CN107216483A - A kind of method for lifting epoxy resin edge flashing intensity - Google Patents
A kind of method for lifting epoxy resin edge flashing intensity Download PDFInfo
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- CN107216483A CN107216483A CN201710453362.XA CN201710453362A CN107216483A CN 107216483 A CN107216483 A CN 107216483A CN 201710453362 A CN201710453362 A CN 201710453362A CN 107216483 A CN107216483 A CN 107216483A
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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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
- C08J7/126—Halogenation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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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
- C08K2201/011—Nanostructured additives
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- General Chemical & Material Sciences (AREA)
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Abstract
The invention discloses a kind of method for lifting epoxy resin edge flashing intensity, comprise the following steps：1) it is nano combined：Al is added during epoxy resin cure machine-shaping2O3Nano particle carries out nano combined processing, obtains epoxy resin samples；2) it is cleaned and dried：It will be dried after the epoxy resin samples cleaning of shaping；3) surface fluorination：Cleaned dried epoxy resin samples are subjected to surface fluorination processing, and fluorinated layer is formed on epoxy resin samples surface.By the method for surface modification, in material surface formation fluorinated layer, the surface conductivity of finished product can be lifted, suppresses the accumulation of surface charge, and it is nano combined, the surface roughness of sample can be increased to a certain extent.Under the comprehensive function of two kinds of modification technologies, the edge flashing intensity of sample is improved.And have the advantages that to realize that simple, cost is low, practicality is good, do not need special equipment and special treatment conditions, can be achieved using simple and mechanical equipment and repeatability is strong.
Description
Technical field
It is specific strong to lift epoxy resin edge flashing the invention belongs to engineering dielectric and electrical engineering technical field
The method of degree.
Background technology
When edge flashing refers to the gas or breakdown liquid dielectric around solid dielectric insulation, along solid dielectric insulation
The phenomenon of surface-discharge, voltage when it discharges is referred to as flashover voltage.After generation flashover, interelectrode voltage quickly falls to zero
Or close to zero.The insulating surface hot-spot that spark or electric arc in flashover passage makes causes charing, reduces surface insulation performance.
Edge flashing as in Modern high-pressure electrical equipment influence and limiting device integral insulation intensity a very important factor,
The size of its flashover voltage is with applying voltage waveform, air pressure or the species and solid dielectric insulation of liquid insulating medium, especially
It is that its surface state has direct relation.
At present, epoxy resin is by feat of its excellent dielectric properties, mechanical performance and acid-alkali-corrosive-resisting performance, it has also become
A kind of indispensable material in Modern high-pressure electrical equipment.But conventional epoxy resin has the easy Accumulating charge in surface
The problem of, particularly in HVDC field, this causes epoxy resin to be easier to occur edge flashing compared to other materials,
Cause its surface insulation performance to be destroyed, and trigger a series of security incidents.
The content of the invention
In view of this, in order to overcome the deficiencies in the prior art, it is an object of the invention to provide a kind of enhancing ring
The method of oxygen tree fat edge flashing intensity.
To reach above-mentioned purpose, the present invention provides following technical scheme：
A kind of method for lifting epoxy resin edge flashing intensity, comprises the following steps：
1) it is nano combined：Al is added during epoxy resin cure machine-shaping2O3Nano particle carries out nano combined place
Reason, obtains epoxy resin samples；
2) it is cleaned and dried：It will be dried after the epoxy resin samples cleaning of shaping；
3) surface fluorination：By step 2) in cleaned dried epoxy resin samples carry out surface fluorination processing, and
Epoxy resin samples surface forms fluorinated layer.
Further, the step 1) in, it is to the method that epoxy resin carries out nano combined processing：By epoxy resin, admittedly
Agent and catalyst by proportion are placed in container, and are put into after magnetic stir bar in container that to be placed in heating magnetic stirring apparatus enterprising
Row heating stirring, obtains the first mixed liquor, and the parameter of heating stirring is：50-100 DEG C of temperature, rotating speed 500-1500r/min,
Mixing time 5-180min；
Then Al is proportionally added into the first obtained mixed liquor2O3Nano particle and coupling agent, continue in magnetic agitation
Heating stirring on device, obtains the second mixed liquor, and the parameter of heating stirring is：50-100 DEG C, rotating speed 500-1500r/min is stirred
Mix time 5-180min；
The second mixed liquor is inserted after the completion of heating stirring ultrasonic agitation is carried out in ultrasonic oscillator, mixing time is 5-
240min；Most afterwards through vacuum outgas and the process machine-shaping that is heating and curing.
Further, the epoxy resin, curing agent, catalyst, Al2O3The weight of nano particle and coupling agent is：
100 parts of epoxy resin；80-90 parts of curing agent；1-2 parts of catalyst；Al2O30.1-5 parts of nano particle；0.1-2 parts of coupling agent.
Further, the step 2) in, the epoxy resin samples absolute ethyl alcohol after shaping and deionized water are handed over first
For cleaning, then cleaned, be finally rinsed again with deionized water using ultrasonic cleaning machine；Epoxy resin sample after cleaning
Product are placed in vacuum drying chamber and are dried, and drying condition is：50-120 DEG C of temperature, time 1-48h.
Further, it is to the method that epoxy resin samples carry out surface fluorination processing：By the epoxy resin after cleaning-drying
Sample is put into progress surface fluorination processing in reactor, and the condition of surface fluorination processing is：Constituted using inert gas and fluorine gas
Mixed gas or the mixed gas that is constituted with fluorine gas of nitrogen be fluorinated, the volumetric concentration of fluorine gas is 1-50% in gaseous mixture,
It is 0.1-1bar to be fluorinated the air pressure that temperature is mixed gas in 20-80 DEG C, reactor, and the fluorination time is 5-240min.
The beneficial effects of the present invention are：
The method of present invention lifting epoxy resin edge flashing intensity, using the method for surface modification, in material surface shape
Into fluorinated layer, the surface conductivity of finished product can be lifted, suppress the accumulation of surface charge, and it is nano combined then can be to a certain degree
The surface roughness of upper increase sample, under the comprehensive function of two kinds of modification technologies, the edge flashing intensity of sample is carried
Rise；And the technical scheme that provides of the present invention have realize simple, required instrument cost it is low, with good practicality, no
Need special equipment and special treatment conditions, can be achieved and the strong advantage of repeatability using simple and mechanical equipment.
Brief description of the drawings
In order that the purpose of the present invention, technical scheme and beneficial effect are clearer, the present invention provides drawings described below and carried out
Explanation：
Fig. 1 be atomic force microscope observation to handled through the inventive method after epoxy resin samples three-dimensional surface shape
Looks；
Fig. 2 is the epoxy resin samples through the inventive method before and after the processing that fourier changes the measurement of infrared spectrum analysis instrument
The infared spectrum on surface；
Wherein, in Fig. 1 for fluorination 60min after epoxy resin samples 3 d surface topography figure；
Wavenumber (cm in Fig. 2-1) represent infared spectrum wave number；Absorptivity (a.u.) represents infrared figure
Compose absorptivity；F0 is the epoxy resin samples without fluorination treatment；F60 is epoxy resin samples after perfluorinated processing 60min.
Embodiment
The invention will be further described with specific embodiment below in conjunction with the accompanying drawings, so that those skilled in the art can be with
It is better understood from the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
Embodiment 1
The method of the lifting epoxy resin edge flashing intensity of the present embodiment, comprises the following steps：
1) it is molded：Al is added during epoxy resin cure machine-shaping2O3Nano particle carries out nano combined processing,
Obtain epoxy resin samples.Specifically, the method for epoxy resin cure machine-shaping is：By epoxy resin, curing agent and catalysis
Agent is placed in container in proportion, and is put into after magnetic stir bar in container to be placed in and is carried out heating on heating magnetic stirring apparatus and stir
Mix, obtain the first mixed liquor, and the parameter of heating stirring is：50-100 DEG C of temperature, rotating speed 500-1500r/min, mixing time
5-180min.Wherein, the weight of epoxy resin, curing agent and catalyst is：100 parts of epoxy resin；Curing agent 80-90
Part；1-2 parts of catalyst.
0.1-5 parts of Al are then proportionally added into the first obtained mixed liquor2O3Nano particle and 0.1-2 coupling agents, after
Continue the heating stirring on magnetic stirring apparatus, obtain the second mixed liquor, and the parameter of heating stirring is：50-100 DEG C, rotating speed 500-
1500r/min, mixing time 5-180min；
The second mixed liquor is inserted after the completion of heating stirring ultrasonic agitation is carried out in ultrasonic oscillator, mixing time is 5-
240min；Most obtain epoxy resin samples through vacuum outgas and the process machine-shaping that is heating and curing afterwards.
The part by weight of 100 parts of epoxy resin, 85 parts of curing agent, 2 parts of catalyst is placed in container by the present embodiment, and
It is put into after magnetic stir bar to be placed on heating magnetic stirring apparatus in container and carries out heating stirring, obtains the first mixed liquor, and heating
The condition of stirring is temperature 70 C, and rotating speed 1000r/min stirs 30min.
Then to 3 parts of Al of addition in the first mixed liquor2O3Nano particle and 2 parts of coupling agents, and continue with magnetic stirring apparatus
Stirring, obtains the second mixed liquor, the condition of heating stirring is temperature 70 C, and rotating speed 1000r/min stirs 30min.Recycle super
Acoustic wave oscillator continues to stir the second mixed liquor 15min.The subsequent vacuum outgas in vacuum drying chamber by the second mixed liquor
15min, then mixed liquor is poured into the mould that thickness is 2mm, and be put into electric air dry oven and solidify in 90 DEG C after 4h, then rise
Warm to 110 DEG C solidification 4h；After being finally cooled and shaped in normal temperature, the demoulding is preserved, and obtains epoxy resin samples.
2) it is cleaned and dried：It will be dried after the epoxy resin samples cleaning of shaping.Specifically, first by the asphalt mixtures modified by epoxy resin after shaping
Fat sample absolute ethyl alcohol and deionized water are alternately cleaned, and then cleaned using ultrasonic cleaning machine, deionization is finally used again
Water is rinsed；Epoxy resin samples after cleaning, which are placed in vacuum drying chamber, to be dried, and drying condition is：Temperature 50-120
DEG C, time 1-48h.
The epoxy resin samples of the present embodiment shaping carry out alternately cleaning with absolute ethyl alcohol and deionized water respectively, then make
Cleaned, then be rinsed with deionized water with ultrasonic cleaning machine, the epoxy resin samples after cleaning are placed in vacuum drying chamber
In be dried, drying condition is：Temperature 60 C, 8 hours time.
3) surface fluorination：By step 2) in cleaned dried epoxy resin samples carry out surface fluorination processing, and
Epoxy resin samples surface forms fluorinated layer.It is to the method that epoxy resin samples carry out surface fluorination processing：It will be cleaned and dried
Epoxy resin samples afterwards are put into progress surface fluorination processing in reactor, and the condition of surface fluorination processing is：Using indifferent gas
The mixed gas that the mixed gas or nitrogen of body and fluorine gas composition are constituted with fluorine gas is fluorinated, and the volume of fluorine gas is dense in gaseous mixture
Spend for 1-50%, fluorination temperature is that the air pressure of mixed gas in 20-80 DEG C, reactor is 0.1-1bar, and the fluorination time is 5-
240min。
Epoxy resin samples after clean dry are put into stainless steel cauldron by the present embodiment, and reactor is vacuumized,
Nitrogen is poured again, and in triplicate to exclude the interference to fluorination reaction such as oxygen, fluorine gas and nitrogen are then poured in reactor
Mixed gas, the volumetric concentration of the fluorine gas in mixed gas is 20%, and fluorination temperature is 55 DEG C, mixed gas in reactor
Air pressure is 0.5bar, and the fluorination time is 60min, and the sample after fluorination cleaned and dried, and can use for reference step 2) in side
Method.
At normal temperatures, in air atmosphere, the edge flashing intensity of sample is measured, it is using finger-type electrode, finger-type electrode is tight
The gap being affixed between sample surfaces, electrode is 10mm.Then between the electrodes apply amplitude be -24kV, the rate of rise for -
200V/s negative polarity linear DC voltage, and using the voltage between oscillograph recording electrode, when occurring between electrode along face
During flashover, it is the flashover voltage specifically measured to take voltage now.Every group of sample duplicate measurements 10 times, takes its average value as sample
The final flashover voltage of product.The inventive method measured before and after the processing sample edge flashing voltage as shown in table 1, can from table
To find out, the processing mode has been obviously improved the edge flashing intensity of epoxy resin samples.
It can manage it front and rear epoxy resin samples DC flashover in air measured by the present invention of table 1
Embodiment 2
The method of the lifting epoxy resin edge flashing intensity of the present embodiment, comprises the following steps：
1) it is molded：Al is added during epoxy resin cure machine-shaping2O3Nano particle carries out nano combined processing,
Obtain epoxy resin samples.Specifically, the method for epoxy resin cure machine-shaping is：By epoxy resin, curing agent and catalysis
Agent is placed in container in proportion, and is put into after magnetic stir bar in container to be placed in and is carried out heating on heating magnetic stirring apparatus and stir
Mix, obtain the first mixed liquor, and the parameter of heating stirring is：50-100 DEG C of temperature, rotating speed 500-1500r/min, mixing time
5-180min.Wherein, the weight of epoxy resin, curing agent and catalyst is：100 parts of epoxy resin；Curing agent 80-90
Part；1-2 parts of catalyst.
0.1-5 parts of Al are then proportionally added into the first obtained mixed liquor2O3Nano particle and 0.1-2 coupling agents, after
Continue the heating stirring on magnetic stirring apparatus, obtain the second mixed liquor, and the parameter of heating stirring is：50-100 DEG C, rotating speed 500-
1500r/min, mixing time 5-180min；
The second mixed liquor is inserted after the completion of heating stirring ultrasonic agitation is carried out in ultrasonic oscillator, mixing time is 5-
240min；Most obtain epoxy resin samples through vacuum outgas and the process machine-shaping that is heating and curing afterwards.
The part by weight of 100 parts of epoxy resin, 80 parts of curing agent, 1 part of catalyst is placed in container by the present embodiment, and
It is put into after magnetic stir bar to be placed on heating magnetic stirring apparatus in container and carries out heating stirring, obtains the first mixed liquor, and heating
The condition of stirring is temperature 50 C, and rotating speed 1500r/min stirs 5min.
Then to 0.1 part of Al of addition in the first mixed liquor2O3Nano particle and 0.1 part of coupling agent, and continue with magnetic force and stir
Device stirring is mixed, the second mixed liquor is obtained, the condition of heating stirring is temperature 50 C, and rotating speed 1500r/min stirs 5min.It is sharp again
Continued to stir the second mixed liquor 5min with ultrasonic oscillator.The subsequent vacuum outgas in vacuum drying chamber by the second mixed liquor
15min, then mixed liquor is poured into the mould that thickness is 2mm, and be put into electric air dry oven and solidify in 90 DEG C after 4h, then rise
Warm to 110 DEG C solidification 4h；After being finally cooled and shaped in normal temperature, the demoulding is preserved, and obtains epoxy resin samples.
2) it is cleaned and dried：It will be dried after the epoxy resin samples cleaning of shaping.Specifically, first by the asphalt mixtures modified by epoxy resin after shaping
Fat sample absolute ethyl alcohol and deionized water are alternately cleaned, and then cleaned using ultrasonic cleaning machine, deionization is finally used again
Water is rinsed；Epoxy resin samples after cleaning, which are placed in vacuum drying chamber, to be dried, and drying condition is：Temperature 50-120
DEG C, time 1-48h.
The epoxy resin samples of the present embodiment shaping carry out alternately cleaning with absolute ethyl alcohol and deionized water respectively, then make
Cleaned, then be rinsed with deionized water with ultrasonic cleaning machine, the epoxy resin samples after cleaning are placed in vacuum drying chamber
In be dried, drying condition is：120 DEG C of temperature, 1 hour time.
3) surface fluorination：By step 2) in cleaned dried epoxy resin samples carry out surface fluorination processing, and
Epoxy resin samples surface forms fluorinated layer.It is to the method that epoxy resin samples carry out surface fluorination processing：It will be cleaned and dried
Epoxy resin samples afterwards are put into progress surface fluorination processing in reactor, and the condition of surface fluorination processing is：Using indifferent gas
The mixed gas that the mixed gas or nitrogen of body and fluorine gas composition are constituted with fluorine gas is fluorinated, and the volume of fluorine gas is dense in gaseous mixture
Spend for 1-50%, fluorination temperature is that the air pressure of mixed gas in 20-80 DEG C, reactor is 0.1-1bar, and the fluorination time is 5-
240min。
Epoxy resin samples after clean dry are put into stainless steel cauldron by the present embodiment, and reactor is vacuumized,
Nitrogen is poured again, and in triplicate to exclude the interference to fluorination reaction such as oxygen, fluorine gas and nitrogen are then poured in reactor
Mixed gas, the volumetric concentration of the fluorine gas in mixed gas is 1%, and fluorination temperature is 80 DEG C, mixed gas in reactor
Air pressure is 1bar, and the fluorination time is 240min, and the sample after fluorination cleaned and dried, and can use for reference step 2) in side
Method.
At normal temperatures, in air atmosphere, the edge flashing intensity of sample is measured, it is using finger-type electrode, finger-type electrode is tight
The gap being affixed between sample surfaces, electrode is 10mm.Then between the electrodes apply amplitude be -24kV, the rate of rise for -
200V/s negative polarity linear DC voltage, and using the voltage between oscillograph recording electrode, when occurring between electrode along face
During flashover, it is the flashover voltage specifically measured to take voltage now.Every group of sample duplicate measurements 10 times, takes its average value as sample
The final flashover voltage of product.Through test, the method for the present embodiment has been obviously improved the edge flashing intensity of epoxy resin samples.
Embodiment 3
The method of the lifting epoxy resin edge flashing intensity of the present embodiment, comprises the following steps：
1) it is molded：Al is added during epoxy resin cure machine-shaping2O3Nano particle carries out nano combined processing,
Obtain epoxy resin samples.Specifically, the method for epoxy resin cure machine-shaping is：By epoxy resin, curing agent and catalysis
Agent is placed in container in proportion, and is put into after magnetic stir bar in container to be placed in and is carried out heating on heating magnetic stirring apparatus and stir
Mix, obtain the first mixed liquor, and the parameter of heating stirring is：50-100 DEG C of temperature, rotating speed 500-1500r/min, mixing time
5-180min.Wherein, the weight of epoxy resin, curing agent and catalyst is：100 parts of epoxy resin；Curing agent 80-90
Part；1-2 parts of catalyst.
0.1-5 parts of Al are then proportionally added into the first obtained mixed liquor2O3Nano particle and 0.1-2 coupling agents, after
Continue the heating stirring on magnetic stirring apparatus, obtain the second mixed liquor, and the parameter of heating stirring is：50-100 DEG C, rotating speed 500-
1500r/min, mixing time 5-180min；
The second mixed liquor is inserted after the completion of heating stirring ultrasonic agitation is carried out in ultrasonic oscillator, mixing time is 5-
240min；Most obtain epoxy resin samples through vacuum outgas and the process machine-shaping that is heating and curing afterwards.
The part by weight of 100 parts of epoxy resin, 90 parts of curing agent, 1.5 parts of catalyst is placed in container by the present embodiment, and
It is put into after magnetic stir bar to be placed on heating magnetic stirring apparatus in container and carries out heating stirring, obtains the first mixed liquor, and add
The condition of thermal agitation is 100 DEG C of temperature, and rotating speed 500r/min stirs 100min.
Then to 5 parts of Al of addition in the first mixed liquor2O3Nano particle and 0.5 part of coupling agent, and continue with magnetic agitation
Device is stirred, and obtains the second mixed liquor, the condition of heating stirring is 100 DEG C of temperature, and rotating speed 500r/min stirs 100min.It is sharp again
Continued to stir the second mixed liquor 240min with ultrasonic oscillator.The subsequent vacuum outgas in vacuum drying chamber by the second mixed liquor
15min, then mixed liquor is poured into the mould that thickness is 2mm, and be put into electric air dry oven and solidify in 90 DEG C after 4h, then rise
Warm to 110 DEG C solidification 4h；After being finally cooled and shaped in normal temperature, the demoulding is preserved, and obtains epoxy resin samples.
2) it is cleaned and dried：It will be dried after the epoxy resin samples cleaning of shaping.Specifically, first by the asphalt mixtures modified by epoxy resin after shaping
Fat sample absolute ethyl alcohol and deionized water are alternately cleaned, and then cleaned using ultrasonic cleaning machine, deionization is finally used again
Water is rinsed；Epoxy resin samples after cleaning, which are placed in vacuum drying chamber, to be dried, and drying condition is：Temperature 50-120
DEG C, time 1-48h.
The epoxy resin samples of the present embodiment shaping carry out alternately cleaning with absolute ethyl alcohol and deionized water respectively, then make
Cleaned, then be rinsed with deionized water with ultrasonic cleaning machine, the epoxy resin samples after cleaning are placed in vacuum drying chamber
In be dried, drying condition is：Temperature 50 C, 48 hours time.
3) surface fluorination：By step 2) in cleaned dried epoxy resin samples carry out surface fluorination processing, and
Epoxy resin samples surface forms fluorinated layer.It is to the method that epoxy resin samples carry out surface fluorination processing：It will be cleaned and dried
Epoxy resin samples afterwards are put into progress surface fluorination processing in reactor, and the condition of surface fluorination processing is：Using indifferent gas
The mixed gas that the mixed gas or nitrogen of body and fluorine gas composition are constituted with fluorine gas is fluorinated, and the volume of fluorine gas is dense in gaseous mixture
Spend for 1-50%, fluorination temperature is that the air pressure of mixed gas in 20-80 DEG C, reactor is 0.1-1bar, and the fluorination time is 5-
240min。
Epoxy resin samples after clean dry are put into stainless steel cauldron by the present embodiment, and reactor is vacuumized,
Nitrogen is poured again, and in triplicate to exclude the interference to fluorination reaction such as oxygen, fluorine gas and nitrogen are then poured in reactor
Mixed gas, the volumetric concentration of the fluorine gas in mixed gas is 50%, and fluorination temperature is 20 DEG C, mixed gas in reactor
Air pressure is 0.1bar, and the fluorination time is 5min, and the sample after fluorination cleaned and dried, and can use for reference step 2) in side
Method.
At normal temperatures, in air atmosphere, the edge flashing intensity of sample is measured, it is using finger-type electrode, finger-type electrode is tight
The gap being affixed between sample surfaces, electrode is 10mm.Then between the electrodes apply amplitude be -24kV, the rate of rise for -
200V/s negative polarity linear DC voltage, and using the voltage between oscillograph recording electrode, when occurring between electrode along face
During flashover, it is the flashover voltage specifically measured to take voltage now.Every group of sample duplicate measurements 10 times, takes its average value as sample
The final flashover voltage of product.Through test, the method for the present embodiment has been obviously improved the edge flashing intensity of epoxy resin samples.
Embodiment 4
The method of the lifting epoxy resin edge flashing intensity of the present embodiment, comprises the following steps：
1) it is molded：Al is added during epoxy resin cure machine-shaping2O3Nano particle carries out nano combined processing,
Obtain epoxy resin samples.Specifically, the method for epoxy resin cure machine-shaping is：By epoxy resin, curing agent and catalysis
Agent is placed in container in proportion, and is put into after magnetic stir bar in container to be placed in and is carried out heating on heating magnetic stirring apparatus and stir
Mix, obtain the first mixed liquor, and the parameter of heating stirring is：50-100 DEG C of temperature, rotating speed 500-1500r/min, mixing time
5-180min.Wherein, the weight of epoxy resin, curing agent and catalyst is：100 parts of epoxy resin；Curing agent 80-90
Part；1-2 parts of catalyst.
0.1-5 parts of Al are then proportionally added into the first obtained mixed liquor2O3Nano particle and 0.1-2 coupling agents, after
Continue the heating stirring on magnetic stirring apparatus, obtain the second mixed liquor, and the parameter of heating stirring is：50-100 DEG C, rotating speed 500-
1500r/min, mixing time 5-180min；
The second mixed liquor is inserted after the completion of heating stirring ultrasonic agitation is carried out in ultrasonic oscillator, mixing time is 5-
240min；Most obtain epoxy resin samples through vacuum outgas and the process machine-shaping that is heating and curing afterwards.
The part by weight of 100 parts of epoxy resin, 87 parts of curing agent, 1.5 parts of catalyst is placed in container by the present embodiment, and
It is put into after magnetic stir bar to be placed on heating magnetic stirring apparatus in container and carries out heating stirring, obtains the first mixed liquor, and add
The condition of thermal agitation is 90 DEG C of temperature, and rotating speed 800r/min stirs 180min.
Then to 1 part of Al of addition in the first mixed liquor2O3Nano particle and 1 part of coupling agent, and continue with magnetic stirring apparatus
Stirring, obtains the second mixed liquor, the condition of heating stirring is 90 DEG C of temperature, and rotating speed 800r/min stirs 180min.Recycle super
Acoustic wave oscillator continues to stir the second mixed liquor 180min.The subsequent vacuum outgas in vacuum drying chamber by the second mixed liquor
15min, then mixed liquor is poured into the mould that thickness is 2mm, and be put into electric air dry oven and solidify in 90 DEG C after 4h, then rise
Warm to 110 DEG C solidification 4h；After being finally cooled and shaped in normal temperature, the demoulding is preserved, and obtains epoxy resin samples.
2) it is cleaned and dried：It will be dried after the epoxy resin samples cleaning of shaping.Specifically, first by the asphalt mixtures modified by epoxy resin after shaping
Fat sample absolute ethyl alcohol and deionized water are alternately cleaned, and then cleaned using ultrasonic cleaning machine, deionization is finally used again
Water is rinsed；Epoxy resin samples after cleaning, which are placed in vacuum drying chamber, to be dried, and drying condition is：Temperature 50-120
DEG C, time 1-48h.
The epoxy resin samples of the present embodiment shaping carry out alternately cleaning with absolute ethyl alcohol and deionized water respectively, then make
Cleaned, then be rinsed with deionized water with ultrasonic cleaning machine, the epoxy resin samples after cleaning are placed in vacuum drying chamber
In be dried, drying condition is：Temperature 50 C, 48 hours time.
3) surface fluorination：By step 2) in cleaned dried epoxy resin samples carry out surface fluorination processing, and
Epoxy resin samples surface forms fluorinated layer.It is to the method that epoxy resin samples carry out surface fluorination processing：It will be cleaned and dried
Epoxy resin samples afterwards are put into progress surface fluorination processing in reactor, and the condition of surface fluorination processing is：Using indifferent gas
The mixed gas that the mixed gas or nitrogen of body and fluorine gas composition are constituted with fluorine gas is fluorinated, and the volume of fluorine gas is dense in gaseous mixture
Spend for 1-50%, fluorination temperature is that the air pressure of mixed gas in 20-80 DEG C, reactor is 0.1-1bar, and the fluorination time is 5-
240min。
Epoxy resin samples after clean dry are put into stainless steel cauldron by the present embodiment, and reactor is vacuumized,
Nitrogen is poured again, and in triplicate to exclude the interference to fluorination reaction such as oxygen, fluorine gas and nitrogen are then poured in reactor
Mixed gas, the volumetric concentration of the fluorine gas in mixed gas is 50%, and fluorination temperature is 20 DEG C, mixed gas in reactor
Air pressure is 0.1bar, and the fluorination time is 65min, and the sample after fluorination cleaned and dried, and can use for reference step 2) in side
Method.
At normal temperatures, in air atmosphere, the edge flashing intensity of sample is measured, it is using finger-type electrode, finger-type electrode is tight
The gap being affixed between sample surfaces, electrode is 10mm.Then between the electrodes apply amplitude be -24kV, the rate of rise for -
200V/s negative polarity linear DC voltage, and using the voltage between oscillograph recording electrode, when occurring between electrode along face
During flashover, it is the flashover voltage specifically measured to take voltage now.Every group of sample duplicate measurements 10 times, takes its average value as sample
The final flashover voltage of product.Through test, the method for the present embodiment has been obviously improved the edge flashing intensity of epoxy resin samples.
Embodiment described above is only the preferred embodiment to absolutely prove the present invention and being lifted, protection model of the invention
Enclose not limited to this.Equivalent substitute or conversion that those skilled in the art are made on the basis of the present invention, in the present invention
Protection domain within.Protection scope of the present invention is defined by claims.
Claims (5)
1. a kind of method for lifting epoxy resin edge flashing intensity, it is characterised in that：Comprise the following steps：
1) it is nano combined：Al is added during epoxy resin cure machine-shaping2O3Nano particle carries out nano combined processing,
Obtain epoxy resin samples；
2) it is cleaned and dried：It will be dried after the epoxy resin samples cleaning of shaping；
3) surface fluorination：By step 2) in cleaned dried epoxy resin samples carry out surface fluorination processing, and in epoxy
Resin sample surface forms fluorinated layer.
2. the method for lifting epoxy resin edge flashing intensity according to claim 1, it is characterised in that：The step 1)
In, it is to the method that epoxy resin carries out nano combined processing：Epoxy resin, curing agent and catalyst by proportion are placed in container
In, and be put into after magnetic stir bar in container to be placed on heating magnetic stirring apparatus and carry out heating stirring, the first mixed liquor is obtained,
And the parameter of heating stirring is：50-100 DEG C of temperature, rotating speed 500-1500r/min, mixing time 5-180min；
Then Al is proportionally added into the first obtained mixed liquor2O3Nano particle and coupling agent, continue on magnetic stirring apparatus
Heating stirring, obtains the second mixed liquor, and the parameter of heating stirring is：50-100 DEG C, rotating speed 500-1500r/min, during stirring
Between 5-180min；
The second mixed liquor is inserted after the completion of heating stirring ultrasonic agitation is carried out in ultrasonic oscillator, mixing time is 5-
240min；Most obtain epoxy resin samples through vacuum outgas and the process machine-shaping that is heating and curing afterwards.
3. the method for lifting epoxy resin edge flashing intensity according to claim 2, it is characterised in that：The asphalt mixtures modified by epoxy resin
Fat, curing agent, catalyst, Al2O3The weight of nano particle and coupling agent is：100 parts of epoxy resin；Curing agent 80-90
Part；1-2 parts of catalyst；Al2O30.1-5 parts of nano particle；0.1-2 parts of coupling agent.
4. the method for lifting epoxy resin edge flashing intensity according to claim 1, it is characterised in that：The step 2)
In, the epoxy resin samples absolute ethyl alcohol after shaping and deionized water are alternately cleaned first, then using ultrasonic cleaning machine
Cleaned, be finally rinsed again with deionized water；Epoxy resin samples after cleaning, which are placed in vacuum drying chamber, to be done
Dry, drying condition is：50-120 DEG C of temperature, time 1-48h.
5. the method for lifting epoxy resin edge flashing intensity according to claim 1, it is characterised in that：To epoxy resin
Sample carry out surface fluorination processing method be：Epoxy resin samples after cleaning-drying are put into progress surface fluorine in reactor
Change is handled, and the condition of surface fluorination processing is：The mixed gas or nitrogen constituted using inert gas and fluorine gas is constituted with fluorine gas
Mixed gas be fluorinated, the volumetric concentration of fluorine gas is 1-50% in gaseous mixture, and fluorination temperature is 20-80 DEG C, in reactor
The air pressure of mixed gas is 0.1-1bar, and the fluorination time is 5-240min.
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