WO2015121996A1 - Résine d'isolation électrique - Google Patents

Résine d'isolation électrique Download PDF

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Publication number
WO2015121996A1
WO2015121996A1 PCT/JP2014/053573 JP2014053573W WO2015121996A1 WO 2015121996 A1 WO2015121996 A1 WO 2015121996A1 JP 2014053573 W JP2014053573 W JP 2014053573W WO 2015121996 A1 WO2015121996 A1 WO 2015121996A1
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WO
WIPO (PCT)
Prior art keywords
resin
polar
elastomer
cold environment
fine
Prior art date
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PCT/JP2014/053573
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English (en)
Japanese (ja)
Inventor
大嶽　敦
昌宏 川崎
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株式会社日立製作所
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Priority to PCT/JP2014/053573 priority Critical patent/WO2015121996A1/fr
Publication of WO2015121996A1 publication Critical patent/WO2015121996A1/fr

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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
    • H01B3/40—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 epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L101/00—Compositions of unspecified macromolecular compounds
    • 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
    • H01B3/28—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances natural or synthetic rubbers
    • 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
    • H01B3/44—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 vinyl resins; acrylic resins
    • H01B3/441—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 vinyl resins; acrylic resins from alkenes
    • 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
    • H01B3/46—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 silicones

Definitions

  • the present invention relates to a resin material for electrical equipment used in cold conditions, and more particularly to an insulating resin material for electrical equipment in a cold environment such as a magnetic resonance imaging apparatus, a superconducting related device, and a cold district receiving / transforming facility.
  • Patent Documents 1 to 6 described below are known.
  • Patent Documents 1-6 there is no description from the viewpoint of a minor axis of 200 nm, and there is no description formula indicating it. Moreover, although limitation of the particle diameter in patent document 2 is in the range of this invention, it is not a description from a viewpoint of a short diameter. Moreover, there is no description about adding a very small amount of fine particles (that is, the minor axis is 200 nm or less).
  • the minor axis of the particulate hydrophobic elastomer makes a very important contribution to the dispersion of the particulates. That is, the minor axis usually determines the superiority or inferiority of the two forces on the balance between intermolecular force and electrostatic force.
  • the fine hydrophobic elastomer when the polar fine particles are added, the fine particles gradually approach the wall (fiber reinforced plastic or metal) with polarity while interacting with the fine particle hydrophobic elastomer. In addition, it causes a strong adhesion.
  • the intermolecular force and the electrostatic force are balanced under the condition that the minor axis of the fine particle is 200 nm, and that the hydrophobic particle is dispersed in the polar liquid when the minor axis is 200 nm or less.
  • a hydrophobic substance does not cause dispersion but also causes sedimentation.
  • many hydrophobic elastomers such as silicone have excellent cold characteristics. The problem is to disperse the hydrophobic elastomer in the resin and take advantage of the characteristics. In order to deal with this problem, there is a method of modifying the surface of the hydrophobic elastomer with a polar group, but there is a problem that the cost is generally increased.
  • an object of the present invention is to provide an electrically insulating resin that exhibits the characteristics of a hydrophobic elastomer without a modifying group, improves the characteristics by an additional effect, and is excellent particularly in a cold environment.
  • the present invention contains a particulate hydrophobic elastomer having an average particle diameter of 200 nm or less in the minor axis, and in addition to the particulate hydrophobic elastomer, polar particulates are included at the same time.
  • a resin and an electric device using the resin are provided.
  • the sedimentation rate becomes very slow or almost negligible because the sedimentation and thermal motion of the particles are balanced.
  • the force acting between the fine particles, between the resins, and between the particle resins is greater than that of gravity.
  • the interaction between the polar (that is, polar) fine particles and the resin becomes stronger, and if the agitation is performed under a sufficient shearing force, the fine particles are dispersed almost uniformly.
  • hydrophobic interaction acts between the hydrophobic particles, the particles tend to approach each other.
  • each particle can be as small as 1 wt% polar fine particles and 2 wt% fine particle hydrophobic elastomer, and it has been found that adding up to a total of about 15 wt% exhibits a sufficient effect. ing. Also, at this time, the size of the minor axis where the size of the minor axis interchanges between the intermolecular force and the electrostatic force is also 200 nm, and whether or not the particle and the resin are bonded is determined by this size as a boundary. Our study has shown that if the particles do not adhere to the resin, delamination occurs and the strength is reduced by as much as 30%.
  • a resin for a cold environment characterized in that the resin described above is a thermosetting resin having polarity, and a high-voltage device using the same are provided.
  • the resin is a polar resin and a thermosetting resin is more effective.
  • a thermosetting resin is more effective.
  • many oxide-based fillers have polarity, and the property is that they are easily dispersed without treating the surface of the polar resin.
  • the thermosetting resin can easily maintain the structure formed inside the resin, and can exhibit performance stably with respect to temperature as compared with the thermoplastic resin.
  • an insulating resin characterized by silica, alumina, a layered silicate compound or a combination thereof as polar fine particles in addition to the fine particle hydrophobic elastomer described above and an electric device using the same are provided.
  • Silica mentioned above is a very common substance and is low in cost, and has high flexibility, high purity, shape, and abundant surface treatment agent, so the desired performance such as dispersibility and particle size can be obtained. It is easy to be done. Therefore, it is most suitable for control of resin properties.
  • alumina has a characteristic that it is less susceptible to chemicals compared to silica and should be used in such an environment.
  • the layered silicate compound is separated into thin layers having a thickness of nm, a card house type structure is formed inside the resin, and there is an effect of improving the strength and dielectric breakdown life of the composite resin.
  • an inorganic or organic filler having an average particle diameter exceeding 5 ⁇ m is added, and a resin for cold environment and a resin and an apparatus using the same are provided. .
  • microparticles having an average particle diameter of more than 5 ⁇ m By simultaneously using so-called microparticles having an average particle diameter of more than 5 ⁇ m, it becomes easier to control the physical properties of the resin for cold environments.
  • the linear expansion coefficient can be almost explained by the volume weighted average of the resin component and the filler contained in the composite resin.
  • the nano-size filler increases the viscosity of the resin, the amount added cannot be increased as the linear expansion coefficient is significantly changed.
  • microparticles can be used at the same time, and in addition to the properties given by fine particles, that is, insulation properties and strength, it is possible to control physical properties that change with volume fraction such as linear expansion coefficient. Become.
  • thermosetting resin is an epoxy resin, an unsaturated polyester resin, a novolac resin, or a composite material thereof.
  • the type of resin needs to be changed depending on the environment used and the required cost. It is possible to provide a resin for a cold environment according to requirements by changing these matrix resins while maintaining the above-described characteristics.
  • a group of fine-particle hydrophobic elastomers is formed in a network. Further, even when the fine particles added in the polar resin are hydrophobic elastomers, the adhesion with the resin material at the interface is maintained. As a result, a skeletal network structure formed from the particulate hydrophobic elastomer population is formed. Further, by adding a small amount of polar fine particles, it can be expected that the concentration of polar fine particles increases in the vicinity of a hydrophilic base material or metal in the fluidized resin (before curing).
  • the skeleton network structure shown on the left serves to increase the fracture toughness and fracture strength of the resin after curing, and the polar isolated particles inhibit the progress of the electrical tree and cause dielectric breakdown. It has been shown to improve lifespan. Further, it has been found that the addition amount of each particle may be a very small amount of addition of 3 wt% of fine particle hydrophobic elastomer and 2 wt% of polar fine particles, and if the total amount is 15 wt% at the maximum, a sufficient effect is exhibited. Moreover, the polar fine particles added in a small amount improve the adhesiveness with a base material, a metal wire, etc., and fulfill the effect of preventing peeling from the resin.
  • the resin used in the present invention does not have to be polar. However, if possible, a polar resin and a thermosetting resin are more effective. The reason is that many oxide-based fillers have polarity, and the property is that they are easily dispersed without treating the surface of the polar resin. In addition, the thermosetting resin has an effect that it is easy to maintain the structure formed inside the resin, and can stably exhibit the performance with respect to the temperature as compared with the thermoplastic resin.
  • the fine particle hydrophobic elastomer is silicone, modified silicone, styrene butadiene rubber, ethylene propylene rubber, or a copolymer, compound or a combination thereof.
  • Silicone can control the polymerization length and has flexibility, so it is suitable for control of resin properties.
  • the linear expansion coefficient can be almost explained by the volume weighted average of the resin component and the filler contained in the composite resin.
  • the nano-size filler increases the viscosity of the resin, the amount added cannot be increased as the linear expansion coefficient is significantly changed.
  • the physical properties such as the linear expansion coefficient can be controlled.
  • the particulate hydrophobic elastomer particles have the effect of improving the toughness of the resin, and can improve the crack resistance of the composite resin described above. Therefore, it is possible to provide a resin for a cold environment that can achieve both fracture toughness, insulation life and mechanical strength.
  • thermosetting resin of the present invention is an epoxy resin, an unsaturated polyester resin, a novolac resin, or a composite material thereof will be described.
  • the type of resin needs to be changed according to the environment used, characteristics, and required cost. It is possible to provide a resin for a cold environment according to market requirements by changing these base resin while maintaining the characteristics described above.
  • a silicone rubber is used as the particulate hydrophobic elastomer, a bisphenol A type epoxy prepolymer and a phthalic anhydride acid anhydride curing agent are used as a resin, and a mixture of a reaction accelerator is used as a composite resin material.
  • a partially extracted surface structure of silicone rubber is shown in the chemical structural formula of FIG.
  • an alkyl group R exists on the surface. Since the bonded Si atom has a small electron withdrawing property, it is almost uncharged if R is an alkyl group.
  • the type of alkyl group can be chemically converted, and there are various types of silicones. Such characteristics have been revealed by molecular orbital calculations and various experiments.
  • sample specimens were prepared as follows. This test piece is for preparing a test piece for measuring the three-point bending fracture strength and the long-term electrical degradation life. The sample preparation procedure is described next.
  • Epoxy is bisphenol A type.
  • reaction accelerator add reaction accelerator to the above solution, add silica (short average particle diameter 200nm) as 0.5wt% polar fine particles with respect to the total amount, and mix with uniaxial rotating blade stirrer.
  • FIG. 2 (A) when submicron-sized silicone is put on the surface
  • FIG. 2 (B) when silicone particles with a short diameter of 200 nm or less are put is shown.
  • the amount of silicone added to the total resin weight ratio is 3 wt%.
  • the silicone particle group forms a network structure.
  • silicone which is a fine particle hydrophobic elastomer, is difficult to disperse and tends to agglomerate, but when it is stirred with a planetary mixer, a tensile stress is applied, resulting in a fibrous network. A structure is formed. Further, since the silica added at the same time has a small particle size, the power of Brownian motion acts and does not settle. By hardening such a structure as it is formed inside the composite resin, the strength is increased. In this case, the bending strength was improved by about 30%.
  • the long-term dielectric breakdown lifetime of the resin was only about 20% longer than when no hydrophobic silica was added.
  • the resin having the structure of FIG. 2 (A) had voids around the silicone, and the strength was reduced by 30% relative to the silicone-free resin.
  • the horizontal axis plots the particle diameter (refers to the minor axis), and the vertical axis plots the strength of the interaction (energy).
  • a particle has a certain size (shorter than 200 nm)
  • dipole interaction works strongly, causing a phenomenon in which substances are separated or approached by electrical force.
  • the particle size becomes smaller, the number of atoms exposed on the surface of the particle increases, and the number of atoms closest to the resin also increases. Will work harder.
  • the “shorter axis 200nm” was the region where intermolecular forces and electrostatic interactions were reversed.
  • FIG. 2A it can be seen that a gap is generated around the silicone. Due to this gap, the resin shown in FIG. 2 (A) has a toughness value of about 70% of the resin with no filler added, and the strength is also reduced. That is, the adhesion between the resin and the filler is essential for increasing the strength.
  • FIG. 2 (B) the size of the silicone filler is further reduced to 16 nm. At this size, the interface between the silicone and the resin disappears and is in an adhesive state.
  • toughness improved by 50% or more (room temperature) and bending strength improved by 20% it was found that toughness improved by 50% or more (room temperature) and bending strength improved by 20%.
  • the skeletal network structure shown in Fig. 2 (A) on the left serves to increase the fracture toughness and fracture strength of the cured resin. It was also found that polar isolated particles hinder the development of electrical trees and improve the breakdown lifetime. That is, it was found that the bending strength was improved by 45% compared to the resin without addition of silica, and the long-term dielectric breakdown life was 100%, that is, doubled.
  • FIG. 4 shows the state of cracking after resin is molded around stainless steel.
  • FIG. 4 (A) shows a resin containing a submicron-sized silicone filler, but generates large cracks.
  • Fig. 4 (B) a small turtle-shaped crack enters and gradually progresses.
  • FIG. 4 (B) no cracks that can be observed until -120 ° C.
  • FIG. 4B is a resin material that is less prone to quench.
  • FIG. 5 shows an example in which, in addition to silicone, nitrile butadiene rubber is added at 0.5 wt% of silicone weight ratio.
  • Nitrile butadiene rubber has a short diameter of 200 nm, but since it is a polar elastomer, its dispersibility is good even if it is larger.
  • the pre-curing resin mixed with these two types of elastomers is well kneaded and the resin is injected, the two types of elastomers that were initially mixed uniformly, but only the polar nitrile butadiene rubber is near the substrate with the polarity. It accumulates in. Such a movement occurs spontaneously because it becomes stable in terms of energy.
  • the adhesion with the resin body is improved. For this reason, even if the strain energy stored inside the resin is released at a low temperature, no large peeling occurs at the substrate-resin interface. Therefore, the released energy is suppressed, and it is difficult to cause quenching in the magnetic resonance imaging apparatus.
  • Example 1 it has been found that the same improvement in mechanical strength and insulation characteristics can be obtained as an effect even with unsaturated polyester, polyphenol, and novolac resin as thermosetting resins. In addition, the effects described in Example 1 can be expected for a resin having polarity.
  • the same effect can be obtained by using silica or highly corrosive alumina as the polar fine particles in Examples 1 and 2 and the layered silicate compound for improving the anti-treeing property or a combination thereof.
  • the use of a mixture of a surface-treated alumina and layered silicate compound with and without a hydrophobic surface significantly improves the dielectric breakdown life in the former, while the latter has a significant increase in both dielectric breakdown life and strength. To improve.
  • an inorganic or organic filler having an average particle diameter exceeding 5 ⁇ m may be added.
  • Such large size fillers do not increase the viscosity of the resin before curing as nano-sized particles. Therefore, it can be added up to about 75 wt%.
  • elastomer particles may be further added.
  • Elastomer particles have the effect of improving the fracture toughness of the resin and are less likely to break.
  • the bending strength has a disadvantage.
  • the elastomer particles include nitrile butadiene rubber, butadiene rubber, silicone rubber, and commercially available core-shell type toughness improving rubber materials.
  • epoxy resin there exists a thing shown below, and these can also be used individually or in mixture of 2 or more types.
  • Bisphenol A type epoxy resin hydrogenated bisphenol A type epoxy resin, bisphenol F type epoxy resin, brominated bisphenol A type epoxy resin, bisphenol S type epoxy resin, biphenyl type epoxy resin, naphthalene type epoxy resin, phenol novolac type epoxy resin, Orthocresol novolac type epoxy resins, alicyclic epoxy resins, triglycidyl isocyanurate type epoxy resins, and the like.
  • the coil includes a bobbin 6c, a resin 6b, and a coil wire 6c.
  • Bobbin 6c is made of FRP or stainless steel.
  • the resin 6b is a resin to which the present invention has been described up to the previously known examples, and has a structure that suppresses large cracks at low temperatures. This cracking of the resin becomes an opportunity and peeling from the bobbin occurs. Therefore, by using such a resin, it is possible to overwhelmingly reduce the chance of quenching due to the impact of cracking.
  • FIG. 7 for explaining the mold transformer using the resin for the cold environment described in the above embodiment is a cross-sectional simulation view of the mold transformer using the resin for the cold environment described in the present invention.
  • the mold transformer is housed in a primary coil, a secondary coil, and mold bodies 71 and 72 for housing the coil, and has a configuration as shown in FIG.
  • a thermosetting resin such as epoxy is used to harden the primary coil and the secondary coil. If the epoxy resin has insufficient toughness, a difference in coefficient of linear expansion from the internal wiring and other insulators will occur, causing cracks.
  • Mold transformers are not only used in temperate regions such as Japan, but may also be used in extremely cold regions such as Takayama and cold regions in the future.
  • the resin of the present invention is also used for such applications. Can be used.
  • the mold resin of the mold transformer is a thermosetting resin such as an epoxy resin, but as described above, a thermal stress is generated between the base material and the resin, and this is the outside air temperature. The lower the value, the larger it. For this reason, the problem that a crack generate
  • the resin provided in the present invention can keep the cracking property at a low temperature very low, and remarkably reduce the possibility of cracking.
  • the resin according to the present invention as a coil mold material for a mold transformer, it is possible to suppress the occurrence of cracks in a cold environment.

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

L'invention concerne une résine adaptée à un environnement froid qui est capable d'améliorer la résistance de la résine d'isolation, et, simultanément, de prolonger la durée de vie de l'isolation avant défaillance, et un dispositif d'imagerie par résonance magnétique et un équipement électrique l'utilisant. Un élastomère en un état de fines particules ayant un diamètre court de 200 nm ou moins et de fines particules polaires ayant un diamètre court de 200 nm ou moins sont inclus dans une résine polaire. Ainsi, il est possible d'améliorer la résistance à la fissuration et les caractéristiques d'isolation électrique de la résine aux basses températures, et d'améliorer la propriété adhésive de la résine sur un matériau de base.
PCT/JP2014/053573 2014-02-17 2014-02-17 Résine d'isolation électrique WO2015121996A1 (fr)

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PCT/JP2014/053573 WO2015121996A1 (fr) 2014-02-17 2014-02-17 Résine d'isolation électrique

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2018002819A (ja) * 2016-06-30 2018-01-11 倉持　浩 熱可塑性エラストマー混合物およびそれを用いた連続体形成方法

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WO2013121571A1 (fr) * 2012-02-17 2013-08-22 株式会社日立製作所 Composition de résine pour isolation électrique, produit durci la comprenant, leurs procédés de fabrication, et dispositifs haute tension et dispositifs de distribution et de transmission d'énergie électrique les utilisant

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2018002819A (ja) * 2016-06-30 2018-01-11 倉持　浩 熱可塑性エラストマー混合物およびそれを用いた連続体形成方法

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