WO2020246663A1 - Matériau isolant à base de siloxane nanohybride hautement résistant à la chaleur et procédé de préparation associé - Google Patents

Matériau isolant à base de siloxane nanohybride hautement résistant à la chaleur et procédé de préparation associé Download PDF

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Publication number
WO2020246663A1
WO2020246663A1 PCT/KR2019/013804 KR2019013804W WO2020246663A1 WO 2020246663 A1 WO2020246663 A1 WO 2020246663A1 KR 2019013804 W KR2019013804 W KR 2019013804W WO 2020246663 A1 WO2020246663 A1 WO 2020246663A1
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WO
WIPO (PCT)
Prior art keywords
weight
parts
oligosiloxane
siloxane
resistant
Prior art date
Application number
PCT/KR2019/013804
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English (en)
Korean (ko)
Inventor
강동준
임현균
강민정
박효열
Original Assignee
한국전기연구원
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Publication of WO2020246663A1 publication Critical patent/WO2020246663A1/fr

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Classifications

    • 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
    • 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
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • 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
    • H01B3/30—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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives

Definitions

  • Conventional heat-resistant materials include fluorine-based organic polymer-based heat-resistant coating materials and inorganic polysilazane-based heat-resistant coating materials.
  • the high heat-resistant nanohybrid siloxane insulating material in the present invention means that the residual inorganic content is high, where the residual inorganic content can be measured as the mass of the inorganic matter remaining when the high heat-resistant nanohybrid siloxane insulating material is burned at 750°C. have.
  • oligosiloxane has a siloxane-based siloxane structure with excellent thermal stability that can withstand high temperatures as its main structure, and has at least one of an alkyl group, an aryl group, and an organic group at the side chains and terminals. It says to include.
  • alkyl group any of methyl group, ethyl group, n-propyl group, isopropyl group, n-butyl group, isobutyl group, t-butyl group, n-pentyl group, isopentyl group, hexyl group, dimethyl group, and trimethyl group
  • the aryl group may be any one or more of a phenyl group, a diphenyl group, and a triphenyl group
  • the organic group may be any one or more of a vinyl group, a methacrylic group, and a hydrogen group.
  • the thermal condensation method is not formed by curing through crosslinking between organic substances, but is formed in a form in which only inorganic powder of siloxane is dried or cured, and an organic silane precursor having an alkyl group or an aryl group is hydrolyzed and condensed using an acid aqueous solution. It is a method of reacting to produce an alkyl or aryl oligosiloxane.
  • thermosetting method is a method of producing a thermosetting oligosiloxane by hydrolysis and condensation reaction in an acid atmosphere using an organosilane precursor having an organic group capable of thermosetting.
  • the surface-treated nanosilica particles of the present invention are mixed with oligosiloxane to improve adhesion, crack resistance, and heat resistance.
  • the organic monomer or organic oligomer of the present invention has a carbonized chain structure and includes a thermosetting organic group at the side chain and the terminal.
  • organic monomers or organic oligomers may be included in an amount of 0.1 to 10 parts by weight in the high heat-resistant nanohybrid siloxane insulating material. If it is less than 0.1 parts by weight, it is difficult to control crack resistance and heat resistance, and if it exceeds 10 parts by weight, the heat resistance is very Since it was confirmed that a phenomenon of deterioration is caused, it is preferable to control crack resistance and heat resistance by using species having different molecular weights together. In the case of an organic monomer or an organic oligomer, it is most preferably added in an amount of 5 parts by weight.
  • the heat condensation reaction accelerator it may be added in the step (S10) of preparing an oligosiloxane or may be added in the step (S20) of preparing a high heat-resistant insulating resin, and the order of addition is not limited.
  • an organic solvent it may be contained in an amount of 50 to 70 parts by weight, and if it is less than 50 parts by weight, the miscibility with other components cannot be properly achieved, and if it exceeds 70 parts by weight, it is significant compared to the case where a less amount is added. Since there is no effect, the organic solvent is preferably included in the range of 50 to 70 parts by weight.
  • Example 1 is a method using an alkyl or aryl oligosiloxane through a thermal condensation method.
  • an alkyl or aryl oligosiloxane was prepared using an aqueous hydrochloric acid solution (T, TD, TQ species).
  • T, TD, TQ species aqueous hydrochloric acid solution
  • the molecular weight was controlled by controlling reaction variables including catalyst concentration and reaction time.
  • Example 1-2 16 parts by weight of methyl-ethyl oligosiloxane, 10 parts by weight of methyl-propyl oligosiloxane, 0.5 parts by weight of surface leveling agent, 1.5 parts by weight of heat condensation accelerator, 2 parts by weight of adhesion promoter, 20 parts by weight of butyl cellosolve Parts and 40 parts by weight of xylene, but unlike Example 1-1, a high heat-resistant nanohybrid siloxane insulating material containing 10 parts by weight of fumed nano-silica particles was prepared.
  • Example 1-5 5 parts by weight of methyl-ethyl oligosiloxane, 5 parts by weight of methyl-propyl oligosiloxane, 5 parts by weight of methyl-phenyl oligosiloxane, 5 parts by weight of methyl oligosiloxane, 5 parts by weight of propyl-TEOS oligosiloxane, Colloidal nanosilica 6 parts by weight, fumed nano silica 5 parts by weight, surface leveling agent 0.5 parts by weight, heat condensation reaction accelerator 1.5 parts by weight, adhesion promoter 2 parts by weight, butyl cellosolve 20 parts by weight and xylene 40 parts by weight A heat-resistant nanohybrid siloxane insulating material was prepared.
  • Example 1-1 Example 1-2 Example 1-3 Example 1-4 Example 1-5 Hardness ⁇ ⁇ ⁇ ⁇ ⁇ Residual inorganic content (%) 70 or more 70 or more 70 or more 65 or more 67 or more Transmittance(%) 91 91 91 91 91 91 Adhesion (B) 5 5 5 5 5 5 crack ⁇ ⁇ ⁇ ⁇ ⁇ Moisture content (%) 0.1 or less 0.1 or less 0.1 or less 0.1 or less 0.1 or less 0.1 or less 0.1 or less 0.1 or less 0.1 or less 0.1 or less 0.1 or less 0.1 or less 0.1 or less Pencil hardness H H HB or less H H H
  • Example 2-4 13 parts by weight of methyl-vinyl oligosiloxane, 13 parts by weight of ethyl-vinyl oligosiloxane, 5 parts by weight of propyl-vinyl oligosiloxane, 5 parts by weight of colloidal nanosilica, 0.5 parts by weight of surface leveling agent, thermal condensation
  • a highly heat-resistant nanohybrid siloxane insulating material consisting of 1.5 parts by weight of a reaction accelerator, 2 parts by weight of an adhesion promoter, 20 parts by weight of butyl cellosolve, and 40 parts by weight of xylene was prepared.

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

Abstract

La présente invention concerne un matériau isolant à base de siloxane nanohybride hautement résistant à la chaleur et un procédé de préparation associé et, plus spécifiquement : un matériau isolant à base de siloxane nanohybride hautement résistant à la chaleur ayant une résistance à la chaleur élevée et ayant également des caractéristiques d'isolation de base par le mélange de nanoparticules de silice traitées en surface et d'un oligosiloxane comprenant une structure de siloxane. L'invention concerne en outre un procédé de préparation associé. Les objets techniques de la présente invention sont : un matériau isolant à base de siloxane nanohybride hautement résistant à la chaleur comprenant des nanoparticules de silice traitées en surface et un oligosiloxane, qui comprend une structure siloxane ayant au moins un groupe parmi un groupe alkyle, un groupe aryle et un groupe organique ; et un procédé de préparation associé.
PCT/KR2019/013804 2019-06-07 2019-10-21 Matériau isolant à base de siloxane nanohybride hautement résistant à la chaleur et procédé de préparation associé WO2020246663A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR1020190067178A KR20200140509A (ko) 2019-06-07 2019-06-07 고내열 나노하이브리드 실록산 절연소재 및 이의 제조방법
KR10-2019-0067178 2019-06-07

Publications (1)

Publication Number Publication Date
WO2020246663A1 true WO2020246663A1 (fr) 2020-12-10

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PCT/KR2019/013804 WO2020246663A1 (fr) 2019-06-07 2019-10-21 Matériau isolant à base de siloxane nanohybride hautement résistant à la chaleur et procédé de préparation associé

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KR (1) KR20200140509A (fr)
WO (1) WO2020246663A1 (fr)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101444820B1 (ko) * 2013-05-21 2014-09-30 한국전기연구원 유연 에너지소자의 절연 및 부식방지용 하이브리드 패키징 소재 제조방법
KR20150010051A (ko) * 2013-07-17 2015-01-28 한국전기연구원 고차단성 투명 하이브리드 패키징 막
KR20160014971A (ko) * 2014-07-30 2016-02-12 한국전기연구원 고투명, 내열성 및 절연성을 갖는 하이브리드 코팅소재의 제조방법
KR20180026259A (ko) * 2016-09-02 2018-03-12 한국전기연구원 실리카-실록산 나노하이브리드 코팅소재 및 그 제조방법
KR101906815B1 (ko) * 2017-07-28 2018-10-11 한국전기연구원 무용매 타입의 열경화성 유무기 하이브리드 절연소재

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101444820B1 (ko) * 2013-05-21 2014-09-30 한국전기연구원 유연 에너지소자의 절연 및 부식방지용 하이브리드 패키징 소재 제조방법
KR20150010051A (ko) * 2013-07-17 2015-01-28 한국전기연구원 고차단성 투명 하이브리드 패키징 막
KR20160014971A (ko) * 2014-07-30 2016-02-12 한국전기연구원 고투명, 내열성 및 절연성을 갖는 하이브리드 코팅소재의 제조방법
KR20180026259A (ko) * 2016-09-02 2018-03-12 한국전기연구원 실리카-실록산 나노하이브리드 코팅소재 및 그 제조방법
KR101906815B1 (ko) * 2017-07-28 2018-10-11 한국전기연구원 무용매 타입의 열경화성 유무기 하이브리드 절연소재

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