KR20120101241A - Epoxy-microsilica-organically modified nano layered silicate mixed composite for insulation using electric field and product thereby - Google Patents

Abstract

PURPOSE: A manufacturing method of an epoxy-micro-silica-organically modified nano interlayered silicate-mixed composite is provided to able to provide a mixed composite with improved thermal properties, mechanical properties and electrical properties. CONSTITUTION: A manufacturing method of an epoxy-microsilica-organically modified nano interlayered silicate-mixed composite comprises: a step of pre-treated a liquid epoxy resin and an organically modified nano interlayered silicate; a step of a electric field-dispersion treatment of the pre-pretreated liquid epoxy resin and an organically modified nano interlayered silicate-mixed composte; a step of mixing epoxy-micro silica-nano interlayered silicate-mixed liquid composite mixture and a hardener-silica mixture, which are respectively obtained by injecting micro silica to each of the liquid composite and a hardener; a step of adding additives to the product; a step of vacuum deairation by injecting the product into a heated mold; a step of hardening the vacuum de-aerated product.

Description

FIELD OF THE INVENTION Epoxy-microsilica-organically modified nano layered silicate mixed composite for insulation using electric field and product according to the method of preparing an epoxy-micro silica-nano organic layered silicate mixed composite for insulation using electric field dispersion

The present invention relates to an epoxy-micro silica-nano organic layered silicate mixed composite, in particular fully dispersed (peeled) the organicized layered silicate nanonized in a liquid epoxy resin, and completely peeled and nanonized organic layered silicate between the micro silica particles. The present invention relates to an epoxy-microsilica-nano organic layered silicate composite composite for insulation using a homogeneously dispersed electric field dispersion and a composite composite prepared therefrom.

Epoxy resins are well known in the field of heavy electric insulation systems. That is, they are used in mold-type transformers, current transformers (CT), potential transformers (PT), metering out-fit (MOF), gas switching gears, insulation spacers, and the like. This is because the electrical, mechanical and thermal properties are excellent.

Over the past decades, many researchers have developed low cost, high reliability epoxy based nanocomposites for electrical applications, and through many fillings of micro silica, dimensional stability and thermal and mechanical improvements have been achieved. In particular, the filling of 65-80 wt% microparticles into the epoxy resin has been filled into the epoxy resin to satisfy the dimensional stability of the high voltage heavy electric machine operated continuously for 40 to 60 ℃.

However, the different components of the organic and inorganic components in the epoxy based mixed composite are not related to each other. The reason is that the micro silica is hydrophilic because it has an OH group on its surface, and the epoxy resin is lipophilic because it is a component extracted from oil. In order to increase the binding of the organic component and the inorganic component, the silane coupling agent, which is an organic / inorganic binder, is treated.

In addition, in the high voltage heavy electric machine, since a metallic material is impregnated into the insulator in the epoxy resin which is an insulator, the heavy electric machine such as a transformer continuously generates electric current by flowing current to the conductor in the insulator, and thus the thermal expansion coefficient of the metallic conductor. When the thermal expansion coefficients of the and insulators have a large difference from each other, microcracks occur at the interface between the metal and the insulator.

When micro cracks are generated in this way, the interface portion becomes a cause of a defect and acts as a discharge source, thereby initiating partial discharge. This constant overload (continuous current supply) results in a breakdown of the heavy electrical insulation. In order to prevent such micro cracks, that is, the filling capacity of the micro silica is maximized and filled by a process of reducing the thermal expansion coefficient of the metal and the thermal expansion coefficient of the insulator to a minimum.

However, the higher the filling content, the wider the interface between the micro silica and the epoxy resin becomes, which causes more interfacial defects. In order to overcome this interface defect, nanoscale silica and / or exfoliated nanoparticles such as organic layered silicates are used. However, when the nanoparticles alone are not used, the thermal expansion coefficient cannot be matched, thereby overcoming this by mixing micro-sized silica particles and nanonized organic layered silicates.

However, it is quite difficult to disperse (peel) the nanonized organic layered silicate completely into the epoxy resin. Therefore, when the organic layered silicate is present in the epoxy resin that is not completely peeled, that is, in an aggregated state, the very part serves as a weak point, resulting in deterioration of the insulating property.

SUMMARY OF THE INVENTION In view of the above-mentioned problems, an object of the present invention is to mix microsilica in a completely peeled and nanonized state of an organic layered silicate, so that the fully peeled and nanonized organic layered silicate penetrates between micro silica particles to have a dense structure. Provided is a method for preparing an epoxy-micro silica-nano organicated layered silicate mixed composite for insulation using electric field dispersion in which the organic layered silicate nanoparticles are homogeneously dispersed (peeled) between the micro silica particles by using a dispersion, and a composite composite prepared therefrom. Is in.

The object of the present invention described above is a first step of preheating the liquid epoxy resin at 80 ° C. for 1 to 5 hours to lower the viscosity; A second step of preheating the nano-organized layered silicate at 100 ° C. for 24 hours to completely remove moisture contained in the nano-organized layered silicate; The preheated liquid epoxy resin of the first stage and the nano-organized layered silicate from which the second stage of water was removed are subjected to a power ultrasonic wave, a homogenizer, and a mechanical stirrer for 30 to 60 minutes. The ultrasonic wave conditioner of the powerful ultrasonic wave disperser is a condition of resonance frequency 20khz, amplitude 60 ~ 68%, output 750 ~ 1500W intensity, homogenizer condition 10000rpm, mechanical stirrer 2000 ~ 3000rpm An epoxy-nano organic layered silicate pretreatment step consisting of a third step of stirring; The mixed and pretreated epoxy-nano organic layered silicate liquid composite of the third step is introduced into an alternating current electric field dispersion chamber, and the cation of the nano-organized layered silicate is vibrated between layers of the nano-organized layered silicate by an alternating electric field to expand the interlayer distance. Dispersing the epoxy resin into the expanded interlayer of the nano-organized layered silicate to allow insertion and exfoliation; Injecting micro silica having an average particle diameter of 3 to 20 μm into the liquid composite and the curing agent of the epoxy-nano organic layered silicate treated with the electric field dispersion of the fourth step, respectively, and agitated under a condition of 2000 to 4500 rpm for 30 to 60 minutes in a mechanical stirrer. A fifth step of mixing the epoxy-micro silica-nano organic layered silicate liquid composite mixture and the hardener-micro silica mixture and mixing and defoaming the mixture for 10-20 minutes for stirring and defoaming; A sixth step of defoaming the second mixed and degassed epoxy-micro silica-nano organic layered silicate liquid composite by adding an antifoaming agent and a dispersing agent to facilitate bubble removal and dispersion; By adding a curing accelerator to the sixth step of the primary mixing and secondary degassed epoxy-micro silica-nano organic layered silicate liquid composite, the secondary mixing for stirring and defoaming with a mechanical stirrer to evenly distribute the added curing accelerator. And a seventh step of defoaming thirdly; Epoxy injected after the curing, curing accelerator, antifoaming agent, and dispersing agent were mixed, and the secondary mixed and tertiary degassed seventh stage epoxy-micro silica-nano organic layered silicate liquid composite was injected into a mold preheated to 80 ° C. An eighth step of performing a vacuum defoaming process for 30 to 60 minutes in a vacuum oven (1 torr) to remove the final bubble of the micro silica-nano organic layered silicate liquid composite; In order to mold the vacuum degassed epoxy-micro silica-nano organic layered silicate liquid composite of the eighth step, the first curing was performed at 120 ° C. for 2 hours in a high temperature oven, followed by the second curing at 150 ° C. for 24 hours. It is achieved by an epoxy-micro silica-nano organic layered silicate mixed composite manufacturing method using an electric field dispersion comprising a ninth step prepared by the step of epoxy-micro silica-nano organic layered silicate.

In the manufacturing method of the epoxy-micro silica-nano organic layered silicate mixed composite for insulation using the electric field dispersion of the present invention, 39.7% by weight of epoxy resin, 60% by weight of micro silica, 0.3% by weight of nano-organized layered silicate or 34.7% by weight of epoxy resin %, 65% by weight of micro silica, and 0.3% by weight of nano-organized layered silicate.

In the method for producing an epoxy-micro silica-nano organic layered silicate mixed composite for insulation using the electric field dispersion of the present invention, the AC field dispersion chamber is provided with a pair of opposed +/- parallel flat electrodes for applying an AC electric field. , AC electric field application conditions are characterized in that the applied voltage 3 ~ 11㎸, the applied frequency 1000㎐, the application time 60 minutes or less.

The thermal properties (glass transition) as the organicized layered silicate nano-organized in the liquid epoxy resin is completely dispersed (peeled) by the above-described technical configuration of the present invention, as well as completely peeled and nano-organized layered silicate is uniformly dispersed between the micro silica particles. Temperature), mechanical properties (DMA Tanδ, tensile strength, flexural strength), and electrical properties (insulation breakdown strength) are improved.

Figure 1 (A) is the third step of the electric field undispersed epoxy-nano organic layered silicate mixed composite of the manufacturing step of the present invention, (B) is the fourth step of the electric field dispersed epoxy-nano organic layered silicate mixed composite This is a transmission electron microscope (TEM) photograph comparing (A) and (B).
Figure 2 is a micro-silica of the fifth step of the manufacturing step of the present invention, the epoxy resin is 34.7% by weight, the micro-silica is 65% by weight, the nano-organic layered silicate prepared by the composition ratio of the epoxy-micro silica 0.3% by weight A transmission electron microscope (TEM) image of a nano-organized layered silicate mixed composite.

The present invention adds a certain amount of micro silica (average particle size 3-20 μm) to an epoxy-nano organic layered silicate liquid composite in which the organic layered silicate nano-dispersed in the liquid epoxy resin is completely dispersed (peeled) by electric field dispersion. The purpose of the present invention is to improve the insulation properties by mixing the micro silica and the exfoliated organic layered silicate under the epoxy resin so that the homogeneous dispersion of the nano organic layered silicate nanoparticles is carried out between the micro silica particles.

Hereinafter, the present invention will be described with reference to Examples.

However, embodiments according to the present invention may be modified in many different forms, and the scope of the present invention should not be construed as limited to the embodiments described below. Embodiments of the present invention are provided to more fully explain the present invention to those skilled in the art.

Epoxy resin of the present invention is a universal basic resin of EEW (g / eq) of 184-190, Viscosity of 11,500-13,500 (cps at 25 ℃), Specific Gravity of 1.17 (at 20 ℃) Diglycidyl ether of bisphenol-A (YD-128 (Kukdo Chem. Co., Korea)).

이고, HT는 hydrogenated tallow(~65% C18; ~30% C16; ~5% C14)이며, 음이온(anion)은 cholride이다. The nano-organized layered silicate uses the trade name Closite®10A, commercially available from Southern Clay Products Inc., USA, which is a natural montmorillonite modified with a + 4-valent ammonium salt.

HT is hydrogenated tallow (˜65% C18; ˜30% C16; ˜5% C14), and the anion is cholride.

Curing agents include cycloaliphatic anhydride hardeners (HN), which are widely used in the application of electrical insulation parts (capacitors, resisters, magnetic colis, transformers, current transformers, bushings, epoxy resin insulators, wiring parts, motor armatures and stators). -2200 (molecular formula: C ₉ H ₁₀ O ₃ , MW: 166, Hitachi Co. Ltd) was used, since the void casting or impregnation had no loss of curing agent at relatively high temperatures. Used in mold products without void).

As the accelerator (Epoxy Resin Accelerator) as the accelerator to connect the end of the epoxy group by the action, BDMA (Benzyl dimethylamine; molecular formula C ₉ H ₁₃ N, molecular weight 135.2, specific gravity 0.92) was used. It is used in combination with acid anhydride-based curing agents, and is generally used to reduce curing temperature and time. Applications are also used for epoxy potting, casting and acid anhydride-based adhesives.

The present invention is a mixture of the liquid epoxy resin and the nano-organic layered silicate by stirring, the pre-treatment step of the epoxy-nano organic layered silicate to perform homogenization and ultrasonic dispersion at the same time with stirring and mixing, and the pre-treated epoxy-nano organic layered silicate liquid composite Epoxy-micro silica-nano organic layered silicate mixed composite for dispersing followed by mixing micro silica was prepared by the main treatment step.

Epoxy-nano organic layered silicate pretreatment step of the present invention,

(1) a first step of preheating the liquid epoxy resin at 80 ° C. for 1 to 5 hours to lower the viscosity;

(2) a second step of preheating the nanoorganization layered silicate at 100 ° C. for 24 hours to completely remove moisture contained in the nanoorganization layered silicate;

(3) 30 minutes to 60 minutes of the preheated liquid epoxy resin of the first step and the nano-organized layered silicate from which the water was removed, the power ultrasonic wave, the homogenizer, and the mechanical Stirring with a combination of mechanical agitator, but the ultrasonic excitation condition of the powerful ultrasonic disperser is the condition of the resonance frequency 20khz, amplitude 60 ~ 68%, output 750 ~ 1500W intensity, homogenizer 10000rpm, mechanical agitator 2000 It consists of a third step of stirring with a condition of ~ 3000rpm.

The third stage of the power ultrasonic wave, the homogenizer, and the mechanical stirrer is installed in one chamber so that the three apparatuses are operated at the same time. The organic layered silicate from which the epoxy resin and the water of the second step are removed is stirred while ultrasonically excited.

The epoxy-micro silica-nano organic layered silicate main treatment step of the present invention,

(4) Injecting the mixed and pretreated epoxy-nano organic layered silicate liquid composite of the third step into the alternating current electric field dispersion chamber, the cations of the nano-organized organic layered silicate vibrate between the layers of the nano-organized organic layered silicate by the alternating current electric field. A fourth step of dispersing the epoxy resin so that the epoxy resin is inserted and peeled into the expanded interlayers of the nanoorganization layered silicates;

(5) Injecting micro silica having an average particle diameter of 3 to 20 µm into the liquid composite and the curing agent of the epoxy-nano organic layered silicate treated in the fourth step, respectively, at 2000 to 4500 rpm for 30 to 60 minutes in a mechanical stirrer. A fifth step of mixing and defoaming the mixture of the epoxy-micro silica-nano organic layered silicate liquid composite mixture and the curing agent-micro silica mixture stirred for 10-20 minutes for stirring and defoaming again. Steps;

(6) a sixth defoaming after adding the antifoaming agent and the dispersant to the first mixed and degassed epoxy-micro silica-nano organic layered silicate liquid composite of the fifth step to facilitate bubble removal and dispersion. Steps;

(7) adding a curing accelerator to the first mixed and secondary degassed epoxy-micro silica-nano organic layered silicate liquid composite of the sixth step to agitate and remove bubbles with a mechanical stirrer to distribute the added curing accelerator evenly. A seventh step of secondary mixing and tertiary defoaming;

(8) After the curing agent, the curing accelerator, the antifoaming agent, and the dispersing agent were mixed and the secondary mixed and tertiary degassed seventh stage epoxy-micro silica-nano organic layered silicate liquid composite was injected into a mold preheated to 80 ° C. An eighth step of performing a vacuum defoaming process for 30 to 60 minutes in a vacuum oven (1 torr) to remove final bubbles of the injected epoxy-micro silica-nano organic layered silicate liquid composite;

(9) In order to mold the vacuum degassed epoxy-micro silica-nano organic layered silicate liquid composite of the eighth step, the first curing was performed at 120 ° C. for 2 hours in a high temperature oven, and then again at 150 ° C. for 24 hours. It consists of a ninth step of manufacturing by performing a secondary hardening.

The content of the epoxy resin, micro silica, and nano-organic layered silicate of the present invention prepared by the above-described method of the first to ninth step is 39.7% by weight of epoxy resin, 60% by weight of micro silica, nano-organized layered silicate It is preferable that it is 0.3 weight% or 34.7 weight% of an epoxy resin, 65 weight% of micro silicas, and 0.3 weight% of nano organic layered silicates.

The electric field dispersion of the present invention described above is an electrophoretic method in which positively charged ions (+ ions) move toward the cathode electrode (-electrode) and negatively charged ions (−ions) move to the anode in an alternating electric field. According to (Electrophoresis; one of the assays such as proteins), the + tetravalent ammonium cation of the organic organic layered silicate, which is an organic modifier having a structure similar to the amino group of a protein, reacts in an alternating electric field.

Therefore, when an alternating electric field is applied, the +4 ammonium cation of the nano-organized layered silicate reacts with the alternating voltage of the interorganization layer of the nano-organized layered silicate and collides with the sidewall of the nano-organized layered silicate, thereby expanding the interlayer of the nano-organized layered silicate. Since the interlayer distance increases, the epoxy resin can easily penetrate between the layers.

According to the present invention, the change of interlayer expansion of nano-organized layered silicate according to the applied time, applied voltage, and applied frequency of alternating electric field, and the dispersion of epoxy resin into the expanded layer of nano-organized layered silicate (inserted) And peeling) were measured.

The AC field dispersion measuring device includes a high voltage generator; An alternating electric field dispersion chamber in which a pair of opposed +/- flat electrodes to which a high voltage is applied by the high voltage generator and a liquid composite is installed between the flat electrodes; And a control program for driving the high voltage generator to control an application time, an applied voltage, and an applied frequency of an AC electric field in a liquid composite, and a hopping current for moving between layers according to the time, voltage, and frequency applied according to the control program. A computer equipped with a monitor for displaying a graph showing how is changed; It includes a transmission electron microscope (TEM) that photographs the dispersion (insertion and exfoliation) of the epoxy resin in the interlaminar expansion and interlayer of the nano-organized layered silicate of the liquid composite according to the alternating electric field.

The above-mentioned AC electric field application condition is preferably an applied voltage of 3 to 11 kHz, an applied frequency of 1000 kHz, and an application time of 30 to 60 minutes.

In the case of alternating electric field applied voltage, the electric field strength (75V / mm) below 3kV can be seen to decrease with time rather than to increase due to the extremely weak current flow, which is between nano organic layered silicate layers. The cations (+ tetravalent ammonium cations) of the intercalated nano-organic layered silicates collide at regular intervals toward the nano-organized layered silicate sidewalls between the layers, and the collision energy is weak, resulting in no significant effect on the dispersion of intercalation and exfoliation. . Therefore, if the applied voltage is continuously increased, the collision energy of the cation of the nano-organic layered silicate is increased and the interlayer distance is increased, so that the dispersion can be made better, but if a high voltage of 11kV or more is applied, the risk may increase and an accident may occur Therefore, 11 kV or less is preferable.

In the case of the alternating electric field applied frequency, when the frequency is low, the vibration of the cations of the nano-organized layered silicate is slowed down, so that the cation of the nano-organized layered silicate is weak in the collision effect to the nano-organized layered silicate wall, so that the interlayer of the nano-organized layered silicate is not expanded. If the frequency is too high, the collision effect is enhanced to increase the interlayer expansion of the nano-organized layered silicate, but the cations of the nano-organized layered silicate in the inter-layer space of the nano-organized layered silicate become extremely fast, thus avoiding collisions. 1000 Hz is most preferable because only vibration makes it difficult to collide the layers, resulting in weak peeling.

In the case of alternating electric field application time, if the application time is applied for too long, not only the temperature rises sharply but also the hopping current increases as the application time increases, and it saturates at 60 minutes, so the distance between layers does not grow any longer. Even if it is further applied, 60 minutes or less is preferable because the distance between layers is the same, so that the dispersion does not increase any more.

Therefore, it can be seen that the conditions for applying the AC electric field are preferably 3 to 11 kW, an applied frequency of 1000 kW, and an application time of 60 minutes or less.

Figure 1 (A) is the third step of the electric field undispersed epoxy-nano organic layered silicate mixed composite of the manufacturing step of the present invention, (B) is the fourth step of the electric field dispersed epoxy-nano organic layered silicate mixed composite This is a transmission electron microscope (TEM) photograph comparing (A) and (B).

In the case of (A), the dark black lines represent the nano-organized layered silicate monolayer, and the interlayer expansion of the nano-organized layered silicate is not performed well, so that the dispersion of the epoxy resin does not occur easily between the layers of the nano-organized layered silicate, resulting in 3.2 nm. It can be seen that the dark black lines with d-spacing are arranged in an orderly and orderly fashion.

(B) is a transmission electron microscope (TEM) photograph of the present invention prepared by applying a frequency of 1000 kHz and a voltage of 11 kV. Unlike (A), nano-organized layered silicates are randomly completely dispersed (peeled off) in a liquid epoxy resin. ) Is showing.

Figure 2 is a micro-silica of the fifth step of the manufacturing step of the present invention, the epoxy resin is 34.7% by weight, the micro-silica is 65% by weight, the nano-organic layered silicate prepared by the composition ratio of the epoxy-micro silica 0.3% by weight A transmission electron microscope (TEM) image of a nano-organized layered silicate mixed composite.

In the first TEM photograph, the micro silica is homogeneously dispersed in the epoxy resin, but the nanonized organic layered silicates are not visible because they are too small in size.

Thus, in the enlarged second TEM picture of the first TEM picture, the inside of the circular area indicated by dots is enlarged and represented by (I) to (IV). Shown by the circular dots are nanonized organic layered silicates, which nanonized organic layered silicates are evenly placed between the micro silica particles. Nanonized organic layered silicates are too faint to the naked eye and too difficult to identify.

The reason is that focusing on the micro silica particles will fade the organic layered silicates of the nanoparticles, while focusing on the nanoparticles' organic layered silicates will only show a fraction of the micro silica particles, so the nano-organized layered silicates in the fully peeled state will be Existing images are shown as third TEM photographs (I), (II), (III) and (IV).

1. Thermal Characteristics (Glass Transition Temperature (Tg))

Glass transition temperature (Tg) (℃) Storage modulus (E ') (J / cm 3) Crosslinking density (mol / cm3) Circular epoxy 133.6 116 10.3 × 10 ^-3 EMC-60 133.8 143 12.7 × 10 ^-3 EMC-65 137.0 201 17.7 × 10 ^-3 EMNC-60-0.3 134.0 179 15.9 × 10 ^-3 EMNC-65-0.3 136.7 221 19.5 × 10 ^-3

According to Table 1, the glass transition temperature of the circular epoxy resin was 133.6 ° C. and 60 wt% of micro silica was added to the epoxy-micro composite (EMC) as a result of DSC (Differential Scanning Calorimeter) (model MDSC 2910, TA Instrument). Glass transition temperature of -60) is 133.8 ° C., and glass transition temperature of epoxy-micro composite (EMC-65) to which 65% by weight of micro silica is added is 137.0 ° C., 60% by weight of micro silica and fully peeled and nanonized organic silicate silicate. The glass transition temperature of the epoxy-micro silica-nano organic layered silicate mixed composite (EMNC-60-0.3) of the present invention to which 0.3 wt% was added was 134.0 ° C., 65 wt% of micro silica and 0.3% of the fully peeled and nanonized organic layered silicate 0.3 The glass transition temperature of the epoxy-micro silica-nano organic layered silicate mixed composite (EMNC-65-0.3) of the present invention to which the weight percent was added was 136.7 ° C. Results showed a.

The relationship between the measurement result of glass transition temperature and the crosslink density is closely related. The crosslink density was obtained from the formula ρ = E '/ 3RT. Where ρ is the crosslink density expressed in mol / cm 3, T is the absolute temperature (273.15K), E (J / cm 3) 'is the storage modulus of the epoxy resin at the absolute temperature T = Tg + 45 ° C. , R is the universal gas constant (8.314472 JK ^-1 mol ^-1 ). As the crosslinking density increases, the glass transition temperature also increases, and as the crosslinking density decreases, the glass transition temperature decreases, indicating that the crosslinking density affects the glass transition temperature.

The crosslinking density of the circular epoxy resin is 10.3 × 10 ⁻³ mol / cm 3, the glass transition temperature is 133.6 ° C., and the crosslinking density of the epoxy-micro composite (EMC-60) to which 60% by weight of micro silica is added is 12.7 × 10 ^−3. mol / cm 3, glass transition temperature is 133.8 ℃, crosslink density of epoxy-micro composite (EMC-65) added with 65% by weight of micro silica is 17.7 × 10 ^-3 mol / cm 3, glass transition temperature is 137.0 ℃, micro silica The crosslinking density of the inventive epoxy-micro silica-nano organic layered silicate mixed composite (EMNC-60-0.3) with 60% by weight and 0.3% by weight of fully peeled and nanonized organic layered silicate was 15.9 × 10 ^-3 mol / Cm 3, glass transition temperature is 134.0 ° C., 65% by weight of micro silica and 0.3% by weight of fully peeled and nanonized organic layered silicate, the present epoxy-micro silica-nano organic layered silicate mixed composite (EMNC-65-0.3) Of autumn Density is 19.5 × 10 ^-3 mol / ㎤, the glass transition temperature exhibited 136.7 ℃.

As described above, the crosslinking density of the epoxy-microcomposite added with 60% by weight of micro silica and 65% by weight increased from 12.7 × 10 ^-3 mol / cm 3 to 17.7 × 10 ^-3 mol / cm 3, and the micro silica Comparing the crosslinking density of the epoxy-micro silica-nano-organized layered silicate mixed composite of the present invention to which 60% by weight and 65% by weight and 0.3% by weight of fully peeled and nanonized organic layered silicate were added, 15.9 × 10 ^-3 mol / cm 3 Increased to 19.5 × 10 ⁻³ mol / cm 3 at.

Accordingly, it can be seen that the crosslinking density increases as the micro silica content increases.

And the epoxy-micro silica-nano organic layered silicate mixture of the present invention to which the crosslinking density of the epoxy-microcomposite added with 60% by weight of micro silica and 60% by weight of micro silica and 0.3% by weight of fully peeled and nanonized organic layered silicate were added. The crosslinking density of the composites was increased from 12.7 × 10 ^-3 mol / cm 3 to 15.9 × 10 ^-3 mol / cm 3, and the crosslinking density of the epoxy-micro composite with 65% by weight of micro silica and 65% by weight of micro silica Comparing the crosslinking density of the epoxy-micro silica-nano organic layered silicate mixed composite of the present invention to which 0.3 wt% of fully peeled and nanonized organic layered silicate was added, it was 19.5 × 10 ^-3 mol / cm at 17.7 × 10 ^-3 mol / cm 3. Increased to cm 3.

Accordingly, it can be seen that the crosslinking density is further increased by 0.3 wt% of the nano-organized layered silicate completely peeled off.

2. Mechanical properties (Tanδ (Delta), flexural strength, tensile strength of DMA)

(1) Tanδ (Delta) characteristics of DMA

The change in storage modulus according to the glass transition temperature of the thermal properties is shown in Table 1 above, and the storage modulus of the circular epoxy resin at T = Tg + 45 ° C. in the rubber state region is 116 ( J / cm 3), and the storage elastic modulus of the epoxy-micro composite (EMC-60) added with 60% by weight of micro silica is 143 (J / cm 3) and the epoxy-micro composite (EMC- added with 65% by weight of micro silica). The storage modulus of 65) is 201 (J / cm 3), and the epoxy-micro silica-nano organic layered silicate mixed composite (EMNC) of the present invention added with 60% by weight of micro silica and 0.3% by weight of fully peeled and nanonized organic layered silicate. -60-0.3) has a storage modulus of 179 (J / cm 3), and the epoxy-micro silica-nano organication of the present invention added 65% by weight of micro silica and 0.3% by weight of fully peeled and nanonized organic layered silicate. The storage modulus of the layered silicate mixed composite (EMNC-65-0.3) was found to be 221 (J / cm 3).

As described above, the storage modulus of the epoxy-micro composites to which 60% by weight of micro silica and 65% by weight was added was increased from 143 (J / cm 3) to 201 (J / cm 3), and 60% by weight of micro silica Comparing the storage modulus of the epoxy-micro silica-nano organic layered silicate mixed composite of the present invention to which 65% by weight and 0.3% by weight of fully peeled and nanonized organic layered silicate were added, the storage modulus of 221 (J / cm 3) was measured at 179 (J / cm 3). Increased to).

Accordingly, it can be seen that the storage modulus increases as the micro silica content increases.

And the epoxy-micro silica- of the present invention to which the storage modulus of the epoxy-micro composite (EMC-60) added with 60% by weight of micro silica and 60% by weight of micro silica and 0.3% by weight of fully peeled and nanonized organic layered silicate were added. Comparison of the storage modulus of the nano-organic layered silicate mixed composite (EMNC-60-0.3) increased from 143 (J / cm 3) to 179 (J / cm 3), and epoxy-micro composite (EMC) with 65% by weight of micro silica added. -65) storage of the present invention epoxy-micro silica-nano organic layered silicate mixed composite (EMNC-65-0.3) added 65% by weight of micro silica and 0.3% by weight of fully peeled and nanonized organic layered silicate In comparison, the modulus increased from 201 (J / cm 3) to 221 (J / cm 3).

Accordingly, it can be seen that the storage modulus is further increased by 0.3 wt% of the nano-organized layered silicate completely peeled off.

(2) flexural strength characteristics

Circular epoxy resin, epoxy-micro composite (EMC-60) added with 60% by weight of micro silica, epoxy-micro composite (EMC-65) with added 60% by weight of micro silica, 60% by weight of micro silica and Epoxy-micro silica-nano organic layered silicate mixed composite (EMNC-60-0.3) of the present invention to which 0.3% by weight of fully peeled and nanonized organic layered silicate is added, and 65% by weight of micro silica and fully peeled and nanonized organic layered Flexural strength for the epoxy-micro silica-nano organic layered silicate mixed composite (EMNC-65-0.3) of 0.3% by weight of silicate added according to Weibull Plot is as follows.

Scale parameter (Mpa) Shape parameters Fracture Probability (B10) (Mpa) Circular epoxy 107.6 65.1 78.2 EMC-60 157.8 24.4 92.4 EMC-65 171.2 31.7 38.1 EMNC-60-0.3 162.7 55.9 98.1 EMNC-65-0.3 176.9 65.0 102.2

According to Table 2, the shape parameter is 65.1 epoxy resin with a circular epoxy resin, 24.4 weight percent epoxy-micro composite (EMC-60) added with 60 wt% micro silica, and 65 weight% micro silica added with epoxy-. Epoxy-micro silica-nano organic layered silicate mixed composite (EMNC-60-) with 31.7 microcomposites (EMC-65) and 60% by weight of micro silica and 0.3% by weight of fully peeled and nanonized organic layered silicates added 0.3) is 55.9, and the epoxy-micro silica-nano organicated layered silicate mixed composite (EMNC-65-0.3) of 65% by weight of micro silica and 0.3% by weight of fully exfoliated and nanonized organic layered silicate is added to 65.0. The result was

As described above, the shape parameters of the epoxy-microcomposite added with 60% by weight of micro silica and 65% by weight increased from 24.4 to 31.7, with 60% by weight of micro silica and 65% by weight and fully peeled and nanonized organicization. Comparing the shape parameters of the epoxy-micro silica-nano organic layered silicate mixed composite of the present invention to which 0.3 wt% of the layered silicate was added, it increased from 55.9 to 65.0. If the shape parameter is large, the inclination of the fitted line means the characteristics of homogeneity. The larger the slope of the fitted line is, the more homogeneous the dielectric breakdown strength is.

Accordingly, the shape parameter increases as the content of the micro silica increases, so that the fitted line of the present invention exhibits more homogeneous characteristics than the epoxy-micro composite.

And the epoxy-micro silica- of the present invention to which the shape parameter of the epoxy-micro composite (EMC-60) to which 60% by weight of micro silica is added, and 60% by weight of micro silica and 0.3% by weight of fully peeled and nanonized organic layered silicate are added. When comparing the shape parameters of the nano-organized layered silicate composite (EMNC-60-0.3), the shape parameters of the epoxy-micro composite (EMC-65) added with 65% by weight of micro silica and micro silica 65 were increased from 24.4 to 55.9. Comparison of the shape parameters of the epoxy-micro silica-nano organic layered silicate mixed composite (EMNC-65-0.3) with the addition of 0.3% by weight and 0.3% by weight of fully peeled and nanonized organic layered silicate increased from 31.7 to 65.0. .

Accordingly, it can be seen that as the shape parameter of the present invention is further increased by 0.3% by weight of the fully peeled and nanonized organic layered silicate, the shape parameter of the present invention is more homogeneous.

The scale parameter is 107.6 Mpa for a circular epoxy resin, 157.8 Mpa for an epoxy-micro composite (EMC-60) added with 60% by weight of micro silica, and an epoxy-micro composite with 65% by weight of micro silica. EMC-65) is 171.2 Mpa, and the epoxy-micro silica-nano organic layered silicate mixed composite of the present invention (EMNC-60-0.3) added with 60% by weight of micro silica and 0.3% by weight of fully peeled and nanonized organic layered silicate (EMNC-60-0.3) Is 162.7 Mpa, and the epoxy-microsilica-nano organic layered silicate mixed composite (EMNC-65-0.3) of the present invention with 65% by weight of micro silica and 0.3% by weight of fully peeled and nanonized organic layered silicate was added at 176.9 Mpa. The result was

As described above, the scale parameter of the epoxy-microcomposite added with 60% by weight of micro silica and 65% by weight increased from 157.8 Mpa to 171.2 Mpa, and with 60% by weight of micro silica and 65% by weight and completely peeled off and nano-ized Comparison of the scale parameters of the epoxy-micro silica-nano organic layered silicate mixed composite of the present invention to which 0.3 wt% of the organic layered silicate was added increased from 162.7 Mpa to 176.9 Mpa.

Accordingly, it can be seen that the scale parameter increases as the micro silica content increases.

And the epoxy-micro silica- of the present invention to which 60% by weight of the micro-silica-added epoxy-micro composite (EMC-60) and 60% by weight of the micro silica and 0.3% by weight of the fully peeled and nanonized organic layered silicate were added. Comparison of the scale parameters of the nano-organic layered silicate composite (EMNC-60-0.3) increased from 157.8 Mpa to 162.7 Mpa, and the scale parameters and micro-scales of the epoxy-micro composite (EMC-65) added 65% by weight of micro silica. Comparison of the scale parameters of the epoxy-micro silica-nano organic layered silicate mixed composite (EMNC-65-0.3) of the present invention to which 65% by weight of silica and 0.3% by weight of fully peeled and nanonized organic layered silicate were added was 176.9 at 171.2 Mpa. Increased to Mpa.

Accordingly, it can be seen that the scale parameter of the present invention is further increased by 0.3 wt% of the fully peeled and nanonized organic layered silicate, compared to the epoxy-micro composite.

The probability of failure (B10 life) is 78.2 Mpa for the epoxy resin, 92.4 Mpa for the epoxy-micro composite (EMC-60) added with 60% by weight of micro silica, and epoxy-micro composite with 65% by weight of the micro silica. EMC-65) is 38.1 Mpa, and the epoxy-micro silica-nano organic layered silicate mixed composite of the present invention (EMNC-60-0.3) added with 60% by weight of micro silica and 0.3% by weight of fully peeled and nanonized organic layered silicate Is 98.1 Mpa, and the epoxy-micro silica-nano organicated layered silicate mixed composite (EMNC-65-0.3) of 65% by weight of micro silica and 0.3% by weight of fully peeled and nanonized organic layered silicate is added to 102.2 Mpa. The result was

As described above, when comparing the failure probability of the epoxy-microcomposite with 60% by weight of the micro silica and 65% by weight, it was reduced from 92.4 Mpa to 38.1 Mpa, but 60% by weight of the micro silica and 65% by weight and completely peeled off and nano-ized. Comparison of the scale parameters of the epoxy-micro silica-nano organic layered silicate mixed composite of the present invention to which 0.3 wt% of the organic layered silicate was added increased from 98.1 Mpa to 102.2 Mpa.

Accordingly, it can be seen that the life span is increased as the content of micro silica increases, unlike the conventional epoxy-micro composite.

And the failure probability of the epoxy-micro composite (EMC-60) to which 60% by weight of micro silica was added, and the epoxy-micro silica- of the present invention to which 60% by weight of micro silica and 0.3% by weight of fully peeled and nanonized organic layered silicate were added. The breakdown probability of nano-organic layered silicate composite (EMNC-60-0.3) was increased from 92.4Mpa to 98.1Mpa, and the breakdown probability of epoxy-micro composite (EMC-65) added with 65% by weight of micro silica Comparing the failure probability of the epoxy-micro silica-nano-organized layered silicate mixed composite (EMNC-65-0.3) with 65% by weight of silica and 0.3% by weight of fully peeled and nanonized organic layered silicate, 102.2 at 38.1 Mpa. Increased to Mpa.

Accordingly, it can be seen that the life span of the present invention is further increased by 0.3% by weight of the fully peeled and nanonized organic layered silicate, compared to the epoxy-micro composite.

(3) tensile strength characteristics

Circular epoxy resin, epoxy-micro composite (EMC-60) added with 60% by weight of micro silica, epoxy-micro composite (EMC-65) with added 60% by weight of micro silica, 60% by weight of micro silica and Epoxy-micro silica-nano organic layered silicate mixed composite (EMNC-60-0.3) of the present invention to which 0.3% by weight of fully peeled and nanonized organic layered silicate is added, and 65% by weight of micro silica and fully peeled and nanonized organic layered Flexural strength for the epoxy-micro silica-nano organic layered silicate mixed composite (EMNC-65-0.3) of 0.3% by weight of silicate added according to Weibull Plot is as follows.

Scale parameter (Mpa) Shape parameters Fracture Probability (B10) (Mpa) Circular epoxy 80.6 78.4 78.2 EMC-60 97.3 39.6 92.4 EMC-65 101.7 78.7 38.1 EMNC-60-0.3 98.9 94.7 98.1 EMNC-65-0.3 105.9 104.6 102.2

According to Table 3, the shape parameter is 78.4 of circular epoxy resin, epoxy-micro composite (EMC-60) added with 60% by weight of micro silica, 39.6, and 65% by weight of micro silica. Epoxy-micro silica-nano organic layered silicate mixed composite of the present invention with 78.7 added epoxy-micro composite (EMC-65) added and 60% by weight of micro silica and 0.3% by weight of fully peeled and nanonized organic layered silicate. EMNC-60-0.3) is 94.7, and the epoxy-micro silica-nano organic layered silicate mixed composite (EMNC-65-0.3) of the present invention is added with 65% by weight of micro silica and 0.3% by weight of fully peeled and nanonized organic layered silicate. ) Results in 104.6.

As described above, the shape parameters of the epoxy-microcomposite added with 60% by weight of micro silica and 65% by weight increased from 39.6 to 78.7, and with 60% by weight of micro silica and 65% by weight and fully peeled and nanonized organicization. Comparing the shape parameters of the epoxy-micro silica-nano organic layered silicate mixed composite of the present invention to which 0.3 wt% of the layered silicate was added, it increased from 94.7 to 104.6. If the shape parameter is large, the inclination of the fitted line means the characteristics of homogeneity. The larger the slope of the fitted line is, the more homogeneous the tensile strength is.

Accordingly, the shape parameter increases as the content of the micro silica increases, and thus the fitted line of the present invention exhibits more uniform tensile properties than the epoxy-micro composite.

And the epoxy-micro silica- of the present invention to which the shape parameter of the epoxy-micro composite (EMC-60) to which 60% by weight of micro silica is added, and 60% by weight of micro silica and 0.3% by weight of fully peeled and nanonized organic layered silicate are added. When comparing the shape parameters of the nano-organic layered silicate composite (EMNC-60-0.3), it increased from 39.6 to 94.7, and the shape parameters of the epoxy-micro composite (EMC-65) added with 65% by weight of micro silica and micro silica 65 Comparison of the shape parameters of the epoxy-micro silica-nano organic layered silicate mixed composite (EMNC-65-0.3) of the present invention with the addition of 0.3% by weight and 0.3% by weight of fully peeled and nanonized organic layered silicate increased from 78.7 to 104.6. .

Accordingly, it can be seen that by 0.3 wt% of the fully peeled and nanonized organic layered silicate, the homogeneous tensile properties are exhibited as the shape parameter of the present invention is further increased as compared with the epoxy-micro composite.

The scale parameter is 80.6 Mpa for the epoxy resin, 97.3 Mpa for the epoxy-micro composite (EMC-60) added with 60% by weight of micro silica, and epoxy-micro composite (65% by weight for the micro silica added). EMC-65) of 101.7 Mpa, epoxy-micro silica-nano organic layered silicate mixed composite of the present invention (EMNC-60-0.3) added with 60% by weight of micro silica and 0.3% by weight of fully peeled and nanonized organic layered silicate Is 98.9 Mpa, and the epoxy-micro silica-nano organic layered silicate mixed composite (EMNC-65-0.3) of the present invention with 65% by weight of micro silica and 0.3% by weight of fully peeled and nanonized organic layered silicate is added at 105.9 Mpa. The result was

As described above, the scale parameters of the epoxy-microcomposite added with 60% by weight of micro silica and 65% by weight increased from 97.3 Mpa to 101.7 Mpa, with 60% by weight of micro silica and 65% by weight and completely peeled off and nano-ized. Comparison of the scale parameters of the epoxy-micro silica-nano organic layered silicate mixed composite of the present invention to which 0.3 wt% of the organic layered silicate added was increased from 98.9 Mpa to 105.9 Mpa.

Accordingly, it can be seen that the scale parameter increases as the micro silica content increases.

And the epoxy-micro silica- of the present invention to which 60% by weight of the micro-silica-added epoxy-micro composite (EMC-60) and 60% by weight of the micro silica and 0.3% by weight of the fully peeled and nanonized organic layered silicate were added. When comparing the scale parameters of the nano-organized layered silicate mixed composite (EMNC-60-0.3), the scale parameters of the epoxy-micro composite (EMC-65) added with 65% by weight of micro silica were increased from 97.3 Mpa to 98.9 Mpa. When comparing the scale parameters of the epoxy-micro silica-nano organic layered silicate mixed composite (EMNC-65-0.3) of the present invention to which 65% by weight of silica and 0.3% by weight of fully peeled and nanonized organic layered silicate were added, it was 105.9 at 101.7 Mpa. Increased to Mpa.

Accordingly, it can be seen that the scale parameter of the present invention is further increased by 0.3% by weight of the fully peeled and nanonized organic layered silicate, compared to the epoxy-micro composite.

The probability of failure (B10 life) is the same as that of the flexural strength.

3. Electrical Characteristics (Insulation Breaking Strength)

Insulation breakdown strength is a very important characteristic for estimating the insulation performance of dielectric materials because it causes fatal defects in high voltage power equipment.

Scale parameter (kV / 0.25㎜) Shape parameters Fracture Probability (B10) (kV / 0.25㎜) Circular epoxy 81.9 6.9 59.2 EMC-60 71.6 4.8 46.6 EMC-65 66.3 4.2 38.1 EMNC-60-0.3 95.4 12.2 79.8 EMNC-65-0.3 87.3 10.3 70.2

Here, the shape parameter represents the data distribution slope, the scale parameter represents the dielectric breakdown strength expected at the failure probability at 63.2% of the cumulative distribution probability density, and the fracture probability is the dielectric breakdown strength characteristic of the plot. The probability of an accident occurring in this bad 10% is an electrical property that has a profound effect on lifespan as the actual breakdown occurs in this area.

According to Table 4, the scale parameters are 81.9 for the epoxy resin, 71.6 for the epoxy-micro composite (EMC-60) added with 60% by weight of micro silica, and 65% by weight for the micro silica added. Epoxy-micro silica-nano organic layered silicate blend composite (EMNC-60-) with 66.3 microcomposites (EMC-65) and 60% by weight of micro silica and 0.3% by weight of fully peeled and nanonized organic layered silicates added 0.3) is 95.4, and the epoxy-micro silica-nano organicated layered silicate mixed composite (EMNC-65-0.3) of the present invention with 65% by weight of micro silica and 0.3% by weight of fully peeled and nanonized organic layered silicate is added to The result was

As described above, the scale parameter of the epoxy-microcomposite added with 60% by weight of micro silica and 65% by weight was reduced from 71.6 to 66.3. It can be seen that the scale parameter was increased by adding 0.3% by weight.

That is, the epoxy-micro silica of the present invention to which 60% by weight of the micro-silica-added epoxy-micro composite (EMC-60) and 60% by weight of the micro silica and 0.3% by weight of the fully peeled and nanonized organic layered silicate were added. The scale parameters of the nano-organic layered silicate mixed composite (EMNC-60-0.3) increased from 71.6 to 95.4, and the scale parameters of the epoxy-microcomposite (EMC-65) and micro silica added 65% by weight of micro silica. Comparison of the scale parameters of the epoxy-micro silica-nano organic layered silicate mixed composite (EMNC-65-0.3) with 65% by weight and 0.3% by weight of fully peeled and nanonized organic layered silicate increased from 66.3 to 87.3 It was.

Shape parameters are 6.9 for round epoxy resins, 4.8 for epoxy-micro composites (EMC-60) with 60% by weight of micro silica added, and epoxy-micro composites with 65% by weight of micro silica (EMC-). 65) is 4.2, and the epoxy-micro silica-nano organic layered silicate mixed composite (EMNC-60-0.3) of the present invention added with 60% by weight of micro silica and 0.3% by weight of fully peeled and nanonized organic layered silicate (EMNC-60-0.3) The epoxy-micro silica-nano organic layered silicate mixed composite (EMNC-65-0.3) of the present invention with the addition of 65% by weight of micro silica and 0.3% by weight of fully peeled and nanonized organic layered silicate resulted in a result of 10.3.

As described above, although the shape parameters of the epoxy-microcomposite added with 60% by weight of micro silica and 65% by weight were reduced from 4.8 to 4.2, the organic layered silicate completely peeled and nano-ized into such epoxy-microcomposite was It can be seen that the shape parameter was increased by adding 0.3% by weight.

That is, the epoxy-micro silica of the present invention to which the shape parameter of the epoxy-micro composite (EMC-60) added with 60% by weight of micro silica, 60% by weight of micro silica and 0.3% by weight of fully peeled and nanonized organic layered silicate were added. When comparing the shape parameters of nano-organic layered silicate mixed composites (EMNC-60-0.3), the scale parameters of the epoxy-micro composites (EMC-65) added with 65% by weight of micro-silica and micro-silica were increased from 4.8 to 12.2. The scale parameters of the inventive epoxy-micro silica-nano organic layered silicate mixed composite (EMNC-65-0.3) added 65% by weight and 0.3% by weight of fully peeled and nanonized organic layered silicate increased from 4.2 to 10.3. It was.

This means that as the fitted line slope increases, the dielectric breakdown strength becomes more homogeneous. These results indicate that the fully peeled and nanonized organic layered silicate having a plate-like form is homogeneously dispersed between the micro silica particles, thereby improving the electrical breakdown strength property.

The electrical breakdown strength is not consistent with the increase in crosslink density shown in Table 1. In the epoxy-micro composites to which 60% by weight and 65% by weight of micro silica were added, the electrical breakdown strength (scale parameter) in Table 4 was decreased despite the increase in the crosslinking density in Table 1.

This is because electrons easily flow around the interface between the spherical micro silica and the epoxy resin, whereby a new electric field is concentrated on the opposite side of the micro silica surface. However, the fully stripped, nano-organized layered silicate in the form of a plate placed between micro silica blocks the electrons, resulting in a surprising increase in the electrical breakdown strength properties.

As described above, the observation of the transmission electron microscope (TEM) confirmed that the nanonized organic layered silicate was completely peeled off, and that the completely peeled and nanonized organic layered silicate was homogeneously dispersed between the micro silica particles. have.

And as the micro silica content increased, the crosslinking density increased, and the crosslinking density was even higher by adding 0.3% by weight of the fully peeled and nanonized organic layered silicate.

Tensile strength and flexural strength were also increased with increasing the amount of micro silica filling, and were further increased by 0.3 wt% of fully peeled and nano-organized layered silicates.

In addition, the electrical breakdown strength was reduced as the amount of micro silica filled increased in the case of 60-% by weight and 65-% by weight of silica, but completely peeled and nano-organized into the epoxy-micro composite. The electrical breakdown strength was increased by adding 0.3 wt% of the layered silicate.

Claims (5)

A first step of preheating the liquid epoxy resin at 80 ° C. for 1 to 5 hours to lower the viscosity;
A second step of preheating the nano-organized layered silicate at 100 ° C. for 24 hours to completely remove moisture contained in the nano-organized layered silicate;
The preheated liquid epoxy resin of the first stage and the nano-organized layered silicate from which the moisture of the second stage was removed are subjected to a power ultrasonic wave, a homogenizer, and a mechanical stirrer for 30 to 60 minutes. stirrer), but the ultrasonic wave of the powerful ultrasonic disperser is the condition of the resonance frequency 20khz, amplitude 60 ~ 68%, output 750 ~ 1500W intensity, the homogenizer is 10000rpm, the mechanical stirrer is 2000 ~ 3000rpm An epoxy-nano organic layered silicate pretreatment step consisting of a third step of stirring under conditions;
The mixed and pretreated epoxy-nano organic layered silicate liquid composite of the third step is introduced into an alternating current electric field dispersion chamber, and the cation of the nano-organized layered silicate is vibrated between layers of the nano-organized layered silicate by an alternating electric field to expand the interlayer distance. Dispersing the epoxy resin into the expanded interlayer of the nano-organized layered silicate to allow insertion and exfoliation;
Injecting micro silica having an average particle diameter of 3 to 20 μm into the liquid composite and the curing agent of the epoxy-nano organic layered silicate treated with the electric field dispersion of the fourth step, respectively, and agitated under a condition of 2000 to 4500 rpm for 30 to 60 minutes in a mechanical stirrer. A fifth step of mixing the epoxy-micro silica-nano organic layered silicate liquid composite mixture and the hardener-micro silica mixture and mixing and defoaming the mixture for 10-20 minutes for stirring and defoaming;
A sixth step of defoaming the second mixed and degassed epoxy-micro silica-nano organic layered silicate liquid composite by adding an antifoaming agent and a dispersing agent to facilitate bubble removal and dispersion;
By adding a curing accelerator to the sixth step of the primary mixing and secondary degassed epoxy-micro silica-nano organic layered silicate liquid composite, the secondary mixing for stirring and defoaming with a mechanical stirrer to evenly distribute the added curing accelerator. And a seventh step of defoaming thirdly;
Epoxy injected after the curing, curing accelerator, antifoaming agent, and dispersing agent were mixed, and the secondary mixed and tertiary degassed seventh stage epoxy-micro silica-nano organic layered silicate liquid composite was injected into a mold preheated to 80 ° C. An eighth step of performing a vacuum defoaming process for 30 to 60 minutes in a vacuum oven (1 torr) to remove the final bubble of the micro silica-nano organic layered silicate liquid composite;
In order to form the vacuum degassed epoxy-micro silica-nano organic layered silicate liquid composite of the eighth step, the first curing was performed at 120 ° C. for 2 hours in a high temperature oven, and then the second curing was performed at 150 ° C. for 24 hours. Epoxy-micro silica-nano-organized layered silicate composite composite manufacturing method using the electric field dispersion comprising the main step of the epoxy-micro silica-nano organic layered silicate comprising the ninth step. The method according to claim 1,
Insulation using electric field dispersion, characterized in that 39.7% by weight of epoxy resin, 60% by weight of micro silica, 0.3% by weight of nano organic layered silicate, or 34.7% by weight of epoxy resin, 65% by weight of micro silica, 0.3% by weight of nanoorganized layered silicate Process for preparing epoxy-micro silica-nano organic layered silicate mixed composite for use. The method according to claim 1 or 2,
The AC electric field dispersion chamber is provided with a pair of opposed +/- parallel plate electrodes for applying an AC electric field, and AC electric field application conditions are applied voltage 3 ~ 11 kHz, applied frequency 1000 kHz, application time 60 minutes or less. A method for producing an epoxy-micro silica-nano organic layered silicate mixed composite for insulation using electric field dispersion. An epoxy-micro silica-nano organic layered silicate mixed composite, which is prepared by a method for preparing an insulating epoxy-micro silica-nano organic layered silicate mixed composite using electric field dispersion. Epoxy-micro silica-nano organic layered silicate mixed composite prepared by the method of manufacturing the epoxy-micro silica-nano organic layered silicate mixed composite for insulation using the electric field dispersion of claim 2.

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