CN105602248A - Polymer insulator material and preparation method thereof - Google Patents
Polymer insulator material and preparation method thereof Download PDFInfo
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- CN105602248A CN105602248A CN201610061479.9A CN201610061479A CN105602248A CN 105602248 A CN105602248 A CN 105602248A CN 201610061479 A CN201610061479 A CN 201610061479A CN 105602248 A CN105602248 A CN 105602248A
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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
- C08K9/10—Encapsulated 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
- 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
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/303—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups H01B3/38 or H01B3/302
- H01B3/306—Polyimides or polyesterimides
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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
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention discloses a polymer insulator material which is prepared from, by mass, 90-99% of polyimide and 1-10% of zinc oxide powder. A preparation method includes the following steps of firstly, adding nanometer zinc oxide powder to a mixed alcohol-water solution containing a coupling agent, dispersing the mixed solution through the ultrasonic oscillation and high-speed stirring combined mode, and conducting grinding after vacuum drying to obtain modified nanometer zinc oxide micro powder; secondly, dispersing the modified nanometer zinc oxide micro powder in the first step in ethyl alcohol, adding polyimide to be evenly stirred and dried to obtain the polymer insulator material powder, and pressing and forming the prepared polymer insulator material powder. The compound sample is prepared through a blending compound mode, operation is easy, conditions are easy to control, the environment is not polluted, and the material can be applied to preparation of polymer insulators of various powder materials. Therefore, the material has the advantages of being wide in application range, high in reliability, simple in process, high in operability and the like.
Description
Technical field
The invention belongs to electric high-voltage insulating materials field, be specifically related to a kind of polymer insulator material and preparation method thereof.
Background technology
Polymer has good electrical insulation properties, wide at field quilts such as aerospace industry, power system insulation, microelectronicsGeneral use is important insulation fabric part in electric high-voltage insulating materials field. But, when solid insulator is in vacuum gapDuring as support or insulation partition, can on insulator and vacuum interface, produce far below insulator intrinsic breakdown field intensity or vacuumThe edge flashing electric discharge phenomena of gap breakdown field intensity. Vacuum flashover phenomenon has seriously restricted the electric strength of compound inslation system, dodgesNetwork discharge pulse not only can interfere with the normal work of sensitive electrical devices on power equipment, and more serious electric discharge even can cause electricitySub-device and insulator part are discharged pulse and burn, and have a strong impact on reliability and the life-span of power equipment. According to related data reportRoad, the problem that the Aerospace Satellite of the accelerator of USDOE and Japan all once caused because of vacuum component generation edge flashing phenomenonAnd be damaged, cause very big economic loss. As can be seen here, edge flashing phenomenon is the core of restriction electrical equipment electric pressureThe Main Bottleneck that heart factor is also current development high voltage, high-power, compact apparatus faces.
Vacuum edge flashing research normally gets according to engineering is actual abstract, and through years of researches, academic circles at present is generalThink that vacuum edge flashing roughly can be divided into following three phases: 1. initial period---produce initiating electron; 2. developing stage---form electron multiplication; 3. the flashover stage---form penetrability gas discharge channel. Therefore, send out for vacuum edge flashingExhibition mechanism, effectively improves the method for insulator edge flashing voltage and just can set about from the following aspects: 1. reduce near negative electrodeInterface electric field intensity, key factor three binding sites (electrode---insulator surface---the vacuum three who makes to cause flashoverIntersection) near local formate field intensity reduce, cause the voltage that flashover development need is higher to trigger; 2. suppress electron avalancheEvolution, has reduced ionization by collision and secondary in charge migration process; 3. reduce the degassed rate of insulator surface.But, be applied to insulator under varying environment and be mainly above-mentioned any or several mechanism and playing a role, and need logicalCrossing which kind of processing mode can the most effectively reach and improve insulator vacuum edge flashing performance and be still a problem demanding prompt solution.
Under direct current high electric field effect, polymeric material very easily forms space charge, and the gathering of space charge can cause local electricity in mediumThe compound of electric charge accelerated, increased to field distortion, thermionic emission and encourage, accelerate the aging and local discharge breakdown of polymeric materialDeng. Due to this distortion effect of space charge to electric field, space charge to the electricity of insulating material of polymer lead, aging, punctureThe electric property of the each side such as destruction has obvious impact, and the French scholar Blaise of foundation and Gressus were 90 years last centuryThe electronics proposing for the initial stage triggers dipole alignment relaxation (ElectronTriggeredPolarizationRelaxation, EPTR) hypothesis modelKnown, the trap parameters in vacuum edge flashing voltage and the medium top layer of insulator has extremely close contacting.
The difference of polymeric material trap parameters can cause material surface charge injection degree difference, thereby forms inhomogeneous on top layerSpace charge and distribution, affect the evolution of electron avalanche, then affect its vacuum flashover property. Improve polymeric material skyBetween a kind of method of electric charge carry out exactly mixed nanometer. Polyimides is the high-molecular organic material of combination property the best in polymerOne of, but in pure polyimides dielectric, the existence of space charge can directly cause the change that its internal electric field distributes, to media tableThe effect that weakens or strengthen is played by the internal field of layer. In prior art, relate to and prepare the compound polyimide that electric durability can be goodThe method of film reaches its maturity, wherein applies with the product of du pont company, company of Ube Industries Ltd. and Zhong Yuan companyThe most extensive, but, good vacuum-resistant edge flashing performance polyimide structures part there is for preparation, for technical know-how etc.Reason, external result of study in recent years does not almost have; The research of domestic related fields, substantially in space state, in recent years shouldFor polyimide insulative structural member generation edge flashing under some particular surroundings causes, the impaired event of equipment happens occasionally, and showsResearch and development high-performance polyimide insulation fabric part is badly in need of in China, to meet the needs of modern electrical equipment.
Chinese patent CN102153858A discloses a kind of composite insulating material, and nylon is matrix, nano titanium oxide and fluorine goldMica is doping phase. The content of nylon is 60～90wt%, and the content of nano titanium oxide is no more than 30wt%, fluorophologopiteContent is no more than 10wt%. Described composite insulating material has high vacuum flashover voltage, low surface second electron emission coefficiency, lowDielectric constant, good weatherability. There is following shortcoming in this patent: the aging and local discharge breakdown of the resistance to electricity of this compositePerformance is lower; The nonlinear conductance characteristic of composite is poor, does not relate to anti-interior chargeding performance; This composite can only be generallyEnvironment under use, cannot be applied to the adverse circumstances such as radiation, high low temperature conversion; Preparation method's forming materials difficulty of this invention.
Summary of the invention
Object of the present invention is exactly for a kind of polymer insulator material and preparation method thereof is provided.
To achieve these goals, the present invention adopts following technical scheme:
A kind of polymer insulator material, comprises matrix resin and Nano filling, described matrix resin be polyimides (preferably:Thermoplastics type's polyimides), described Nano filling is Zinc oxide powder.
This polymer insulator material is in the application of preparing in vacuum high-pressure insulating device.
The mass percent of the above-mentioned each component of polymer insulator material is: matrix resin is that 90-99%, zinc oxide filler are1％-10％。
The median particle diameter 40-60 of described matrix resin (preferably 50) μ m, the median particle diameter 10-30 of described Nano filling is (excellentSelect 20) nm.
The preparation method of above-mentioned polymer insulator material, comprises the following steps:
(1) nano zine oxide powder is joined in the mixed alcohol aqueous solution that contains coupling agent (preferably in the mixed alcohol aqueous solution, secondThe volume ratio of alcohol and water is: 95:5, and coupling agent consumption is the 3%-5% of nano zine oxide powder quality, coupling agent is γ-ammonia thirdEthyl triethoxy silicane alkane), more above-mentioned mixed solution is carried out to sonic oscillation and carries out dispersion treatment in conjunction with the mode of high-speed stirred (excellentChoosing: 30-60min), after vacuum drying (preferably: 105-120 DEG C, vacuum 10Pa condition), grinding can obtain after modificationNano oxidized zinc powder;
(2) the nano oxidized zinc powder after step (1) modification is scattered in to alcohol (that is: absolute ethyl alcohol) afterwards (preferably: wineEssence volumetric usage is nano zine oxide and polyimide molding powder 3～5 times), then add polyimides (preferably: polyimides existsBefore use: be placed in vacuum drying chamber 12-24h, baking temperature 120-150 DEG C, vacuum 10Pa. ) rapid stirring stirs evenly post-drying,The composite powder that must handle well, can obtain polymer insulation by compressing the polymer insulator material powder preparingSub-material.
A preparation method for composite insulator, comprises the following steps: comprise step (1) and the step (2) of said method, alsoComprise: (3) cold moudling: briquetting pressure is 10-15MPa, the duration is 10-15s; (4) segmented HTHP moulding:The preformed stage starts 40-60min by room temperature and rises to 270 DEG C, and high pressure keeps 10MPa; Holding stage is at 270 DEG C, under 10MPaInsulation 20min, now composite is in molten state; Rise to temperature 300-320 DEG C with 5-10min again, insulation 30-40min,High pressure keeps 15MPa to make composite material forming, cools to 200 DEG C of composite insulators that can take out moulding.
First the present invention adopts chemical reagent to carry out modification to nanoparticle surface, to reduce nanoparticle surface activity, subtractsThe surface polarity of weak particle, improves the surperficial wettability of particle, reaches and improves the boundary of nano particle in polymeric matrixFace compatibility, make nanometer additive in PI resin good dispersion to obtain good nano effect; Secondly, the present invention is by adoptingCarry out dispersion phase mixed solution by high-speed stirred and supersonic oscillations mode, it is strong that homogenizer generates while rotation in solutionThe nanoparticle of shearing force meeting agglomerated is disperseed again, and in addition, hyperacoustic cavitation also can play the dispersion of nano particleGood result. Nanoclusters aggressiveness is in the time that stirring action can not disperse completely, and the pressure that ultrasonic wave produces can cause liquid mediumMolecule sharp pounding, acts on aggregate and makes it to be dispersed into single nano particle; Meanwhile, be coated on the coupling of nanoparticle surfaceAgent also can impel nanoparticle subsolution reunite and to its modifying surface processing; Last the present invention adopts the moulding of segmented HTHPLegal system is made composite sample, makes unmanageable polyimide molding powder can well moulding.
Zinc oxide is stronger than titanium oxide to the absorbability of light, and nano zine oxide has UV absorption bandwidth, the advantage that ability is strong,Long to ultraviolet shielded wave band, nano zine oxide, having obvious superiority aspect anti-light degradation, can improve material significantlyAgeing-resistant performance. The preferred ZnO additive of the present invention is for ZnO, ultraviolet absorption characteristic to be conducive to carry on the one handAging and the local discharge breakdown performance of the resistance to electricity of high polymer material, it is significant that this is applied to extreme environment to material; SeparatelyOn the one hand, the matrix resin that adds ZnO has good non-linear C-V characteristic, makes it have better anti-interior chargeding performance,This is that titanium oxide can not possess.
The present invention is by nano inorganic zinc oxide ultra_fine powders and special engineering plastics polyimide matrix are carried out to blend moulding, at matrixBetween resin and additive, form a large amount of interface traps, and because the less interface trap that causes of size of filler is darker, poly-In compound, introduce a large amount of deep traps, increased catching and the detrapping time of carrier, reduced the mobility of carrier. Direct current is highUnder electric field action, in polymeric material, carrier mobility very easily forms space charge, and the gathering of space charge can cause in medium localElectric field distortion, thermionic emission are accelerated, are increased the compound of electric charge and hit with the aging and shelf depreciation of excitation, acceleration polymeric materialWear etc.
The prepared compound polyimide material of the present invention is compared with pure polyimides, and nano modification has improved deep trap density, fallsThe low mobility of electric charge carrier, has reduced ionization by collision and the secondary in transition process, has limited electric charge and has been situated betweenWith the transporting of interface, suppress the development of flashover in plastid, therefore can significantly improve the vacuum edge flashing electricity of composite insulatorPress.
Technical scheme of the present invention has following beneficial effect:
1, the present invention adopts composite legal system for composite sample, and simple to operate, condition is easily controlled, free from environmental pollution, can be applicable toThe polymer insulator preparation of multiple powder body material. Therefore there is wide application, reliability is high, technique is simple, workableEtc. advantage;
2, sample preparation process of the present invention is not subject to the effects limit such as external environment condition temperature, humidity;
3, the present invention can accurate adjustment filer content, optimizes the composite sample of best proportioning.
Brief description of the drawings
Fig. 1 is nano zine oxide scatter diagram in the present invention;
In figure: 1, ultrasonic dispersion machine, 2, high speed agitator, 3, beaker, 4, support;
Fig. 2 is the compound polyimide insulator vacuum edge flashing voltage pattern with different content nano zine oxide filler;
Fig. 3 is the compound polyimide insulator trap level variation diagram with different content nano zine oxide filler.
Detailed description of the invention
Below in conjunction with accompanying drawing and embodiment, the invention will be further described.
Embodiment 1:
Step 1: thermoplastics type's polyimide molding powder pretreatment: take the polyimide molding powder of default quality, then putIn vacuum drying chamber 24h, 120 DEG C of baking temperatures, vacuum 10Pa, obtains polyimide matrix raw material after pretreatment;
Step 2: cold moudling: dry step 1 rear pure polyimide material powder is placed in to grinding tool and carries out cold moudling, becomeType pressure is 10MPa, and the duration is 15s;
Step 3: segmented HTHP moulding: the sample after step 2 cold moudling is placed in to moulding press, and to carry out segmented highTemperature high-pressure molding, starts 60min by room temperature and rises to 270 DEG C, and high pressure keeps 10MPa; 270 DEG C, under 10MPa, be incubated 20min,Now pure polyimide material is in molten state; Rise to 300 DEG C of temperature with 5min again, insulation 40min, high pressure keeps 15MPaMake polyimide material moulding; Naturally cool to 200 DEG C and take out sample.
Embodiment 2:
Step 1: nano zine oxide fillers dispersed and surface treatment: first ethanol, deionized water are mixed according to the ratio of 95:5After closing, the alcohol solution that adds coupling agent to be prepared into contain coupling agent, then joins nano zine oxide powder to contain coupling agentThe mixed alcohol aqueous solution in. Wherein coupling agent consumption is 3% of nano zine oxide powder quality. Again above-mentioned mixed solution is placed in superIn acoustic wave oscillator, carry out sonic oscillation and in conjunction with the mode of high-speed stirred, inorganic microparticle-dispersed processed to 30min, as shown in Figure 1.Subsequently above-mentioned scattered suspension is put into vacuum drying chamber and be dried processing, 105 DEG C of baking temperatures, vacuum 10Pa,Grinding obtains the inorganic nano zinc oxide ultra_fine powders after modification, and described coupling agent is gamma-aminopropyl-triethoxy-silane.
The pretreatment of thermoplastics type's polyimide molding powder, takes the polyimide molding powder of presetting quality, is then placed on vacuum dryDry case 24h, 120 DEG C of baking temperatures, vacuum 10Pa, obtains polyimide matrix raw material after pretreatment;
Step 2: liquid phase blending and stirring and drying and processing: take the modification rear oxidation zinc inorganic powder of default quality, add certainIn the alcohol of volume, then the suspension of micro mist and alcohol is placed in to ultrasonic vibration instrument and disperses 30min, treat that micro mist is uniformly dispersedAfter, add the polyimide molding powder of presetting quality, make zinc oxide content account for 1% of compound gross mass percentage, in beakerAdding volume is the alcohol formation suspension of 3 times of mixture volumes, and with after high speed agitator stirring 30min, puts into baking ovenDry 48h, 105 DEG C of bake out temperatures, the composite powder that obtains handling well;
Step 3: cold moudling: step 2 is dried to rear composite material powder and be placed in grinding tool and carry out cold moudling, briquetting pressureFor 10MPa, the duration is 15s;
Step 4: segmented HTHP moulding: the sample after step 3 cold moudling is placed in to moulding press, and to carry out segmented highTemperature high-pressure molding, starts 50min by room temperature and rises to 270 DEG C, and high pressure keeps 10MPa; 270 DEG C, under 10MPa, be incubated 20min,Now composite is in molten state; Rise to 310 DEG C of temperature with 5min again, insulation 30min, high pressure keeps 15MPa to make compoundForming materials; Naturally cool to 200 DEG C and take out sample.
Embodiment 3:
Step 1: nano zine oxide fillers dispersed and surface treatment: first ethanol, deionized water are mixed according to the ratio of 95:5After closing, the alcohol solution that adds coupling agent to be prepared into contain coupling agent, then joins nano zine oxide powder to contain coupling agentThe mixed alcohol aqueous solution in. Wherein coupling agent consumption is 3% of nano zine oxide powder quality. Again above-mentioned mixed solution is placed in superIn acoustic wave oscillator, carry out sonic oscillation and in conjunction with the mode of high-speed stirred, inorganic microparticle-dispersed processed to 30min, as shown in Figure 1.Subsequently above-mentioned scattered suspension is put into vacuum drying chamber and be dried processing, 105 DEG C of baking temperatures, vacuum 10Pa,Grinding obtains the inorganic nano zinc oxide ultra_fine powders after modification, and described coupling agent is gamma-aminopropyl-triethoxy-silane.
The pretreatment of thermoplastics type's polyimide molding powder, takes the polyimide molding powder of presetting quality, is then placed on vacuum dryDry case 24h, 120 DEG C of baking temperatures, vacuum 10Pa,, obtain polyimide matrix raw material after pretreatment;
Step 2: liquid phase blending and stirring and drying and processing: take the modification rear oxidation zinc inorganic powder of default quality, add certainIn the alcohol of volume, then the suspension of micro mist and alcohol is placed in to ultrasonic vibration instrument and disperses 30min, treat that micro mist is uniformly dispersedAfter, add the polyimide molding powder of presetting quality, make zinc oxide content account for 3% of compound gross mass percentage, in beakerAdding volume is the alcohol formation suspension of 3 times of mixture volumes, and with after high speed agitator stirring 60min, puts into baking ovenDry 24h, 120 DEG C of bake out temperatures, the composite powder that obtains handling well;
Step 3: cold moudling: step 2 is dried to rear composite material powder and be placed in grinding tool and carry out cold moudling, briquetting pressureFor 15MPa, the duration is 10s;
Step 4: segmented HTHP moulding: the sample after step 3 cold moudling is placed in to moulding press, and to carry out segmented highTemperature high-pressure molding, starts 50min by room temperature and rises to 270 DEG C, and high pressure keeps 10MPa; 270 DEG C, under 10MPa, be incubated 20min,Now composite is in molten state; Rise to 300 DEG C of temperature with 5min again, insulation 40min, high pressure keeps 15MPa to make compoundForming materials; Naturally cool to 200 DEG C and take out sample.
Embodiment 4:
Step 1: nano zine oxide fillers dispersed and surface treatment: first ethanol, deionized water are mixed according to the ratio of 95:5After closing, the alcohol solution that adds coupling agent to be prepared into contain coupling agent, then joins nano zine oxide powder to contain coupling agentThe mixed alcohol aqueous solution in. Wherein coupling agent consumption is 5% of nano zine oxide powder quality. Again above-mentioned mixed solution is placed in superIn acoustic wave oscillator, carry out sonic oscillation and in conjunction with the mode of high-speed stirred, inorganic microparticle-dispersed processed to 30min, as shown in Figure 1.Subsequently above-mentioned scattered suspension is put into vacuum drying chamber and be dried processing, 105 DEG C of baking temperatures, vacuum 10Pa,Grinding obtains the inorganic nano zinc oxide ultra_fine powders after modification, and described coupling agent is gamma-aminopropyl-triethoxy-silane.
The pretreatment of thermoplastics type's polyimide molding powder, takes the polyimide molding powder of presetting quality, is then placed on vacuum dryDry case 24h, 120 DEG C of baking temperatures, vacuum 10Pa, obtains polyimide matrix raw material after pretreatment;
Step 2: liquid phase blending and stirring and drying and processing: take the modification rear oxidation zinc inorganic powder of default quality, add certainIn the alcohol of volume, then the suspension of micro mist and alcohol is placed in to ultrasonic vibration instrument and disperses 30min, treat that micro mist is uniformly dispersedAfter, add the polyimide molding powder of presetting quality, make zinc oxide content account for 5% of compound gross mass percentage, in beakerAdding volume is the alcohol formation suspension of 3 times of mixture volumes, and with after high speed agitator stirring 60min, puts into baking ovenDry 24h, 120 DEG C of bake out temperatures, the composite powder that obtains handling well;
Step 3: cold moudling: step 2 is dried to rear composite material powder and be placed in grinding tool and carry out cold moudling, briquetting pressureFor 15MPa, the duration is 10s;
Step 4: segmented HTHP moulding: the sample after step 3 cold moudling is placed in to moulding press, and to carry out segmented highTemperature high-pressure molding, starts 50min by room temperature and rises to 270 DEG C, and high pressure keeps 10MPa; 270 DEG C, under 10MPa, be incubated 20min,Now composite is in molten state; Rise to 305 DEG C of temperature with 5min again, insulation 40min, high pressure keeps 15MPa to make compoundForming materials; Naturally cool to 200 DEG C and take out sample.
Embodiment 5:
Step 1: nano zine oxide fillers dispersed and surface treatment: first ethanol, deionized water are mixed according to the ratio of 95:5After closing, the alcohol solution that adds coupling agent to be prepared into contain coupling agent, then joins nano zine oxide powder to contain coupling agentThe mixed alcohol aqueous solution in. Wherein coupling agent consumption is 5% of nano zine oxide powder quality. Again above-mentioned mixed solution is placed in superIn acoustic wave oscillator, carry out sonic oscillation and in conjunction with the mode of high-speed stirred, inorganic microparticle-dispersed processed to 30min, as shown in Figure 1.Subsequently above-mentioned scattered suspension is put into vacuum drying chamber and be dried processing, 105 DEG C of baking temperatures, vacuum 10Pa,Grinding obtains the inorganic nano zinc oxide ultra_fine powders after modification, and described coupling agent is gamma-aminopropyl-triethoxy-silane.
The pretreatment of thermoplastics type's polyimide molding powder, takes the polyimide molding powder of presetting quality, is then placed on vacuum dryDry case 24h, 120 DEG C of baking temperatures, vacuum 10Pa, obtains polyimide matrix raw material after pretreatment;
Step 2: liquid phase blending and stirring and drying and processing: take the modification rear oxidation zinc inorganic powder of default quality, add certainIn the alcohol of volume, then the suspension of micro mist and alcohol is placed in to ultrasonic vibration instrument and disperses 60min, treat that micro mist is uniformly dispersedAfter, add the polyimide molding powder of presetting quality, make zinc oxide content account for 10% of compound gross mass percentage, to beakerIn to add volume be that the alcohol of 4 times of mixture volumes forms suspension, and stir after 60min with high speed agitator, put into baking ovenMiddle oven dry 24h, 120 DEG C of bake out temperatures, the composite powder that obtains handling well;
Step 3: cold moudling: step 2 is dried to rear composite material powder and be placed in grinding tool and carry out cold moudling, briquetting pressureFor 15MPa, the duration is 10s;
Step 4: segmented HTHP moulding: the sample after step 3 cold moudling is placed in to moulding press, and to carry out segmented highTemperature high-pressure molding, starts 50min by room temperature and rises to 270 DEG C, and high pressure keeps 10MPa; 270 DEG C, under 10MPa, be incubated 20min,Now composite is in molten state; Rise to 320 DEG C of temperature with 5min again, insulation 30min, high pressure keeps 15MPa to make compoundForming materials; Naturally cool to 200 DEG C and take out sample.
Polyimides sample before and after modification is respectively got to 5, be less than 10 at temperature 298K, air pressure-4Continuous direct current in Pa vacuum chamberFlashover 30 times, pressuring method takes ladder to boost, gradient is 100V/s, adjacent twice arcing time be spaced apart 60s, electrodeThe circular gold-plated membrane electrode that adopts Φ 20mm, thickness is 1 μ m, spacing 2mm.
Adopt the method in the present invention, the sub-sample vacuum of the polyimide insulative direct current edge flashing after inorganic nano-filler modificationBefore average voltage is more unmodified, be significantly improved, as shown in Figure 2. From Fig. 2 and Fig. 3, can also find, containing Nano fillingComposite sample trap level and trap density be significantly higher than pure polyimides sample, and along with nanometer additive mass fractionIncrease present first rise, downward trend again, and the Changing Pattern of the vacuum edge flashing voltage of insulator and sample trap levelVariation there is the high goodness of fit. Nano modification has improved deep trap density, has reduced the mobility of electric charge carrier, reducesIonization by collision and secondary in transition process, limited electric charge in dielectric with the transporting of interface, suppressedThe development of flashover, has improved flashover voltage.
By reference to the accompanying drawings the specific embodiment of the present invention is described although above-mentioned, not the limit to protection domain of the present inventionSystem, one of ordinary skill in the art should be understood that on the basis of technical scheme of the present invention, those skilled in the art do not need to payGo out various amendments that creative work can make or distortion still in protection scope of the present invention.
Claims (10)
1. a polymer insulator material, is characterized in that: comprise matrix resin and Nano filling, described matrix resin is polyamidesImines, described Nano filling is Zinc oxide powder.
2. polymer insulator material as claimed in claim 1, is characterized in that: described matrix material is thermoplastics type's polyimides.
3. polymer insulator material as claimed in claim 1, is characterized in that: the described each component of polymer insulator materialMass percent is: matrix resin is that 90-99%, zinc oxide filler are 1%-10%.
4. polymer insulator material as claimed in claim 1, is characterized in that: the median particle diameter of described matrix resin40-60 μ m, the median particle diameter 10-30nm of described Nano filling.
5. the arbitrary described polymer insulator material of claim 1-4 is in the application of preparing in vacuum high-pressure insulating device.
6. the preparation method of the arbitrary described polymer insulator material of claim 1-4, is characterized in that: comprise the following steps:
(1) nano zine oxide powder is joined in the mixed alcohol aqueous solution that contains coupling agent, more above-mentioned mixed solution is surpassedSound oscillation is also carried out dispersion treatment in conjunction with the mode of high-speed stirred, grinds the nano zine oxide that can obtain after modification after vacuum dryingMicro mist;
(2) the nano oxidized zinc powder after step (1) modification is scattered in after alcohol, then after adding polyimides to stir evenlyDry, obtain polymer insulator material powder, by compressing the polymer insulator material powder preparing.
7. preparation method as claimed in claim 6, is characterized in that: described in described step (1) in the mixed alcohol aqueous solution, and secondThe volume ratio of alcohol and water is: 95:5, coupling agent consumption is the 3%-5% of nano zine oxide powder quality.
8. preparation method as claimed in claim 6, is characterized in that: described in described step (1), coupling agent is γ-aminopropyl threeEthoxysilane.
9. a preparation method for composite insulator, is characterized in that: comprise step claimed in claim 6 (1) and step (2),Also comprise: step (3) cold moudling: briquetting pressure is 10-15MPa, the duration is 10-15s; Step (4) segmentedHTHP moulding: the preformed stage starts 40-60min by room temperature and rises to 270 DEG C, high pressure keeps 10MPa; Holding stage exists270 DEG C, under 10MPa, be incubated 20min; Rise to temperature 300-320 DEG C with 5-10min again, insulation 30-40min, high pressure keeps15MPa makes composite material forming can obtain composite insulator.
10. the composite insulator being prepared by preparation method claimed in claim 9.
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Cited By (4)
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| CN110256849A (en) * | 2019-07-19 | 2019-09-20 | 扬州苏伟新材料科技有限公司 | A kind of high flashover voltage polyamide acidic group compound resin and preparation method thereof |
| CN111334041A (en) * | 2020-03-26 | 2020-06-26 | 中国科学院兰州化学物理研究所 | Polyimide lubricating material filled with nano titanium nitride and preparation method thereof |
| CN111995774A (en) * | 2020-08-20 | 2020-11-27 | 株洲时代新材料科技股份有限公司 | Preparation method of wear-resistant polyamide-imide molding powder |
| WO2024099008A1 (en) * | 2022-11-10 | 2024-05-16 | 电子科技大学长三角研究院(湖州) | Method and system for improving internal electrification resistance of polyimide medium |
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| CN104134499A (en) * | 2014-08-05 | 2014-11-05 | 国家电网公司 | High-voltage composite insulator |
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| US20120229981A1 (en) * | 2011-03-09 | 2012-09-13 | Chen-Lung Lin | Electrically insulating and thermally conductive composition and electronic device |
| CN102391646A (en) * | 2011-11-07 | 2012-03-28 | 西安交通大学 | Enhanced high-insulation composite material and preparation method thereof |
| CN104134499A (en) * | 2014-08-05 | 2014-11-05 | 国家电网公司 | High-voltage composite insulator |
| CN105153699A (en) * | 2015-07-31 | 2015-12-16 | 江苏省电力公司泰州供电公司 | Preparation method of hyper branched copolymerized polyimide/zinc oxide (ZnO) hybrid insulated film |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110256849A (en) * | 2019-07-19 | 2019-09-20 | 扬州苏伟新材料科技有限公司 | A kind of high flashover voltage polyamide acidic group compound resin and preparation method thereof |
| CN111334041A (en) * | 2020-03-26 | 2020-06-26 | 中国科学院兰州化学物理研究所 | Polyimide lubricating material filled with nano titanium nitride and preparation method thereof |
| CN111334041B (en) * | 2020-03-26 | 2021-07-23 | 中国科学院兰州化学物理研究所 | Polyimide lubricating material filled with nano titanium nitride and preparation method thereof |
| CN111995774A (en) * | 2020-08-20 | 2020-11-27 | 株洲时代新材料科技股份有限公司 | Preparation method of wear-resistant polyamide-imide molding powder |
| CN111995774B (en) * | 2020-08-20 | 2023-02-07 | 株洲时代新材料科技股份有限公司 | Preparation method of wear-resistant polyamide-imide molding powder |
| WO2024099008A1 (en) * | 2022-11-10 | 2024-05-16 | 电子科技大学长三角研究院(湖州) | Method and system for improving internal electrification resistance of polyimide medium |
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