CN102863936A - Heating solidification type dual-component epoxy pouring sealant and preparation method thereof - Google Patents
Heating solidification type dual-component epoxy pouring sealant and preparation method thereof Download PDFInfo
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Abstract
The invention provides a heating solidification type dual-component epoxy pouring sealant which comprises an A component and a B component. The A component comprises the following ingredients of, by weight, 70-130 parts of an epoxy resin, 150-280 parts of a first inorganic filler, 0-25 parts of a dilution agent, 0-15 parts of a toughening agent, 0-3 parts of an organosilicon antifoaming agent and 0-3 parts of pigment; and the B component comprises the following ingredients of, by weight, 70-150 parts of acid anhydride, 150-280 parts of a second inorganic filler and 0-15 parts of a wetting dispersing agent. The preparation method of the sealant includes respectively preparing the A component and the B component, then, respectively heating the A component and the B component, and evenly mixing the A component and the B component to obtain the heating solidification type dual-component epoxy pouring sealant. The heating solidification type dual-component epoxy pouring sealant is good in comprehensive performance and fluidity and long in storage period.
Description
Technical field
The present invention relates to the joint sealant field, particularly heat-curing type bi-component epoxy joint sealant and preparation method thereof.
Background technology
Resins, epoxy is to the organic high molecular compound that refers to contain in the molecule two or more epoxide groups.The dielectric properties of Resins, epoxy, mechanical property, adhesiveproperties and excellent anti-corrosion performance, cure shrinkage and linear expansivity are little, the cured article dimensional stabilizing, good manufacturability has splendid over-all properties.Because formulating of recipe handiness and the diversity of epoxide resin material make it be used widely in field of electronic devices.
The epoxy pouring sealant for preparing take Resins, epoxy as main component is the globality of strengthening electronic device effectively, improve electron device to the resistibility of external shock, vibrations, the insulation that keeps electron device, be conducive to miniaturization, the lightweight of electron device, avoid the direct exposure of electronic component and circuit, can greatly improve waterproof and the moistureproof ability of electron device, greatly prolong the work-ing life of electron device and reduce use cost.
The epoxy encapsulating divides from the curing process condition, can be divided into normal temperature cured type and heat-curing type two classes; Divide from formulation, can be divided into two-component-type and one-pack type two classes.The normal temperature cured type epoxy pouring sealant is generally two-pack, and need not to heat room temperature after the embedding can solidify.Although the normal temperature cured type epoxy pouring sealant is not high to equipment requirements; use also more convenient; but mixture operation viscosity is large; infiltration property is poor; working life is short; be difficult to be applied in the automatic production, and cured article thermotolerance and electrical property are often not ideal enough, use than the occasion that the seal protection that is more suitable for small power Low-voltage Electronic device maybe should not be heating and curing.Heat-curing type bi-component epoxy joint sealant; it is the most widely joint sealant kind of present consumption maximum, purposes; have advantages of many; such as stably stored cycle length, permeate well, the cured article dimensional stability is high, heat-drawn wire is higher and electric insulating quality is splendid etc.; be very suitable for encapsulation and the seal protection of powerful electron device, can satisfy the service requirements that automatic production line is produced.
Heat-curing type bi-component epoxy joint sealant is comprised of Resins, epoxy and other substance.Because pure epoxy resin has very high crosslinking structure, thus have that matter is crisp, the shortcoming such as fatiguability and heat dispersion thereof are poor.The researchist is general through Resins, epoxy and various substance being adjusted and being optimized, and to improve the epoxy pouring sealant over-all properties, as improving flame retardant properties and heat conductivility, reduces internal stress and linear expansivity.Described substance mainly comprises mineral filler, but inorganic filler content is too much, and the viscosity increase of epoxy pouring sealant is larger, thereby affects its flowability and perviousness; The epoxy pouring sealant memory cycle shortens in addition, causes filler to sink in a large number, increases to use operation.Inorganic filler content is few, and the epoxy pouring sealant over-all properties is poor.
Summary of the invention
The technical problem that the present invention solves is to provide a kind of heat-curing type bi-component epoxy joint sealant, and inorganic filler content is high, good combination property.
The invention provides a kind of heat-curing type bi-component epoxy joint sealant, comprise A component and B component,
Described A component comprises the composition of following weight part:
Resins, epoxy 70 ~ 130;
The first mineral filler 150 ~ 280;
Thinner 0 ~ 25;
Toughner 0 ~ 15;
Silicone antifoam agent 0 ~ 3;
Pigment 0 ~ 3;
Described B component comprises the composition of following weight part:
Acid anhydrides 70 ~ 150;
The second mineral filler 150 ~ 280;
Wetting dispersing agent 0 ~ 15.
Preferably, the mass ratio of described A component and B component is (1:100)～(100:1).
Preferably, described the first filler and the second filler independently are selected from one or more in crystalline silicon powder, activated Calcium carbonate and the active aluminium hydroxide, and described the first filler and the second filler median size are 1～100 μ m.
Preferably, be in bisphenol A type epoxy resin, bisphenol f type epoxy resin, novolac epoxy, glycidyl amine type epoxy resin and the aliphatic epoxy resin one or more.
Preferably, described thinner is one or more in n-butyl glycidyl ether, glycidyl allyl ether, benzyl glycidyl ether and the BDDE.
Preferably, it is characterized in that, described acid anhydrides is one or more in methylhexahydrophthalic anhydride, methyl tetrahydrophthalic anhydride, isomerized methyltetrahydro phthalate anhydride, MNA, methyl carbic anhydride and the carbic anhydride.
Preferably, described wetting dispersing agent is stearate.
Preferably, described toughner is one or more in carboxyl end of the liquid acrylonitrile-butadiene rubber, polyurethane toughened dose, hydroxyl terminated butyl nitrile (HTBN) rubber and the Qi Shi toughner.
The invention discloses a kind of preparation method of heat-curing type bi-component epoxy joint sealant, may further comprise the steps:
The Resins, epoxy of 70 ~ 130 weight parts, the thinner of 0 ~ 25 weight part, the toughner of 0 ~ 15 weight part, the silicone antifoam agent of 0 ~ 3 weight part, the pigment of 0 ~ 3 weight part are mixed with the first mineral filler of 150 ~ 280 weight parts, obtain the A component;
The acid anhydrides of 70 ~ 150 weight parts, the wetting dispersing agent of 1 ~ 15 weight part are mixed with the second mineral filler of 150 ~ 280 weight parts, obtain the B component;
A component and B component are heated respectively, after mixing, obtain heat-curing type bi-component epoxy joint sealant.
Preferably, the mass ratio of described A component and B component is (1:100)～(100:1).
Compared with prior art, heat-curing type bi-component epoxy joint sealant of the present invention comprises A component and B component.All contain mineral filler in described two components, improved the content of mineral filler in epoxy pouring sealant, thereby the over-all propertieies such as thermal conductivity, insulating property, physical strength of epoxy pouring sealant have been improved, to work-ing life of improving high-power electronic component with reduce maintenance cost great effect is arranged.Secondly, heat-curing type bi-component epoxy joint sealant viscosity of the present invention is low, good fluidity.Again, two components that all contain mineral filler can separately be preserved, and mix in use again, and the mineral filler in two components all is difficult for deposition, thereby has prolonged the memory cycle.Experimental result shows, the heat-curing type bi-component epoxy joint sealant mixing initial viscosity of the present invention's preparation is less than 15Pa.s, and Shao Shi D hardness is greater than 85, and thermal conductivity is greater than 0.8, and volume specific resistance is greater than 2.6 * 10
16Ω m, disruptive strength is greater than 25KV/mm.
Embodiment
In order further to understand the present invention, below in conjunction with embodiment the preferred embodiment of the invention is described, but should be appreciated that these describe just as further specifying the features and advantages of the present invention, rather than to the restriction of claim of the present invention.
The embodiment of the invention discloses a kind of heat-curing type bi-component epoxy joint sealant, comprise A component and B component,
Described A component comprises the composition of following weight part:
Resins, epoxy 70 ~ 130;
The first mineral filler 150 ~ 280;
Thinner 0 ~ 25;
Toughner 0 ~ 15;
Silicone antifoam agent 0 ~ 3;
Pigment 0 ~ 3;
Described B component comprises the composition of following weight part;
Acid anhydrides 70 ~ 150;
The second mineral filler 150 ~ 280;
Wetting dispersing agent 0 ~ 15.
According to the present invention, in the A component, described Resins, epoxy is preferably one or more in bisphenol A type epoxy resin, bisphenol f type epoxy resin, novolac epoxy, glycidyl amine type epoxy resin and the aliphatic epoxy resin.The present invention does not have particular restriction to the source of described Resins, epoxy, is bought by market to get final product.The content of described Resins, epoxy is 70 ~ 130 weight parts, is preferably 80 ~ 120 weight parts.
According to the present invention, in the A component, described the first mineral filler is preferably one or more in crystalline silicon powder, activated Calcium carbonate and the active aluminium hydroxide, and the median size of described the first mineral filler is preferably 1～100 μ m, more preferably 30～70 μ m.The adding of mineral filler can improve the over-all properties of epoxy pouring sealant, plays the effect of heat-resisting, fire-retardant, low-expansion coefficient, heat radiation.The present invention does not have particular restriction to the source of described the first mineral filler, is bought by market to obtain to get final product.The content of described the first mineral filler is 150 ~ 280 weight parts, is preferably 170 ~ 250 weight parts.
According to the present invention, in the A component, the viscosity that act as the reduction epoxy pouring sealant of described thinner is so that further processing, described thinner is preferably one or more in n-butyl glycidyl ether, glycidyl allyl ether, benzyl glycidyl ether and the BDDE.The present invention does not have particular restriction to the source of described thinner, is bought by market to obtain to get final product.The content of described thinner is 0 ~ 25 weight part, is preferably 8 ~ 20 weight parts.
According to the present invention, in the A component, described toughner is preferably one or more in carboxyl end of the liquid acrylonitrile-butadiene rubber, polyurethane toughened dose, hydroxyl terminated butyl nitrile (HTBN) rubber and the Qi Shi toughner.The present invention does not have particular restriction to the source of described toughner, is bought by market to get final product.The content of described toughner is 0 ~ 15 weight part, is preferably 5 ~ 12 weight parts.
According to the present invention, in the A component, the kind of described silicone antifoam agent there is not particular restriction, select get final product according to kind well known to those skilled in the art, the source of described silicone antifoam agent there is not particular restriction yet, the market purchase gets final product.The content of described silicone antifoam agent is 0 ~ 3 weight part, is preferably 1 ~ 2 weight part.
According to the present invention, in the A component, flaw is covered in acting as of described pigment, and what be conducive to is attractive in appearance.Described pigment optimization is carbon black or nigrosine.The present invention does not have particular restriction to the source of pigment, and market is bought and got final product.The content of described pigment is 0 ~ 3 weight part, is preferably 1 ~ 2 weight part.
According to the present invention, described B component is solidifying agent.In the B component, described acid anhydrides is preferably one or more in methylhexahydrophthalic anhydride, methyl tetrahydrophthalic anhydride, isomerized methyltetrahydro phthalate anhydride, MNA, methyl carbic anhydride and the carbic anhydride.The present invention does not have particular restriction to the source of described acid anhydrides, is bought by market to get final product.The content of described acid anhydrides is 70 ~ 150 weight parts, is preferably 80 ~ 120 weight parts.
According to the present invention, in described B component, described the second mineral filler is preferably one or more in crystalline silicon powder, activated Calcium carbonate and the active aluminium hydroxide, and the median size of described the second mineral filler is preferably 1～100 μ m, more preferably 30～70 μ m.The adding of mineral filler can improve the over-all properties of epoxy pouring sealant, plays the effect of heat-resisting, fire-retardant, low-expansion coefficient, heat radiation.The second mineral filler can be identical with the first mineral filler, also can be not identical.The present invention does not have particular restriction to the source of described the second mineral filler, is bought by market to get final product.The content of described the second mineral filler is 150 ~ 280 weight parts, is preferably 180 ~ 260 parts.
According to the present invention, in described B component, acting as of described wetting dispersing agent improves dispersiveness and the wetting property of mineral filler in epoxy pouring sealant, is conducive to prevent that mineral filler from sinking and the flowability of raising epoxy pouring sealant.Described wetting dispersing agent is preferably stearate.The present invention does not have particular restriction to the source of described wetting dispersing agent, is bought by market to get final product.The content of described wetting dispersing agent is 0 ~ 15 weight part, is preferably 6 ~ 12 weight parts.
According to the present invention, the mass ratio of described A component and B component is preferably (1:100)～(100:1), more preferably (1:50): (50 ~ 1) most preferably are 1:1.
The invention provides a kind of preparation method of heat-curing type bi-component epoxy joint sealant, may further comprise the steps:
The Resins, epoxy of 70 ~ 130 weight parts, the thinner of 0 ~ 25 weight part, the toughner of 0 ~ 15 weight part, the silicone antifoam agent of 0 ~ 3 weight part, the pigment of 0 ~ 3 weight part are mixed with the first mineral filler of 150 ~ 280 weight parts, obtain the A component;
The acid anhydrides of 70 ~ 150 weight parts, the wetting dispersing agent of 1 ~ 15 weight part are mixed with the second mineral filler of 150 ~ 280 weight parts, obtain the B component;
A component and B component are heated respectively, after mixing, obtain heat-curing type bi-component epoxy joint sealant.
According to the present invention, at first prepare the A component take Resins, epoxy, the first mineral filler, thinner, toughner, silicone antifoam agent and pigment as raw material.
According to the present invention, in the A component, described Resins, epoxy is preferably one or more in bisphenol A type epoxy resin, bisphenol f type epoxy resin, novolac epoxy, glycidyl amine type epoxy resin and the aliphatic epoxy resin.The present invention does not have particular restriction to the source of described Resins, epoxy, is bought by market to get final product.The content of described Resins, epoxy is 70 ~ 130 weight parts, is preferably 80 ~ 120 weight parts.
According to the present invention, in the A component, described the first mineral filler is preferably one or more in crystalline silicon powder, activated Calcium carbonate and the active aluminium hydroxide, and the median size of described the first mineral filler is preferably 1～100 μ m, more preferably 30～70 μ m.The adding of mineral filler can improve the over-all properties of epoxy pouring sealant, plays the effect of heat-resisting, fire-retardant, low-expansion coefficient, heat radiation.The present invention does not have particular restriction to the source of described the first mineral filler, is bought by market to obtain to get final product.The content of described the first mineral filler is 150 ~ 280 weight parts, is preferably 170 ~ 250 weight parts.
According to the present invention, in the A component, the viscosity that act as the reduction epoxy pouring sealant of described thinner is so that further processing, described thinner is preferably one or more in n-butyl glycidyl ether, glycidyl allyl ether, benzyl glycidyl ether and the BDDE.The present invention does not have particular restriction to the source of described thinner, is bought by market to obtain to get final product.The content of described thinner is 0 ~ 25 weight part, is preferably 8 ~ 20 weight parts.
According to the present invention, in the A component, described toughner is preferably one or more in carboxyl end of the liquid acrylonitrile-butadiene rubber, polyurethane toughened dose, hydroxyl terminated butyl nitrile (HTBN) rubber and the Qi Shi toughner.The present invention does not have particular restriction to the source of described toughner, is bought by market to get final product.The content of described toughner is 0 ~ 15 weight part, is preferably 5 ~ 12 weight parts.
According to the present invention, in the A component, the kind of described silicone antifoam agent there is not particular restriction, select get final product according to kind well known to those skilled in the art, the source of described silicone antifoam agent there is not particular restriction yet, the market purchase gets final product.The content of described silicone antifoam agent is 0 ~ 3 weight part, is preferably 1 ~ 2 weight part.
According to the present invention, in the A component, flaw is covered in acting as of described pigment, and what be conducive to is attractive in appearance.Described pigment optimization is carbon black or nigrosine.The present invention does not have particular restriction to the source of pigment, and market is bought and got final product.The content of described pigment is 0 ~ 3 weight part, is preferably 1 ~ 2 weight part.
In preparation A component process, Resins, epoxy, thinner, toughner, silicone antifoam agent, pigment are mixed with the first mineral filler, preferably can obtain the A component through vacuum defoamation.In order to mix, add again pigment and the first mineral filler after preferably Resins, epoxy, thinner, toughner and silicone antifoam agent being mixed.In the described mixing process, preferably stir, stirring velocity is preferably 1800 ~ 2500rmp, and churning time is preferably 20 ~ 40 minutes
According to the present invention, the B component prepares take acid anhydrides, wetting dispersing agent and the second mineral filler as raw material.
In the B component, described acid anhydrides is preferably one or more in methylhexahydrophthalic anhydride, methyl tetrahydrophthalic anhydride, isomerized methyltetrahydro phthalate anhydride, MNA, methyl carbic anhydride and the carbic anhydride.The present invention does not have particular restriction to the source of described acid anhydrides, is bought by market to get final product.The content of described acid anhydrides is 70 ~ 150 weight parts, is preferably 80 ~ 120 weight parts.
According to the present invention, in described B component, described the second mineral filler is preferably one or more in crystalline silicon powder, activated Calcium carbonate and the active aluminium hydroxide, and the median size of described the second mineral filler is preferably 1～100 μ m, more preferably 30～70 μ m.The adding of mineral filler can improve the over-all properties of epoxy pouring sealant, plays the effect of heat-resisting, fire-retardant, low-expansion coefficient, heat radiation.The second mineral filler can be identical with the first mineral filler, also can be not identical.The present invention does not have particular restriction to the source of described the second mineral filler, is bought by market to get final product.The content of described the second mineral filler is 150 ~ 280 weight parts, is preferably 180 ~ 260 parts.
According to the present invention, in described B component, acting as of described wetting dispersing agent improves dispersiveness and the wetting property of mineral filler in epoxy pouring sealant, is conducive to prevent that mineral filler from sinking and the flowability of raising epoxy pouring sealant.Described wetting dispersing agent is preferably stearate.The present invention does not have particular restriction to the source of described wetting dispersing agent, is bought by market to get final product.The content of described wetting dispersing agent is 0 ~ 15 weight part, is preferably 6 ~ 12 weight parts.
In the process of preparation B component, acid anhydrides, wetting dispersing agent and the second mineral filler are mixed, preferably pass through vacuum defoamation after, can obtain the B component.In order to mix, after preferably acid anhydrides and wetting dispersing agent being mixed, to add again the second mineral filler and mix.In the described mixing process, preferably stir, stirring velocity is preferably 1200 ~ 1800rmp, and churning time is preferably 20 ~ 40 minutes.
The A component for preparing and B component separately store, and preferably airtight, dry, temperature is lower than in 25 ℃ the environment and stores.
According to the present invention, obtain A component and B component after, A component and B component are heated respectively, after mixing, can obtain heat-curing type bi-component epoxy joint sealant.The mass ratio of described A component and B component is preferably (1:100)～(100:1), more preferably (1:50): (50 ~ 1) most preferably are 1:1.The temperature of described heating is preferably 50 ~ 80 ℃, more preferably 55 ~ 75 ℃.The heat-curing type bi-component epoxy joint sealant that obtains can carry out embedding.
The heat-curing type bi-component epoxy joint sealant of the present invention's preparation is applicable to the embedding of high-power electronic device, is preferably high-power thyristor (SCR), power transistor (GTR), power field effect pipe (PMOSFET), high-power bipolar power transistor (IGBT), high-power metallic-zone of oxidation-semi-conductor-field-effect transistor(FET) (MOSFET), high-power integrated gate commutated thyristor (IGCT), SPM (IPM), state induction transistor (SIT) are carried out embedding.
The epoxy pouring sealant that obtains is carried out performance test, and the result shows, its initial viscosity＜15Pa.s, Shao Shi D hardness＞85, thermal conductivity＞0.8, volume specific resistance＞2.6 * 10
16Ω m, disruptive strength＞25KV/mm.
In order further to understand the present invention, below in conjunction with embodiment heat-curing type bi-component epoxy joint sealant provided by the invention is described, protection scope of the present invention is not limited by the following examples.
In following examples, bisphenol A type epoxy resin E-51 is that the model that the Ba Ling petrochemical iy produced is produced is the bisphenol A type epoxy resin of E-51; Bisphenol F epoxy resin Epikate-235 is that the model that DOW Chemical is produced is the bisphenol F epoxy resin of Epikate-235; The DER-736 aliphatic epoxy resin is that the model that DOW Chemical is produced is the aliphatic epoxy resin of DER-736; Bisphenol A type epoxy resin E-44 is that the model that the Ba Ling petrochemical iy produced is produced is the bisphenol A type epoxy resin of E-44; The F-44 novolac epoxy is that the model that Hunan Jia Shengde material Science and Technology Ltd. produces is the novolac epoxy of F-44; The machine silicon defoaming agent is that the model of Bi Ke chemical production is the silicone antifoam agent of BYK-A530; Polyurethane toughened dose is the toughner that Yantai ten thousand China produce; Wetting dispersing agent is that the model of Bi Ke chemical production is the wetting dispersing agent of BKY-163; Active micro silicon powder is 400 active micro silicon powders that the East Sea, Lianyun Harbour gold rose silicon powder factory produces; Active aluminium hydroxide is the aluminium hydroxide that the Jinan rising sun in morning chemical industry company limited produces.
Embodiment 1
With 120 gram bisphenol A type epoxy resin E-51,15 gram BDDEs, polyurethane toughened dose of 8 grams and 1.5 gram silicone antifoam agents mix and are stirred to evenly, and the stirrer rotating speed is 2000rpm, and churning time is 30 minutes.Then add while stirring 2.5 gram carbon blacks and 190 gram active micro silicon powders, continue to stir 30 minutes, after mixing, vacuum defoamation obtains the A component.The A component is placed on airtight, dry, temperature is lower than in 25 ℃ the environment and stores.
With 97 gram methyl hexahydrophthalic anhydrides and 15 gram wetting dispersing agent mix and blends, stirring velocity is 1500rpm, and churning time is 15 minutes, is stirred to mix.Then add while stirring 200 gram active micro silicon powders, continue to stir 30 minutes, after mixing, vacuum defoamation obtains the B component.The B component is placed on airtight, dry, temperature is lower than in 25 ℃ the environment and stores.
Get 100 gram A components and 100 gram B components respectively 60 ℃ of lower heating, strongly stir and make muddy and mix, after the vacuum defoamation, obtain 200 gram heat-curing type bi-component epoxy joint sealants, can carry out embedding.
Performance to the epoxy pouring sealant that obtains is tested, and the result is referring to table 1.
Embodiment 2
With 50 gram bisphenol A type epoxy resin E-51,70 gram bisphenol F epoxy resin Epikate-235,15 grams 1, the 4-butanediol diglycidyl ether, polyurethane toughened dose of 18 grams and 1.5 gram silicone antifoam agents mix and are stirred to evenly, and the stirrer rotating speed is 2000rpm, and churning time is 30 minutes.Then add while stirring 2 gram carbon blacks, 65 gram active micro silicon powders, 50 gram calcium carbonate and 60 gram active aluminium hydroxides continue to stir 30 minutes, and after mixing, vacuum defoamation obtains the A component.The A component is placed on airtight, dry, temperature is lower than in 25 ℃ the environment and stores.
With 98 gram methyl tetrahydro phthalic anhydrides and 15 gram wetting dispersing agent mix and blends, stirring velocity is 1500rpm, and churning time is 15 minutes, is stirred to mix.Then add while stirring 100 gram active micro silicon powders and 100 gram calcium carbonate, continue to stir 30 minutes, after mixing, vacuum defoamation obtains the B component.The A component is placed on airtight, dry, temperature is lower than in 25 ℃ the environment and stores.
Get 100 gram A components and 100 gram B components respectively 60 ℃ of lower heating, strongly stir and make muddy and mix, after the vacuum defoamation, obtain 200 gram heat-curing type bi-component epoxy joint sealants, can carry out embedding.
Performance to the epoxy pouring sealant that obtains is tested, and the result is referring to table 1.
Embodiment 3
With 60 gram bisphenol A type epoxy resin E-44,40 gram bisphenol F epoxy resin Epikate-235,20 gram F-44 novolac epoxys, 14 gram n-butyl glycidyl ethers, polyurethane toughened dose of 10 grams and 1.5 gram silicone antifoam agents mix and are stirred to evenly, the stirrer rotating speed is 2000rpm, and churning time is 30 minutes.Then add while stirring 2 gram carbon blacks, 100 gram active micro silicon powders, 85 gram active aluminium hydroxides continue to stir 30 minutes, and after mixing, vacuum defoamation obtains the A component.The A component is placed on airtight, dry, temperature is lower than in 25 ℃ the environment and stores.
With 60 gram methyl tetrahydro phthalic anhydrides, 40 gram methyl Na Dike acid anhydrides and 15 gram wetting dispersing agent mix and blends, stirring velocity is 1500rpm, churning time is 15 minutes, is stirred to mix.Then add while stirring 100 gram active micro silicon powders and 100 gram activated aluminas, continue to stir 30 minutes, after mixing, vacuum defoamation obtains the B component.The A component is placed on airtight, dry, temperature is lower than in 25 ℃ the environment and stores.
Get 100 gram A components and 100 gram B components respectively 60 ℃ of lower heating, strongly stir and make muddy and mix, after the vacuum defoamation, obtain 200 gram heat-curing type bi-component epoxy joint sealants, can carry out embedding.
Performance to the epoxy pouring sealant that obtains is tested, and the result is referring to table 1.
Embodiment 4
With 60 gram bisphenol A type epoxy resin E-51,40 gram bisphenol F epoxy resin Epikate-235,20 gram DER-736 aliphatic epoxy resins, 15 gram benzyl glycidyl ethers, polyurethane toughened dose of 10 grams and 1.5 gram silicone antifoam agents mix and are stirred to evenly, the stirrer rotating speed is 2000rpm, and churning time is 30 minutes.Then add while stirring 2 gram carbon blacks, 90 gram active micro silicon powders and 90 gram active aluminium hydroxides continue to stir 30 minutes, and after mixing, vacuum defoamation obtains the A component.The A component is placed on airtight, dry, temperature is lower than in 25 ℃ the environment and stores.
With 60 gram methyl tetrahydro phthalic anhydrides, 40 gram methyl Na Dike acid anhydrides and 10 gram wetting dispersing agent mix and blends, stirring velocity is 1500rpm, churning time is 15 minutes, is stirred to mix.Then add while stirring 200 gram activated aluminas, continue to stir 30 minutes, after mixing, vacuum defoamation obtains the B component.The A component is placed on airtight, dry, temperature is lower than in 25 ℃ the environment and stores.
Get 100 gram A components and 100 gram B components respectively 60 ℃ of lower heating, strongly stir and make muddy and mix, after the vacuum defoamation, obtain 200 gram heat-curing type bi-component epoxy joint sealants, can carry out embedding.
Performance to the epoxy pouring sealant that obtains is tested, and the result is referring to table 1.
The performance of the epoxy pouring sealant of each embodiment preparation of table 1
| Project | Unit | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Hardness | Shao D | 87.5 | 88.9 | 88.6 | 87.9 |
| Tensile strength | MPa | 42 | 45 | 47 | 43 |
| Elongation at break | % | 5.0 | 4.5 | 4.8 | 5.0 |
| Flexural strength | MPa | 63.2 | 63.5 | 67.1 | 61.0 |
| Thermal linear expansion coefficient | ppm/℃ | 82 | 95 | 104 | 89 |
| Thermal conductivity | W/mK | 0.89 | 0.82 | 0.79 | 0.96 |
| Volume specific resistance | Ω·m | 2.6×10 16 | 1.8×10 16 | 2.1×10 16 | 1.5×10 16 |
| Dielectric strength | MV/m | 25.0 | 25.4 | 24.6 | 24.9 |
| Flame retardant properties detects | / | UL94V-0 | UL94V-0 | UL94V-0 | UL94V-0 |
| Initial viscosity | Pa.s | 10 | 5 | 6 | 7 |
The explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be apparent concerning those skilled in the art, and General Principle as defined herein can be in the situation that do not break away from the spirit or scope of the present invention, in other embodiments realization.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (10)
1. a heat-curing type bi-component epoxy joint sealant comprises A component and B component,
Described A component comprises the composition of following weight part:
Resins, epoxy 70 ~ 130;
The first mineral filler 150 ~ 280;
Thinner 0 ~ 25;
Toughner 0 ~ 15;
Silicone antifoam agent 0 ~ 3;
Pigment 0 ~ 3;
Described B component comprises the composition of following weight part:
Acid anhydrides 70 ~ 150;
The second mineral filler 150 ~ 280;
Wetting dispersing agent 0 ~ 15.
2. epoxy pouring sealant according to claim 1 is characterized in that, the mass ratio of described A component and B component is (1:100)～(100:1).
3. epoxy pouring sealant according to claim 1, it is characterized in that, described the first filler and the second filler independently are selected from one or more in crystalline silicon powder, activated Calcium carbonate and the active aluminium hydroxide, and described the first filler and the second filler median size are 1～100 μ m.
4. epoxy pouring sealant according to claim 1 is characterized in that, described Resins, epoxy is one or more in bisphenol A type epoxy resin, bisphenol f type epoxy resin, novolac epoxy, glycidyl amine type epoxy resin and the aliphatic epoxy resin.
5. epoxy pouring sealant according to claim 1 is characterized in that, described thinner is one or more in n-butyl glycidyl ether, glycidyl allyl ether, benzyl glycidyl ether and the BDDE.
6. epoxy pouring sealant according to claim 1, it is characterized in that, described acid anhydrides is one or more in methylhexahydrophthalic anhydride, methyl tetrahydrophthalic anhydride, isomerized methyltetrahydro phthalate anhydride, MNA, methyl carbic anhydride and the carbic anhydride.
7. epoxy pouring sealant according to claim 1 is characterized in that, described wetting dispersing agent is stearate.
8. epoxy pouring sealant according to claim 1 is characterized in that, described toughner is one or more in carboxyl end of the liquid acrylonitrile-butadiene rubber, polyurethane toughened dose, hydroxyl terminated butyl nitrile (HTBN) rubber and the Qi Shi toughner.
9. the preparation method of a heat-curing type bi-component epoxy joint sealant may further comprise the steps:
The Resins, epoxy of 70 ~ 130 weight parts, the thinner of 0 ~ 25 weight part, the toughner of 0 ~ 15 weight part, the silicone antifoam agent of 0 ~ 3 weight part, the pigment of 0 ~ 3 weight part are mixed with the first mineral filler of 150 ~ 280 weight parts, obtain the A component;
The acid anhydrides of 70 ~ 150 weight parts, the wetting dispersing agent of 1 ~ 15 weight part are mixed with the second mineral filler of 150 ~ 280 weight parts, obtain the B component;
A component and B component are heated respectively, after mixing, obtain heat-curing type bi-component epoxy joint sealant.
10. preparation method according to claim 9 is characterized in that, the mass ratio of described A component and B component is (1:100)～(100:1).
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Effective date of registration: 20180724 Address after: 412199 Industrial Park, Lukou Economic Development Zone, Zhuzhou County, Zhuzhou, Hunan Patentee after: Zhuzhou Times Electric Insulation Co., Ltd. Address before: 412007 Haitian Road, Tianyuan District, Zhuzhou, Hunan Province, No. 18 Patentee before: Zhuzhou Shidai New Material Sci-Tech Co., Ltd. |