CN103059515B - 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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- CN103059515B CN103059515B CN201210560087.9A CN201210560087A CN103059515B CN 103059515 B CN103059515 B CN 103059515B CN 201210560087 A CN201210560087 A CN 201210560087A CN 103059515 B CN103059515 B CN 103059515B
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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
It is simple that epoxy pouring sealant has moulding process, the advantages such as thermotolerance is good, excellent electrical property, if but use out of doors, its weathering resistance then shows slightly not enough, can not ensure outdoor life-time service.The existing joint sealant used out of doors be mostly with epoxy resin-anhydride system, tetrafluoroethylene, silicon rubber, urethane for main raw material(s), there is good weathering resistance, preservative property, resistance to acids and bases, electrical property and mechanical property.Vinyl ester resin is used as anti-corrosion resin at first, is used in gas flue, outdoor coating, along with the improvement of its performance, and then is applied in again communications and transportation, the communication aspect such as material, wind-powered electricity generation material.But yet there are no useful vinyl ester resin modification epoxy pouring sealant and for the report of outdoor Embedding Material.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of weathering resistance and corrosion resistance nature is better, can be used as epoxy pouring sealant of the vinyl ester resin modification of outdoor Embedding Material and preparation method thereof.
The epoxy pouring sealant of vinyl ester resin modification of the present invention, be made up of component A and B component, by weight, component A consist of epoxy resin 100 parts, silicon powder 150 ~ 300 parts, described epoxy resin is made up of the bisphenol A type epoxy resin of 50 ~ 90 parts and the polyfunctional epoxy resin of 10 ~ 50 parts; B component consist of 80 ~ 120 parts, acid anhydrides, vinyl ester resin 10 ~ 40 parts, initiator 0.05 ~ 0.5 part, promotor 0.1 ~ 3 part.
Vinyl ester resin is both containing more unsaturated double-bond, radical crosslinking curing is provided, main chain basic structure is the basic segment of epoxy resin---benzene ring structure simultaneously, therefore with the characteristic of epoxy resin and unsaturated polyester resin, and have good corrosion resistance nature and weathering resistance, the anticorrosion weathering resistance of epoxy pouring sealant can be improved.Applicant takes the lead in using it in the modification of epoxy pouring sealant, the modified epoxy joint sealant obtained is made to have better weathering resistance and corrosion resistance nature while the resistance toheat substantially keeping matrix resin (bisphenol A type epoxy resin and polyfunctional epoxy resin), to be more suitable for being used as outdoor Embedding Material.
In technique scheme, by weight, preferred component A consists of epoxy resin 100 parts, silicon powder 150 ~ 180 parts.By weight, preferred B component consists of 90 ~ 110 parts, acid anhydrides, vinyl ester resin 20 ~ 35 parts, initiator 0.1 ~ 0.3 part, promotor 0.1 ~ 2 part.
In above technical scheme:
Described bisphenol A type epoxy resin is preferably the bisphenol A type epoxy resin that oxirane value is 0.3 ~ 0.54, can be specifically any one or two or more combinations in E51 epoxy resin, E44 epoxy resin, E42 epoxy resin and E35 epoxy resin.When bisphenol A type epoxy resin is wherein two or more arbitrarily combination, the proportioning between them can proportioning arbitrarily.
Described polyfunctional epoxy resin to be oxirane value be 0.7 ~ 0.9 polyfunctional epoxy resin, can be specifically any one or the two or more combinations that are selected from four glycidyl group two amido ditane epoxy resin, p-aminophenol three-glycidyl base epoxy, resorcinol formaldehyde four tetraglycidel ether epoxy resin and dimethyl hydantion 2-glycidyl amine type epoxy resin.When polyfunctional epoxy resin is wherein two or more arbitrarily combination, the proportioning between them can proportioning arbitrarily.
Described acid anhydrides is for being selected from one or more the combination in methylhexahydrophthalic anhydride (MHHPA), methylnadic anhydride (MNA), methyl tetrahydrophthalic anhydride (MTHPA) and 70# acid anhydrides.Described methylhexahydrophthalic anhydride (MHHPA), methylnadic anhydride (MNA), mol ratio between methyl tetrahydrophthalic anhydride (MTHPA) and 70# acid anhydrides are generally: 0 ~ 2:0 ~ 1:0 ~ 1:0 ~ 1.
Described vinyl ester resin is any one or the two or more combinations that are selected from standard type bisphenol-A epoxide vinylester resin, methacrylic acid epoxy novolac type vinyl ester resin and isocyanate-modified acrylic type vinyl ester resin 3201#.When vinyl ester resin is wherein two or more arbitrarily combination, the proportioning between them can proportioning arbitrarily.
Described initiator is any one or two or more combinations in peroxidized t-butyl perbenzoate (TBPB), hydrogen phosphide cumene (CHP) and the peroxidation isocaprylic acid tert-butyl ester (TBPO).When initiator is wherein two or more arbitrarily combination, the proportioning between them can 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, comprises the following steps:
1) component A is prepared: according to the composition of component A (by weight, component A consist of epoxy resin 100 parts, silicon powder 150 ~ 300 parts, described epoxy resin is made up of the bisphenol A type epoxy resin of 50 ~ 90 parts and the polyfunctional epoxy resin of 10 ~ 50 parts) take each raw material, under 80 ~ 120 DEG C of conditions, mix and blend 1 ~ 2h, obtains component A;
2) B component is prepared: the composition (the consisting of 80 ~ 120 parts, acid anhydrides, vinyl ester resin 10 ~ 40 parts, initiator 0.05 ~ 0.5 part, promotor 0.1 ~ 3 part of B component) according to B component takes each raw material, under 50 ~ 70 DEG C of conditions, mix and blend 20 ~ 30min, obtains B component;
3) preparation of epoxy pouring sealant: component A and B component are mixed under 50 ~ 70 DEG C of conditions, then vacuum defoamation is to completely, to obtain final product.
The step 3 of aforesaid method) in, by component A and B component, mix and blend 5 ~ 10min under 50 ~ 70 DEG C of conditions can reach the object mixed usually.In this step, after deaeration, the joint sealant of gained solidifies routinely carry out when solidifying, concrete curing schedule preferably includes: first by die needed preheating 2 ~ 5h at 60 ~ 100 DEG C in advance, then by the joint sealant cast after vacuum defoamation in a mold, according to the solidification of 60 DEG C × 1h+100 DEG C × 2h+120 DEG C × 2h staged, after cooling, the demoulding, take out under sample is placed on 160 DEG C of conditions and solidify 10 ~ 20h.
Compared with prior art, the present invention utilizes vinyl ester resin to epoxy pouring sealant modification, the epoxy sealing adhesive capacity obtained low (mixing initial viscosity < 2Pa.s (60 DEG C)), operable time are longer (at 25 DEG C of temperature, > 24h), the performances such as solidification rear electric property, thermotolerance, preservative property, water-absorbent are all better, specifically see with shown in following table 1, the requirement that outdoor embedding device uses can be met.
Table 1:
| Performance | Scope |
| Shock strength, KJ/m 2 | 9～15 |
| Dielectric strength, KV/mm | 18～24 |
| Heat-drawn wire, DEG C | 155～208 |
| Thermal shock intensity, (-40 ~ 155 DEG C) 6 times | Do not ftracture |
Embodiment
With specific embodiment, the invention will be further described below, but the present invention is not limited to these embodiments.
Embodiment 1
By the epoxy pouring sealant taking each raw material with the composition in following table 2 and prepare vinyl ester resin modification, concrete preparation technology comprises the following steps:
1) component A is prepared: the bisphenol A type epoxy resin taken (E51 epoxy resin), polyfunctional epoxy resin (resorcinol formaldehyde four tetraglycidel ether epoxy resin) and silicon powder are placed in mix and blend 2h under 120 DEG C of conditions, obtain component A;
2) prepare B component: by take acid anhydrides (methylhexahydrophthalic anhydride), vinyl ester resin (bisphenol type epoxy type vinyl ester resin), initiator (peroxidized t-butyl perbenzoate) and promotor (dimethyl benzylamine), at 60 DEG C, be uniformly mixed 30min, obtain B component;
3) preparation of epoxy pouring sealant: during use, by component A and B component mixing, under 60 DEG C of conditions, stir 10min, then vacuum defoamation is to completely, obtains required joint sealant.Carry out in the steps below during solidification: by die needed preheating 2h under 80 DEG C of conditions in advance, then by the joint sealant cast after vacuum defoamation in a mold, according to the solidification of 60 DEG C × 1h+100 DEG C × 2h+120 DEG C × 2h staged, after cooling, the demoulding, take out under sample is placed on 160 DEG C of conditions and solidify 10h.
Embodiment 2
By the epoxy pouring sealant taking each raw material with the composition in following table 2 and prepare vinyl ester resin modification, concrete preparation technology comprises the following steps:
1) component A is prepared: the bisphenol A type epoxy resin taken (E44 epoxy resin), polyfunctional epoxy resin (resorcinol formaldehyde four tetraglycidel ether epoxy resin) and silicon powder are placed in mix and blend 2h under 120 DEG C of conditions, obtain component A;
2) B component is prepared: by acid anhydrides (methylhexahydrophthalic anhydride, methylnadic anhydride and the 70# acid anhydrides) mixing taken, heated and stirred is clear liquid, namely mixed type solidifying agent is obtained, then vinyl ester resin (methacrylic acid epoxy novolac type vinyl ester resin), initiator (peroxidized t-butyl perbenzoate) and promotor (dimethyl benzylamine) is added, at 60 DEG C, be uniformly mixed 30min, obtain B component;
3) preparation of epoxy pouring sealant: during use, by component A and B component mixing, under 60 DEG C of conditions, stir 10min, then vacuum defoamation is to completely, obtains required joint sealant.Carry out in the steps below during solidification: die needed preheating 2h under 80 DEG C of conditions in advance, then by the pre-polymer mix cast after vacuum defoamation in a mold, according to the solidification of 60 DEG C × 1h+100 DEG C × 2h+120 DEG C × 2h staged, after cooling, the demoulding, take out under sample is placed on 160 DEG C of conditions and solidify 10h.
Embodiment 3
By the epoxy pouring sealant taking each raw material with the composition of embodiment 3 in following table 2 and prepare vinyl ester resin modification, concrete preparation technology is with embodiment 2.
Embodiment 4
By the epoxy pouring sealant taking each raw material with the composition of embodiment 4 in following table 2 and prepare vinyl ester resin modification, concrete preparation technology is with embodiment 2.
Embodiment 5
By the epoxy pouring sealant taking each raw material with the composition of embodiment 5 in following table 2 and prepare vinyl ester resin modification, concrete preparation technology is with embodiment 2.
Embodiment 6
By the epoxy pouring sealant taking each raw material with the composition of embodiment 6 in following table 2 and prepare vinyl ester resin modification, concrete preparation technology is with embodiment 2.
Comparative example 1
By the epoxy pouring sealant taking each raw material with the composition of comparative example 1 in following table 2 and prepare vinyl ester resin modification, concrete preparation technology comprises the following steps:
1) component A is prepared: the bisphenol A type epoxy resin taken (E51 epoxy resin), polyfunctional epoxy resin (four glycidyl group two amido ditane epoxy resin) and silicon powder are placed in mix and blend 2h under 120 DEG C of conditions, obtain component A;
2) B component is prepared: by acid anhydrides (methylhexahydrophthalic anhydride, methylnadic anhydride and the 70# acid anhydrides) mixing taken, heated and stirred is clear liquid, namely mixed type solidifying agent is obtained, then promotor (2-ethyl-4-methylimidazole) is added, at 80 DEG C, be uniformly mixed 30min, obtain B component;
3) preparation of epoxy pouring sealant: by component A and B component mixing, stir 10min under 60 DEG C of conditions, then vacuum defoamation is to completely, obtains required joint sealant.Carry out in the steps below during solidification: by die needed preheating 2h under 80 DEG C of conditions in advance, then by the pre-polymer mix cast after vacuum defoamation in a mold, according to the solidification of 60 DEG C × 1h+100 DEG C × 2h+120 DEG C × 2h staged, after cooling, the demoulding, take out under sample is placed on 200 DEG C of conditions and solidify 10h.
Comparative example 2
By the epoxy pouring sealant taking each raw material with the composition of comparative example 2 in following table 2 and prepare vinyl ester resin modification, concrete preparation technology is:
By take vinyl ester resin (methacrylic acid epoxy novolac type vinyl ester resin), initiator (peroxidized t-butyl perbenzoate, the peroxidation isocaprylic acid tert-butyl ester) and promotor (dimethyl benzylamine), 30min is uniformly mixed at 60 DEG C, then vacuum defoamation is to completely, obtains required joint sealant.Carry out in the steps below during solidification: by die needed preheating 2h under 80 DEG C of conditions in advance, then by the pre-polymer mix cast after vacuum defoamation in a mold, according to the solidification of 60 DEG C × 1h+100 DEG C × 2h+120 DEG C × 2h staged, after cooling, the demoulding, take out under sample is placed on 200 DEG C of conditions and solidify 10h.
Comparative example 3
By the epoxy pouring sealant taking each raw material with the composition of comparative example 3 in following table 2 and prepare vinyl ester resin modification, concrete preparation technology is with embodiment 5.
Comparative example 4
By the epoxy pouring sealant taking each raw material with the composition of comparative example 4 in following table 2 and prepare vinyl ester resin modification, concrete preparation technology is with embodiment 5.
Table 2
The epoxy pouring sealant that the epoxy pouring sealant of vinyl ester resin modification obtained for above-described embodiment 1 ~ 6 and comparative example 1 ~ 4 obtain is carried out traditional performance test and corrosion resistance nature test, and result is respectively as 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 example
Table 4: the corrosion resistance nature contrast table of the epoxy resin embedding adhesive of each embodiment and each comparative example
The performance of comprehensive above-mentioned table 3 and table 4, when the add-on of vinyl ester resin is very few (as comparative example 3), under same process condition the cold-hot impact of the epoxy pouring sealant of gained and erosion resistance all bad; And when the add-on of vinyl ester resin is too much (as comparative example 4), though the epoxy pouring sealant of gained can keep good cold-hot impact and erosion resistance under same process condition, its shock strength has larger decline; When the amount of vinyl ester resin is 100 weight part (as comparative example 2), cost is higher, though the epoxy pouring sealant of gained can keep good erosion resistance, its cold-hot impact is deteriorated, and shock strength is also not high enough.Data in comparative example 1 further show that adding of vinyl ester resin is greatly improved to the corrosion resistance nature of joint sealant.Visible, by vinyl ester resin is used in the modification of epoxy pouring sealant, make the modified epoxy joint sealant obtained the corrosion resistance nature of modified epoxy joint sealant and weather resistance can be brought up to new height while the resistance toheat of basic maintenance matrix resin itself, thus there is better over-all properties, to be more suitable for being used as outdoor Embedding Material.
Claims (10)
1. the epoxy pouring sealant of vinyl ester resin modification, it is characterized in that: it is made up of component A and B component, by weight, component A consist of epoxy resin 100 parts, silicon powder 150 ~ 300 parts, described epoxy resin is made up of the bisphenol A type epoxy resin of 50 ~ 90 parts and the polyfunctional epoxy resin of 10 ~ 50 parts; B component consist of 80 ~ 120 parts, acid anhydrides, vinyl ester resin 10 ~ 40 parts, initiator 0.05 ~ 0.5 part, promotor 0.1 ~ 3 part.
2. the epoxy pouring sealant of vinyl ester resin modification according to claim 1, is characterized in that: by weight, component A consist of epoxy resin 100 parts, silicon powder 150 ~ 180 parts.
3. the epoxy pouring sealant of vinyl ester resin modification according to claim 1, is characterized in that: by weight, B component consist of 90 ~ 110 parts, acid anhydrides, vinyl ester resin 20 ~ 35 parts, initiator 0.1 ~ 0.3 part, promotor 0.1 ~ 2 part.
4. the epoxy pouring sealant of the vinyl ester resin modification according to any one of claims 1 to 3, is characterized in that: described bisphenol A type epoxy resin to be oxirane value be 0.3 ~ 0.54 bisphenol A type epoxy resin.
5. the epoxy pouring sealant of the vinyl ester resin modification according to any one of claims 1 to 3, is characterized in that: described polyfunctional epoxy resin to be oxirane value be 0.7 ~ 0.9 polyfunctional epoxy resin.
6. the epoxy pouring sealant of the vinyl ester resin modification according to any one of claims 1 to 3, is characterized in that: described acid anhydrides is be selected from one or more the combination in methylhexahydrophthalic anhydride, methylnadic anhydride, methyl tetrahydrophthalic anhydride and 70# acid anhydrides.
7. the epoxy pouring sealant of the vinyl ester resin modification according to any one of claims 1 to 3, is characterized in that: described vinyl ester resin is any one or the two or more combinations that are selected from standard type bisphenol-A epoxide vinylester resin, methacrylic acid epoxy novolac type vinyl ester resin and isocyanate-modified acrylic type vinyl ester resin 3201#.
8. the epoxy pouring sealant of the vinyl ester resin modification according to any one of claims 1 to 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 isocaprylic acid tert-butyl ester (TBPO).
9. the epoxy pouring sealant of the vinyl ester resin modification according to any one of claims 1 to 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 according to claim 1, comprises the following steps:
1) prepare component A: take each raw material according to the composition of component A, under 80 ~ 120 DEG C of conditions, mix and blend 1 ~ 2h, obtains component A;
2) prepare B component: take each raw material according to the composition of B component, under 50 ~ 70 DEG C of conditions, mix and blend 20 ~ 30min, obtains B component;
3) preparation of epoxy pouring sealant: component A and B component are mixed under 50 ~ 70 DEG C of conditions, then vacuum defoamation is to completely, to obtain final product.
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| CN105754072B (en) * | 2016-04-07 | 2018-07-03 | 中国人民解放军国防科学技术大学 | Composition epoxy resin 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 |
| 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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| CN101225156B (en) * | 2007-12-13 | 2010-05-19 | 桂林电器科学研究所 | Epoxide resin curing agent, epoxide resin embedding glue and confecting method thereof |
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