EP1585784A1 - Systeme de resine de coulee fortement charge - Google Patents

Systeme de resine de coulee fortement charge

Info

Publication number
EP1585784A1
EP1585784A1 EP04703396A EP04703396A EP1585784A1 EP 1585784 A1 EP1585784 A1 EP 1585784A1 EP 04703396 A EP04703396 A EP 04703396A EP 04703396 A EP04703396 A EP 04703396A EP 1585784 A1 EP1585784 A1 EP 1585784A1
Authority
EP
European Patent Office
Prior art keywords
filler
resin system
casting resin
fraction
cast resin
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.)
Withdrawn
Application number
EP04703396A
Other languages
German (de)
English (en)
Inventor
Wolfgang Von Gentzkow
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.)
Siemens AG
Original Assignee
Siemens 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 Siemens AG filed Critical Siemens AG
Publication of EP1585784A1 publication Critical patent/EP1585784A1/fr
Withdrawn legal-status Critical Current

Links

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
    • 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
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • 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
    • C08K3/28—Nitrogen-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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • 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
    • C08K3/28—Nitrogen-containing compounds
    • C08K2003/282—Binary compounds of nitrogen with aluminium
    • 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
    • C08K2201/002—Physical properties
    • C08K2201/005—Additives being defined by their particle size in general
    • 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
    • C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K

Definitions

  • the invention relates to cast resin systems in which the proportion of filler is increased compared to conventional cast resin systems without an increase in viscosity restricting the processability of the cast resin.
  • Casting resin is to be understood as a low-viscosity reaction resin mixture that has a viscosity ⁇ 20,000 mPas at low processing temperature at a low shear rate.
  • core / shell particles are organic particles and typically do not fall under the generic term fillers
  • the viscosity increases due to the core / shell particles from 700-1000 mPas to 3500-5000 mPas, that is to say five times. This effect is even more pronounced with filler-containing systems. For these reasons, reaching filler concentrations ⁇ 70% by weight of quartz powder in a system that can be processed as casting resin does not appear credible.
  • the proportion of filler in the casting resin is the degree of filling.
  • filler combinations consisting of at least 2 fillers has been described several times in the literature. However, this does not result in increased fill levels of ⁇ 50% by volume.
  • JP11092622 describes filled injection molding systems with filler mixtures composed of at least two types of filler particles. However, the filler content is only a maximum of 35% by weight.
  • an ax. Is defined by a mixture of two fillers consisting of potassium titanate wiskers and potassium titanate powder. Filler concentration of 62.5 wt .-% realized. This corresponds to a degree of volume filling of ⁇ 30%.
  • JP63288977 describes molding compositions which contain a mixture of several fillers. However, this does not result in higher fill levels either.
  • the cast resin system comprises a combination of three filler fractions which differ in their particle size.
  • the D 50 particle size of the smallest particle fraction is preferably 1 to 10 ⁇ m, that of the medium particle fraction 10 to 100 ⁇ m and that of the largest particle fraction 100 to 1000 ⁇ m.
  • the cast resin system comprises a filler fraction which at least partially comprises particles whose surface is coated.
  • the surface of the filler particles can be coated with organic or inorganic layers.
  • the cast resin system comprises a bimodal filler mixture in which the volume fraction of the finer particle fraction is between 5 and 50 vol.%, Preferably between 10 and 25 vol.%, Based on the total filler.
  • the liquid portion of the filler-containing cast resin systems according to the invention consists of commercially available epoxy resins which are liquid at room temperature, unsaturated polyester resins (UP resins), polyurethane resins (PU resins), acrylic resins and silicone resins.
  • UP resins unsaturated polyester resins
  • PU resins polyurethane resins
  • acrylic resins acrylic resins and silicone resins.
  • Aromatic, aliphatic and cycloaliphatic di- or polyglycidyl ethers are suitable as epoxy compounds.
  • aromatic di- or polyglycidyl ethers used are bisphenol F diglycidyl ether and bisphenol A diglycidyl ether.
  • Cycloaliphatic glycidyl compounds and ⁇ -methylglycidyl compounds are used as aliphatic di- or polyglycidyl ethers.
  • epoxy resins with cycloalkylene oxide structures are bis (2,3-epoxycyclopentyl) ether, 2,3-epoxycyclopentylglycidyl ether, 1,2-bis (2,3-epoxycyclopentyl) ethane, vinylcyc- lohexene dioxide, 3, 4-epoxycyclohexylmethyl-3 x , 4 -epoxycyclo-hexane-carboxylate, 3, 4-epoxy-6-methylcyclohexylmethyl-3 ⁇ , 4 ⁇ - epoxy-6-methyl-cyclohexane carboxylate, bis (3, 4-epoxycyclo - hexylmethyl) adipate and bis (3, 4-epoxy-6-methylcyclohexylethyl1) adipate.
  • Preferred cycloaliphatic epoxy resins are bis (4-hydroxycyclohexyl) methane diglycidyl ether, 2,2-bis (4-hydroxycyclohexyl) propane diglycidyl ether, tetrahydrophthalic acid diglycidyl ester, 4-methyltetrahydrophthalic acid diglycidyl ester,
  • the cycloaliphatic epoxy resins can also be used in combination with aliphatic epoxy resins.
  • Epoxidation products of unsaturated fatty acid esters can be used as “aliphatic epoxy resins *.
  • Epoxy-containing compounds which are derived from mono- and polyfatty acids having 12 to 22 carbon atoms and an iodine number between 30 and 400 are preferably used, such as, for example, oleic acid, galdic acid, erucic acid, ricinoleic acid, linoleic acid, linolenic acid, elaidic acid, Likanic acid, arachidonic acid and clupanodonic acid.
  • the cast resin systems according to the invention can be used for the production of high-quality composite materials and / or material composites, for example as insulation and construction materials in electrical engineering, as floor coatings, plastic plasters, joint filling materials and facade claddings in the construction industry and for decorative applications in the interior and sanitary sector ,
  • a filled epoxy resin for example, is referred to as a composite material.
  • a “material composite” is when one or more materials are functionally “connected” to one another by a (hardened) casting resin.
  • the invention is explained in more detail below with the aid of examples:
  • the examples are filler-containing cast resin systems.
  • the fillers are mixed separately into the resin component and the hardener component. This happens at room temperature or at temperatures between 60 and 80 ° C.
  • the viscosity of the resin component containing the filler By measuring the viscosity of the resin component containing the filler, one can already study the viscosity-increasing influence of the fillers and filler mixtures.
  • the filled resin component and the filled hardener component are mixed together, degassed in a vacuum and measured immediately.
  • the filler mixtures can be mixed directly into the finished resin mixture.
  • Table 1 shows the fillers used in Examples 1 to 25. For this, density, particle size Size distribution and width of the particle size distribution are given.
  • Table 3 in Examples 7 to 10 shows the viscosities of an epoxy resin component, comprising 100 parts of bisphenol A diglycidyl ether CY 228 from Vantico, 4 parts of polypropylene glycol DY 049 from Vantico and 0.3 part of a flow aid from Vantico Byk (density of the mixture 1.15 g / cm 3 ) with various fillers and filler mixtures, which are obtained at different fill levels at 70 ° C depending on the shear rate.
  • the results show that despite the comparatively high viscosity of the epoxy resin component of approx. 1000 mPas at 70 ° C volume Fill levels up to 59% can be obtained. These correspond to fill levels of up to 77% by weight.
  • Silica flour comprising 100 parts of bisphenol A diglycidyl ether CY 228 from Vantico, 4 parts of polypropylene glycol DY 049 from Vantico and 0.3 part of a flow aid from Vantico Byk (density of the mixture 1.15 g
  • the enthalpy of reaction important for the curing process drops from 85 (Example 11, monomodal mixture) to 65 J / g (Examples 12 and 13, bimodal mixtures).
  • the loss of reaction and the linear expansion coefficient also decrease, which reduces the stress in connection with inorganic storage components and thus significantly improves the properties of the compound.
  • the thermal conductivity is increased, as a result of which the curing temperature can be reduced and the cycle time in the molding material production can be reduced. This measure significantly improves the mechanical properties of the composite materials, such as modulus of elasticity, flexural strength and fracture toughness.
  • Examples 17 and 18 show that 5 with the same filler composition as in Example 16 with UP resins (Example 17) and PU resins (Example 18) similar viscosity values are obtained as with epoxy resins.
  • Table 8 Viscosity values of unsaturated polyester resin filled with aluminum oxide Resin matrix: unsaturated polyester Altana (UP 3400) flow aid, density 1.18 g / cm 3
  • Resin matrix PU casting compound 4204: 4900 (2: 1) Altana, flow aid, density 1.07 g / cm 3
  • compositions according to the invention can be used to produce sufficiently flowable cast resin mixtures with very high filler contents which were previously not considered processable.
  • the degree of filling is achieved with which noticeable improvements in properties can be achieved, e.g. for the flame resistance, the linear coefficient of thermal expansion, the thermal conductivity, the fracture toughness, the specific fracture energy, the modulus of elasticity, the reaction shrinkage and the reaction enthalpy.
  • the technological improvements mentioned can then be used to derive further technological advantages for the products made from the highly filled epoxy resin molding materials.
  • By better dissipating the cross-linking reaction local temperature peaks are avoided and in connection with the lower coefficient of thermal expansion and the reduced reaction shrinkage there is less cooling stress and improved resistance to temperature changes.
  • the curing or molding temperatures can be reduced or the curing or cycle times can be shortened while maintaining the temperatures, without having to accept poorer demolding rigidity. Together with the lower material costs for highly filled cast resin systems, this leads to a higher one
  • Figure 1 Viscosity of filler-containing epoxy resin mixtures as a function of the filler content using the example of the Rütapox VE 4518 resin mixture from Bakelite AG

Landscapes

  • 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 un système de résine de coulée selon lequel, comparativement à des systèmes de résine de coulée traditionnels, la proportion de charge est élevée de 50% en volume, à des valeurs Φ, sans qu'une augmentation de la viscosité ne réduise la moulabilité de la résine de coulée. L'augmentation du niveau de charge est obtenue par répartition multimodale de la charge.
EP04703396A 2003-01-23 2004-01-20 Systeme de resine de coulee fortement charge Withdrawn EP1585784A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10302642 2003-01-23
DE10302642 2003-01-23
PCT/EP2004/000431 WO2004065469A1 (fr) 2003-01-23 2004-01-20 Systeme de resine de coulee fortement charge

Publications (1)

Publication Number Publication Date
EP1585784A1 true EP1585784A1 (fr) 2005-10-19

Family

ID=32747485

Family Applications (1)

Application Number Title Priority Date Filing Date
EP04703396A Withdrawn EP1585784A1 (fr) 2003-01-23 2004-01-20 Systeme de resine de coulee fortement charge

Country Status (2)

Country Link
EP (1) EP1585784A1 (fr)
WO (1) WO2004065469A1 (fr)

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102004060765A1 (de) * 2004-12-15 2006-07-06 Bene_Fit Gmbh Verfahren zur Herstellung von Verbundwerkstoffen, Verbundwerkstoff und dessen Verwendung
GB0515088D0 (en) * 2005-07-22 2005-08-31 Imerys Minerals Ltd Particulate glass compositions and methods of production
US8586654B2 (en) 2009-04-21 2013-11-19 Dow Global Technologies, Llc Anisotropic composite
US9481759B2 (en) 2009-08-14 2016-11-01 Boral Ip Holdings Llc Polyurethanes derived from highly reactive reactants and coal ash
US8846776B2 (en) 2009-08-14 2014-09-30 Boral Ip Holdings Llc Filled polyurethane composites and methods of making same
DE102010046627A1 (de) * 2010-09-17 2012-03-22 Schock Gmbh Formteil, wie beispielsweise Küchenspülbecken, Waschbecken oder dergleichen, sowie Verfahren zum Herstellen eines solchen Formteils
US9932457B2 (en) 2013-04-12 2018-04-03 Boral Ip Holdings (Australia) Pty Limited Composites formed from an absorptive filler and a polyurethane
US20160130385A1 (en) * 2013-06-07 2016-05-12 Covestro Deutschland Ag Polyol formulations containing fillers and polyurethanes produced therefrom
US10138341B2 (en) 2014-07-28 2018-11-27 Boral Ip Holdings (Australia) Pty Limited Use of evaporative coolants to manufacture filled polyurethane composites
DE102019204191A1 (de) * 2019-03-27 2020-10-01 Siemens Aktiengesellschaft Gießharz, Formstoff daraus, Verwendung dazu und eine elektrische Isolierung
CN113583390A (zh) * 2021-09-08 2021-11-02 深圳先进电子材料国际创新研究院 一种环氧基封装材料增韧改性的方法

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5576362A (en) * 1992-04-20 1996-11-19 Denki Kagaku Kogyo Kabushiki Kaisha Insulating material and a circuit substrate in use thereof
FR2742763B1 (fr) * 1995-12-22 1998-03-06 Rhone Poulenc Chimie Elastomere silicone a haute conductibilite thermique
US6054222A (en) * 1997-02-20 2000-04-25 Kabushiki Kaisha Toshiba Epoxy resin composition, resin-encapsulated semiconductor device using the same, epoxy resin molding material and epoxy resin composite tablet
US6096414A (en) * 1997-11-25 2000-08-01 Parker-Hannifin Corporation High dielectric strength thermal interface material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO2004065469A1 *

Also Published As

Publication number Publication date
WO2004065469A1 (fr) 2004-08-05

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