CN108587069A - A kind of preparation method of the epoxy resin composite material of resistance to electricity tree characteristic - Google Patents
A kind of preparation method of the epoxy resin composite material of resistance to electricity tree characteristic Download PDFInfo
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- CN108587069A CN108587069A CN201810487199.3A CN201810487199A CN108587069A CN 108587069 A CN108587069 A CN 108587069A CN 201810487199 A CN201810487199 A CN 201810487199A CN 108587069 A CN108587069 A CN 108587069A
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- epoxy resin
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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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
- C08K9/00—Use of pretreated ingredients
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
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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
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Organic Insulating Materials (AREA)
Abstract
The invention discloses a kind of preparation methods of the epoxy resin composite material of resistance to electricity tree characteristic, it is compounded using nanoscale and micron grade aluminum oxide as inorganic filler, since inorganic particle has the function of stopping electrical treeing, so that electricity tree channel is blocked by inorganic particle, to enhance the inhibition electric branch growth ability of epoxy resin；Different-grain diameter filler is used cooperatively the generation that can effectively reduce air gap between filler particles and epoxy polymer, and after carrying out coupling agent low-temperature plasma synergistic processing to inorganic filler, promote being bonded for different-grain diameter filler and epoxy resin-base, to effectively improve the combination density between filler and resin matrix, simultaneously in the solidification process of epoxy resin composite material, ultrasonication, Fruit storage through interval, the generation for reducing air gap in epoxy systems, to achieve the purpose that secondary electrical tree construction is inhibited to generate.
Description
Technical field
The invention belongs to high voltage insulating materials technical fields, and in particular to a kind of epoxy resin composite wood of resistance to electricity tree characteristic
The preparation method of material.
Background technology
The aging of insulating materials is the important factor in order of cable run safe operation, includes mainly voltage ageing and heat ageing
2 kinds of forms, and the voltage ageing caused by electric branch is common ageing form.Cable termination in the fabrication process, may be
The other forms defect such as bubble and impurity is introduced inside epoxy resin insulation material, internal field is caused to concentrate, and part is caused to be put
Electricity and charge injection, and then lead to the formation in electric branch channel.Under the continuous action of highfield, electric branch is fast-developing, most
Lead to insulation breakdown eventually, seriously threatens the safe and stable operation of cable transmission systems.
Invention content
The present invention provides it is a kind of it is resistance to electricity tree characteristic epoxy resin composite material preparation method, using nanoscale with it is micro-
Meter level aluminium oxide as inorganic filler, it is evenly dispersed in the epoxy, enhance the inhibition electric branch growth energy of epoxy resin
Power.
In order to achieve the above objectives, the present invention uses following technical scheme：
A kind of preparation method of the epoxy resin composite material of resistance to electricity tree characteristic, includes the following steps：
（1）Take micrometer alumina, nano aluminium oxide according to 1:The mass ratio of 0.8-1.5 is put into acetone solvent, ultrasonic disperse 25-
45min, for use；A certain amount of KH-550 silane coupling agents are added in boiling solution, with salt acid for adjusting pH value to 5.0-
6.5, it is hydrolyzed, alumina fluid dispersion is then added, 30-60min is stirred in 55-65 DEG C of water bath with thermostatic control, be filtered under diminished pressure,
It is washed with deionized to no chlorion, product activates 6-9h at 140-155 DEG C after drying；
（2）Low Temperature Plasma Treating：
Alumina powder after above-mentioned activation modification is placed in repetition pulse dielectric barrier discharge（DBD）Region of discharge in, make
Micro/nano level particle receives atmosphere air surface modification of low temperature plasma, after 2-6min, acquires low temperature plasma
Modified micro/nano level aluminium oxide particles, are sealed；
（3）It takes pure epoxy resin to be added in beaker, is placed in heating mantle and stirs in heating and be warming up to 85-95 DEG C, and keep
10-20min reduces epoxy resin viscosity, the above-mentioned alumina packing after Low Temperature Plasma Treating is added in beaker, surely
Determine blender speed governing 1500-2000r/min, composite material uniform stirring 20-35min be then placed in supersonic wave cleaning machine,
Ultrasonication 10-15min is carried out under conditions of 45-60 DEG C of water bath with thermostatic control, then at 1500-2000r/min mechanical agitations 20-
30min carries out ultrasonic wave-mechanical treatment again later, 2-3 times repeatedly, makes Al2O3Filler is sufficiently mixed in epoxy resin；
（4）Curing agent is sequentially added into above-mentioned epoxy resin, accelerating agent is stirred mixed processing, in 45-60 DEG C of thermostatted water
Under conditions of bath, continue ultrasonication, and the mechanical agitation 20-30min under 1200-1600r/min；
（5）After waiting for ultrasonication, takes out beaker and be placed in vacuum pump, taken out under conditions of -7.5MPa, 55-70 DEG C
After vacuum carries out deaeration processing 25-40min, pours into and preheat and be coated in the mold of releasing agent and vacuumize 20-30min in advance；
（6）It finally puts it into the drying box of constant temperature from taking-up mold, is adjusted with the speed that heats of 10 DEG C/h since 90 DEG C
Temperature is finally warming up to 128-132 DEG C with 18-20 DEG C/h speed later to 105-110 DEG C, and one is finally kept at 140-150 DEG C
Hour, after curing reaction, taken out after cooled to room temperature.
Wherein, the micrometer alumina average grain diameter is at 5-10 μm, and the nano aluminium oxide average grain diameter is in 10-20nm.
Wherein, the use of medium is radius 5cm, thickness 0.1cm quartz glass, high-voltage electricity in the Low Temperature Plasma Treating
Pole and ground electrode radius be 2.5cm, thickness 3cm, discharging gap 0.3cm.
Beneficial effects of the present invention are as follows：
It uses nanoscale to be compounded with micron grade aluminum oxide in the present invention and is used as inorganic filler, since inorganic particle has blocking electricity tree
The effect of growth so that electricity tree channel is blocked by inorganic particle, to enhance the inhibition electric branch growth ability of epoxy resin；
Different-grain diameter filler is used cooperatively the generation that can effectively reduce air gap between filler particles and epoxy polymer, and to inorganic filler
After carrying out coupling agent-low-temperature plasma synergistic processing, filler surface roughness can be improved so that aluminium oxide particles surface is coupled
Agent grafting rate improves, and promotes being bonded for different-grain diameter filler and epoxy resin-base, uniform filling is made to be dispersed in resin matrix
In, to effectively improve the combination density between filler and resin matrix, while in the solidification process of epoxy resin composite material
In, ultrasonication, Fruit storage through interval reduce the generation of air gap in epoxy systems, inhibit secondary to reach
The purpose that electric tree construction generates.
Specific implementation mode
Embodiment 1
A kind of preparation method of the epoxy resin composite material of resistance to electricity tree characteristic, includes the following steps：
（1）Take micrometer alumina, nano aluminium oxide according to 1:1.2 mass ratio is put into acetone solvent, ultrasonic disperse 35min,
For use；The micrometer alumina average grain diameter is at 5-10 μm, and the nano aluminium oxide average grain diameter is in 10-20nm；
A certain amount of KH-550 silane coupling agents are added in boiling solution, with salt acid for adjusting pH value to 5.0, carry out water
Solution, alumina fluid dispersion is then added, stirs 40min in 60 DEG C of waters bath with thermostatic control, is filtered under diminished pressure, be washed with deionized to
Without chlorion, product activates 8h at 150 DEG C after drying；
（2）Low Temperature Plasma Treating：
Alumina powder after above-mentioned activation modification is placed in repetition pulse dielectric barrier discharge（DBD）Region of discharge in, make
Micro/nano level particle receives atmosphere air surface modification of low temperature plasma, after 4min, acquires low-temperature plasma structural reform
Micro/nano level aluminium oxide particles after property, are sealed；
It is radius 5cm, thickness 0.1cm quartz glass that medium is used in the Low Temperature Plasma Treating, and high-field electrode is electric with ground
Polar radius is 2.5cm, thickness 3cm, discharging gap 0.3cm.
（3）It takes 100g pure epoxy resins to be added in beaker, is placed in heating mantle to stir in heating and is warming up to 90 DEG C, and
15min is kept, epoxy resin viscosity is reduced, beaker is added in the above-mentioned alumina packings after Low Temperature Plasma Treating of 18g
In, stablize blender speed governing 1600r/min and is then placed in composite material uniform stirring 30min in supersonic wave cleaning machine,
Ultrasonication 15min is carried out under conditions of 60 DEG C of waters bath with thermostatic control to carry out again later then at 1600r/min mechanical agitation 25min
Ultrasonic wave-mechanical treatment 2 times repeatedly, makes Al2O3Filler is sufficiently mixed in epoxy resin；
（4）Curing agent is sequentially added into above-mentioned epoxy resin, accelerating agent is stirred mixed processing, in 60 DEG C of waters bath with thermostatic control
Under the conditions of, continue ultrasonication, and the mechanical agitation 30min under 1400r/min；
（5）After waiting for ultrasonication, takes out beaker and be placed in vacuum pump, vacuumized under conditions of -7.5MPa, 60 DEG C
After carrying out deaeration processing 30min, pours into and preheat and be coated in the mold of releasing agent and vacuumize 30min in advance；
（6）It finally puts it into the drying box of constant temperature from taking-up mold, is adjusted with the speed that heats of 10 DEG C/h since 90 DEG C
Temperature is finally warming up to 130 DEG C with 20 DEG C/h speed later to 110 DEG C, is finally kept for one hour at 150 DEG C, curing reaction knot
Shu Hou takes out after cooled to room temperature.
Claims (4)
1. a kind of preparation method of the epoxy resin composite material of resistance to electricity tree characteristic, which is characterized in that include the following steps：
（1）Take micrometer alumina, nano aluminium oxide according to 1:The mass ratio of 0.8-1.5 is put into acetone solvent, ultrasonic disperse 25-
45min, for use；A certain amount of KH-550 silane coupling agents are added in boiling solution, with salt acid for adjusting pH value to 5.0-
6.5, it is hydrolyzed, alumina fluid dispersion is then added, 30-60min is stirred in 55-65 DEG C of water bath with thermostatic control, be filtered under diminished pressure,
It is washed with deionized to no chlorion, product activates 6-9h at 140-155 DEG C after drying；
（2）Low Temperature Plasma Treating：
Alumina powder after above-mentioned activation modification is placed in repetition pulse dielectric barrier discharge（DBD）Region of discharge in, make
Micro/nano level particle receives atmosphere air surface modification of low temperature plasma, after 2-6min, acquires low temperature plasma
Modified micro/nano level aluminium oxide particles, are sealed；
（3）It takes pure epoxy resin to be added in beaker, is placed in heating mantle and stirs in heating and be warming up to 85-95 DEG C, and keep
10-20min reduces epoxy resin viscosity, the above-mentioned alumina packing after Low Temperature Plasma Treating is added in beaker, surely
Determine blender speed governing 1500-2000r/min, composite material uniform stirring 20-35min be then placed in supersonic wave cleaning machine,
Ultrasonication 10-15min is carried out under conditions of 45-60 DEG C of water bath with thermostatic control, then at 1500-2000r/min mechanical agitations 20-
30min carries out ultrasonic wave-mechanical treatment again later, 2-3 times repeatedly, makes Al2O3Filler is sufficiently mixed in epoxy resin；
（4）Curing agent is sequentially added into above-mentioned epoxy resin, accelerating agent is stirred mixed processing, in 45-60 DEG C of thermostatted water
Under conditions of bath, continue ultrasonication, and the mechanical agitation 20-30min under 1200-1600r/min；
（5）After waiting for ultrasonication, takes out beaker and be placed in vacuum pump, taken out under conditions of -7.5MPa, 55-70 DEG C
After vacuum carries out deaeration processing 25-40min, pours into and preheat and be coated in the mold of releasing agent and vacuumize 20-30min in advance；
（6）It finally puts it into the drying box of constant temperature from taking-up mold, is adjusted with the speed that heats of 10 DEG C/h since 90 DEG C
Temperature is finally warming up to 128-132 DEG C with 18-20 DEG C/h speed later to 105-110 DEG C, and one is finally kept at 140-150 DEG C
Hour, after curing reaction, taken out after cooled to room temperature.
2. a kind of preparation method of the epoxy resin composite material of resistance to electricity tree characteristic according to claim 1, feature exist
In the micrometer alumina average grain diameter is at 5-10 μm, and the nano aluminium oxide average grain diameter is in 10-20nm.
3. a kind of preparation method of the epoxy resin composite material of resistance to electricity tree characteristic according to claim 1, feature exist
In it is radius 5cm, thickness 0.1cm quartz glass, high-field electrode and ground electrode to use medium in the Low Temperature Plasma Treating
Radius is 2.5cm, thickness 3cm, discharging gap 0.3cm.
4. a kind of preparation method of the epoxy resin composite material of resistance to electricity tree characteristic according to claim 1, feature exist
In additive amount of the micro-nano aluminium oxide mixed fillers in epoxy resin composite material is 15-25%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810487199.3A CN108587069A (en) | 2018-05-21 | 2018-05-21 | A kind of preparation method of the epoxy resin composite material of resistance to electricity tree characteristic |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810487199.3A CN108587069A (en) | 2018-05-21 | 2018-05-21 | A kind of preparation method of the epoxy resin composite material of resistance to electricity tree characteristic |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591496A (en) * | 2019-08-23 | 2019-12-20 | 安徽锦华氧化锌有限公司 | Preparation method of modified nano-zinc oxide filled exterior wall coating |
| CN111154227A (en) * | 2019-12-26 | 2020-05-15 | 苏州巨峰先进材料科技有限公司 | High-thermal-conductivity insulating layer material, metal substrate and preparation method |
| CN111276645A (en) * | 2020-03-23 | 2020-06-12 | 成都科成精化科技有限公司 | Design method of filler reinforcing system of lithium battery aluminum plastic film adhesive |
| CN111517371A (en) * | 2020-04-28 | 2020-08-11 | 铜陵同达兴实业有限责任公司 | Production process of nanoscale iron oxide |
| CN113583390A (en) * | 2021-09-08 | 2021-11-02 | 深圳先进电子材料国际创新研究院 | Method for toughening and modifying epoxy-based packaging material |
-
2018
- 2018-05-21 CN CN201810487199.3A patent/CN108587069A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591496A (en) * | 2019-08-23 | 2019-12-20 | 安徽锦华氧化锌有限公司 | Preparation method of modified nano-zinc oxide filled exterior wall coating |
| CN111154227A (en) * | 2019-12-26 | 2020-05-15 | 苏州巨峰先进材料科技有限公司 | High-thermal-conductivity insulating layer material, metal substrate and preparation method |
| CN111276645A (en) * | 2020-03-23 | 2020-06-12 | 成都科成精化科技有限公司 | Design method of filler reinforcing system of lithium battery aluminum plastic film adhesive |
| CN111517371A (en) * | 2020-04-28 | 2020-08-11 | 铜陵同达兴实业有限责任公司 | Production process of nanoscale iron oxide |
| CN113583390A (en) * | 2021-09-08 | 2021-11-02 | 深圳先进电子材料国际创新研究院 | Method for toughening and modifying epoxy-based packaging material |
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Application publication date: 20180928 |
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