EP1480813A1 - Procede pour produire et traiter des matieres a mouler en resine epoxy - Google Patents

Procede pour produire et traiter des matieres a mouler en resine epoxy

Info

Publication number
EP1480813A1
EP1480813A1 EP03708109A EP03708109A EP1480813A1 EP 1480813 A1 EP1480813 A1 EP 1480813A1 EP 03708109 A EP03708109 A EP 03708109A EP 03708109 A EP03708109 A EP 03708109A EP 1480813 A1 EP1480813 A1 EP 1480813A1
Authority
EP
European Patent Office
Prior art keywords
mixer
molding
molding compositions
production
components
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
EP03708109A
Other languages
German (de)
English (en)
Inventor
Heinz-Gunter Reichwein
Michael Schwab
Jens Steinmann
Thomas Dressen
Gunda Panik
Frank Bayerl
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hexion GmbH
Original Assignee
Bakelite AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Bakelite AG filed Critical Bakelite AG
Publication of EP1480813A1 publication Critical patent/EP1480813A1/fr
Ceased legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C67/00—Shaping techniques not covered by groups B29C39/00 - B29C65/00, B29C70/00 or B29C73/00
    • B29C67/24—Shaping techniques not covered by groups B29C39/00 - B29C65/00, B29C70/00 or B29C73/00 characterised by the choice of material
    • B29C67/246—Moulding high reactive monomers or prepolymers, e.g. by reaction injection moulding [RIM], liquid injection moulding [LIM]
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/12—Powdering or granulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2063/00—Use of EP, i.e. epoxy resins or derivatives thereof, as moulding material
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/31504—Composite [nonstructural laminate]
    • Y10T428/31511—Of epoxy ether

Definitions

  • the invention relates to a new process for the production and processing of molding compositions based on epoxy resins.
  • Epoxy resin molding compounds are granules made of epoxy resin, hardener as well as fillers and additives that can be processed into thermally curable molded parts without the addition of an additive.
  • the molded articles produced in this way are distinguished by good mechanical and electrical properties.
  • the other fillers and additives are mixed into a liquid mixture of epoxy resin and hardener. At a moderately elevated temperature, the epoxy resins are allowed to prereact until the mass is tack-free and free-flowing at room temperature. Despite good wetting of the fillers, this process has the disadvantage that the setting of the pre-reaction is not exactly reproducible, so that the corresponding molding compositions differ in their reactivity from batch to batch. In addition, these molding compositions are not stable in storage.
  • the object is achieved by a process for the production and processing of epoxy resin molding compositions according to claims 1 to 7.
  • the molding compositions produced by the process are particularly suitable for the production of molded parts in the reaction injection molding process, for the encapsulation of electronic or electrical components or component components and for the production of mechatronic components, as claimed in claims 8 to 10.
  • the solution is achieved by mixing all the constituents of the molding composition together in a high-speed mixer and processing them into loose, free-flowing granules.
  • the direct further use of this granulate as a molding composition for the production of molded parts in the known manner by pressing in a mold does not lead to high-quality moldings, since the homogenization is not sufficient.
  • the granules have the property of forming a flowable mass under pressure.
  • This is used according to the invention in that the granules are homogenized under pressure shortly before shaping and hardening.
  • the granules which are not yet sufficiently homogeneous, are pressed under pressure and, if appropriate, with heating by a continuous mixer upstream of the molding tool, shortly before it is fed to the molding tool, and homogenized in the process.
  • this also works with molding compositions whose filler content is up to 95% by weight, based on the total composition.
  • the granulate is produced very quickly and easily.
  • the granules are storable and do not clump together in normal storage, but remain free-flowing. Only when using pressures> 5 bar, such as those that occur when passing through transport devices such as extruder screws or piston pumps, are these mixtures plasticized and can be homogenized in continuous mixers.
  • the homogeneous molding compound obtained is then injected directly into the mold. It is a further advantage of the method according to the invention that both the mixing machines and the device components, such as the devices and continuous mixers required for pressure generation, are common machines in the plastics processing industry and can be connected upstream of a molding tool in a simple manner. The previously customary production of shaped bodies is not significantly changed by this.
  • the structure of the epoxy resin molding compositions produced in accordance with the invention essentially corresponds to the epoxy resin molding compositions which have been customary to date.
  • epoxy resins with at least two epoxy groups per molecule whose melting range is below 70 ° C.
  • Preferred are epoxy compounds which are liquid at room temperature, such as diglycidyl ether from Bisphenols or pre-extended resins based on bisphenol A diglycidyl ethers.
  • Low-viscosity resins such as epoxy resins based on cycloolefins or tetraglycidyldianiline, or else mixtures of solid epoxy resins, such as, for example, epoxidized novolaks with what are known as reactive diluents, are particularly preferred.
  • the epoxy resins can optionally be modified with other polymers such as polyesters, acrylates, silicone polymers or polyvinyl derivatives.
  • latent hardeners are used as hardeners, such as, for example, alkyl-substituted aromatic amines, polycarboxylic acids and anhydrides, BC1 3 or BF 3 complexes, latent hetero compounds based on nitrogen or phosphorus or metal complex compounds.
  • latent hardeners are also microencapsulated hardeners. Hardeners which, in free form, lead to curing of the epoxy resins at room temperature, such as aliphatic or aromatic amines or polyamines, novolaks or imidazole derivatives, are encapsulated with an inert material.
  • the capsule walls are destroyed either by the thermal energy introduced or by the shear forces occurring during the homogenization, and the hardener is released and homogenized with the rest of the molding compound mixture.
  • the amount of hardener used is chosen in a manner known per se so that it is sufficient for the epoxy compounds to be fully cured.
  • All inorganic and / or organic fillers customary for such molding compositions with the grain sizes usually used can be used as fillers.
  • Examples are hydrophobized or untreated chalk, dolomite, precipitated or ground silica, wollastonite, mica, talc, silicates, clays, titanium dioxide, lithopone, aluminum oxide hydrate, antimony trioxide but also cellulose or polyamide powder.
  • fibers in particular short fibers with an average length of 0.5 to 4 mm, can also be used as particularly reinforcing fillers.
  • fibers are glass, ceramic, aramid, cellulose, polyester, polyamide or C fibers.
  • the amount of fillers used is up to 95% by weight, preferably up to 85% by weight, based on the total molding composition.
  • additives such as lubricants or release agents such as waxes, metal soaps or substituted fatty acid amides, pigments, flexibilizers, coupling reagents, accelerators or flame retardants can also be mixed into the epoxy resin molding materials prepared according to the invention in amounts which are customary per se.
  • the mixing process takes place in a mixer with rapidly rotating mixing tools, e.g. a multi-shaft dissolver, a fluidized bed, turbo internal or high performance centrifugal mixer. Preference is given to high-speed mixers in which there is the possibility of also tempering the mix so that the temperature rise resulting from the energy input is limited so that the temperature of the mixture can be kept below the starting point of the curing reaction of the epoxy resin. If necessary, a cooling mixer can be installed downstream of the mixer. Within a short mixing time, if vortex or high-performance centrifugal mixers are used within a mixing time of less than one minute, the not yet homogeneous molding compound is obtained as loose, pressure-stable granules and can be stored as such at room temperature for several months. The mixing process must be ended when the granules have formed, because the mixture clumps together if the mixing time is extended.
  • mixing tools e.g. a multi-shaft dissolver, a fluidized bed, turbo internal or high performance centrifug
  • this granulate can be used as a molding compound for the production of molded parts.
  • the fillers have not been wetted intensively by the mixing process and the mixture is not sufficiently homogeneous, the mechanical properties of the moldings produced therefrom are unsatisfactory.
  • the granules are therefore homogenized shortly before shaping and curing under pressure. This is done in that the granules, optionally with heating to a temperature which is below the light-off temperature of the curing of the epoxy resin or below the melting temperature of the capsule wall material, possibly used encapsulated hardener, by means of a pressure-building conveyor device, about a piston pump or a screw is pressed through a continuous mixer upstream of the molding tool.
  • Continuous mixers with built-in screw are continuously running single-shaft or multi-shaft mixers or cocneters. A simpler but equally effective homogenization can be achieved if the continuous mixer upstream of the molding tool is a static mixer which is preceded by a pressure-building conveyor device which plasticizes the granules and presses them through the static mixer.
  • the molding compositions produced according to the invention are suitable for all applications in which epoxy resin molding compositions are used. In particular, however, they are suitable for the production of molded parts in the reaction injection molding process, for the encapsulation of electronic or electrical components or component components and for the production of mechatronic components.

Abstract

La présente invention concerne un procédé pour produire et traiter des matières à mouler en résine époxy, lesdites matières à mouler comprenant des résines époxy, des agents de durcissement, des substances de charge et des additifs. Selon l'invention, les résines époxy sont mélangées avec les composantes restantes de la matière à mouler dans un mélangeur comprenant des outils de mélange à grande vitesse, puis mises sous forme de granules, le granulat apte à l'écoulement ainsi obtenu étant homogénéisé sous pression peu avant mise en forme et durcissement.
EP03708109A 2002-02-28 2003-02-19 Procede pour produire et traiter des matieres a mouler en resine epoxy Ceased EP1480813A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE2002108644 DE10208644A1 (de) 2002-02-28 2002-02-28 Verfahren zur Herstellung und Verarbeitung von Epoxidharz-Formmassen
DE10208644 2002-02-28
PCT/EP2003/001639 WO2003072339A1 (fr) 2002-02-28 2003-02-19 Procede pour produire et traiter des matieres a mouler en resine epoxy

Publications (1)

Publication Number Publication Date
EP1480813A1 true EP1480813A1 (fr) 2004-12-01

Family

ID=27740504

Family Applications (1)

Application Number Title Priority Date Filing Date
EP03708109A Ceased EP1480813A1 (fr) 2002-02-28 2003-02-19 Procede pour produire et traiter des matieres a mouler en resine epoxy

Country Status (13)

Country Link
US (1) US20060286385A1 (fr)
EP (1) EP1480813A1 (fr)
JP (1) JP2005518957A (fr)
KR (1) KR20040088488A (fr)
CN (1) CN1638947A (fr)
AU (1) AU2003212250B8 (fr)
BR (1) BR0303325A (fr)
DE (1) DE10208644A1 (fr)
MX (1) MXPA04006905A (fr)
PL (1) PL370424A1 (fr)
RU (1) RU2308374C2 (fr)
WO (1) WO2003072339A1 (fr)
ZA (1) ZA200406199B (fr)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2372725B1 (fr) * 2010-03-26 2013-09-11 ABB Research Ltd. Production d'une isolation électrique et produits isolés
RU2460641C1 (ru) * 2011-03-15 2012-09-10 Государственное образовательное учреждение высшего профессионального образования "Тихоокеанский государственный университет" Способ формования изделий из эпоксидной смолы
CN102785326A (zh) * 2011-05-19 2012-11-21 深圳市安托山特种机电有限公司 一种新型封装材料注射机
CN104924593B (zh) * 2015-07-17 2018-02-23 威海两岸环保新材料科技有限公司 一步法制备聚乳酸薄膜的方法
CN106477969B (zh) * 2016-09-14 2019-03-01 九牧厨卫股份有限公司 一种制备砂浆的组合物、由其制备的砂浆、包含该砂浆的树脂浆组合物及其制备方法
JP6546623B2 (ja) * 2017-06-26 2019-07-17 矢崎総業株式会社 端子付き電線の製造方法

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AT350248B (de) * 1970-06-11 1979-05-25 Rother Dr Franz Verfahren zur herstellung von formkoerpern aus einer mischung aus anorganischen pulvern und epoxidharz
JPS5137152A (ja) * 1974-09-25 1976-03-29 Tokyo Nippon Yoki Kogyo Kk Ehokishijushifuntaisoseibutsu
JPS5692011A (en) * 1979-12-26 1981-07-25 Nitto Electric Ind Co Ltd Production of epoxy resin molding material
EP0038292B2 (fr) * 1980-02-21 1993-07-28 Ciba-Geigy Ag Utilisation de silicate de calcium synthétique cristallin
JPS5924762A (ja) * 1982-07-31 1984-02-08 Toto Kasei Kk 速硬化性粉体塗料組成物
JPS6155123A (ja) * 1984-08-27 1986-03-19 Nitto Electric Ind Co Ltd 粉末状エポキシ樹脂組成物の製造方法
JPH01129035A (ja) * 1987-11-12 1989-05-22 Nitto Denko Corp 粉末状エポキシ樹脂組成物の製造方法
EP0376884A3 (fr) * 1988-12-21 1991-06-05 Ciba-Geigy Ag Granulat coulant
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DE69722106T2 (de) * 1996-08-29 2004-04-01 Mitsubishi Denki K.K. Epoxidharzzusammensetzung und damit eingekapselte Halbleiteranordnungen
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Also Published As

Publication number Publication date
CN1638947A (zh) 2005-07-13
RU2308374C2 (ru) 2007-10-20
AU2003212250B2 (en) 2008-09-11
KR20040088488A (ko) 2004-10-16
AU2003212250A1 (en) 2003-09-09
PL370424A1 (en) 2005-05-30
MXPA04006905A (es) 2004-12-06
RU2004129283A (ru) 2005-08-10
US20060286385A1 (en) 2006-12-21
ZA200406199B (en) 2005-09-09
AU2003212250B8 (en) 2009-03-26
WO2003072339A1 (fr) 2003-09-04
DE10208644A1 (de) 2003-09-11
BR0303325A (pt) 2004-03-30
JP2005518957A (ja) 2005-06-30

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