Direct filling

FIELD: chemistry.

SUBSTANCE: invention relates to a curing composition for producing electrically insulating structural material for electrical or electronic components. The curing composition contains epoxy resin, a curing agent and a filler composition. The filler composition contains wollastonite and amorphous silicon dioxide. The surface of one of the fillers is treated with silane. A cured product is obtained by curing said curing composition.

EFFECT: invention enables to use said curing composition directly in the ceramic housing of a switching device and has high cracking resistance.

9 cl, 3 tbl, 2 ex

 

The present invention relates to a curing composition containing epoxy resin and a filler composition, to otverzhdennom product obtained by curing the specified curing of the composition and to the use of hardened products as insulating structural material for electric or electronic components. In addition, the present invention relates to the use of the cured composition to obtain components or parts of electrical equipment, as well as to a method for insulating equipment.

The components of the switching devices are subject to very strict requirements. Usually provides the electrical components with the shell, which consists of insulating synthetic resin. In addition to the required dielectric characteristics of the membrane are important mechanical properties such as impact strength and resistance to cracking.

A critical factor of the resin sheath for electrical components with high performance, such as vacuum switching devices or transformers operating in voltage ranges up to about 40 kV, is resistant to cracking during temperature fluctuations.

An indicator of the resistance to cracking when Ter is atilirovanie is the so-called cracking index (IL) (RI).

In order to avoid cracking the shell material, the prototype suggests that the vacuum chamber of the switching devices and other items installed in the dielectric parts and kapsulirovanie in the bearing load shell composed of epoxy resin. To prevent cracking form the composition comprises a powder filler, such as quartz powder or powder of synthetic silicon dioxide.

However, the cracking index (IL)(RI)obtained by the above method is inadequate for electrical components with high performance.

In addition, electrical components capsulised in silicone or polyurethane, or soft, molded resin, which is a type of buffer that is resistant to the stresses resulting from differences in thermal extensions.

The technology of encapsulation means that the vacuum switching chamber and the inserted part must be depreciated for mechanical reasons by the elastomeric material prior to introduction into the epoxy resin. The requirements for this material are:

high dielectric strength and adequate flexibility to absorb thermal stresses and mechanical stresses.

Elastomeric snubbing absorbs stresses that have places is encapsulated components in the process of work as a result of differences in thermal extensions kapsulirujushchej material and capsulerebel component.

However, this technology requires at least two stages of the method, which is less efficient and, in addition, intensive.

Thus, preferred is a method of casting, in which epoxy resin is applied directly in the vacuum chamber of the switching device and which does not require additional amortizatory.

WO-A1-2004/090913 describes a method of producing castings for switching devices for discovolante, srednetonnazhnyh and vysokovoltnyh applications, in which a mixture of glass beads with a given distribution of diameters of size Dx is entered in kapsulirujushchej compound, thus creating a direct encapsulation of components. However, the method of direct pouring switching devices discussed in WO-A1-2004/090913, has the disadvantage of high cost of hollow spheres, and, in addition, the hollow spheres can partially mechanically break down during mixing, which reduces the efficiency.

In addition, the deals that can be used more fillers such as amorphous silicon dioxide and wollastonite. However, not described in the application, in which some combination of these two fillers is suitable as a filler for epoxy systems used for direct casting of vacuum switching devices.

EP-A2-1176171 rassmatrivavshijsja material for direct pouring of the switching devices, containing matrix termotorgmash resin containing epoxy resin and modified acid anhydride, and inorganic particles and rubber particles having the structure of the core/ sheath. However, the combination of inorganic particles, rubber particles having the structure of the core/sheath is very expensive.

US-B1-6638567 considers cured composition containing:

(a) a cycloaliphatic epoxy resin which is liquid at room temperature and suspended in the polymer core/shell;

(b) an anhydride of the polybasic carboxylic acids;

(C) two different filler (C1) and (C2), where C1 is a filler which is capable of releasing water when the temperature rises above room temperature, and (C2) is a reinforcing material; and the total proportion of fillers (C1) and (C2) is from 58 to 73 wt.%. in relation to the total amount of components (a), (b), (C1) and (C2) in the composition, and the mass ratio fillers (C1):(C2) is in the range from 1:3 to 1:1.

Cured composition can be used for direct casting of vacuum switching devices and other electrical components with high performance. However, the considered polymer systems core/shell is full-time is expensive.

The aim of the present invention is to solve the problems associated with the systems discussed in the prototypes. In addition, the aim is the creation of a cured composition that can be directly applied in a ceramic housing of the switching device and which has a high resistance to cracking temperature ceramic shell.

Now unexpectedly found that the above problems can be solved curing the epoxy resin composition containing a combination of different fillers.

The first variant of the present invention is a cured composition containing

(a) epoxy resin and

b) composition of fillers containing

i) wollastonite and

ii) amorphous silicon dioxide.

An integral component of the cured compositions of the present invention is a composition of fillers containing wollastonite and amorphous silicon dioxide.

The wollastonite is a naturally occurring acicular calcium silicate formula Ca3[Si3O9]having a particle size in the micron range. Artificially obtained wollastonite is also the needle. The wollastonite is supplied commercially, e.g. under the trademark Nyad company Nyco Company or under the trademark Tremin firm uarzwerke, Germany, for example, Tremin 283-100 EST or Tremin 283-600 EST.

According to a preferred variant of the wollastonite is a powder having an average particle size of d501-100 μm, more preferably from 2 to 50 μm and most preferably from 3 to 25 μm, determined according to ISO 13320-1:1999.

In addition, it is preferable curing the composition in which the wollastonite has an average particle size of d501-200 μm, more preferably from 2 to 100 μm and most preferably from 5 to 90 μm, determined according to ISO 13320-1:1999.

Figure d50known as the average diameter of the particles. This means that the powder contains 50% of the particles having a larger particle size, and 50% of the particles having a smaller particle size than the value of d50. Figure d95means that 95% of the particles have a smaller particle size and 5% of the particles have a larger particle size than the value of d95.

The wollastonite preferably has a bulk density of 0.40-0,90 g/cm3more preferably 0,49-0,80 g/cm3and most preferably from 0.55 to 0.76 g/cm3defined according to DIN 52466.

Especially preferred is a wollastonite having a specific surface area by BET method 2-5 m2/g determined according to DIN 66132.

Curing the composition according to the present invention predpochtitel what about the contains wollastonite, the surface is treated. Preferably the surface of the wollastonite is treated with silane, preferably selected from the group consisting of aminosilane, epoxysilane, (meth)acrylic silane, methylsilane and vinylsilane.

Preferably the silane is selected from silane according to the following formula:

where R represents methyl or ethyl.

The second essential component of the filler is amorphous silica. Preferably amorphous silicon dioxide is a natural amorphous silica or fused quartz. Fused silica with an average particle size (d50) of 10.5 μm is commercially available under the trademark Tecosil from CE Minerals, Greenville, TN, USA. Natural amorphous silicon dioxide sold under the trademark Amosil firm Quarzwerke, Germany.

According to a preferred variant of amorphous silicon dioxide has an average particle size (d50) 1-100 μm, more preferably from 2 to 50 μm and most preferably from 5 to 25 μm, determined according to ISO 13320-1:1999.

Preferably amorphous silicon dioxide has a treated surface. Preferably the surface of the amorphous silicon dioxide is treated with silane, more preferably selected from the group consisting of aminosilane, epoxysilane, (methacrylic silane, methylsilane and vinylsilane.

Preferably the silane is selected from silane according to the following formula:

where R represents methyl or ethyl.

According to a preferred variant of the cured composition according to the present invention contains the composition of the fillers, in which the mass ratio of silica/wollastonite is from 10:1 to 1:10, preferably from 9:1 to 1:9, more preferably from 85:15 to 15:85, particularly preferably from 70:30 to 30:70 and most preferably from 60:40 to 40:60.

Preferably cured composition comprises the composition of fillers, in which the wollastonite and/or amorphous silicon dioxide has an average particle size (d50in the interval from 2 to 50 μm, determined according to ISO 13320-1:1999.

In addition, it is preferable that at least one of the fillers of the composition of the filler is surface treated with silane.

Especially preferred is a cured composition, in which the surface of the wollastonite and/or amorphous silica treated with silane selected from the group consisting of aminosilane, epoxysilane, (meth)acrylic silane, methylsilane and vinylsilane.

Another integral component of the cured compositions according to the present invention is an epoxy see the La.

Preferably the epoxy resin is liquid at 25°C.

To obtain compositions according to the present invention epoxy resins suitable as component (a)are epoxy resin, the usual technology of epoxy resins. Examples of epoxy resins are:

I) Polyglycidyl and poly(β-methylpyridine) esters obtained by the interaction of the compounds having at least two hydroxyl groups in the molecule with epichlorohydrin and β-methylephedrine respectively. The reaction is mainly carried out in the presence of bases.

As compounds having at least two hydroxyl groups in the molecule, can be used aliphatic polybasic carboxylic acid. Examples of polybasic carboxylic acids are oxalic acid, succinic acid, glutaric acid, adipic acid, Emelyanova acid, cork acid, azelaic acid or diarizonae or trimmeresana linoleic acid.

It is also possible, however, to use cycloaliphatic polybasic carboxylic acids, for example hexahydrophthalic acid or 4-methylhexahydrophthalic acid.

Can also be used aromatic polybasic carboxylic acids, for example phthalic acid, isophthalic acid sludge is terephthalic acid, and partially hydrogenated aromatic polybasic carboxylic acids, such as tetrahydrophtalic acid or 4-methyltetrahydrophthalic acid.

II) Polyglycidyl and poly(β-methylpyridine) ethers, obtained by the interaction of the compounds having at least two free alcoholic hydroxyl groups and/or phenolic hydroxyl groups with epichlorohydrin and β-methylephedrine under alkaline conditions or in the presence of an acid catalyst with subsequent alkali treatment.

Glycidyloxy esters of the specified type are derived, for example, acyclic alcohols such as ethylene glycol, diethylene glycol or higher poly(oksietilenom)glycols, propane-1,2-diol or poly(oxypropylene)glycols, propane-1,3-diol, butane-1,4-diol, poly(oxytetracyline)glycols, pentane-1,5-diol, hexane-1,6-diol, hexane-2,4,6-triol, glycerol, 1,1,1-trimethylolpropane, pentaerythritol, sorbitol, and polyepichlorohydrins.

Other simple glycidyloxy esters of the specified type are derived from cycloaliphatic alcohols, such as 1,4-cyclohexanedimethanol, bis-(4-hydroxycyclohexyl)methane or 2,2-bis-(4-hydroxycyclohexyl)propane, or from alcohols, which contain aromatic groups and/or other functional groups, such as N,N-bis-(2-hydroxyethyl)aniline or p,p'-bis-(2-hydroxic the laminitis)difenilmetana. Simple glycidyloxy esters can also be based on mononuclear phenols, such as resorcinol or hydroquinone, or on the basis of multinuclear phenols, for example bis-(4-hydroxyphenyl)methane, 4,4'-dihydroxybiphenyl, bis-(4-hydroxyphenyl)sulfone, 1,1,2,2-tetrakis-(4-hydroxyphenyl)ethane, 2,2-bis-(4-hydroxyphenyl)propane or 2,2-bis-(3,5-dibromo-4-hydroxyphenyl)propane.

Other hydroxidealuminum that are appropriate for simple glycidyloxy esters are novolak obtained by condensation of aldehydes, such as formaldehyde, acetaldehyde, chloral or furfural, phenols or bisphenolate, which are unsubstituted or substituted by chlorine atoms or With1-C9-alkyl groups, such as phenol, 4-chloro-phenol, 2-METHYLPHENOL or 4-tert-butylphenol.

III) Poly(N-glycidyl)new compounds obtained by dehydrochlorination of the reaction products of epichlorhydrin with amines containing at least two amine hydrogen atom. Such amines are, for example, aniline, n-butylamine, bis-(4-AMINOPHENYL)methane, motacillidae or bis-(4-methylaminophenol)methane.

Poly(N-glycidyl)new compounds also include, however, tripyridyltriazine, N,N'-diglycidyl derivatives cycloalkylation, such as etilenmocevina or 1,3-propylenimine, and diglycidyl derivatives guide is stoinov, such as 5,5-dimethylhydantoin.

IV) Poly(S-glycidyl)inhibiting compounds, for example di-S-glycidyloxy derivatives come from developed, for example ethane-1,2-dithiol or simple bis-(4-mercaptomethyl)ether.

V) Cycloaliphatic epoxy resins, for example, a simple bis-(2,3-epoxycyclohexyl)ether, 2,3 simple-amoxicillingeneric ether, 1,2-bis-(2,3-amoxicillinamoxil)ethane or 3,4-epoxycyclohexylmethyl-3',4'-epoxycyclohexanecarboxylate.

It is also possible, however, to use epoxy resins in which the 1,2-epoxypropyl linked to different heteroatoms or functional groups; these compounds include, for example, N,N,O-triglycidyl derivative of 4-aminophenol, (simple ether(ester) salicylic acid, N-glycidyl-N'-(2-glycidyloxy)-5,5-dimethylhydantoin and 2 glycidyloxy-1,3-bis-(5,5-dimethyl-1-glycidylester-3-yl)propane.

Compositions according to the present invention are polymeric systems from medium to relatively high viscosity, which can be completely solidified by heating. In dry condition they are thermosetting materials of relatively high rigidity, having a glass transition temperature of about 80-140°C. the Term "cycloaliphatic epoxy resin" in the context of this invention means any epoxy resin having C is kalifatidis structural units, i.e. it includes both cycloaliphatic glycidyloxy compounds, and β-methylpyridine compounds and epoxy-based cycloalkylation. The term "liquid at room temperature (RT)(RT)" should be understood as meaning pour compounds that are liquid at 25°C, i.e. they are low to medium viscosity (viscosity less than about 20,000 MPa * s, determined Rheomat equipment type 1154 MS DIN 125; D=11/c at 25°C).

Suitable cycloaliphatic glycidyloxy compounds and β-methylpyridinium compounds are glycidyloxy esters and β-methylglycerol esters of cycloaliphatic polybasic carboxylic acids, such as tetrahydrophtalic acid, 4-methyltetrahydrophthalic acid, hexahydrophthalic acid, 3-methylhexahydrophthalic acid and 4-methylhexahydrophthalic acid.

Other suitable cycloaliphatic epoxy resins are simple diglycidyl esters and simple β-methylglycerol esters of cycloaliphatic alcohols, such as 1,2-dihydrocyclopenta, 1,3-dihydroxytoluene and 1,4-dihydrocyclopenta, 1,4-cyclohexanedimethanol, 1,1-bis-(hydroxymethyl), cyclohex-3-ene, bis-(4-hydroxycyclohexyl)methane, 2,2-bis-(4-hydroxycyclohexyl)propane and (4-hydroxycyclohexyl)sulfon.

Examples of epoxy resins having cycloalkenes the derivative structure, are simple bis-(2,3-epoxycyclohexyl)ether, 2,3 simple-amoxicillingeneric ether, 1,2-bis-(2,3-epoxycyclohexyl)ethane, vinylcyclohexane, 3,4-epoxycyclohexylmethyl-3',4'-epoxycyclohexanecarboxylate, 3,4-epoxy-6-methylcyclohexyl-3',4'-epoxy-6'-methylcyclohexanecarboxylic, bis-(3,4-epoxycyclohexylmethyl)adipate and bis-(3,4-epoxy-6-methylcyclohexyl)adipate.

Preferred cycloaliphatic epoxy resins are simple bis-(4-hydroxycyclohexyl)metadirectory ether, simple, 2,2-bis-(4-hydroxycyclohexyl)perpendicularity ether, diglycidyl ether tetrahydrophthalic acid, diglycidyl ether 4-methyltetrahydrophthalic acid, diglycidyl ether 4-methylhexahydrophthalic acid, 3,4-epoxycyclohexylmethyl-3',4'-epoxycyclohexanecarboxylate and especially diglycidyl ether hexahydrophthalic acid.

Can also be used aliphatic epoxy resin. As the "aliphatic epoxy resins", you can use the epoxidation products of esters of unsaturated fatty acids. It is preferable to use epoxydodecane compounds, derivatives of one - and polybasic fatty acids having from 12 to 22 carbon atoms and an iodine number of from 30 to 400, for example eurolingua acid, Mirandolina acid, palmitoleic acid,oleic acid, gadolinia acid, erucic acid, ricinoleic acid, linoleinovoy acid, linolenic acid, elaidic acid, lisanova acid, arachidonic acid and kopandanova acid.

For example, suitable are the products of the epoxidation of soybean oil, linseed oil, perelomova oil, Tung oil, oiticica oil, safflower oil, poppy oil, hemp oil, cottonseed oil, sunflower oil, rapeseed oil, polyunsaturated triglycerides, triglycerides of Euphorbia, peanut oil, olive oil, oils of olive seed oil, almond oil, kapok oil, oil of nutmeg, oil of apricot pits, oil, beech nut, luminophore oil, corn oil, sesame oil, grapeseed oil, oil lallemantia, castor oil, herring oil, oil sardines, Menhaden-oil, whale blubber, tall oil and derivatives thereof.

Also suitable are higher unsaturated derivatives, which can be obtained by the sequential dehydrogenation reactions of these oils.

Olefinic double bonds of the radicals of unsaturated fatty acids of the above compounds can be epoxydecane in accordance with known methods, for example by reaction with hydrogen peroxide, optionally in the presence of a catalyst, and is calligraphed or nagkalat, for example, naturaline acid or peracetic acid. In the scope of the invention for component (a) can be used as a fully epoxydecane and partially epoxydecane derivatives, which still contain free double bonds.

Preference is given to using epoxidizing soybean oil and epoxidizing linseed oil.

Can also be used mixtures of epoxy resins (I)-(V)above. Curing the composition according to the present invention preferably contains a liquid at 25°C or solid aromatic or cycloaliphatic simple glycidyloxy ether or complex glycidyloxy ether, particularly preferably simple diglycidyl ether or complex diglycidyl ether of bisphenol a or bisphenol F. the Preferred epoxy resin can also be obtained by the reaction of simple polyglycidyl ether and complex polyglycerol ester with alcohols, such as diols. Interaction with dialami increases the molecular weight.

Particularly preferred is an epoxy resin, which is a simple glycidyloxy ether of bisphenol a, which interacts with less than equimolecular amount of bisphenol A.

According to a preferred variant of the cured composition contains epoxy resin, wybran the Yu group, consisting of complex polyglycidyl ether complex of poly(β-methylglycyl)new ether, simple polyglycidyl ether, simple poly(β-methylglycyl)new ether.

Preferably cured composition according to the present invention contains a cycloaliphatic epoxy resin, which is preferably selected from the group consisting of simple bis-(4-hydroxycyclohexyl)metadigital.gov.co ether, simple 2,2-bis-(4-hydroxycyclohexyl)propertyholding ether, diglycidylether ether tetrahydrophthalic acid, dipyridamole ether 4-methyltetrahydrophthalic acid, dipyridamole ether 4-methylhexahydrophthalic acid, 3,4-epoxycyclohexylmethyl-3',4'-epoxycyclohexanecarboxylate and diglycidylether ether hexahydrophthalic acid.

Preferably cured composition further comprises a curing agent, more preferably anhydrous compound.

More preferably cured composition further comprises an anhydride of the polybasic carboxylic acid.

Anhydrite hardener may be a linear aliphatic polymeric anhydrides, for example policeacademy polyanhydride, or polianilinovyh polyanhydride, or cyclic anhydrides of carboxylic acids.

The cyclic anhydrides of carboxylic acids are especially predpochtite lname.

Examples of cyclic anhydrides of carboxylic acids are succinic anhydride, citraconic anhydride, itacademy anhydride, alkenylamine succinic anhydrides, dodecanesulfonyl anhydride, maleic anhydride and tricarballylic anhydride, the adduct of maleic anhydride with cyclopentadiene or methylcyclopentadiene, adduct of linoleic acid with maleic anhydride, alkylated andalternative anhydrides, methyltetrahydrophthalic anhydride and tetrahydrophthalic anhydride, and isomeric mixtures of the latter two compounds are especially preferred.

Preferably the curing agent is anhydrous hardener, which is more preferably selected from the group consisting of methyltetrahydrophthalic anhydride, methyl-4-endo-methylentetrahydrofolate anhydride, methylhexahydrophthalic anhydride, tetrahydrophthalic anhydride.

More preferably anhydrous hardener is a poly(ester)anhydride, which is obtained by the interaction of the dianhydride with less than equimolecular number diols.

Especially preferred is the product of the interaction methyltetrahydrophthalic anhydride with ethylene glycol, which is commercially available under the trademark XB 5993 (provider - Huntsman, Switzerland).

Songs from the according to the present invention optionally contain a curing accelerator as an additional component. Suitable curing accelerators known to specialists in this field of technology. Examples which may be mentioned are:

complexes of amines, especially tertiary amines, with trichloride boron or boron TRIFLUORIDE;

tertiary amines, such as benzyldimethylamine;

derivatives of urea, such as N-4-course-N',N'-dimethyloxetane (monuron);

unsubstituted or substituted imidazoles, such as imidazole or 2-phenylimidazol.

The preferred accelerators for the above compositions, which contain epoxydecane oil, are tertiary amines, especially benzyldimethylamine, and imidazoles (e.g., 1-Mei).

Hardeners and, when applicable, accelerators are used in conventional effective amounts, i.e. in amounts sufficient for the curing of the compositions according to the present invention. The ratio of the components (polymer system)/hardener/accelerator depends on the nature of the compounds, the desired rate of curing and the desired properties of the final product and can be easily determined by a person skilled in the art. Typically used from 0.4 to 1.6 equivalents, preferably from 0.8 to 1.2 equivalents, anhydrite groups on amoxicillin.

The curing accelerators are generally used in quantities of from 0.1 to 20 parts by weight per 100 parts by weight of epoxy is Noah resins (resins).

Curing the composition according to the present invention may optionally contain other additives such as plasticizer, additives that prevent delamination of the mixture, dyes, antifoam, light, additives that improve the release of forms, supplements that increase impact strength, adhesion promoter, flame retardants and curing accelerators.

Curing the composition according to the present invention can be used to obtain components or parts of electrical equipment.

Therefore, another option of the present invention is the application of the curing composition according to the present invention for obtaining components or parts of electrical equipment. Preferably, the electrical component is selected from the group consisting of transformers, insulating bushings, insulators, switches, sensors, converters and cable sealing ends. Preferably cured composition is used to directly fill the vacuum chamber of the switching device.

Curing the composition according to the present invention preferably termomaterialy. The resulting cured products show unexpectedly superior mechanical properties, particularly in terms of resistance to cracking when thermocyclers the AI.

Therefore, another option of the present invention is a cured product obtained by curing curing composition according to the present invention.

Cured products according to the present invention are preferably used as insulating structural material for electric or electronic components, it is preferable for the vacuum chambers of the switching devices.

Another option of the present invention is a method of obtaining electrical equipment containing the following stages:

a) applying a cured composition according to the present invention in the case of electrical components; and

b) curing curing of the composition.

The preferred option of the present invention to provide electrical insulation that contains the following stages:

a) applying a cured composition according to the present invention in a ceramic housing of the switching device; and

b) curing curing of the composition.

Curing the composition according to the present invention preferably is used for direct casting ceramic shell of the vacuum chamber of the switching device. Therefore, according to the preferred variant of the method according to the present from which retenu cured composition is applied directly to the ceramic housing of the switching device. The value of this application direct application means that the cured composition is applied directly to the ceramic surface without separation of the elastic buffer layer.

According to a preferred variant of the method according to the present invention, the cured composition is applied, preferably injected in a pre-heated form, which contains the ceramic housing of the switching device.

Preheated form has a temperature in the range from 130 to 160°C. it is also preferable that the cured composition is cured by heating, preferably in the range from 130 to 160°C. Usually cured composition is cured for at least 10 minutes, preferably 10-60 minutes

The method according to the present invention preferably contains the following stages:

a) injection of curing of the composition in a pre-heated form, having a temperature in the range from 130 to 160°C, where this form contains a ceramic housing of the switching device,

b) at least partially curing curing of the composition,

(C) removing forms and

d) an optional curing curing of the composition.

Especially, it is preferable that the cured composition is in direct contact with the again the ceramic housing of the switching device.

EXAMPLES

Table 1
The raw materials used in the examples
XB 5992®Liquid, modified, low viscosity epoxy resin bisphenol a with amoxicillinum 4,9-5,1 EQ./kg Supplier: Huntsman, Switzerland
XB 5993®Liquid, modified, pre-accelerated anhydrous compound. Supplier: Huntsman, Switzerland
Bayferrox®225Dye - pigment iron oxide. Supplier: Bayer, Germany
Tecosil®44iFused silica with an average particle size (d50) to 10.5 μm. Supplier: CE Minerals, Greenville, Texas, USA
Amosil®520Amosil®520 derived from natural amorphous silica by grinding with subsequent air separation. The average particle size (d50) 21 μm. Supplier of: Quarzwerke, Germany
Tremin®283-100ESTThe wollastonite surface-treated epoxysilane with an average particle size (d50) of 8 μm. Supplier of: Quarzwerke, Germany
Tremin®283-600ESTThe wollastonite surface-treated epoxysilane with an average particle size (d50) 3.5 µm. Supplier of: Quarzwerke, Germany

1. Comparative example C1

(only fused silica Tecosil®44i)

In a heated steel vessel 100 g XB 5992®mixed with 90 g XB 5993®and the mixture is heated under weak stirring propeller stirrer at 60°C for about 5 minutes Then the stirrer is stopped, add 2 g of Bayferrox®225 and again let the mixer for about 1 min. Then under stirring added in several portions 342 g Tecosil®44i and the mixture is heated at 60°C under stirring for about 10 minutes Then the stirrer is stopped and the vessel carefully Tegaserod tabulation of vacuum for about 1 minutes

A small portion of the mixture is used to measure the viscosity at 60°C on a Rheomat equipment (type 115, MS DIN 125 D=11). The main part of the mixture is poured into heated to 140°C steel form with receiving plates to determine the characteristics (thickness 4 mm). The form is then installed in the heat chamber at 140°C for 30 min After the heat of the casting form is then removed from the heating Cabinet and the plate is cooled to ambient temperature (25°C).

2. Comparative example C2

(tol is to the wollastonite Tremin ®283-100 EST)

In a heated steel vessel 100 g XB 5992®mixed with 90 g XB 5993, and the mixture is heated under weak stirring propeller stirrer at 60°C for about 5 minutes Then the stirrer is stopped, add 2 g of Bayferrox®225 and again let the mixer for about 1 min. Then under stirring added in several portions 342 g Tremin®283-100 EST and the mixture is heated at 60°C under stirring for about 10 minutes Then the stirrer is stopped and the vessel carefully Tegaserod tabulation of vacuum for about 1 min. a Small portion of the mixture is used to measure the viscosity at 60°C on a Rheomat equipment (type 115, MS DIN 125 D=11). The main part of the mixture is poured into heated to 140°C steel form with receiving plates to determine the characteristics (thickness 4 mm). The form is then installed in the heat chamber at 140°C for 30 min After the heat of the casting form is then removed from the heating Cabinet and the plate is cooled to ambient temperature (25°C).

3. Example 1 according to the invention

(50% Tecosil®44i + 50% Tremin®283-100 EST)

In a heated steel vessel 100 g XB 5992®mixed with 90 g XB 5993®and the mixture is heated under weak stirring propeller stirrer at 60°C for about 5 minutes Then the stirrer is stopped, add 2 g of Bayferrox®225 and again let the mixer in each is about 1 minutes Then under stirring added in several portions 171 g Tremin®283-100 EST and 171 g Tecosil®44i and the mixture is heated at 60°C under stirring for about 10 minutes Then the stirrer is stopped and the vessel carefully Tegaserod tabulation of vacuum for about 1 min. a Small portion of the mixture is used to measure the viscosity at 60°C on a Rheomat equipment (type 115, MS DIN 125 D=11). The main part of the mixture is poured into heated to 140°C steel form with receiving plates to determine the characteristics (thickness 4 mm). The form is then installed in the heat chamber at 140°C for 30 min After the heat of the casting form is then removed from the heating Cabinet and the plate is cooled to ambient temperature (25°C).

4. Comparative example C3

(only natural amorphous silica Amosil®520)

In a heated steel vessel 100 g XB 5992®mixed with 90 g XB 5993®and the mixture is heated under weak stirring propeller stirrer at 60°C for about 5 minutes Then the stirrer is stopped, add 2 g of Bayferrox®225 and again let the mixer for about 1 min. Then under stirring added in several portions 342 g Amosil®520 and the mixture is heated at 60°C under stirring for about 10 minutes Then the stirrer is stopped and the vessel carefully Tegaserod tabulation of vacuum for about 1 minutes

The nothing is a part of the mixture used to measure the viscosity at 60°C on a Rheomat equipment (type 115, MS DIN 125 D=11). The main part of the mixture is poured into heated to 140°C steel form with receiving plates to determine the characteristics (thickness 4 mm). The form is then installed in the heat chamber at 140°C for 30 min After the heat of the casting form is then removed from the heating Cabinet and the plate is cooled to ambient temperature (25°C).

5. Comparative example C4

(wollastonite Tremin®283-600 EST)

In a heated steel vessel 100 g XB 5992®mixed with 90 g XB 5993®and the mixture is heated under weak stirring propeller stirrer at 60°C for about 5 minutes Then the stirrer is stopped, add 2 g of Bayferrox®225 and again let the mixer for about 1 min. Then under stirring added in several portions 342 g Tremin®283-600 EST and the mixture is heated at 60°C under stirring for about 10 minutes Then the stirrer is stopped and the vessel carefully Tegaserod tabulation of vacuum for about 1 minutes

A small portion of the mixture is used to measure the viscosity at 60°C on a Rheomat equipment (type 115, MS DIN 125 D=11). The main part of the mixture is poured into heated to 140°C steel form with receiving plates to determine the characteristics (thickness 4 mm). The form is then installed in the heat chamber at 140°C for 30 min After the heat of the casting form is then removed from the heating Cabinet and plates ohlord the Ute to the ambient temperature (25°C).

6. Example 2 according to the invention

(85% Amosil®520 + 15% Tremin®283-600 EST)

In a heated steel vessel 100 g XB 5992®mixed with 90 g XB 5993®and the mixture is heated under weak stirring propeller stirrer at 60°C for about 5 minutes Then the stirrer is stopped, add 2 g of Bayferrox®225 and again let the mixer for about 1 min. Then under stirring portions add to 51.3 g Tremin 283-600 EST and 290,7 g Amosil®520 and the mixture is heated at 60°C under stirring for about 10 minutes Then the stirrer is stopped and the vessel carefully Tegaserod tabulation of vacuum for about 1 minutes

A small portion of the mixture is used to measure the viscosity at 60°C on a Rheomat equipment (type 115, MS DIN 125 D=11). The main part of the mixture is poured into heated to 140°C steel form with receiving plates to determine the characteristics (thickness 4 mm). The form is then installed in the heat chamber at 140°C for 30 min After the heat of the casting form is then removed from the heating Cabinet and the plate is cooled to ambient temperature (25°C).

The number listed in the subsequent table are in parts by weight of

All connections involved in the experiment condition for 48 h at 23°C and 50%relative humidity.

Table 2
ComponentsComparative example C1Comparative example C2Example 1 (according to the image-acquisition)Average (C1; C2)Effect outside the middle
XB 5992®100100100
XB 5993®909090
Bayferrox®225222
Fused silica (Tecosil®44i)342-171
The wollastonite Tremin®283-100 EST-342171
The viscosity at 60°C1)Pa.s29,028,520,028,830%
The ultimate tensile strength2)MPa838490to 83.58%
Elongation at break3)%1,00,91,11,016%
Bending strength4)MPa114120135117,015%
The voltage of fiber5)%1,11,21,21,24%
The viscosity at the destruction To1Cis the 6)MPa/m22,02,72,72,415%
The viscosity at the destruction of G1C7)J/m2298565475431,510%
KTR (below TC)8)hours/million/K29,931,728,630,8
TC (Tg) (1st run)°C10410098102,0
IR=f(TA,KTR,G1Cextension)10)°C-50-65-97-6062%

Table 3
Comp the components Comparative example C3Comparative example C4Example 2 (according to the image-acquisition)The expectations radiated 3-4Effect outside the expected
XB 5992®100100100
XB 5993®909090
Bayferrox®225222
Amosir®520342-290,7
The wollastonite Tremin®283-600 EST-34251,3
The viscosity at 60°C1)Pa.s7,6too high8,610,014%
The ultimate tensile strength2)MPa80the concentration is8680,08%
Elongation at break3)%0,9the concentration is1,10,922%
Bending strength4)MPa108the concentration is128108,019%
The voltage of fiber5)%1,0the concentration is1,11,010%
The viscosity at the destruction To1C6)MPa/m2 2,1the concentration is2,42,29%
The viscosity at the destruction of G1C7)J/m2335the concentration is441335,032%
KTR (below TC)8)hours/million/K27,5the concentration is25,727,5
TC (Tg) (1st run)°C102the concentration is105102,0
IR=f(TA,KTR,G1Cextension)10)°C-76-131-7671%
concentration (not defined)
1)Determined at 60°C on a Rheomat equipment (type 115, MS DIN 125 D=11/C).
2)Determined according to ISO 527-1 (1993), a model for type tests In (190×20,5×4 mm); the velocity of the test: 1.00 mm/min
3)Determined according to ISO 527-1 (1993), a model for type tests In (190×20,5×4 mm); test speed: 1.00 mm/min
4)Determined according to ISO 178, the sample size for tests of 80×10×4 mm; test speed: 2.00 mm/min
5)Determined according to ISO 178, the sample size for tests of 80×10×4 mm; test speed: 2.00 mm/min
6),7)The viscosity at the destruction of the expressed values of K1Cand G1Cdefined according to the RM 216, the size of test specimens 80×34×4 mm; test speed: 0.50 mm/min
8)CTE (CTE - Coefficient of thermal expansion, specified according to ISO 11359-2:1999, interval: 20-60°C.
9)Determined according to ISO 11359-2:1999, 10-20 mg; temperature change: 10,0 K/min, sample size: 50×4×4 mm; temperature change: 2 K/min
10)IL (RI) - index of cracking

The cracking index, are shown in tables 2 and 3, is a function of various mechanical parameters, each of which can influence the characteristic cracking in the case of voltage caused by temperature changes, combined with the formation of a single parameter, the so-called index of cracking. The cracking index allows to make easier the comparison of the mechanical properties of various systems.

The following qualitative state regarding the effects of individual changes the parameters on the behavior of the temperature change can be obtained empirically:

1. The higher the value TC (Tg), the worse the behavior when the temperature changes.

2. The lower the value of G1Cthe worse behavior when the temperature changes.

3. The lower the elongation, the worse the behavior when the temperature changes.

4. The higher the coefficient of thermal expansion (CTE) (CTE), the worse the behavior when the temperature changes.

However, when multiple parameters are changed simultaneously, it is no longer possible to obtain high-quality state with respect to the resulting behavior when the temperature changes. When, for example, as the value of TC and the value of G1Cincrease, but the value of CTE is reduced, it is no longer possible to make predictions about the expected behavior when the temperature changes.

When Ciba Spezialitattenchemie statistical evaluation of measurement values using a large number of extremely changeable systems gave a formula to calculate a new parameter, the so-called index of cracking, which is extremely useful from the point of view of application technology. This option is now possible even in the case of multiple changes with the receiving state regarding get the expected behavior when the temperature changes.

The formula is as follows:

IL=-498,08 Z0,18480890G0,194114801(A-18)-0,391334273T-0,18387791 +224,25,

where IL is the index of cracking; Z represents an elongation at break in %; G=G1Cin j/m2;

Rather it represents a coefficient of thermal expansion in h/m/K, and T=TC in °C.

When using this formula, the lower values of the index cracking indicates the expected improvement of the resistance to temperature change. The cracking index correlates very well with the average temperature cracking in °C, which can be defined in practical test cracking. The specified temperature cracking and, thus, also the cracking index provide an indication of temperature, beyond which, probably, cracks (caused by tension in the case of temperature fluctuations and the difference between the coefficients of thermal expansion of the molding compound and the metal insert).

Discussion of results

Table 2. Comparison of comparative examples C1 and C2 from example 1 according to the present invention

a) Aspects viscosity

Composition or with a filler Tecosil®44i (in order to get a low CTE), or only with wollastonite Tremin®283-100 EST (in order to obtain good toughness - high To1Cand G1C) are not the appropriate solution to solve issues on which they both systems (comparative examples 1C and 2C) show the viscosity, which are too high. From 1:1-mixture of C1 and C2 could in principle be expected that the obtained values are shown in column average (C1, C2)". It is also clear that the expected viscosity of the mixture will be too high for the purpose of the invention (providing and casting system for direct casting of vacuum switching devices). It was therefore unexpected to find that the viscosity of example 1 (which represents in principle a mixture of 1:1 C1 and C2) is much lower and therefore is applicable for the desired application.

b) Mechanical aspects

The ultimate tensile strength for C1 and C2 is approximately the same as expected for the mixture. However, example 1 even gives the ultimate tensile strength is 8% higher than expected when calculating the average.

The characteristic bending strength is consistent with this observation and is 15% higher than expected.

Comparative example 2, the system with wollastonite

The needle shape of the filler expected high values of K1Cand G1C. However, the observed high impact strength is still insufficient to obtain a very low overall index cracking "IR". Comparative example C2 gives only the index cracking "IL" -65°C. experience has shown that a value of about -100°C is usually necessary to withstand on the order, which are bathed in direct pouring of vacuum switching devices. Thus, C2 is not suitable for direct casting of vacuum switching devices.

Comparative example C1 is a system that contains only fused quartz.

The value of CTE is lower than in C2, but the values of K1Cand G1Care lower than for the composition according to comparative example 2 containing wollastonite. Taking into account all the factors C1 gives only the temperature of the cracking -50°C, which is too high for direct casting of vacuum switching devices.

It was unexpectedly found that a mixture of 1:1 C1 and C2 does not give the expected medium-To1Cbut much higher values. It was unexpectedly found that the cured composition as defined in example 1 gives the temperature of the cracking -97°C, which is sufficient for direct casting of vacuum switching devices. This low temperature cracking is 62% better (lower)than the temperature calculated based on the average mechanical values for a mixture of both formulations.

Table 2. Comparison of comparative examples C3 and C4 with example 2 according to the present invention

a) Aspects viscosity

The composition according to comparative example C3 contains ka is este filler only natural amorphous silica. The measured viscosity is low enough for direct pouring of the switching devices.

The composition according to comparative example C4 contains as filler only wollastonite. The specified viscosity of the composition is too high, and, as a consequence, it was impossible to measure the viscosity. High viscosity makes the composition according to comparative example C4 is not suitable for direct fill.

While specified type of wollastonite dramatically increases the viscosity, it was unexpectedly found that the replacement of 15% wt. silicon dioxide wollastonite has only a weak impact on the viscosity.

b) Mechanical aspects

The composition of comparative example C3 gives the same mechanical properties as the composition of comparative example C1. Temperature cracking IL defined for utverzhdenii composition according to comparative example C3 is -76°C, which is too high for the desired application.

The composition of comparative example C4 has a viscosity that is too high to get plates for testing and to determine mechanical properties.

The composition of example 2 contains only a small portion of wollastonite compared to silicon dioxide (15:85) in order to experience more extreme conditions.

There is no data for the ecapture, containing only the wollastonite type Tremin®283-600 EST, as it was impossible to mold the samples for testing due to high viscosity. Therefore, can be made only rough estimates of the expected improvements when combining both fillers shown in table 3. It was expected that a small introduction only 15% of wollastonite should not have a dramatic impact. However, it turns out that the mechanical properties increase significantly. Indeed, all properties are much better than the properties of the composition containing only filler Amosil 520 (C3). Temperature cracking is reduced to -131°C, which is 71% higher than the temperature of cracking obtained only with filler Amosil 520. Due to the low viscosity of the formulation according to example 2 is suitable for direct casting of vacuum switching devices.

1. Curing the composition to obtain electrical equipment containing
(a) epoxy resin and
b) a filler composition that contains
i) wollastonite and
ii) amorphous silicon dioxide,
c) a hardener,
where the surface of at least one of the fillers of the composition of the filler is treated with the silane and the mass ratio (amorphous silicon dioxide):wollastonite is from 70:30 to 30:70.

2. Cured composition is I according to claim 1, in which the wollastonite and/or amorphous silicon dioxide has an average particle size (d50in the interval from 2 to 50 microns.

3. Cured composition according to claim 1, in which the surface of the wollastonite and/or amorphous silicon dioxide is treated with silane selected from the group consisting of aminosilane, epoxysilane, (meth)acrylicana, methylsilane and vinylsilane.

4. Cured composition according to claim 1 or 2, in which the amorphous silicon dioxide is a natural amorphous silica or fused quartz.

5. Cured composition according to claim 1 or 2, in which the mass ratio (amorphous silicon dioxide):wollastonite is from 60:40 to 40:60.

6. Cured composition according to claim 1 or 2, containing as a hardener anhydride polybasic carboxylic acid.

7. The method of obtaining electrical equipment, comprising the following stages:
a) injection of curing of the composition in a pre-heated form, having a temperature in the range from 130 to 160°C, where this form contains a ceramic housing of the switching device,
b) at least partially curing curing of the composition,
c) removal of forms and
d) an optional curing curing of the composition.

8. The method according to claim 7, in which the cured composition is in the bar is dstvennogo contact with the surface of the ceramic housing of the switching device.

9. The cured product obtained by curing curing composition according to claims 1-6.



 

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2 tbl, 7 ex

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2 tbl

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2 tbl

FIELD: chemistry.

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15 cl, 3 tbl, 27 ex

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16 cl, 2 tbl, 8 ex

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32 cl, 1 tbl, 2 ex

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8 cl, 3 dwg, 2 tbl, 9 ex

Polymer composition // 2528681

FIELD: chemistry.

SUBSTANCE: invention relates to production of high-strength polymer compositions using cycloaliphatic dioxides and can be used to produce binder for composite materials, coatings, adhesives and for other purposes. A polymer composition for producing binder and coatings based on epoxy resins and a nitrogen-containing curing agent, which is a product of reacting an amine with cycloaliphatic or cycloaliphatic-aliphatic dioxides obtained by direct epoxidation of unsaturated compounds, wherein during the reaction, a liquid or molten aliphatic, aromatic, cycloaliphatic or alkylene aromatic amine is fed into the reactor at the beginning, followed by a dioxide with respect to 3-20 times the molar excess of amine, followed by an acrylate and amino alcohol; the reaction mixture is stirred for 20-180 minutes at temperature of 30-180°C and then added to a mixture of epoxy resin with an active or passive diluent and a low-molecular aliphatic or aromatic hydroxyl-containing compound is added and stirred at T=15-95°C for 20-120 minutes.

EFFECT: invention improves processing properties of the polymer composition and raises the heat distortion temperature while simultaneously improving dielectric properties at temperature of 150-200°C and after exposure to hot and superheated water.

2 tbl, 1 ex

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