CN110724434A - Nano SiC/epoxy coating material, preparation method and application thereof - Google Patents
Nano SiC/epoxy coating material, preparation method and application thereof Download PDFInfo
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- CN110724434A CN110724434A CN201910979286.5A CN201910979286A CN110724434A CN 110724434 A CN110724434 A CN 110724434A CN 201910979286 A CN201910979286 A CN 201910979286A CN 110724434 A CN110724434 A CN 110724434A
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- 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
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention provides a nano SiC/epoxy coating material, a preparation method and application thereof, comprising the following steps: step 1: putting the nano SiC into a plasma fluidized bed device for powder treatment, and introducing CF4And Ar, turning on a high-frequency alternating current power supply of the plasma fluidized bed device, setting current and voltage parameters, and treating for a preset time to obtain plasma fluorinated nano SiC; step 2: and stirring and mixing the nano SiC subjected to plasma fluorination treatment with epoxy resin by using a vacuum mechanical stirrer, and then continuously adding a curing agent and an accelerator for stirring and mixing to obtain the nano SiC/epoxy coating material. According to the method, the epoxy composite coating is prepared after plasma fluorination treatment is carried out on the nano SiC, and the insulator is coated, so that the flashover voltage of the insulator can be obviously improved, and the probability of failure of power equipment is reduced.
Description
Technical Field
The invention relates to the technical field of insulating material preparation, in particular to a nano SiC/epoxy coating material, a preparation method and application thereof.
Background
The insulator is widely applied to various power equipment, and mainly has the main function of fixedly supporting a current-carrying conductor so as to form effective insulation between the conductor and the ground. However, as the voltage class of power equipment is continuously increased, the breakdown phenomenon often occurs on the surface of the insulating material rather than inside the insulating material, and the main reason is that the bulk breakdown of the insulating material requires a larger electric field intensity than the planar flashover, so the planar flashover phenomenon becomes a main cause of the failure of the power equipment.
The normal operation of the power equipment is seriously threatened by the flashover along the surface, so that the improvement of the flashover voltage of the insulator in the power equipment has important significance. Compared with the direct modification of insulator materials, the coating does not need to replace the original insulating materials, and the direct coating of the coating on the insulator has the advantages of convenience, economy and easy implementation. The nano filler/epoxy composite coating material has good application prospect, the current treatment methods for the filler comprise a physical grinding method and a coupling agent treatment method, however, the improvement of the electrical property of the coating material along the surface is not large by the surface treatment methods, so that how to carry out surface treatment on the filler becomes very critical.
Disclosure of Invention
The invention provides a nano SiC/epoxy coating material, a preparation method and application thereof, which are used for coating an insulator to improve the surface flashover voltage.
In order to achieve the purpose, the invention adopts the following technical scheme.
The invention provides a preparation method of a nano SiC/epoxy coating material, which comprises the following steps:
step 1: putting the nano SiC into a plasma fluidized bed device for powder treatment, and introducing CF4And Ar, turning on a high-frequency alternating current power supply of the plasma fluidized bed device, setting current and voltage parameters, and treating for a preset time to obtain plasma fluorinated nano SiC;
step 2: and stirring and mixing the nano SiC subjected to plasma fluorination treatment with epoxy resin by using a vacuum mechanical stirrer, and then continuously adding a curing agent and an accelerator for stirring and mixing to obtain the nano SiC/epoxy coating material.
Preferably, the plasma fluidized bed apparatus in step 1 comprises: fluidized bed, high frequency AC power supply and reaction gas;
the center part of the fluidized bed is a metal electrode which is connected with the high-frequency alternating current power supply, a quartz glass sleeve is arranged outside the metal electrode, and the quartz glass sleeve is surrounded by a quartz glass cavity and is not contacted with each other; wrapping a metal film outside the quartz glass cavity, wherein the metal film is connected with the ground; the quartz glass cavity is provided with a gas inlet and a gas outlet, the gas inlet is positioned at the lower part of the quartz glass cavity and is connected with the reaction gas and the gas flow meter for controlling the flow rate of the gas, and the gas outlet is positioned at the upper part of the quartz glass cavity and is used for being connected with the activated carbon block and the vacuum pump.
Preferably, in the step 1, CF is introduced into every 5-8g of nano SiC4At a flow rate of 1slm, said introduction of CF4And Ar flow ratio of 1: 10.
preferably, in the step 1, the current is set to be 10-15 mA, the voltage is 10-15 kV, the air pressure of a cavity of the plasma fluidized bed device is 50-100 Pa, and the preset time is 10-12 min.
Preferably, the mass ratio of the nano SiC to the epoxy resin after the plasma fluorination treatment is (3-8): 100.
Preferably, in the step 2, the mass ratio of the epoxy resin, the curing agent and the accelerator is (50-85) to (1-10) 100.
Preferably, the epoxy resin in the step 2 is an E51 type epoxy resin, the curing agent is methyl tetrahydrophthalic anhydride, and the accelerator is DMP-30.
Preferably, the stirring speed is 1000r/min for 20-30 min of each stirring and mixing in the step 2.
The invention also provides a nano SiC/epoxy coating material which is prepared by the method.
The nano SiC/epoxy coating material obtained by the invention is coated on the insulator in a spraying, dipping and brushing way and is used for coating the insulator.
According to the technical scheme provided by the nano SiC/epoxy coating material, the preparation method and the application thereof, the method can effectively treat the filler by adopting a plasma treatment method of a chemical surface treatment method, is efficient, environment-friendly and convenient, can enable the epoxy composite coating to play a role in accelerating charge dissipation by using a plasma fluidized bed to perform fluorination treatment on the filler, can remarkably improve flashover voltage and reduce the probability of failure of power equipment when being used for coating an insulator after performing plasma fluorination treatment on the nano SiC.
Additional aspects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic structural view of a plasma fluidized bed apparatus used in this embodiment;
FIG. 2 is an XPS test chart of nano SiC before and after plasma fluorination treatment in examples 1, 2 and 3;
fig. 3 is a graph of normalized surface potential decay test for coated and uncoated insulators prepared in examples 1, 2 and 3.
Description of reference numerals:
1-high-frequency alternating current power supply 2-vacuum pump 3-gas outlet 4-metal electrode 5-quartz glass sleeve 6-quartz glass cavity 7-metal film 8-gas inlet 9-gas flowmeter 10-reaction gas 11-activated carbon block
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
As used herein, the singular forms "a", "an", "the" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms "comprises" and/or "comprising," when used in this specification, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof. It should be understood that the term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
It will be understood by those skilled in the art that, unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
For the convenience of understanding the embodiments of the present invention, the following description will be further explained by taking several specific embodiments as examples in conjunction with the drawings, and the embodiments are not to be construed as limiting the embodiments of the present invention.
Example 1
The preparation method of the nano SiC/epoxy coating material comprises the following steps:
step 1: putting 5g of nano SiC into a plasma fluidized bed device for powder treatment, opening a vacuum pump, keeping the air pressure of a cavity at 50-100 pa, and sequentially introducing CF with the gas flow of 1slm4And 10slm of Ar, wherein after a stable fluidized bed is formed in the reaction cavity, a high-frequency alternating current power supply is turned on, the voltage is 10-15 kV, the current is 10-15 mA, and the nano SiC subjected to plasma fluorination treatment is obtained after 10-12 min.
Step 2: adding the nano SiC subjected to plasma fluorination treatment into E51 epoxy resin in an amount which accounts for 3% of the amount of the E51 epoxy resin, and stirring for 20-30 min by using a vacuum mechanical stirrer with the speed of 1000 r/min; and then adding a methyl tetrahydrophthalic anhydride curing agent and a DMP-30 accelerator into the mixture, wherein the mass ratio of the E51 epoxy resin to the methyl tetrahydrophthalic anhydride curing agent to the DMP-30 accelerator is 100: 85: 1; and then mechanically stirring for 20-30 min in vacuum at the speed of 1000r/min to obtain the nano SiC/epoxy coating material.
Fig. 1 is a schematic structural view of a plasma fluidized bed apparatus used in this embodiment, and referring to fig. 1, the plasma fluidized bed apparatus includes three parts, i.e., a fluidized bed, a high-frequency ac power supply 1, and a reaction gas 10.
The center part of the fluidized bed is a metal electrode 4, the metal electrode 4 is connected with a high-frequency alternating current power supply 1, a quartz glass sleeve 5 is arranged outside the electrode, and a quartz glass cavity 6 surrounds the quartz glass sleeve 5 and is not in contact with the quartz glass sleeve 5. And a metal film 7 is wrapped outside the quartz glass cavity 6, and the metal film 7 is connected with the ground. The quartz glass cavity 6 is provided with an air inlet 8 and an air outlet 3, the air inlet 8 is positioned at the lower part of the quartz glass cavity 6 and is connected with a reaction gas 10 and a gas flow meter 9 for controlling the flow rate of the gas, and the air outlet 3 is positioned at the upper part of the quartz glass cavity 6 and is connected with an active carbon block 11 for preventing the powder in the fluidized bed from blowing out and a vacuum pump 2 for carrying out vacuum treatment on the cavity.
Wherein, the high-frequency alternating current power supply 1 is a power supply with adjustable voltage and current, different parameters can be adjusted, the nano SiC material is processed, and the reaction gas 10 is carbon tetrafluoride (CF)4) And argon (Ar) gas flow rate of which can be controlled by a gas flow meter 9 so that CF passing through the hollow quartz glass sleeve 54And Ar gas have different flow rates and ratios to meet production requirements.
The plasma fluidized bed device is operated by the following processes of firstly, placing the nano SiC at the bottom of a quartz glass cavity of a fluidized bed, turning on a vacuum pump, keeping the interior of the cavity at negative pressure or vacuum, and introducing CF (carbon fiber) through an air inlet of the quartz glass cavity4And Ar, the gas flow of the two gases can be adjusted by a gas flowmeter, and after the gas is introduced, the nano SiC is acted by the gas from the bottom to the top to form a stable fluidized bed; and then turning on a high-frequency alternating current power supply, adjusting corresponding parameters, forming stable glow discharge plasma in the quartz glass tube and the quartz glass cavity, and finishing plasma fluorination treatment on the nano SiC filler after a period of treatment.
Example 2
The preparation method of the nano SiC/epoxy coating material comprises the following steps:
step 1: putting 5g of nano SiC into a plasma fluidized bed device, opening a vacuum pump, keeping the air pressure of a cavity at 50-100 pa, and sequentially introducing CF with the gas flow of 1slm4And 10slm of Ar, wherein after a stable fluidized bed is formed in the reaction cavity, a high-frequency alternating current power supply is turned on, the voltage is 10-15 kV, the current is 10-15 mA, and the nano SiC subjected to plasma fluorination treatment is obtained after 10-12 min.
Step 2: adding the nano SiC subjected to plasma fluorination treatment into E51 epoxy resin in an amount accounting for 5% of the E51 epoxy resin, and stirring for 20-30 min by using a vacuum mechanical stirrer with the speed of 1000 r/min; and then adding a methyl tetrahydrophthalic anhydride curing agent and a DMP-30 accelerator into the mixture, wherein the mass ratio of the E51 epoxy resin to the methyl tetrahydrophthalic anhydride curing agent to the DMP-30 accelerator is 100: 85: 1; and then mechanically stirring for 20-30 min in vacuum at the speed of 1000r/min to obtain the nano SiC/epoxy coating material.
Example 3
The preparation method of the nano SiC/epoxy coating material comprises the following steps:
step 1: putting 5g of nano SiC into a plasma fluidized bed device, opening a vacuum pump, keeping the air pressure of a cavity at 50-100 pa, and sequentially introducing CF with the gas flow of 1slm4And 10slm of Ar, wherein after a stable fluidized bed is formed in the reaction cavity, a high-frequency alternating current power supply is turned on, the voltage is 10-15 kV, the current is 10-15 mA, and the nano SiC subjected to plasma fluorination treatment is obtained after 10-12 min.
Step 2: adding the nano SiC subjected to plasma fluorination treatment into E51 epoxy resin in an amount accounting for 8 percent of the amount of the E51 epoxy resin, and stirring for 20-30 min by using a vacuum mechanical stirrer with the speed of 1000 r/min; and then adding a methyl tetrahydrophthalic anhydride curing agent and a DMP-30 accelerator into the mixture, wherein the mass ratio of the E51 epoxy resin to the methyl tetrahydrophthalic anhydride curing agent to the DMP-30 accelerator is 100: 85: 1; and then mechanically stirring for 20-30 min in vacuum at the speed of 1000r/min to obtain the nano SiC/epoxy coating material.
Application example 1
And (3) coating the nano SiC/epoxy coating material obtained in the embodiment 1-3 on an insulator by using a spraying method, setting the air pressure of a spray gun to be 0.1-0.15 Mpa, spraying for 5-10 s at a single point, pre-curing the coated insulator in a drying oven at 100 ℃ for 2-3h, and then curing in the drying oven at 120 ℃ for 2-3h to finally form a coating with the thickness of 0.2-0.4 mm on the surface of the insulator.
In the spraying method, the thickness of the coating can be controlled by controlling the air pressure (0.02-1 Mpa) of the spray gun and the spraying time (2-10 s), and the thicker the air pressure of the spray gun is, the thicker the spraying time is, and the thicker the coating is. The parameters can be controlled in actual production to meet actual requirements. The coated insulator can form a uniform coating on the surface of the insulator after a curing process, and the coating can effectively improve the flashover voltage of the insulator.
The embodiment can also use a dip coating method for coating, specifically:
in the dipping coating method, the viscosity of the coating is controlled by temperature, the insulator is wholly soaked in the coating material, and the insulator is taken out at a certain pulling speed after a period of time, so that the insulator coated with the uncured coating is obtained. The thickness of the coating is influenced by the viscosity (100-300 cp) of the coating and the pulling speed (2-10 cm/s), the coating is thicker when the viscosity of the coating is larger, and the coating is thicker when the pulling speed is larger.
Fig. 2 is an XPS test chart of the SiC nanoparticles before and after the plasma fluorination treatment in examples 1, 2 and 3, and it can be seen from fig. 1 that the F element content of the SiC nanoparticles increases and the O element content decreases after the plasma fluorination treatment. This indicates that: after the nano SiC is subjected to plasma fluorination treatment, the F-containing functional group can be effectively grafted on the surface of the nano SiC.
The coated insulator and the uncoated insulator prepared in examples 1, 2 and 3 were respectively tested by isothermal surface potential attenuation, and the planar portion of the insulator was charged with a pin electrode having a radius of curvature of 5mm and a distance of 10mm from the surface of the insulator under an applied voltage of 7kV for 1 min. After charging is finished, the surface potential of the charged part is tested by using an electrostatic potentiometer, the probe of the electrostatic potentiometer is 5mm away from the surface of the insulator, the testing time is 30mm, and the testing result is shown in fig. 3. as shown in fig. 2, it can be seen that the more the content of plasma fluorinated nano SiC in the coating is, the larger the surface potential attenuation is, and the coating material of which the mass of the plasma fluorinated nano SiC is 8% of that of the epoxy resin is added in the embodiment 3, so that the surface potential attenuation speed of the insulator reaches the maximum value. The potential of the surface of the insulator is positively correlated with the charge density, the faster the surface potential decays indicates the faster the charge dissipation, and the coatings of examples 1, 2 and 3 can accelerate the dissipation of the surface charge of the insulator.
The coated and uncoated insulators prepared in examples 1, 2 and 3 were tested for flashover results along the surface.
The insulator coated with the plasma fluorinated nano SiC/epoxy composite coating in the above example was subjected to a surface flashover test, with fingertip electrodes having a radius of curvature of 1cm and a distance of 10mm, the two electrodes were tightly attached to the surface of the insulator, a negative polarity dc power supply was applied, a voltage step-up rate was 1kV/s, the average value was obtained by repeating each group 10 times, and the measured surface flashover voltage was as shown in table 1 below. As can be seen from Table 1, the flashover voltage of the insulator sample coated with the plasma fluorinated nano SiC/epoxy composite coating prepared in each example is higher than that of the sample without the coating, and the coating and the preparation process thereof can effectively improve the flashover voltage of the insulator.
TABLE 1
| Sample (I) | Flashover Voltage (kV) |
| Without coating | 8.26 |
| Example 1 | 9.13 |
| Example 2 | 9.25 |
| Example 3 | 9.85 |
It will be appreciated by those skilled in the art that the foregoing types of applications are merely exemplary, and that other types of applications, whether presently existing or later to be developed, that may be suitable for use with the embodiments of the present invention, are also intended to be encompassed within the scope of the present invention and are hereby incorporated by reference.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A preparation method of a nano SiC/epoxy coating material is characterized by comprising the following steps:
step 1: putting the nano SiC into a plasma fluidized bed device for powder treatment, and introducing CF4And Ar, turning on a high-frequency alternating current power supply of the plasma fluidized bed device, setting current and voltage parameters, and treating for a preset time to obtain plasma fluorinated nano SiC;
step 2: and stirring and mixing the nano SiC subjected to plasma fluorination treatment with epoxy resin by using a vacuum mechanical stirrer, and then continuously adding a curing agent and an accelerator for stirring and mixing to obtain the nano SiC/epoxy coating material.
2. The method of claim 1, wherein the plasma fluidized bed apparatus of step 1 comprises: fluidized bed, high frequency AC power supply and reaction gas;
the center part of the fluidized bed is a metal electrode which is connected with the high-frequency alternating current power supply, a quartz glass sleeve is arranged outside the metal electrode, and the quartz glass sleeve is surrounded by a quartz glass cavity and is not contacted with each other; wrapping a metal film outside the quartz glass cavity, wherein the metal film is connected with the ground; the quartz glass cavity is provided with a gas inlet and a gas outlet, the gas inlet is positioned at the lower part of the quartz glass cavity and is connected with the reaction gas and the gas flow meter for controlling the flow rate of the gas, and the gas outlet is positioned at the upper part of the quartz glass cavity and is used for being connected with the activated carbon block and the vacuum pump.
3. The method according to claim 1, wherein in the step 1, CF is introduced into every 5-8g of nano SiC4Has a flow rate of 1slm, soIntroduction of CF4And Ar flow ratio of 1: 10.
4. the method according to claim 1, wherein the current is set to 10 to 15mA, the voltage is set to 10 to 15kV, the chamber gas pressure of the plasma fluidized bed device is 50 to 100Pa, and the predetermined time is 10 to 12min in the step 1.
5. The method according to claim 1, wherein the mass ratio of the nano SiC to the epoxy resin after the plasma fluorination treatment is (3-8): 100.
6. The method as claimed in claim 1, wherein in the step 2, the mass ratio of the epoxy resin, the curing agent and the accelerator is 100 (50-85) to (1-10).
7. The method of claim 1, wherein the epoxy resin in step 2 is an epoxy resin E51, the curing agent is methyl tetrahydrophthalic anhydride, and the accelerator is DMP-30.
8. The method according to claim 1, wherein the stirring speed in step 2 is 1000r/min for 20-30 min per stirring and mixing.
9. A nano SiC/epoxy coating material, wherein the material is prepared by the method of any one of claims 1 to 8.
10. The nano SiC/epoxy coating material as claimed in claim 9, wherein the material is applied to an insulator by spraying, dipping or brushing, and is used for coating the insulator.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112358806A (en) * | 2021-01-12 | 2021-02-12 | 广东大自然家居科技研究有限公司 | Modified coating for ceramic tile-like wood floor and preparation method thereof |
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