CN101506301A - Casting resin composition, insulating material using the same, and insulating structure - Google Patents
Casting resin composition, insulating material using the same, and insulating structure Download PDFInfo
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- CN101506301A CN101506301A CNA2007800312162A CN200780031216A CN101506301A CN 101506301 A CN101506301 A CN 101506301A CN A2007800312162 A CNA2007800312162 A CN A2007800312162A CN 200780031216 A CN200780031216 A CN 200780031216A CN 101506301 A CN101506301 A CN 101506301A
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Abstract
An insulating cast resin composition including an epoxy resin having two or more epoxy groups per single molecule; a micro-particle including one or more substances selected from the group of silica, alumina and mullite; an elastomer particle; and a nano-particle including one or more substances selected from the group of layer silicates, oxides and nitrides.
Description
Technical field
The present invention relates to send in the high-tension machines of employing such as power transformation machine and play the casting resin composition of insulating effect and adopt its insulating material, insulating structure.
Background technology
Power delivery network from the power station to the user, transmitting and transforming equipment is set everywhere, in each transmitting and transforming equipment, send the power transformation machine in order to open and close high voltage circuit etc., be provided with in the distribution clutch of depositing vacuum valve, the gas insulation opening and closing arrangement of enclosing sulfur hexafluoride gas and the pipeline gas power transmission device etc.Send in the power transformation machine at these,, can utilize the insulating material of resinous composition for making the insulation of vacuum valve and high-pressure conductor.
The insulating material that uses in the above-mentioned purpose must have physical strength, thermotolerance and electrical insulating property, and considers from the viewpoint that reduces cost, and can adopt the Resins, epoxy as thermosetting resin.In addition, from improving purposes such as mechanical characteristics and electrical insulating property, the known employing is dispersed in technology in the Resins, epoxy to various particles.The spy opens the 2002-15621 communique, the spy opens the 2001-160342 communique and the special 2006-57017 communique of opening discloses relevant technology.
Summary of the invention
The insulating material that adopts above-mentioned each correlation technique to make, when with it when being molded as the casting type resin of conductor, the generation several technical issues.At first, insufficient approaching as the thermal expansivity of the thermal expansivity of insulating material and conductor, then have to produce the worry of peeling off in conductor boundary with molding.In addition, because conductor and insulating material very closely bond, take place in the part so the insulating material that discharge causes wears out, the position that the patience in the insulating material is low develops rapidly and is dendroid (referring to the application Fig. 2, being called branchization (treeing) below).Because this progress is exceedingly fast, the insulation breakdown time of casting type resin depends on anti-branch voltinism specially.Research according to the inventor, adopt the special insulating material of opening 2002-15621 number disclosed technology, the inadequate shortcoming of anti-branch voltinism is arranged, open the insulating material of the disclosed technology of 2006-57017 communique according to the spy, because big, so there is the easy shortcoming of peeling off between conductor and the insulating material with the difference of the coefficient of thermal expansion of conductor.
The present invention its objective is that for the shortcoming that overcomes these technology proposes providing a kind of has binding property with conductor molding, and the insulating material, the insulating structure that have the casting resin composition of high anti-branch voltinism and adopt it.
According to the 1st aspect of the present invention, the insulativity casting resin composition contains: the epoxy compounds that has 2 above epoxy group(ing) in per 1 molecule; Contain the micropartical of material more than a kind that is selected from silicon-dioxide, aluminum oxide, mullite; Contain the nanoparticle of material more than a kind that is selected from laminar silicic acid salt compound, oxide compound, nitride; And elastomerics particle.
According to the 2nd aspect of the present invention, insulating material contains the cured article of above-mentioned casting resin composition.
According to the 3rd aspect of the present invention, insulating structure has: conductor; And contain above-mentioned insulating material, carrying out the insulating insulating component between above-mentioned conductor and other members.
Description of drawings
Fig. 1 is a particle dispersion state mimic diagram in the insulating material that relates to of one of the present invention embodiment.
Fig. 2 is the aging route state of progress mimic diagram from the pin electrode front end.
Fig. 3 is the erosion state mimic diagram that is produced from the discharge of clavate electrode front end.
Fig. 4 is one of the insulating structure that a present invention relates to illustration.
Fig. 5 is the another illustration of insulating structure that the present invention relates to.
Fig. 6 is the SEM image of the insulating material section of comparative example 1.
Embodiment
As follows about embodiment of the present invention with reference to description of drawings.
As using in the scope of this specification and claims book, the sentence of so-called " branchization is aging " mean " it is aging to develop into dendritic electricity in the insulating material ", and the implication of " branchization " speech means its progress.
The casting resin composition of one of the present invention embodiment roughly contains: (A) epoxy compounds that has 2 above epoxy group(ing) in per 1 molecule; (B) contain the micropartical of material more than a kind that is selected from silicon-dioxide, aluminum oxide, mullite; (C) elastomerics particle; And (D) contain the nanoparticle of material more than a kind that is selected from laminar silicic acid salt compound, oxide compound, nitride.
(A) epoxy compounds
As above-mentioned epoxy compounds, so long as contain in per 1 molecule that the compound by 3 yuan of rings that 2 carbon atoms and 1 Sauerstoffatoms constituted more than 2 is solidified and the suitable compound that obtains gets final product, any all can employing and not being particularly limited.
This epoxy compounds, as its preferred example, can enumerate: the bisphenol A type epoxy resin that polyatomic phenol such as Epicholorohydrin and bisphenols or polyvalent alcohol obtain by condensation, the bisphenol A type epoxy resin that polyatomic phenol such as Epicholorohydrin and bisphenols or polyvalent alcohol obtain by condensation, brominated bisphenol a type epoxy resin, the hydrogenation bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol-s epoxy resin, bisphenol AF type Resins, epoxy, bisphenol-type epoxy resin, naphthalene type Resins, epoxy, fluorenes type Resins, epoxy, phenolic resin varnish type epoxy resin, phenol novolak type epoxy resin, adjacent methane type Resins, epoxy, three (hydroxy phenyl) methane type Resins, epoxy, Racemic glycidol ether type epoxies such as four phenolic group (Tetraphenicol) ethane type Resins, epoxy, and the glycidyl ester type epoxy resin that obtains by condensation of Epicholorohydrin and carboxylic acid, the hetero ring type Resins, epoxy such as glycolylurea type Resins, epoxy that three-glycidyl based isocyanate or Epicholorohydrin and glycolylurea (Hidaiton) class obtains by reaction.In addition, these both can use separately also and can use as mixture more than 2 kinds.
In order to solidify above-mentioned epoxy compounds, add the epoxy compounds solidifying agent.As the epoxy compounds solidifying agent, as long as carry out chemical reaction the epoxy compounds solidified material can suitably be adopted with epoxy compounds, its kind is limited.As this epoxy compounds solidifying agent, for example, can enumerate amine curing agent, acid anhydride type curing agent, imidazole curing agent, polythiol class solidifying agent, phenols curing agent, Louis's acids solidifying agent, isocyanates solidifying agent.
Object lesson as above-mentioned amine curing agent, for example, can enumerate quadrol, 1, the 3-diaminopropanes, 1, the 4-diaminobutane, hexamethylene-diamine, dipropylenediamine, polyether diamine, 2,5-dimethyl hexamethylene-diamine, trimethylhexamethylenediamine, diethylenetriamine, the two propyl group amine of imino-, two (hexamethyl) triamine, Triethylenetetramine (TETA), tetren, penten, amino ethyl ethanolamine, three (methylamino) hexane, dimethylamino propylamine, diethyl amino propylamine, the two propylamine of methyl-imino, menthanediamine (menthanedimine), isophorone diamine, two (4-amino-3-methyl bicyclic hexyl) methane, diamino-dicyclohexyl methane, two (amino methyl) hexanaphthene, N-aminoethyl piperazine, 3, two (the 3-aminopropyls) 2 of 9-, 4,8,10-four oxaspiros (5,5) undecane, m-xylenedimaine, mphenylenediamine, diaminodiphenyl-methane, diamino diphenyl sulfone, diamino diethyl ditan, the dicyano diamide, organic acid dihydrazide.
Object lesson as above-mentioned acid anhydride type curing agent, for example, dodecenyl succinic anhydride, poly-adipic anhydride, poly-nonane diacid acid anhydride, poly sebacic polyanhydride, poly-(ethyl octadecane diacid) acid anhydride, poly-(phenyl Thapsic acid) acid anhydride, methyl tetrahydrochysene anhydride phthalic acid, methyl six hydrogen anhydride phthalic acids, methyl Himic acid anhydrides, six hydrogen anhydride phthalic acids, the tetrahydrochysene anhydride phthalic acid, trialkyl tetrahydrochysene anhydride phthalic acid, the methylcyclohexane dicarboxylic anhydride, anhydride phthalic acid, trimellitic acid 1,2-anhydride, pyromellitic dianhydride, the benzophenone tetracarboxylic acid, the ethylene glycol bis trimellitate, glycerol three trimellitates, the hexachloro endoethylene tetrahydrophthalic acid acid anhydride, tetrabromophthalic anhydride Rou Dou guan acid anhydrides, methyl Rou Dou guan acid anhydrides, poly-nonane diacid acid anhydride.
As the object lesson of above-mentioned imidazole curing agent, for example, can enumerate glyoxal ethyline, 2-ethyl-4-methylimidazole, 2-heptadecyl imidazoles.In addition, as the object lesson of polythiol class solidifying agent, for example, can enumerate polysulphide, monothioester.
In addition, with above-mentioned epoxy compounds with solidifying agent and usefulness, also can add and promote or the epoxy compounds curing catalyst of gate ring oxygen compound curing reaction.Particularly, when adding acid anhydride type curing agent, because comparing, other solidifying agent such as its curing reaction and amine curing agent want slow, so many employing epoxy compounds curing catalysts.As the curing catalyst that acid anhydride type curing agent is used, tertiary amine or its salt, quaternary ammonium compound, imidazoles, alkali metal alcoholates etc. are preferred.
(B) micropartical
As above-mentioned micropartical, can enumerate any particle that contains silicon-dioxide, aluminum oxide, mullite, or its mixture more than 2 kinds.
Above-mentioned micropartical, above-mentioned relatively epoxy compounds 100 weight parts, it is preferred mixing with the ratio of 100～500 weight parts.Above-mentioned atomic use level, when above-mentioned relatively epoxy compounds 100 weight parts are lower than 100 weight parts, the coefficient of thermal expansion of casting resin composition strengthens because poor with the coefficient of thermal expansion of metallic conductor, then become and the metallic conductor of molding between produce the reason of peeling off.On the other hand, when relative epoxy compounds 100 weight parts of above-mentioned atomic use level surpassed 500 weight parts, the resin combination viscosity of cast molding rises, and was unfavorable to atomic mixture operation and cast molding operation.
The scope that above-mentioned atomic primary particle size is in 1～100 μ m is preferred.When above-mentioned atomic primary particle size was not in the scope of 1～100 μ m, the resin combination viscosity of cast molding rises, and was unfavorable to atomic mixture operation and cast molding operation.
(C) elastomerics particle
As above-mentioned elastomerics particle, contain elastomerics, can adopt the particle of core shell structure.As the ideal elastomerics, can enumerate styrene butadiene-Sipacril 2739OF, acrylic rubber, styrene butadiene ribber etc.These can separately or mix more than 2 kinds and use.In addition, do not have the elastomerics particle of core shell structure, as long as adopt special dispersion agent or dispersing method in resin, can homodispersely can adopt yet.
Above-mentioned relatively epoxy compounds 100 weight parts of above-mentioned elastomerics particle are preferred with the mixed of 1～30 weight part.When above-mentioned relatively epoxy compounds 100 weight parts of the use level of above-mentioned elastomerics particle were lower than 1 weight part, the toughness of cast molding resin combination cured article reduced.On the other hand, when above-mentioned relatively epoxy compounds 100 weight parts of the use level of above-mentioned elastomerics particle during greater than 30 weight parts, the viscosity of cast molding resin combination rises, and is unfavorable to atomic mixture operation and cast molding operation.
The scope that the primary particle size of above-mentioned elastomerics particle is in 0.1～10 μ m is preferred.When the primary particle size of above-mentioned elastomerics particle was not in the scope of 0.1～10 μ m, the toughness of cast molding resin combination cured article reduced.In addition, the resin combination viscosity of cast molding rises, and is unfavorable to atomic mixture operation and cast molding operation.
(D) nanoparticle
As above-mentioned nanoparticle, can enumerate any particle that contains laminar silicic acid salt compound, oxide compound, nitride, or its mixture more than 2 kinds.
As the laminar silicic acid salt compound, can enumerate and be selected from least a of the mineral substance that comprises smectites, mica group (mica), vermiculite class, mica group (mica isinglass).As the laminar silicic acid salt compound that belongs to smectites, for example, can enumerate montmorillonite, hectorite, saponite, sauconite, beidellite, white antimony, nontronite.As the laminar silicic acid salt compound that belongs to mica group, for example, can enumerate muriate, phlogopite, lithionite, white mica, biotite, paragonite, margarodite, taincolite, tetrasilicic acid mica.As the laminar silicic acid salt compound that belongs to the vermiculite class, for example, can enumerate three or eight stratiform vermiculites (trioctahedral vermiculite), three or eight stratiform vermiculites (dioctahedralvermiculite).As the laminar silicic acid salt compound that belongs to mica group, for example, can enumerate white mica, biotite, paragonite, lithionite, margarodite, brittle mica, barium iron brittle mica.Wherein, from the considerations such as dispersiveness epoxy compounds, it is preferred adopting the laminar silicic acid salt compound that belongs to the montmorillonite group.The laminar silicic acid salt compound can contain the independent mixture more than a kind or 2 kinds in these any materials.
In addition, the laminar silicic acid salt compound has silicate layer and carries out stacked structure, by ion exchange reaction (interior exchange), can keep various materials such as ion, molecule, atomic group at each interlayer.For example, each interlayer of laminar silicic acid salt compound can keep various organic compound, gives the laminar silicic acid salt compound with specific effect by this organic compound.For example, the organic compound of epoxy compounds being given affinity remains on each interlayer, keeps the laminar silicic acid salt compound of this organic compound to give affinity to epoxy compounds.Be not limited to insert the organic compound of each interlayer, when considering by the degree between the ion exchange treatment interposed layer, quaternary ammonium ion is preferred.
As quaternary ammonium ion, can enumerate the TBuA ion, the tetrahexyl ammonium ion, dihexyl Dimethyl Ammonium ion, dioctyl Dimethyl Ammonium ion, hexyl trimethyl ammonium ion, octyl group trimethyl ammonium ion, the dodecyl trimethyl ammonium ion, six decyl trimethyl ammonium ions, stearyl trimethyl ammonium ion, docosene base trimethyl ammonium ion, the cetyltrimethyl ammonium ion, hexadecyl triethyl ammonium ion, six decyl ammonium ions, four decyl dimethyl benzyl ammonium ions, stearyl dimethyl benzyl ammonium ion, two oil base Dimethyl Ammonium ions, N-methyl di-alcohol lauryl ammonium ion, two propyl alcohol monomethyl lauryl ammonium ions, dimethyl one ethanol lauryl ammonium ion, polyoxyethylene dodecyl ammonium ion, dimethyl six decyls eight decyl ammonium ions, the tricaprylmethylammonium ion, tetramethyl ammonium, the tetrapropyl ammonium ion.These quaternary ammonium ions can be separately or the mixture more than 2 kinds remain on each interlayer of laminar silicic acid salt compound.
As oxide compound, can enumerate silicon-dioxide, aluminum oxide, titanium oxide, Bismuth Trioxide, cerium dioxide, cobalt monoxide, cupric oxide, Indian red, Neodymium trioxide, Indium sesquioxide, manganese oxide, stannic oxide, yttrium oxide, zinc oxide.Above-mentioned oxide compound can comprise the independent mixture more than a kind or 2 kinds of these materials.
As nitride, can enumerate the nitride of Ti, Ta, Nb, Mo, Co, Fe, Cr, V, Mn, Al, Si etc.Above-mentioned nitride can contain the independent mixture more than a kind or 2 kinds of these materials.
The primary particle size of above-mentioned nanoparticle, the scope of preferred 1～1000nm.When the primary particle size of above-mentioned nanoparticle was not in the scope of 1～1000nm, the raising of electrical insulation capability was insufficient.In addition, the viscosity of cast molding resin combination rises, and is unfavorable to atomic mixture operation and cast molding operation.
Suitable modification or coating also can be implemented in the surface of above-mentioned micropartical, above-mentioned elastomerics particle and above-mentioned nanoparticle.Modification or coating be in order to improve the cementability with epoxy compounds, or the cohesion that is suppressed in the epoxy compounds are implemented.As the coupler that is used for modification, can enumerate silane coupling agents such as γ-glycidoxy-propyl trimethoxy silicane, gamma-amino propyl group-Trimethoxy silane, vinyltriethoxysilane, 3-metacryloxy propyl trimethoxy silicane, 3-glycidoxypropyl-Trimethoxy silane, the titanate ester coupler, aluminium class coupler.In addition, as the surface treatment agent that is used for modification, can enumerate Aluminum trilaurate, aluminum stearate, iron stearate, aluminum oxide, silicon-dioxide, zirconium white, polysiloxane.Perhaps, these reagent mix more than 2 kinds to use and also can.
Above-mentioned cast molding resin combination can also suitably cooperate curtain coating to prevent that agent, sedimentation from preventing additives such as agent, defoamer, flow agent, antiseize paste, dispersion agent, base material wetting agent.
Above-mentioned cast molding resin combination based on above-mentioned various raw materials, is made by laxative remedy.At first, the limit applies the shearing force limit and mixes above-mentioned nanoparticle in above-mentioned epoxy compounds.By applying shearing force, nanoparticle can be dispersed in the epoxy compounds.As being used for the blended device, so long as applying the device that the shearing force limit can mixed powder, the limit gets final product, anyly all can use, its kind is not particularly limited.As its object lesson, for example, can enumerate sheet grinder-mixer, 3 roller grinder-mixers, homogenize mixing machine, Labo PlastmillMixer (the smart mechanism of Japan is done society of institute and made), Miracle KCK (shallow field ironworker institute society make), Distromix (エ-テ Network ジ ャ パ Application society makes), Clear S55 (manufacturing of エ system テ Network ニ ッ Network society).
At the blended initial stage, above-mentioned nanoparticle is owing to be in mutually weak state of aggregation, presents opaque outward appearance with the mixture of above-mentioned epoxy compounds.Along with the blended progress, the dispersion of above-mentioned nanoparticle in mixture enlarges, and when further thorough mixing, said mixture presents transparent outward appearance.By the outward appearance of confirming that this is transparent, can judge and carry out sufficient mixing.
Above-mentioned nanoparticle surface also can be carried out modification with coupler or surface treatment agent in advance.Can make the contact interface of epoxy compounds and nanoparticle firm thus.In addition, when adopting the laminar silicic acid salt compound as nanoparticle, also can handle in advance, promptly be the processing that maintains organic compounds (for example, quaternary ammonium ion) at its interlayer.Thus, give nanoparticle the affinity to epoxy compounds, in epoxy compounds, can easily reach more uniform dispersion.
Secondly, in having disperseed the above-mentioned epoxy compounds of above-mentioned nanoparticle, after above-mentioned micropartical, above-mentioned elastomerics particle mixed, disperse, the interpolation epoxy compounds mixed with solidifying agent, can obtain purpose cast molding resin combination.And, this cast molding resin combination is flowed in the mould, be heating and curing after the vacuum defoamation, can obtain insulating material (cast molding insulant).Also have, in the manufacturing process of above-mentioned cast molding resin combination, the additive of above-mentioned any interpolation can suitably add as required, mix.
Because nanoparticle is very trickle, with the Nano grade homodisperse, so must carry out shear-mixed.By carrying out shear-mixed, filled micropartical and elastomerics particle after, between nanoparticle-micropartical, the interparticle interval of nanoparticle-elastomerics, any all below 1 μ m.When interparticle interval reaches 1 μ m when following, can present high toughness and excellent electrical insulating property.
Fig. 1 is each particle dispersion state mimic diagram in the insulating material of the present embodiment.Insulating material contains Resins, epoxy 1, elastomerics particle 2, micropartical 3 and nanoparticle 4.Break-up shot gonosome particle 2 in Resins, epoxy 1, disperse particles 3 in the gap between elastomerics particle 2, and then in these gaps dispersing nanometer particle 4.Elastomerics particle 2, micropartical 3 and nanoparticle 4 are dispersed in respectively in the Resins, epoxy 1.
The insulating material of the present embodiment, owing to have high tenacity and excellent electric insulation, for example, in the distribution clutch of built-in switching arrangement with vacuum valve, the lining vacuum valve, insulating insulating component in addition between vacuum valve and other members, and in the gas-insulated switchgear device, pipeline gas in the power transmission device etc., to support to use in the structural member etc. of high-pressure conductor be suitable in insulation in metal vessel.
Also have, the insulating material of the present embodiment is not limited to the structural member used with insulating component, gas-insulated switchgear device as above-mentioned distribution clutch, also can use in various uses such as insulating bar, insulation compound, profiled insulation parts, solvent impregnated resin, cable coating materials with the coating varnish of turbine terminal part, interceptor at generator.In addition, according to occasion, also can adopt in high thermal conduction insulating trip, IC substrate, LSI element with interlayer dielectric, laminated substrate, sealing material for semiconductor etc. at power unit insulated enclosure material.
Therefore, the insulating material of the present embodiment can be suitable for various uses.Promptly, in recent years, be accompanied by miniaturization, high capacity, high frequencyization, the Towards Higher Voltage of industry heavy electric machinery and electric and electronic, harshization of environment for use etc., to the cast molding resin combination, require the stabilization etc. of the contour performanceization of raising, high reliabilityization, high quality and the quality of electrical insulation capability.Insulating material of the present invention and these requirements coincide, and by selecting to use above-mentioned constituent material, as epoxy cast molding insulant and epoxy impregnation insulant etc., go for various industry heavy electric machineries and electric and electronic.
Below, embodiments of the invention are illustrated.
Embodiment 1
In epoxy compounds (bisphenol A type epoxy resin) 100 weight parts, interpolation applies shearing force and carries out mixing as laminar silicic acid salt compound 10 weight parts between the quaternary ammonium ion interposed layer of nanoparticle (primary particle size is 1～hundreds of nm) and epoxy silane class coupler 1 weight part.Adopt mixing that shearing force carries out, proceed to this mixture never be clear to transparent till.Secondly, compounding mixes, disperses as the styrene butadiene with core shell structure-Sipacril 2739OF particle 10 weight parts of elastomerics particle, as atomic silicon dioxide granule 340 weight parts in this mixture.Secondly, in this mixing thing, add epoxy compounds, carry out mixing in 10 minutes, make the cast molding resin combination in 80 ℃ with acid anhydride type curing agent 86 weight parts, acid anhydride type curing agent curing catalyst 1 weight part.This cast molding resin combination is flowed in the mould that is heated to 100 ℃ in advance, after the vacuum defoamation, under the condition of 100 ℃ * 3 hours (1 curing)+150 ℃ * 15 hours (2 curing), implement solidification treatment, make purpose cast molding insulant (insulating material).This cast molding insulant is made for following evaluating characteristics.
In epoxy compounds (bisphenol A type epoxy resin) 100 weight parts, add Titanium particles 10 weight parts (primary particle size 15nm) and metatitanic acid class coupler 1 weight part as nanoparticle, apply shearing force and carry out mixing.Secondly, compounding mixes, disperses as the styrene butadiene with core shell structure-Sipacril 2739OF particle 10 weight parts of elastomerics particle, as atomic silicon dioxide granule 340 weight parts in this mixing thing.Secondly, add epoxy compounds with acid anhydride type curing agent 86 weight parts, acid anhydride type curing agent curing catalyst 1 weight part, carry out mixing in 10 minutes, make the cast molding resin combination in 80 ℃ toward this mixing thing.This cast molding resin combination is flowed in the mould that is heated to 100 ℃ in advance, after the vacuum defoamation, under the condition of 100 ℃ * 3 hours (1 curing)+150 ℃ * 15 hours (2 curing), implement solidification treatment, make purpose cast molding insulant (insulating material).This cast molding insulant is made for following evaluating characteristics.
In epoxy compounds (bisphenol A type epoxy resin) 100 weight parts, add silicon dioxide granule 35 weight parts (primary particle size 12nm) as nanoparticle, apply shearing force and mix.Secondly, compounding mixes, disperses as the styrene butadiene with core shell structure-Sipacril 2739OF particle 10 weight parts of elastomerics particle, as atomic silicon dioxide granule 340 weight parts in this mixing thing.In this mixing thing, add epoxy compounds, carry out mixing in 10 minutes, make the cast molding resin combination in 80 ℃ with acid anhydride type curing agent 86 weight parts, acid anhydride type curing agent curing catalyst 1 weight part.This cast molding resin combination is flowed in the mould that is heated to 100 ℃ in advance, after the vacuum defoamation, under the condition of 100 ℃ * 3 hours (1 curing)+150 ℃ * 15 hours (2 curing), implement solidification treatment, make purpose cast molding insulant (insulating material).This cast molding insulant is made for following evaluating characteristics.
Comparative example 1
In epoxy compounds (bisphenol A type epoxy resin) 100 weight parts, compounding mixes, disperses as the styrene butadiene with core shell structure-Sipacril 2739OF particle 10 weight parts of elastomerics particle, as atomic silicon dioxide granule 340 weight parts.Secondly, in this mixing thing, add epoxy compounds, carry out mixing in 10 minutes, make the cast molding resin combination in 80 ℃ with acid anhydride type curing agent 86 weight parts, acid anhydride type curing agent curing catalyst 1 weight part.This cast molding resin combination is flowed in the mould that is heated to 100 ℃ in advance, after the vacuum defoamation, under the condition of 100 ℃ * 3 hours (1 curing)+150 ℃ * 15 hours (2 curing), implement solidification treatment, make purpose cast molding insulant (insulating material).This cast molding insulant is made for following evaluating characteristics.
The section SEM image of the cast molding insulant of comparative example 1 is shown in Fig. 6.The micropartical 102 in Resins, epoxy 101 about dispersion number μ m and the situation of elastomerics particle 103 are observed, but do not observe than its little nanometer particle.
Comparative example 2
In epoxy compounds (bisphenol A type epoxy resin) 100 weight parts, compounding is as laminar silicic acid salt compound 10 weight parts between the quaternary ammonium ion interposed layer of nanoparticle (primary particle size 1～hundreds of nm), apply shearing force carry out mixing, by shearing force carry out mixing proceed to this mixture never be clear to transparent till.Secondly, in this mixture, add epoxy compounds, carry out mixing in 10 minutes, make the cast molding resin combination in 80 ℃ with acid anhydride type curing agent 86 weight parts, acid anhydride type curing agent curing catalyst 1 weight part.This cast molding resin combination is flowed in the mould that is heated to 100 ℃ in advance, after the vacuum defoamation, under the condition of 100 ℃ * 3 hours (1 curing)+150 ℃ * 15 hours (2 curing), implement solidification treatment, make purpose cast molding insulant (insulating material).This cast molding insulant is made for following evaluating characteristics.
Comparative example 3
In epoxy compounds (bisphenol A type epoxy resin) 100 weight parts, compounding applies shearing force and carries out mixing as laminar silicic acid salt compound 10 weight parts between the quaternary ammonium ion interposed layer of nanoparticle (primary particle size 1～hundreds of nm).Apply mixing that shearing force carries out, proceed to this mixture never be clear to transparent till.Secondly, interpolation mixes, disperses as the styrene butadiene with core shell structure-Sipacril 2739OF particle 10 weight parts of elastomerics particle in this mixture.Then, in this mixing thing, add epoxy compounds, carry out mixing in 10 minutes, make the cast molding resin combination in 80 ℃ with acid anhydride type curing agent 86 weight parts, acid anhydride type curing agent curing catalyst 1 weight part.This cast molding resin combination is flowed in the mould that is heated to 100 ℃ in advance, after the vacuum defoamation, under the condition of 100 ℃ * 3 hours (1 curing)+150 ℃ * 15 hours (2 curing), implement solidification treatment, make purpose cast molding insulant (insulating material).This cast molding insulant is made for following evaluating characteristics.
The particle filled composite and the manufacturing process of the cast molding resin combination in embodiment 1～3, the comparative example 1 are summarized in table 1.
[table 1]
Secondly, to the cast molding insulant in embodiment 1～3 and the comparative example 1～3, adopt following method to measure respectively and destroy toughness, insulation breakdown time, the aging property of anti-partial discharge the, coefficient of thermal expansion, the preceding resin viscosity of curing.
(destroying the flexible measuring method)
According to ASTM D5045-91, make the initial be full of cracks of small-sized tension force test piece generation, apply the stretching loading, the loading when rupturing from the be full of cracks development is calculated and is destroyed toughness value (K
IC).In addition, the translational speed of pinblock is that 1mm/ minute, mensuration temperature are room temperature.
(measuring method of insulation breakdown time)
Make the sample of molding pin with the cast molding resin combination, at the bottom of sample coated with conductive coating, be arranged on fix on the plate electrode after, pin is applied the voltage of 10kV-1kHz, mensuration reaches the time of insulation breakdown.Gap from the front end of pin electrode to plate electrode is 3mm.
(mensuration of the aging degree of depth that partial discharge produces)
Cut the plate tensile sample of thickness 1mm from the cast molding insulant, the space that forms from specimen surface 0.2mm is provided with bar electrode.Bar electrode is applied the voltage of 4kV, make dull and stereotyped specimen surface be exposed to partial discharge.Discharge after 1440 hours, measure the aging degree of depth of maximum of the aging part of discharge.
(measuring method of coefficient of thermal expansion)
Cut vertical 5mm * laterally rectangular parallelepiped test piece of 5mm * height 10mm from the cast molding insulant of making, obtain coefficient of thermal expansion (α with the thermo-mechanical analysis device
1).Heat-up rate is 2 ℃/minute, compressive load 0.05N.
(measuring method of resin viscosity)
After epoxy compounds disperses various particles, add the epoxy compounds solidifying agent, the cast molding insulant before being heating and curing is heated to 60 ℃, measure with Brookfield viscometer.
The evaluation result of the cast molding resin combination before the cast molding insulant of embodiment 1～3, comparative example 1～3 and the curing is summarized in table 2.
[table 2]
Shown in the measurement result of table 2, compare as can be known with the cast molding insulant of comparative example 1～3 by the cast molding insulant of embodiment 1～3, have high tenacity and have excellent electric insulation, and coefficient of thermal expansion is also low.Comparison below with reference to embodiment and comparative example are carried out illustrates concrete effect of the present invention, effect.
At first, compare, effect, the effect of bringing by the destruction toughness of mix nanoparticles described by embodiment 1,2 and comparative example 1.The cast molding insulant of embodiment 1,2 by the effect of the nanoparticle of filling, destroys toughness than comparative example 1 height.This is owing to dispersive nanoparticle in the Resins, epoxy, suppresses to tear the resulting effect of progress.Shown in comparative example 1, by the filled elastomer particle, can improve destruction toughness, this is generally known, but owing to while filled elastomer particle and nanoparticle in embodiment 1, so reach than original high destruction toughness.
In addition, by the comparison of embodiment 1,2 and comparative example 2,3, effect, effect that hybrid fine particles and elastomerics particle are brought describe.When adopting the cast molding insulant of embodiment 1,2, epoxy compounds 100 weight parts relatively are owing to fill micropartical in the scope of 100～500 weight parts, so form and as the low-thermal-expansion rate of the normally used aluminium of conductor with degree.By making the cast molding insulant consistent with the coefficient of thermal expansion of conductor, can prevent since high voltage installation when operation the heat that takes place, make the interface peel of conductor and cast molding insulant.On the other hand, do not fill the coefficient of thermal expansion of the cast molding insulant of atomic comparative example 2,3, compare with the cast molding insulant of embodiment 1,2 and reach very high.When the difference of the coefficient of thermal expansion of conductor and cast molding insulant was big, the cast molding insulant that partial discharge takes place at the place of peeling off of conductor/resin boundary surface took place aging.
In addition, compare with comparative example 1,2 by embodiment 1,2, the effect that micropartical, elastomerics particle and nanoparticle are sneaked into epoxy compounds simultaneously and brought is illustrated.The mensuration of insulation breakdown time by adopting pin electrode, the cast molding insulant of embodiment 1,2 is compared with the cast molding insulant of comparative example 1,2, the rapid prolongation of insulation breakdown time.From with comparative example 1 more as can be known, the mixing of nanoparticle can prolong the insulation breakdown time.On the other hand, compare with the comparative example 2 of mix nanoparticles, the insulation breakdown time of the cast molding insulant of embodiment 1,2 is long, and this result can be understood as and can not describe by the independent effect of nanoparticle, but has the composite effect of micropartical and elastomerics particle.
The weathering process of the cast molding insulant in the insulation breakdown of employing pin electrode is illustrated by following.Shown in Fig. 2 (b), when adopting the cast molding insulant of comparative example 1, from aging route (electric tree network) P2 that the front end of pin electrode NE presents, low Resins, epoxy 1 part and the elastomerics particle 3 of the ageing resistance under high electric field optionally wear out.On the other hand, the cast molding insulant of embodiment 1,2, shown in Fig. 2 (a), the nanoparticle 4 that the progress of aging route P1 is had patience disperses, and can suppress the progress of aging route P1 in Resins, epoxy 1 part.Elastomerics particle 3 is owing to surrounded by nanoparticle 4, so the progress of the route that wears out is protected.In addition, the cast molding insulant of embodiment 1,2 is compared with the cast molding insulant of the comparative example 2 of only filling nanoparticle, shows the long insulation breakdown time.The cast molding insulant of comparative example 2, the nanoparticle of filling, the progress that can suppress electric tree network, but embodiment 1,2, except that the effect of this nanoparticle, mix filling by nanoparticle with atomic and since electric tree network the capacity of the Resins, epoxy part of easy progress reduce, so show the insulation breakdown time of growing very much.
In addition, both made in the mensuration of the anti-partial discharge characteristic that adopts bar electrode RE, the cast molding insulant of embodiment 1,2 is compared with the cast molding insulant of comparative example 1,2, and the known aging degree of depth is little.Shown in Fig. 3 (b), the cast molding insulant of comparative example 1, owing to wearing out that partial discharge D causes, Resins, epoxy 1 part that the ageing resistance under the high electric field is low and elastomerics particle 3 are corroded (in the accompanying drawing, E represents with reference symbol) by selectivity.On the other hand, the cast molding insulant of embodiment 1～2 is shown in Fig. 3 (a), because the high nanoparticle of partial discharge D ageing resistance 4 is disperseed, so can suppress the erosion E of Resins, epoxy 1 part that partial discharge D causes.In addition, owing to elastomerics particle 3 is surrounded by nanoparticle 4, so be protected from corroding E.In addition, the cast molding insulant of embodiment 1,2 is compared with the cast molding insulant of the comparative example 2 of only filling nanoparticle, and degree of aging is little.Shown in Fig. 2 (c), the cast molding insulant of comparative example 2, owing to filled nanoparticle, that can suppress that partial discharge causes is aging.Otherwise embodiment 1,2, and the partial discharge of nanoparticle aging had the inhibition effect, simultaneously, nanoparticle mixes filling with atomic, and the capacity of the most serious aging erosive Resins, epoxy part that partial discharge causes reduces, so the aging erosion that partial discharge causes becomes very little.
Secondly, by the comparison of embodiment 1 with embodiment 3, the primary particle size of each particle and use level are illustrated influence, the effect of resin viscosity.Resin viscosity before the curing of the cast molding insulant of embodiment 1 is compared only highly slightly with original comparative example 1, the cast molding resin combination flows in the cast molding operation of mould can be guaranteed to carry out easily.On the other hand, the resin viscosity before the curing of the cast molding insulant of embodiment 3 becomes very high.
In addition, compare, the surface modification of bringing particle and effect, the effect of shear-mixed are described by embodiment 1 and embodiment 3.The cast molding insulant of record among the embodiment 1 is dispersed in the Resins, epoxy by shear-mixed as the laminar silicic acid salt compound of nanoparticle.In addition, each particle surface carries out surface treatment by silane coupling agent.On the other hand, the cast molding insulant of record among the embodiment 3, the common mixing by as the silicon dioxide granule of nanoparticle is dispersed in the Resins, epoxy.In addition, each particle surface does not carry out surface treatment by coupler.
By the dispersion of nanoparticle shear-mixed, the particle dispersion state in the cast molding insulant is produced big influence.By applying shearing force; the mixture of Resins, epoxy and nanoparticle is mixing to reach transparent embodiment 1; and the mixture that adopts common blended Resins, epoxy and nanoparticle; by the particle dispersion state in the cast molding insulant of opaque embodiment 3; observe by electron microscope; in the cast molding insulant of embodiment 1, between nanoparticle-elastomerics particle and the interval between nanoparticle-micropartical, any all below 1 micron.On the other hand, the cast molding insulant of embodiment 3, each interparticle interval does not reach below 1 micron.Therefore, the cast molding insulant of embodiment 3, the loading level of nanoparticle be not only than embodiment more than 1, and, destroy any rerum natura of toughness, insulation breakdown time, the aging degree of depth, also all poor than the cast molding insulant of embodiment 1.
In addition, adopt the laminar silicic acid salt compound that carried out organic decoration by quaternary ammonium ion, can reduce the surface energy of silicate layer by quaternary ammonium ion, and interlayer forms the lipophilicity atmosphere.Carry out the effect of organic decoration by quaternary ammonium ion, affinity to the Resins, epoxy of laminar silicic acid salt compound uprises, mix by applying shear-stress, the laminar silicic acid salt compound is peeled off at interlayer, and each layer be homodisperse in the cast molding composition.In addition, by the surface treatment of silane coupling agent, because Chemical bond takes place at the interface of particle and resin, easily the macromolecular chain of confinement ring epoxy resins can suppress the molecular chain movement that heat causes, the particle/resin boundary surface that becomes crack progress weakness reaches firm.
Fig. 4, Fig. 5 illustrate the example of the insulating structure that the present invention relates to respectively.Fig. 4 illustrates the resin moulded valve that uses in the distribution clutch.In Fig. 4, comprise the vacuum valve 5 of fixation side conductor 51, movable side conductor 52, end plate 53,54, insulating cylinder 55, overlayed on the insulating component 6.By this insulating component 6,, and insulate between other members (not shown) that have in the distribution clutch the fixation side conductor 51 that flows through high-tension current, movable side conductor 52.Here, this insulating component 6 contains the insulating material as the cured article of cast molding resin combination of the present invention.
Fig. 5 illustrates the insulation system member that uses in the gas insulation opening and closing arrangement.In Fig. 5, flow through the conductor 11 of high-tension current, in the metal vessel 12 of enclosing insulating gas (sulfur hexafluoride gas), by insulation system member 13 support of being insulated.Here, insulation system member 13 contains the insulating material as the cured article of cast molding resin combination of the present invention.As Fig. 4, shown in Figure 5, adopt the insulating structure of insulating material of the present invention, can improve the characteristic and the reliability of high-voltage machine.
With reference to several embodiment preferred the present invention is illustrated, but the present invention is not subjected to the qualification of above-mentioned embodiment again.Based on above-mentioned disclosed content, the personnel with the common technology in present technique field can implement the present invention by the correction or the improvement of embodiment.
The possibility of utilizing on the industry
The invention provides: have cohesive with the conductor of molding, and have high anti-branch The cast molding resin combination of property and adopt its insulating materials, insulating structure.
Claims (11)
1. insulativity cast molding resin combination wherein contains: the epoxy compounds that has 2 above epoxy group(ing) in per 1 molecule; Contain the micropartical of material more than a kind that is selected from silicon-dioxide, aluminum oxide, mullite; The elastomerics particle; And contain the nanoparticle of material more than a kind that is selected from laminar silicic acid salt compound, oxide compound, nitride.
2. the cast molding resin combination of claim 1, wherein, above-mentioned micropartical is gone up relatively and is stated epoxy compounds 100 weight parts mutually and mix with the ratio of 100～500 weight parts.
3. the cast molding resin combination of claim 1, wherein, above-mentioned atomic primary particle size is 1～100 μ m.
4. the cast molding resin combination of claim 1, wherein, above-mentioned relatively epoxy compounds 100 weight parts of above-mentioned elastomerics particle mix with the ratio of 1～30 weight part.
5. the cast molding resin combination of claim 1, wherein, the primary particle size of above-mentioned elastomerics particle is 0.1～10 μ m.
6. the cast molding resin combination of claim 1, wherein, above-mentioned relatively epoxy compounds 100 weight parts of above-mentioned nanoparticle mix with the ratio of 1～30 weight part.
7. the cast molding resin combination of claim 1, wherein, the primary particle size of above-mentioned nanoparticle is 1～1000nm.
8. the cast molding resin combination of claim 1, wherein, above-mentioned micropartical, above-mentioned elastomerics particle, above-mentioned nanoparticle, by be selected from coupler and surface treatment agent a kind with on implement surface modification.
9. insulating material wherein contains the cured article of the cast molding resin combination of claim 1.
10. the insulating material of claim 9, in above-mentioned cured article, above-mentioned nanoparticle and the interparticle interval of above-mentioned elastomerics, and above-mentioned nanoparticle and above-mentioned atomic interval, any all below 1 μ m.
11. insulating structure wherein possesses conductor; And contain right require 9 insulating material, carrying out the insulating insulating component between above-mentioned conductor and other members.
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| JP226745/2006 | 2006-08-23 | ||
| JP2006226745 | 2006-08-23 | ||
| JP202179/2007 | 2007-08-02 |
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| CN101506301A true CN101506301A (en) | 2009-08-12 |
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| CNA2007800312162A Pending CN101506301A (en) | 2006-08-23 | 2007-08-21 | Casting resin composition, insulating material using the same, and insulating structure |
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| CN101845222A (en) * | 2010-05-21 | 2010-09-29 | 南京大学 | Mullite/polyaniline composite material with core-shell structure and preparation method thereof |
| CN102816411A (en) * | 2011-06-10 | 2012-12-12 | 株式会社日立产机系统 | Electrical insulating material and high voltage equipment |
| CN103059513A (en) * | 2013-02-17 | 2013-04-24 | 桂林理工大学 | Castable for manufacturing high-voltage motor nano composite main insulation |
| CN103694636A (en) * | 2013-12-10 | 2014-04-02 | 中国科学院过程工程研究所 | Electric insulating epoxy resin composition, preparation method and use of composition |
| CN103814415A (en) * | 2011-09-26 | 2014-05-21 | 西门子公司 | Insulation systems with improved resistance to partial discharge, production method for this |
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| CN101845222A (en) * | 2010-05-21 | 2010-09-29 | 南京大学 | Mullite/polyaniline composite material with core-shell structure and preparation method thereof |
| CN102816411A (en) * | 2011-06-10 | 2012-12-12 | 株式会社日立产机系统 | Electrical insulating material and high voltage equipment |
| CN102816411B (en) * | 2011-06-10 | 2015-11-18 | 株式会社日立产机系统 | Electrically insulating material and use its high voltage installation |
| CN103814415B (en) * | 2011-09-26 | 2017-06-13 | 西门子公司 | Insulation system with improved partial discharge resistant and preparation method thereof |
| CN103814415A (en) * | 2011-09-26 | 2014-05-21 | 西门子公司 | Insulation systems with improved resistance to partial discharge, production method for this |
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| CN104094361A (en) * | 2012-02-17 | 2014-10-08 | 株式会社日立制作所 | Resin composition for electric insulation, cured product thereof, methods for manufacturing same, and high-voltage devices and electric power transmission and distribution devices using same |
| CN104185876A (en) * | 2012-04-05 | 2014-12-03 | 西门子公司 | Insulating material for rotating machines |
| US9771464B2 (en) | 2012-04-05 | 2017-09-26 | Siemens Aktiengesellschaft | Insulating material for rotating machines |
| CN104185876B (en) * | 2012-04-05 | 2017-10-03 | 西门子公司 | The insulating materials of rotating machinery |
| CN104508760A (en) * | 2012-09-07 | 2015-04-08 | 积水化学工业株式会社 | Insulating resin material and multilayer substrate |
| CN104508760B (en) * | 2012-09-07 | 2016-11-09 | 积水化学工业株式会社 | Dielectric resin material and multilager base plate |
| CN103059513A (en) * | 2013-02-17 | 2013-04-24 | 桂林理工大学 | Castable for manufacturing high-voltage motor nano composite main insulation |
| CN103694636A (en) * | 2013-12-10 | 2014-04-02 | 中国科学院过程工程研究所 | Electric insulating epoxy resin composition, preparation method and use of composition |
| CN104559058A (en) * | 2014-12-28 | 2015-04-29 | 湖南新科绝缘材料有限公司 | Preparation method of novel casting resin for transformers, electric reactor coils and high-voltage switches |
| CN105017508A (en) * | 2015-08-21 | 2015-11-04 | 广州聚合电子材料有限公司 | Anti-breakdown and corrosion-resistant epoxy resin system as well as preparation method and application thereof |
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Application publication date: 20090812 |