CN103059515A - Vinyl ester resin modified epoxy pouring sealant and preparation method thereof - Google Patents
Vinyl ester resin modified epoxy pouring sealant and preparation method thereof Download PDFInfo
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- CN103059515A CN103059515A CN2012105600879A CN201210560087A CN103059515A CN 103059515 A CN103059515 A CN 103059515A CN 2012105600879 A CN2012105600879 A CN 2012105600879A CN 201210560087 A CN201210560087 A CN 201210560087A CN 103059515 A CN103059515 A CN 103059515A
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Abstract
The invention discloses a vinyl ester resin modified epoxy pouring sealant which is composed of a component A and a component B. By weight, the component A comprises 100 parts of epoxy resin and 150-300 parts of silica powder, the epoxy resin is composed of 50-90 parts of bisphenol A type epoxy resin and 10-50 parts of polyfunctional group epoxy resin, and the component B comprises 80-120 parts of anhydride, 10-40 parts of vinyl ester resin, 0.05-0.5 part of initiator and 0.1-3 parts of accelerant. The epoxy pouring sealant manufactured through the preparation method is low in viscosity (mixed initial viscosity is smaller than 2Pa.s at 60 DEG C), long in operable time (under temperature of 25 DEG C, the operable time is longer than 24 hours), good in properties such as electricity property, heat resistance, corrosion resistance and hydroscopicity after solidified, and capable of meeting the using requirements for outdoors pouring sealing devices.
Description
Technical field
The present invention relates to epoxy pouring sealant, be specifically related to epoxy pouring sealant of vinyl ester resin modification and preparation method thereof.
Background technology
Epoxy pouring sealant has the advantages such as moulding process is simple, and thermotolerance is good, electrical property is excellent, if but use out of doors, its weathering resistance is then slightly inadequate, can not guarantee outdoor life-time service.The existing joint sealant that uses out of doors mostly be with Resins, epoxy-anhydride system, tetrafluoroethylene, silicon rubber, urethane as main raw material(s), have preferably weathering resistance, preservative property, resistance to acids and bases, electrical property and mechanical property.Vinyl ester resin as anti-corrosion resin, is used in gas flue, the outdoor coating at first, along with the improvement of its performance, and then is applied in again the aspects such as communications and transportation, communication material, wind-powered electricity generation material.But the epoxy pouring sealant that yet there are no useful vinyl ester resin modification also is used for the report of outdoor Embedding Material.
Summary of the invention
The technical problem to be solved in the present invention provide a kind of weathering resistance and corrosion resistance nature better, can be used as the epoxy pouring sealant and preparation method thereof of the vinyl ester resin modification of outdoor Embedding Material.
The epoxy pouring sealant of vinyl ester resin modification of the present invention, formed by A component and B component, by weight, the A component consist of 100 parts of Resins, epoxy, 150～300 parts of silicon powders, described Resins, epoxy is comprised of 50～90 parts bisphenol A type epoxy resin and 10～50 parts polyfunctional epoxy resin; The B component consist of 80～120 parts on acid anhydrides, 10～40 parts of vinyl ester resins, 0.05～0.5 part of initiator, 0.1～3 part of promotor.
Vinyl ester resin had both contained more unsaturated double-bond, the radical crosslinking curing is provided, main chain basic structure is the basic segment of Resins, epoxy---benzene ring structure simultaneously, therefore with the characteristic of Resins, epoxy and unsaturated polyester resin, and good corrosion resistance nature and weathering resistance are arranged, can improve the anticorrosion weathering resistance of epoxy pouring sealant.The applicant takes the lead in using it in the modification of epoxy pouring sealant, make the modified epoxy joint sealant that obtains have better weathering resistance and corrosion resistance nature in basic the maintenance in the resistance toheat of matrix resin (bisphenol A type epoxy resin and polyfunctional epoxy resin), to be more suitable for as outdoor Embedding Material.
In the technique scheme, by weight, preferred A component consists of 100 parts of Resins, epoxy, 150～180 parts of silicon powders.By weight, preferred B component consists of 90～110 parts on acid anhydrides, 20～35 parts of vinyl ester resins, 0.1～0.3 part of initiator, 0.1～2 part of promotor.
In the above technical scheme:
It is 0.3～0.54 bisphenol A type epoxy resin that described bisphenol A type epoxy resin is preferably oxirane value, specifically can be any one or two or more combinations in E51 Resins, epoxy, E44 Resins, epoxy, E42 Resins, epoxy and the E35 Resins, epoxy.When bisphenol A type epoxy resin is wherein arbitrarily during two or more combination, the proportioning between them is proportioning arbitrarily.
Described polyfunctional epoxy resin is that oxirane value is 0.7～0.9 polyfunctional epoxy resin, specifically can be any one or the two or more combinations that is selected from four glycidyl group two amido ditane Resins, epoxy, p-aminophenol triglycidyl group Resins, epoxy, resorcinol formaldehyde four tetraglycidel ether epoxy resins and the dimethyl hydantion 2-glycidyl amine type Resins, epoxy.When polyfunctional epoxy resin is wherein arbitrarily during two or more combination, the proportioning between them is proportioning arbitrarily.
Described acid anhydrides is for being selected from one or more the combination in methylhexahydrophthalic anhydride (MHHPA), methyl carbic anhydride (MNA), methyl tetrahydrophthalic anhydride (MTHPA) and the 70# acid anhydrides.Mol ratio between described methylhexahydrophthalic anhydride (MHHPA), methyl carbic anhydride (MNA), methyl tetrahydrophthalic anhydride (MTHPA) and the 70# acid anhydrides is generally: 0～2:0～1:0～1:0～1.
Described vinyl ester resin is any one or the two or more combination that is selected among standard type bisphenol-A epoxide vinylester resin, methacrylic acid phenolic aldehyde epoxy type vinyl ester resin and the isocyanate-modified acrylic type vinyl ester resin 3201#.When vinyl ester resin is wherein arbitrarily during two or more combination, the proportioning between them is proportioning arbitrarily.
Described initiator is any one or the two or more combination in peroxidized t-butyl perbenzoate (TBPB), hydrogen phosphide cumene (CHP) and the peroxidation acid tert-butyl ester (TBPO).When initiator is wherein arbitrarily during two or more combination, the proportioning between them is proportioning arbitrarily.
Described promotor is dimethyl benzylamine (BDMA), glyoxal ethyline or 2-ethyl-4-methylimidazole.
The preparation method of the epoxy pouring sealant of above-mentioned vinyl ester resin modification may further comprise the steps:
1) preparation A component: according to the composition of A component (by weight, the A component consist of 100 parts of Resins, epoxy, 150～300 parts of silicon powders, described Resins, epoxy is comprised of 50～90 parts bisphenol A type epoxy resin and 10～50 parts polyfunctional epoxy resin) take by weighing each raw material, mix and blend 1～2h under 80～120 ℃ of conditions obtains the A component;
2) preparation B component: take by weighing each raw material according to the composition of B component (B component consist of 80～120 parts on acid anhydrides, 10～40 parts of vinyl ester resins, 0.05～0.5 part of initiator, 0.1～3 part of promotor), mix and blend 20～30min under 50～70 ℃ of conditions obtains the B component;
3) preparation of epoxy pouring sealant: A component and B component are mixed under 50～70 ℃ of conditions, and then vacuum defoamation is extremely complete, and get final product.
The step 3 of aforesaid method) in, mix and blend 5～10min under 50～70 ℃ of conditions can reach the purpose that mixes with A component and B component usually.In this step, the joint sealant of gained solidifies routinely when solidifying and gets final product after the deaeration, concrete curing schedule preferably includes: first with die needed in advance at 60～100 ℃ of lower preheating 2～5h, then the joint sealant after the vacuum defoamation is cast in the mould, solidify according to 60 ℃ * 1h+100 ℃ * 2h+120 ℃ * 2h staged, after cooling, the demoulding, the taking-up sample is placed under 160 ℃ of conditions and solidifies 10～20h, gets final product.
Compared with prior art, the present invention utilizes vinyl ester resin to the epoxy pouring sealant modification, the epoxy sealing adhesive capacity that obtains low (mixing initial viscosity＜2Pa.s (60 ℃)), operable time are grown (under 25 ℃ of temperature,＞24h), the performances such as electric property, thermotolerance, preservative property, water-absorbent are all better after solidifying, specifically see shown in the following table 1, can satisfy the requirement that outdoor embedding device uses.
Table 1:
| Performance | Scope |
| Shock strength, KJ/m 2 | 9～15 |
| Dielectric strength, KV/mm | 18～24 |
| Heat-drawn wire, ℃ | 155～208 |
| Thermal shock intensity, (40～155 ℃) 6 times | Do not ftracture |
Embodiment
The invention will be further described with specific embodiment for the below, but the present invention is not limited to these embodiment.
Embodiment 1
Take by weighing the epoxy pouring sealant that each raw material prepares the vinyl ester resin modification by the composition in the following table 2, concrete preparation technology may further comprise the steps:
1) preparation A component: the bisphenol A type epoxy resin (E51 Resins, epoxy), polyfunctional epoxy resin (resorcinol formaldehyde four tetraglycidel ether epoxy resins) and the silicon powder that take by weighing are placed mix and blend 2h under 120 ℃ of conditions, obtain the A component;
2) preparation B component: with acid anhydrides (methylhexahydrophthalic anhydride), vinyl ester resin (bisphenol type epoxy type vinyl ester resin), initiator (peroxidized t-butyl perbenzoate) and the promotor (dimethyl benzylamine) that takes by weighing, under 60 ℃, mix 30 min, obtain the B component;
3) preparation of epoxy pouring sealant: during use, A component and B component are mixed, stir 10 min under 60 ℃ of conditions, then vacuum defoamation obtains required joint sealant to fully.Carry out in the steps below during curing: with die needed in advance preheating 2h under 80 ℃ of conditions, then the joint sealant after the vacuum defoamation is cast in the mould, solidify according to 60 ℃ * 1h+100 ℃ * 2h+120 ℃ * 2h staged, after cooling, the demoulding, the taking-up sample is placed under 160 ℃ of conditions and solidifies 10h, gets final product.
Embodiment 2
Take by weighing the epoxy pouring sealant that each raw material prepares the vinyl ester resin modification by the composition in the following table 2, concrete preparation technology may further comprise the steps:
1) preparation A component: the bisphenol A type epoxy resin (E44 Resins, epoxy), polyfunctional epoxy resin (resorcinol formaldehyde four tetraglycidel ether epoxy resins) and the silicon powder that take by weighing are placed mix and blend 2h under 120 ℃ of conditions, obtain the A component;
2) preparation B component: the acid anhydrides (methylhexahydrophthalic anhydride, methyl carbic anhydride and 70# acid anhydrides) that takes by weighing is mixed, heated and stirred is clear liquid, namely obtain mixed type solidifying agent, then add vinyl ester resin (methacrylic acid phenolic aldehyde epoxy type vinyl ester resin), initiator (peroxidized t-butyl perbenzoate) and promotor (dimethyl benzylamine), under 60 ℃, mix 30 min, obtain the B component;
3) preparation of epoxy pouring sealant: during use, A component and B component are mixed, stir 10 min under 60 ℃ of conditions, then vacuum defoamation obtains required joint sealant to fully.Carry out in the steps below during curing: die needed in advance preheating 2h under 80 ℃ of conditions, then the pre-polymerization mixture after the vacuum defoamation is cast in the mould, solidify according to 60 ℃ * 1h+100 ℃ * 2h+120 ℃ * 2h staged, after cooling, the demoulding, the taking-up sample is placed under 160 ℃ of conditions and solidifies 10h, gets final product.
Embodiment 3
Composition by embodiment 3 in the following table 2 takes by weighing the epoxy pouring sealant that each raw material prepares the vinyl ester resin modification, and concrete preparation technology is with embodiment 2.
Embodiment 4
Composition by embodiment 4 in the following table 2 takes by weighing the epoxy pouring sealant that each raw material prepares the vinyl ester resin modification, and concrete preparation technology is with embodiment 2.
Embodiment 5
Composition by embodiment 5 in the following table 2 takes by weighing the epoxy pouring sealant that each raw material prepares the vinyl ester resin modification, and concrete preparation technology is with embodiment 2.
Embodiment 6
Composition by embodiment 6 in the following table 2 takes by weighing the epoxy pouring sealant that each raw material prepares the vinyl ester resin modification, and concrete preparation technology is with embodiment 2.
Comparative Examples 1
Composition by Comparative Examples 1 in the following table 2 takes by weighing the epoxy pouring sealant that each raw material prepares the vinyl ester resin modification, and concrete preparation technology may further comprise the steps:
1) preparation A component: the bisphenol A type epoxy resin (E51 Resins, epoxy), polyfunctional epoxy resin (four glycidyl group two amido ditane Resins, epoxy) and the silicon powder that take by weighing are placed mix and blend 2h under 120 ℃ of conditions, obtain the A component;
2) preparation B component: the acid anhydrides (methylhexahydrophthalic anhydride, methyl carbic anhydride and 70# acid anhydrides) that takes by weighing is mixed, heated and stirred is clear liquid, namely obtain mixed type solidifying agent, then add promotor (2-ethyl-4-methylimidazole), under 80 ℃, mix 30 min, obtain the B component;
3) preparation of epoxy pouring sealant: during use, A component and B component are mixed, stir 10 min under 60 ℃ of conditions, then vacuum defoamation obtains required joint sealant to fully.Carry out in the steps below during curing: with die needed in advance preheating 2h under 80 ℃ of conditions, then the pre-polymerization mixture after the vacuum defoamation is cast in the mould, solidify according to 60 ℃ * 1h+100 ℃ * 2h+120 ℃ * 2h staged, after cooling, the demoulding, the taking-up sample is placed under 200 ℃ of conditions and solidifies 10h, gets final product.
Comparative Examples 2
Composition by Comparative Examples 2 in the following table 2 takes by weighing the epoxy pouring sealant that each raw material prepares the vinyl ester resin modification, and concrete preparation technology is:
With vinyl ester resin (methacrylic acid phenolic aldehyde epoxy type vinyl ester resin), initiator (peroxidized t-butyl perbenzoate, the peroxidation acid tert-butyl ester) and the promotor (dimethyl benzylamine) that takes by weighing, under 60 ℃, mix 30 min, then vacuum defoamation obtains required joint sealant to fully.Carry out in the steps below during curing: with die needed in advance preheating 2h under 80 ℃ of conditions, then the pre-polymerization mixture after the vacuum defoamation is cast in the mould, solidify according to 60 ℃ * 1h+100 ℃ * 2h+120 ℃ * 2h staged, after cooling, the demoulding, the taking-up sample is placed under 200 ℃ of conditions and solidifies 10h, gets final product.
Comparative Examples 3
Composition by Comparative Examples 3 in the following table 2 takes by weighing the epoxy pouring sealant that each raw material prepares the vinyl ester resin modification, and concrete preparation technology is with embodiment 5.
Comparative Examples 4
Composition by Comparative Examples 4 in the following table 2 takes by weighing the epoxy pouring sealant that each raw material prepares the vinyl ester resin modification, and concrete preparation technology is with embodiment 5.
Table 2
The epoxy pouring sealant of the vinyl ester resin modification that above-described embodiment 1～6 is made and the epoxy pouring sealant that Comparative Examples 1～4 makes carry out the traditional performance test and corrosion resistance nature is tested, and the result is respectively shown in following table 3 and table 4:
Table 3: the traditional performance contrast table of the epoxy resin embedding adhesive of each embodiment and each Comparative Examples
Table 4: the corrosion resistance nature contrast table of the epoxy resin embedding adhesive of each embodiment and each Comparative Examples
The performance of comprehensive above-mentioned table 3 and table 4, when the add-on of vinyl ester resin is very few (such as Comparative Examples 3), the cold-hot impact of the epoxy pouring sealant of gained and erosion resistance are all bad under the same process condition; And when the add-on of vinyl ester resin is too much (such as Comparative Examples 4), though the epoxy pouring sealant of gained can keep preferably cold-hot impact and erosion resistance under the same process condition, its shock strength has larger decline; When the amount of vinyl ester resin is 100 weight part (such as Comparative Examples 2), cost is higher, though the epoxy pouring sealant of gained can keep preferably erosion resistance, and its cold-hot impact variation, shock strength is also not high enough.The adding that data in the Comparative Examples 1 further show vinyl ester resin is greatly improved to the corrosion resistance nature of joint sealant.As seen, by vinyl ester resin being used for the modification of epoxy pouring sealant, make the modified epoxy joint sealant that obtains corrosion resistance nature and the weather resistance of modified epoxy joint sealant can be brought up to new height in basic the maintenance in the resistance toheat of matrix resin itself, thereby has better over-all properties, to be more suitable for as outdoor Embedding Material.
Claims (10)
1. the epoxy pouring sealant of vinyl ester resin modification, it is characterized in that: it is comprised of A component and B component, by weight, the A component consist of 100 parts of Resins, epoxy, 150～300 parts of silicon powders, described Resins, epoxy is comprised of 50～90 parts bisphenol A type epoxy resin and 10～50 parts polyfunctional epoxy resin; The B component consist of 80～120 parts on acid anhydrides, 10～40 parts of vinyl ester resins, 0.05～0.5 part of initiator, 0.1～3 part of promotor.
2. the epoxy pouring sealant of vinyl ester resin modification according to claim 1 is characterized in that: by weight, the A component consist of 100 parts of Resins, epoxy, 150～180 parts of silicon powders.
3. the epoxy pouring sealant of vinyl ester resin modification according to claim 1 is characterized in that: by weight, the B component consist of 90～110 parts on acid anhydrides, 20～35 parts of vinyl ester resins, 0.1～0.3 part of initiator, 0.1～2 part of promotor.
4. the epoxy pouring sealant of each described vinyl ester resin modification according to claim 1～3 is characterized in that: described bisphenol A type epoxy resin is that oxirane value is 0.3～0.54 bisphenol A type epoxy resin.
5. the epoxy pouring sealant of each described vinyl ester resin modification according to claim 1～3 is characterized in that: described polyfunctional epoxy resin is that oxirane value is 0.7～0.9 polyfunctional epoxy resin.
6. the epoxy pouring sealant of each described vinyl ester resin modification according to claim 1～3 is characterized in that: described acid anhydrides is one or more the combination that is selected from methylhexahydrophthalic anhydride, methyl carbic anhydride, methyl tetrahydrophthalic anhydride and the 70# acid anhydrides.
7. the epoxy pouring sealant of each described vinyl ester resin modification according to claim 1～3 is characterized in that: described vinyl ester resin is any one or the two or more combination that is selected among standard type bisphenol-A epoxide vinylester resin, methacrylic acid phenolic aldehyde epoxy type vinyl ester resin and the isocyanate-modified acrylic type vinyl ester resin 3201#.
8. the epoxy pouring sealant of each described vinyl ester resin modification according to claim 1～3 is characterized in that: described initiator is one or more the combination in peroxidized t-butyl perbenzoate (TBPB), hydrogen phosphide cumene (CHP) and the peroxidation acid tert-butyl ester (TBPO).
9. the epoxy pouring sealant of each described vinyl ester resin modification according to claim 1～3 is characterized in that: described promotor is dimethyl benzylamine (BDMA), glyoxal ethyline or 2-ethyl-4-methylimidazole.
10. the preparation method of the epoxy pouring sealant of vinyl ester resin modification claimed in claim 1 may further comprise the steps:
1) preparation A component: the composition according to the A component takes by weighing each raw material, and mix and blend 1～2h under 80～120 ℃ of conditions obtains the A component;
2) preparation B component: the composition according to the B component takes by weighing each raw material, and mix and blend 20～30min under 50～70 ℃ of conditions obtains the B component;
3) preparation of epoxy pouring sealant: A component and B component are mixed under 50～70 ℃ of conditions, and then vacuum defoamation is extremely complete, and get final product.
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| CN105754072A (en) * | 2016-04-07 | 2016-07-13 | 中国人民解放军国防科学技术大学 | Epoxy resin composition and preparation method thereof |
| CN106520048A (en) * | 2016-11-29 | 2017-03-22 | 广西大学 | Adhesive applied to stone curtain wall |
| CN106634756A (en) * | 2017-01-04 | 2017-05-10 | 濮阳惠成电子材料股份有限公司 | Two-component LED pouring sealant |
| CN108752943A (en) * | 2018-05-24 | 2018-11-06 | 昆明理工大学 | A kind of preparation method of epoxy resin-matrix ambroin |
| CN111057490A (en) * | 2019-12-10 | 2020-04-24 | 广州席风机电设备工程有限公司 | Preparation method of high-adhesion polyacrylate-based pouring sealant |
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| CN105754072A (en) * | 2016-04-07 | 2016-07-13 | 中国人民解放军国防科学技术大学 | Epoxy resin composition and preparation method thereof |
| CN106520048A (en) * | 2016-11-29 | 2017-03-22 | 广西大学 | Adhesive applied to stone curtain wall |
| CN106634756A (en) * | 2017-01-04 | 2017-05-10 | 濮阳惠成电子材料股份有限公司 | Two-component LED pouring sealant |
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| CN111057490A (en) * | 2019-12-10 | 2020-04-24 | 广州席风机电设备工程有限公司 | Preparation method of high-adhesion polyacrylate-based pouring sealant |
| CN114231233A (en) * | 2021-11-22 | 2022-03-25 | 深圳先进电子材料国际创新研究院 | Low-viscosity-distribution cavity conductive adhesive and preparation method and application thereof |
| CN115449278A (en) * | 2022-10-20 | 2022-12-09 | 沈阳大学 | Graphene-loaded titanium dioxide composite anticorrosive paint and preparation method thereof |
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