temperature of the constant temperature drying oven in the step 4 is set to be 60 ℃, and the drying time is 1 hour;
wherein the step 5 specifically comprises the following steps: heating and diluting the epoxy resin weighed in the step 1 at 60 ℃ for 30min, removing water, adding the RTV silicone rubber weighed in the step 1 and a curing agent, then sequentially adding the glass fiber, the nano zinc oxide and the nano silicon dioxide dried in the step 4, stirring and ultrasonically treating under the water bath condition, and uniformly mixing; the water bath temperature is 25-30 ℃, the mechanical rotation speed is 200-250 r/min, the ultrasonic frequency is 40kHz, and the stirring time is 10 min.
The invention has the beneficial effects that:
according to the invention, the glass fiber, the nano zinc oxide and the nano silicon dioxide co-modified RTV silicone rubber/epoxy resin can ensure the excellent insulating property of the epoxy-based material, improve the mechanical strength of the epoxy-based material, and enhance the aging resistance and the heat conductivity of the epoxy-based material; the preparation method of the insulating composite coating is low in cost.
Drawings
FIG. 1 is a flow chart of a method for preparing a nano-modified polymer insulation repair coating according to the present invention;
FIG. 2 is a volume resistivity test curve of a sample of the nano-modified polymer insulation repair coating of the present invention;
FIG. 3 is a relative dielectric constant test curve of a sample of the nano-modified polymer insulation repair coating of the present invention;
FIG. 4 is a dielectric loss test curve of a sample of the nano-modified polymer insulation repair coating of the present invention;
FIG. 5 is a curve of the AC breakdown field strength test of samples of the nano-modified polymer insulation repair coating of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention provides a nano modified high-molecular insulation repair coating which comprises the following components in parts by mass: every 100g of epoxy resin is added with 50g of RTV silicon rubber, 15g of normal temperature curing agent, 6.111-13.750 g of glass fiber, 6.111-13.750 g of nano zinc oxide, 6.111-13.750 g of nano silicon dioxide, 1.222-2.750 g of coupling agent, 28.722-64.625 g of absolute ethyl alcohol and 0.611-1.375 g of purified water;
the epoxy resin is bisphenol A type epoxy resin E-51; the normal temperature curing agent is 593 type epoxy curing agent; the coupling agent is KH 550; the glass fiber is 100 meshes; the grain size of the nano zinc oxide is 50 +/-5 nm; the particle size of the nano silicon dioxide is 50 +/-5 nm.
The invention also provides a preparation method of the nano modified polymer insulation repair coating, which is implemented according to the following steps as shown in figure 1:
step 1, weighing the following components in parts by mass: 100g of epoxy resin, 50g of RTV silicon rubber, 15g of normal-temperature curing agent, 6.111-13.750 g of glass fiber, 6.111-13.750 g of nano zinc oxide, 6.111-13.750 g of nano silicon dioxide, 1.222-2.750 g of coupling agent, 28.722-64.625 g of absolute ethyl alcohol and 0.611-1.375 g of purified water;
step 2, adding the dried nano zinc oxide into absolute ethyl alcohol, and mechanically and ultrasonically stirring for 20min under the condition of a water bath at the temperature of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; mixing the coupling agent and purified water, and adding an absolute ethanol solution to obtain a coupling agent hydrolysate; mixing the coupling agent hydrolysate with the nano zinc oxide solution, and mechanically and ultrasonically stirring for 40min under the same condition; finally, placing the coupling agent modified nano zinc oxide solution in a constant-temperature drying oven for drying for 4-6 hours, and grinding for later use;
step 3, adding the dried nano silicon dioxide into absolute ethyl alcohol, and mechanically and ultrasonically stirring for 20min under the same condition as the step 2; mixing the coupling agent and purified water, and adding an absolute ethanol solution to obtain a coupling agent hydrolysate; mixing the coupling agent hydrolysate with the nano-silica solution, and mechanically and ultrasonically stirring for 40min under the same condition; finally, placing the coupling agent modified nano silicon dioxide solution in a constant-temperature drying oven for drying for 4-6 hours, and grinding for later use;
step 4, heating and diluting the epoxy resin at 60 ℃ for 30min, removing water, adding RTV silicone rubber and a curing agent, then sequentially adding dried glass fiber, nano zinc oxide and nano silicon dioxide, and mechanically and ultrasonically stirring for 10min under the same condition as that in the step 2 to prepare the glass fiber, nano zinc oxide and nano silicon dioxide co-modified RTV silicone rubber/epoxy resin composite repair coating;
and 5, brushing the composite repairing paint on the surface of the damaged and cracked insulating material, and curing and forming to realize insulation repairing.
Example 1
Step 1, weighing the following components in parts by mass: bisphenol A type epoxy resin E-51100 g, RTV silicon rubber 50g and 593 type epoxy curing agent 15 g;
step 2, heating and diluting bisphenol A type epoxy resin E-51 at 60 ℃ for 30min, removing water, and adding RTV silicone rubber and 593 type epoxy curing agent; under the condition of water bath at 25-30 ℃, mechanically and ultrasonically stirring for 10min at the mechanical rotating speed of 200-250 r/min and the ultrasonic frequency of 40kHz to prepare the RTV silicone rubber/epoxy resin composite repair coating;
and 3, brushing the composite repairing paint on the surface of the damaged and cracked insulating material, and curing and forming to realize insulating repair.
Example 2
Step 1, weighing the following components in parts by mass: bisphenol A type epoxy resin E-51100 g, RTV silicon rubber 50g, 593 type epoxy curing agent 15g, glass fiber 6.111g, nano zinc oxide 6.111g, nano silicon dioxide 6.111g, absolute ethyl alcohol 28.722g, purified water 0.611g and KH5501.222g;
step 2, adding dried nano zinc oxide into 12.222g of absolute ethyl alcohol, and mechanically and ultrasonically stirring for 20min under the condition of a water bath at the temperature of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; mixing 0.611g of KH550 and 0.306g of purified water, and adding 2.139g of absolute ethanol solution to obtain coupling agent hydrolysate; mixing the coupling agent hydrolysate with the nano zinc oxide solution, and mechanically and ultrasonically stirring for 40min under the condition of water bath at the temperature of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; and finally, placing the coupling agent modified nano zinc oxide solution in a constant-temperature drying oven for drying for 4-6 hours, and grinding for later use.
Step 3, adding dried nano silicon dioxide into 12.222g of absolute ethyl alcohol, and mechanically and ultrasonically stirring for 20min under the condition of a water bath at the temperature of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; mixing 0.611g of KH550 with 0.306g of purified water, and adding 2.139g of absolute ethanol solution to obtain coupling agent hydrolysate; mixing the coupling agent hydrolysate with the nano-silica solution, and mechanically and ultrasonically stirring for 40min under the condition of water bath at the temperature of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; and finally, placing the coupling agent modified nano silicon dioxide solution in a constant-temperature drying oven for drying for 4-6 hours, and grinding for later use.
Step 4, heating and diluting the epoxy resin at 60 ℃ for 30min, removing water, adding RTV silicone rubber and a curing agent, then sequentially adding dried glass fiber, nano-zinc oxide and nano-silica, and mechanically and ultrasonically stirring for 10min at the mechanical rotation speed of 200-250 r/min and the ultrasonic frequency of 40kHz under the condition of a water bath at 25-30 ℃ to prepare the glass fiber, nano-zinc oxide and nano-silica co-modified RTV silicone rubber/epoxy resin composite repair coating;
and 5, brushing the composite repairing paint on the surface of the damaged and cracked insulating material, and curing and forming to realize insulation repairing.
Example 3
Step 1, weighing the following components in parts by mass: bisphenol A type epoxy resin E-51100 g, RTV silicon rubber 50g, 593 type epoxy curing agent 15g, glass fiber 7.500g, nano zinc oxide 7.500g, nano silicon dioxide 7.500g, absolute ethyl alcohol 35.25g, purified water 0.750g and KH5501.500g;
step 2, adding the dried nano zinc oxide into 15.000g of absolute ethyl alcohol, and mechanically and ultrasonically stirring for 20min under the water bath condition of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; mixing 0.750g KH550 and 0.375g purified water, and adding 2.625g absolute ethanol solution to obtain coupling agent hydrolysate; mixing the coupling agent hydrolysate with the nano zinc oxide solution, and mechanically and ultrasonically stirring for 40min under the condition of water bath at the temperature of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; and finally, placing the coupling agent modified nano zinc oxide solution in a constant-temperature drying oven for drying for 4-6 hours, and grinding for later use.
Step 3, adding the dried nano silicon dioxide into 15.000g of absolute ethyl alcohol, and mechanically and ultrasonically stirring for 20min under the water bath condition of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; mixing 0.750g KH550 and 0.375g purified water, and adding 2.625g absolute ethanol solution to obtain coupling agent hydrolysate; mixing the coupling agent hydrolysate with the nano-silica solution, and mechanically and ultrasonically stirring for 40min under the condition of water bath at the temperature of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; and finally, placing the coupling agent modified nano silicon dioxide solution in a constant-temperature drying oven for drying for 4-6 hours, and grinding for later use.
Step 4, heating and diluting the epoxy resin at 60 ℃ for 30min, removing water, adding RTV silicone rubber and a curing agent, then sequentially adding dried glass fiber, nano-zinc oxide and nano-silica, and mechanically and ultrasonically stirring for 10min at the mechanical rotation speed of 200-250 r/min and the ultrasonic frequency of 40kHz under the condition of a water bath at 25-30 ℃ to prepare the glass fiber, nano-zinc oxide and nano-silica co-modified RTV silicone rubber/epoxy resin composite repair coating;
and 5, brushing the composite repairing paint on the surface of the damaged and cracked insulating material, and curing and forming to realize insulating repair.
Example 4
Step 1, respectively weighing the following components in parts by mass: bisphenol A epoxy resin E-51100 g, RTV silicon rubber 50g, 593 type epoxy curing agent 15g, glass fiber 8.954g, nano zinc oxide 8.954g, nano silicon dioxide 8.954g, absolute ethyl alcohol 42.081g, purified water 0.895g, KH5501.791g;
step 2, adding dried nano zinc oxide into 17.907g of absolute ethyl alcohol, and mechanically and ultrasonically stirring for 20min under the condition of a water bath at the temperature of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; then 0.895g KH550 and 0.448g purified water are mixed, and 3.134g absolute ethyl alcohol solution is added to obtain coupling agent hydrolysate; mixing the coupling agent hydrolysate with the nano zinc oxide solution, and mechanically and ultrasonically stirring for 40min under the condition of water bath at the temperature of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; and finally, placing the coupling agent modified nano zinc oxide solution in a constant-temperature drying oven for drying for 4-6 hours, and grinding for later use.
Step 3, adding dried nano silicon dioxide into 17.907g of absolute ethyl alcohol, and mechanically and ultrasonically stirring for 20min under the condition of a water bath at the temperature of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; then 0.895g KH550 and 0.448g purified water are mixed, and 3.134g absolute ethyl alcohol solution is added to obtain coupling agent hydrolysate; mixing the coupling agent hydrolysate with the nano-silica solution, and mechanically and ultrasonically stirring for 40min under the condition of water bath at the temperature of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; and finally, placing the coupling agent modified nano silicon dioxide solution in a constant-temperature drying oven for drying for 4-6 hours, and grinding for later use.
Step 4, heating and diluting the epoxy resin at 60 ℃ for 30min, removing water, adding RTV silicone rubber and a curing agent, then sequentially adding dried glass fiber, nano-zinc oxide and nano-silica, and mechanically and ultrasonically stirring for 10min at the mechanical rotation speed of 200-250 r/min and the ultrasonic frequency of 40kHz under the condition of a water bath at 25-30 ℃ to prepare the glass fiber, nano-zinc oxide and nano-silica co-modified RTV silicone rubber/epoxy resin composite repair coating;
and 5, brushing the composite repairing paint on the surface of the damaged and cracked insulating material, and curing and forming to realize insulation repairing.
Example 5
Step 1, weighing the following components in parts by mass: bisphenol A type epoxy resin E-51100 g, RTV silicon rubber 50g, 593 type epoxy curing agent 15g, glass fiber 10.476g, nano zinc oxide 10.476g, nano silicon dioxide 10.476g, absolute ethyl alcohol 49.238g, purified water 1.048g and KH5502.095g;
step 2, adding dried nano zinc oxide into 20.952g of absolute ethyl alcohol, and mechanically and ultrasonically stirring for 20min under the condition of a water bath at the temperature of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; mixing 1.048g of KH550 with 0.524g of purified water, and adding 3.667g of absolute ethanol solution to obtain coupling agent hydrolysate; mixing the coupling agent hydrolysate with the nano zinc oxide solution, and mechanically and ultrasonically stirring for 40min under the condition of water bath at the temperature of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; and finally, placing the coupling agent modified nano zinc oxide solution in a constant-temperature drying oven for drying for 4-6 hours, and grinding for later use.
Step 3, adding dried nano silicon dioxide into 20.952g of absolute ethyl alcohol, and mechanically and ultrasonically stirring for 20min under the condition of a water bath at the temperature of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; mixing 1.048g of KH550 and 0.524g of purified water, and adding 3.667g of absolute ethanol solution to obtain coupling agent hydrolysate; mixing the coupling agent hydrolysate with the nano-silica solution, and mechanically and ultrasonically stirring for 40min under the condition of water bath at the temperature of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; finally, placing the coupling agent modified nano silicon dioxide solution in a constant-temperature drying oven for drying for 4-6 hours, and grinding for later use;
step 4, heating and diluting the epoxy resin at 60 ℃ for 30min, removing water, adding RTV silicone rubber and a curing agent, then sequentially adding dried glass fiber, nano-zinc oxide and nano-silica, and mechanically and ultrasonically stirring for 10min at the mechanical rotation speed of 200-250 r/min and the ultrasonic frequency of 40kHz under the condition of a water bath at 25-30 ℃ to prepare the glass fiber, nano-zinc oxide and nano-silica co-modified RTV silicone rubber/epoxy resin composite repair coating;
and 5, brushing the composite repairing paint on the surface of the damaged and cracked insulating material, and curing and forming to realize insulation repairing.
Example 6
Step 1, weighing the following components in parts by mass: bisphenol A epoxy resin E-51100 g, RTV silicon rubber 50g, 593 type epoxy curing agent 15g, glass fiber 12.073g, nano zinc oxide 12.073g, nano silicon dioxide 12.073g, absolute ethyl alcohol 56.744g, purified water 1.207g and KH5502.415g;
step 2, adding dried nano zinc oxide into 24.146g of absolute ethyl alcohol, and mechanically and ultrasonically stirring for 20min under the condition of a water bath at the temperature of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; mixing 1.207g KH550 and 0.604g purified water, and adding 4.226g absolute ethanol solution to obtain coupling agent hydrolysate; mixing the coupling agent hydrolysate with the nano zinc oxide solution, and mechanically and ultrasonically stirring for 40min under the condition of water bath at the temperature of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; and finally, placing the coupling agent modified nano zinc oxide solution in a constant-temperature drying oven for drying for 4-6 hours, and grinding for later use.
Step 3, adding dried nano silicon dioxide into 24.146g of absolute ethyl alcohol, and mechanically and ultrasonically stirring for 20min under the condition of a water bath at the temperature of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; mixing 1.207g KH550 and 0.604g purified water, and adding 4.226g absolute ethanol solution to obtain coupling agent hydrolysate; mixing the coupling agent hydrolysate with the nano-silica solution, and mechanically and ultrasonically stirring for 40min under the condition of water bath at the temperature of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; and finally, placing the coupling agent modified nano silicon dioxide solution in a constant-temperature drying oven for drying for 4-6 hours, and grinding for later use.
Step 4, heating and diluting the epoxy resin at 60 ℃ for 30min, removing water, adding RTV silicone rubber and a curing agent, then sequentially adding dried glass fiber, nano-zinc oxide and nano-silica, and mechanically and ultrasonically stirring for 10min at the mechanical rotation speed of 200-250 r/min and the ultrasonic frequency of 40kHz under the condition of a water bath at 25-30 ℃ to prepare the glass fiber, nano-zinc oxide and nano-silica co-modified RTV silicone rubber/epoxy resin composite repair coating;
and 5, brushing the composite repairing paint on the surface of the damaged and cracked insulating material, and curing and forming to realize insulation repairing.
Example 7
Step 1, weighing the following components in parts by mass: bisphenol A type epoxy resin E-51100 g, RTV silicon rubber 50g, 593 type epoxy curing agent 15g, glass fiber 13.750g, nano zinc oxide 13.750g, nano silicon dioxide 13.750g, absolute ethyl alcohol 64.625g, purified water 1.375g and KH5502.75g;
step 2, adding dried nano zinc oxide into 27.500g of absolute ethyl alcohol, and mechanically and ultrasonically stirring for 20min under the condition of a water bath at the temperature of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; mixing 1.375g KH550 and 0.688g purified water, and adding 4.813g anhydrous ethanol solution to obtain coupling agent hydrolysate; mixing the coupling agent hydrolysate with the nano zinc oxide solution, and mechanically and ultrasonically stirring for 40min under the condition of water bath at the temperature of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; and finally, placing the coupling agent modified nano zinc oxide solution in a constant-temperature drying oven for drying for 4-6 hours, and grinding for later use.
Step 3, adding the dried nano silicon dioxide into 27.500g of absolute ethyl alcohol, and mechanically and ultrasonically stirring for 20min under the water bath condition of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; mixing 1.375g KH550 and 0.688g purified water, and adding 4.813g anhydrous ethanol solution to obtain coupling agent hydrolysate; mixing the coupling agent hydrolysate with the nano-silica solution, and mechanically and ultrasonically stirring for 40min under the condition of water bath at the temperature of 25-30 ℃, wherein the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz; and finally, placing the coupling agent modified nano silicon dioxide solution in a constant-temperature drying oven for drying for 4-6 hours, and grinding for later use.
Step 4, heating and diluting the epoxy resin at 60 ℃ for 30min, removing water, adding RTV silicone rubber and a curing agent, then sequentially adding dried glass fiber, nano-zinc oxide and nano-silica, and mechanically and ultrasonically stirring for 10min at the mechanical rotation speed of 200-250 r/min and the ultrasonic frequency of 40kHz under the condition of a water bath at 25-30 ℃ to prepare the glass fiber, nano-zinc oxide and nano-silica co-modified RTV silicone rubber/epoxy resin composite repair coating;
and 5, brushing the composite repairing paint on the surface of the damaged and cracked insulating material, and curing and forming to realize insulation repairing.
The actual operation condition of the repair coating is further simulated by a cold-hot circulation method, and electric performance tests are carried out on samples before and after cold-hot circulation, the comparison shows the characteristics of the high-molecular insulation repair coating, the tests comprise volume resistivity, relative dielectric constant, dielectric loss and alternating-current breakdown field strength, and the test results are shown in attached figures 2-5.
FIG. 2 and FIG. 3 are volume resistivity and relative dielectric constant test curves of a nano modified polymer insulation repair coating sample; after the cold and hot circulation, the volume resistivity of the sample is obviously increased by one order of magnitude and is 10 12 Omega.m; and the relative dielectric constant of the sample is averagely improved by 0.2, which shows that the insulating property of the insulating repair coating is improved.
FIG. 4 and FIG. 5 are dielectric loss and AC breakdown field strength test curves of the nano modified polymer insulation repair coating sample, respectively; after the cold and hot circulation, the dielectric loss tangent value of the repair material is increased, the alternating current breakdown field strength is reduced, and the compressive strength is reduced to a certain extent, but the whole body still meets the requirement of the actual working condition.
The electrical performance test shows that the epoxy resin-based material can effectively repair the insulation damaged part and effectively prolong the service life of equipment while ensuring the excellent insulation performance of the epoxy resin-based material.

Claims (10)

1. The nano modified high polymer insulation repair coating is characterized by comprising the following components in percentage by mass: 50g of RTV silicon rubber, 15g of normal-temperature curing agent, 6.111-13.750 g of glass fiber, 6.111-13.750 g of nano zinc oxide, 6.111-13.750 g of nano silicon dioxide, 1.222-2.750 g of coupling agent, 28.722-64.625 g of absolute ethyl alcohol and 0.611-1.375 g of purified water are added into every 100g of epoxy resin.
2. The nano modified polymer insulation repair coating material as claimed in claim 1, wherein the epoxy resin is bisphenol a type epoxy resin E-51; the normal temperature curing agent is 593 type epoxy curing agent; the coupling agent is gamma-aminopropyl triethoxysilane KH 550; the glass fiber is 100 meshes, and the purity is more than or equal to 99 percent; the particle size of the nano zinc oxide is 50 +/-5 nm, and the purity is more than or equal to 99 percent; the particle size of the nano silicon dioxide is 50 +/-5 nm, and the purity is more than or equal to 99%.
3. The preparation method of the nano modified high-molecular insulation repair coating is characterized by comprising the following steps:
step 1, weighing the following components in parts by mass: adding 50g of RTV silicon rubber, 15g of normal-temperature curing agent, 6.111-13.750 g of glass fiber, 6.111-13.750 g of nano zinc oxide, 6.111-13.750 g of nano silicon dioxide, 1.222-2.750 g of coupling agent, 28.722-64.625 g of absolute ethyl alcohol and 0.611-1.375 g of purified water into 100g of epoxy resin;
step 2, carrying out surface treatment on the nano zinc oxide powder weighed in the step 1;
step 3, carrying out surface treatment on the nano silicon dioxide powder weighed in the step 1;
step 4, placing the nano zinc oxide subjected to the surface treatment in the step 2, the nano silicon dioxide subjected to the surface treatment in the step 3 and the glass fiber weighed in the step 1 into a constant-temperature drying box for drying;
and 5, diluting the epoxy resin weighed in the step 1, adding the RTV silicone rubber and a normal-temperature curing agent, sequentially adding the glass fiber, the nano zinc oxide and the nano silicon dioxide dried in the step 4, and uniformly mixing to obtain the glass fiber, nano zinc oxide and nano silicon dioxide co-modified RTV silicone rubber/epoxy resin composite repair coating.
4. The preparation method of the nano modified polymer insulation repair coating according to claim 3, wherein the step 2 is specifically implemented according to the following steps:
step 2.1, drying the weighed nano zinc oxide;
step 2.2, after the step 2.1, putting the dried nano zinc oxide into absolute ethyl alcohol with the mass 2 times of that of the dried nano zinc oxide, and mechanically and ultrasonically stirring the mixture uniformly under the condition of water bath;
step 2.3, putting a coupling agent with the mass of 0.1 time of that of the nano zinc oxide into a beaker, and adding purified water with the mass of 0.5 time of that of the coupling agent for hydrolysis; adding absolute ethyl alcohol with the mass of 3.5 times of that of the coupling agent to obtain coupling agent hydrolysate;
step 2.4, adding the hydrolysate obtained in the step 2.3 into the nano zinc oxide solution obtained in the step 2.2, and mechanically and ultrasonically stirring the hydrolysate uniformly under the condition of water bath to enable the coupling agent and the nano zinc oxide to fully react; the stirring time is more than or equal to 40min, and the water bath temperature is 25-30 ℃; the mechanical rotating speed is 200-250 r/min; ultrasonic frequency 40 kHz;
and 2.5, placing the coupling agent modified nano zinc oxide solution obtained in the step 2.4 into a constant-temperature drying oven for drying for 4-6 hours, and grinding for later use after drying.
5. The preparation method of the composite repair paint according to claim 4, wherein the temperature of the constant temperature drying oven in the step 2.1 is set to 80 ℃, and the drying time is 4-6 hours.
6. The preparation method of the composite repair coating according to claim 4, wherein in the step 2.2, the stirring time is not less than 20min, the water bath temperature is 25-30 ℃, the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz.
7. The preparation method of the composite repair paint according to claim 3, wherein the step 3 is specifically performed according to the following steps:
step 3.1, drying the weighed nano silicon dioxide;
step 3.2, adding the dried nano silicon dioxide into absolute ethyl alcohol with the mass 2 times of that of the dried nano silicon dioxide, and mechanically and ultrasonically stirring the mixture uniformly under the condition of water bath to completely dissolve the dried nano silicon dioxide;
step 3.3, putting a coupling agent with the mass of 0.1 time of that of the nano silicon dioxide into a beaker, and adding purified water with the mass of 0.5 time of that of the coupling agent to completely hydrolyze the nano silicon dioxide; adding absolute ethyl alcohol with the mass of 3.5 times of that of the coupling agent to obtain coupling agent hydrolysate;
step 3.4, adding the hydrolysate obtained in the step 3.3 into the nano-silica solution obtained in the step 3.2, and mechanically and ultrasonically stirring the hydrolysate uniformly under the condition of water bath to enable the coupling agent and the nano-silica to fully react; the stirring time is more than or equal to 40min, and the water bath temperature is 25-30 ℃; the mechanical rotating speed is 200-250 r/min; ultrasonic frequency 40 kHz;
and 3.5, placing the coupling agent modified nano silicon dioxide solution obtained in the step 3.4 in a constant-temperature drying oven for drying for 4-6 hours, and grinding for later use after drying.
8. The preparation method of the composite repair coating material according to claim 7, wherein in the step 3.1, the temperature of the constant-temperature drying oven is set to 80 ℃, and the drying time is 4-6 hours; and 3.2, the water bath temperature is 25-30 ℃, the stirring time is more than or equal to 20min, the mechanical rotation speed is 200-250 r/min, and the ultrasonic frequency is 40 kHz.
9. The preparation method of the composite repair paint according to claim 3, wherein the temperature of the constant temperature drying oven in the step 4 is set to 60 ℃ and the drying time is 1 hour.
10. The preparation method of the composite repair paint according to claim 3, wherein the step 5 is specifically: heating and diluting the epoxy resin weighed in the step 1 at 60 ℃ for 30min, removing water, adding the RTV silicone rubber weighed in the step 1 and a curing agent, then sequentially adding the glass fiber, the nano zinc oxide and the nano silicon dioxide dried in the step 4, stirring and ultrasonically treating under the water bath condition, and uniformly mixing; the water bath temperature is 25-30 ℃, the mechanical rotation speed is 200-250 r/min, the ultrasonic frequency is 40kHz, and the stirring time is 10 min.
CN202210850801.1A 2022-07-20 2022-07-20 Nano modified high-molecular insulation repair coating and preparation method thereof Pending CN114958152A (en)

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