CN103305132A - Fast-curing structural adhesive and preparation method thereof - Google Patents
Fast-curing structural adhesive and preparation method thereof Download PDFInfo
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- CN103305132A CN103305132A CN2012100584884A CN201210058488A CN103305132A CN 103305132 A CN103305132 A CN 103305132A CN 2012100584884 A CN2012100584884 A CN 2012100584884A CN 201210058488 A CN201210058488 A CN 201210058488A CN 103305132 A CN103305132 A CN 103305132A
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Abstract
The invention discloses a fast-curing structural adhesive comprising the following components: 20-60 parts of epoxy resin, 10-40 parts of acrylic resin, 5-30 parts of acrylate monomers, 2-30 parts of a latent epoxy resin curing agent, 0.5-5 parts of an one-component epoxy stabilizer, 2-5 parts of an acrylate photoinitiator, 1-20 parts of fillers, and 0.1-2 parts of an auxiliary agent. The invention further discloses a preparation method of the fast-curing structural adhesive. The fast-curing structural adhesive prepared according to the components and the preparation method effectively solves defects and insufficiencies of long positioning time and fully cured time, and poor resistance to heat aging properties.
Description
Technical field
The present invention relates to the adhesive technology field, especially refer to a kind of fast setting sqtructural adhesive, simultaneously, the invention also discloses the preparation method of tackiness agent.
Background technology
Epoxyn has metal base bonding strength height, shrinking percentage is low, the ageing-resistant performance excellence, plurality of advantages such as electrical property excellence, in field widespread uses such as aerospace, automobile, electronics, machineries, the part but epoxyn also comes with some shortcomings, as: curing speed is slow, setting time is longer, and is low to the plastic basis material bonding strength.Wherein, the single-component epoxy resin adhesive need be heated to more than 80 ℃ could solidify at least, and solidifying faster, two-component epoxy resin adhesive also needs could locate about at least 10 minutes.These defectives and deficiency have had a strong impact on the application of epoxyn in allegro modernization industry is produced.Because the component in each field such as aerospace, automobile, electronics, machinery not only comprise metal bases such as aluminium, magnesium, stainless steel, also comprise plastic basis materials such as PC, ABS, PET, PMMA, PEI or plastic blend material.Epoxyn long defective setting time is difficult to adapt to modern streamline production, has a strong impact on production efficiency.
It is fast that acrylic ester adhesive has curing speed, and setting time is short, the advantage good to the plastic basis material cementability.But have the wet and heat ageing resistant poor performance, shrinking percentage is big, easily causes the bond internal stress big, causes shortcomings such as warpage, distortion.
So it is fast to develop a kind of curing speed, setting time is short, and wet and heat ageing resistant is strong, and to metal, plastic basis material all being had the focus that has become industry research than the tackiness agent of high-adhesive-strength.
Summary of the invention
In order to solve the deficiencies in the prior art and defective, the present invention provides and can locate fast by the blend of epoxyn and acrylic ester adhesive, simultaneously metal, plastic basis material are had than high-adhesive-strength, and the tackiness agent of wet and heat ageing resistant excellent property.
In order to realize the foregoing invention purpose, the invention provides following technical scheme:
A kind of fast setting sqtructural adhesive of the present invention comprises following component:
Wherein, described Resins, epoxy comprises E-51 Resins, epoxy, the mixture of one or more any ratios in E-44 Resins, epoxy or the E-20 Resins, epoxy.
Wherein, described acrylic resin comprises urethane acrylate, polyether acrylate, the mixture of any ratio of one or more in polyester acrylate or the epoxy acrylate; Described acrylate monomer comprises methyl methacrylate, hydroxyethyl methylacrylate, Rocryl 410, (methyl) vinylformic acid tetrahydrofuran ester, (methyl) isobornyl acrylate, N, the N DMAA, polyfunctionality (methyl) acrylate, polyethyleneglycol diacrylate, the mixture of one or more any ratios in ethoxyquin bisphenol a diacrylate or (methyl) vinylformic acid.
Wherein, described latent epoxy resin curing agent comprises the Dyhard RU 100 class, imidazoles, anhydrides, the mixture of any ratio of one or more in boron trifluoride amine or the polythiol.
Wherein, described single-component epoxy stablizer is barbituric acid.
Wherein, described acrylate light trigger comprises 2; 4; 6-trimethylbenzoyl-diphenyl phosphine oxide; the benzophenone of benzophenone and replacement, the methyl phenyl ketone of methyl phenyl ketone and replacement, bitter almond oil camphor and alkyl ester thereof; the xanthone of xanthone and replacement; phosphine oxide, diethoxy acetophenone, benzoin methylether; ethoxybenzoin; benzoin iso-propylether, diethoxy xanthone, chloro thio-xanthene-one; N methyldiethanol amine benzophenone, 2-hydroxy-2-methyl-1-phenyl third-1-ketone or 2-benzyl-2-(dimethylamino)-1-[4-(4-morpholinyl) phenyl]-mixture of one or more any ratios in the 1-butanone.
Wherein, described filler comprises aerosil, calcium carbonate, the mixture of one or more any ratios in nano aluminium oxide or the shell nuclear rubber powder.Described auxiliary agent comprises silane coupling agent, defoamer, epoxy-resin systems stablizer, the mixture of any ratio of one or more in curing catalyst or the adhesion promoter.
Simultaneously, the invention also discloses the preparation method of above-mentioned fast setting sqtructural adhesive, comprise the steps:
(1) acrylate resin and acrylate monomer evenly mix;
(2) add the acrylate light trigger, intensification is stirred to the acrylate light trigger and dissolves fully;
(3) adding Resins, epoxy, single-component epoxy stablizer and auxiliary agent successively stirs;
(4) after the cooling, add the latent epoxy curing agent, high-speed stirring is to being uniformly dispersed;
(5) add filler such as aerosil, high-speed stirring
(6) under vacuum state, remove bubble, get finished product.
Wherein, the intensification temperature described in the step (2) is 30-50 ℃.Cooling temperature described in the step (4) is below 25 ℃.
Beneficial effect of the present invention is: can finish the location second at 5-30 under the uviolizing according to the fast setting sqtructural adhesive of component prescription disclosed by the invention and preparation method thereof preparation, the bond behind the location can move and not influence final bonding strength; Back fast setting sqtructural adhesive is finished curing under heating condition, the condition that is heating and curing is 80-150 ℃, 30-120 minute.The setting time that fast setting sqtructural adhesive of the present invention has solved prior art effectively is long, defective and deficiencies such as wet and heat ageing resistant poor performance.Fast setting sqtructural adhesive of the present invention is applicable to that having at least a kind of in two kinds of bonding base materials is transparent substrate, and the situation that two kinds of base materials can both anti-at least 80 ℃ of temperature.
Embodiment
Describe the present invention below in conjunction with specific embodiment.
Embodiment one
Get 25Kg urethane acrylate and 15Kg N, stirred 10-30 minute in the N DMAA adding stirring tank, until mixing; Add 2Kg 2,4, behind 6-trimethylbenzoyl-diphenyl phosphine oxide, be warming up to 40 ℃, dissolved fully until 2,4,6-trimethylbenzoyl-diphenyl phosphine oxide in high-speed stirring 30-60 minute; After add 35.5Kg E-51 Resins, epoxy, 1Kg barbituric acid, 0.5Kg silane coupling agent successively and stir 10-30 minute to evenly, the control whipping temp is no more than 50 ℃; Cool to below 25 degrees centigrade, add the 18Kg polythiol, high-speed stirring 30-60 minute, be uniformly dispersed, the control temperature is no more than 25 ℃ in the whipping process; Add fillers such as 3Kg aerosil, high-speed stirring 15-30 minute, the control whipping temp was not higher than 25 ℃, vacuumized and removed bubble, and the control temperature is no more than 25 ℃, gets finished product A, and canned, the finished product storing temp must not be higher than 5 ℃.
Embodiment two
Get in 10Kg polyether acrylate and 30Kg (methyl) the isobornyl acrylate adding stirring tank and stirred 10-30 minute, until mixing; After adding the benzophenone of 5Kg benzophenone and replacement, be warming up to 30 ℃, dissolved fully until the benzophenone of benzophenone and replacement in high-speed stirring 30-60 minute; After add 50.9KgE-44 Resins, epoxy, 0.5Kg barbituric acid, 0.1Kg epoxy-resin systems stablizer successively and stir 10-30 minute to evenly, the control whipping temp is no more than 50 ℃; Cool to below 25 degrees centigrade, add 2.5Kg boron trifluoride amine, high-speed stirring 30-60 minute, be uniformly dispersed, the control temperature is no more than 25 ℃ in the whipping process; Add fillers such as 1Kg calcium carbonate, high-speed stirring 15-30 minute, the control whipping temp was not higher than 25 ℃, vacuumized and removed bubble, and the control temperature is no more than 25 ℃, gets finished product B, and canned, the finished product storing temp must not be higher than 5 ℃.
Embodiment three
Get in 40Kg polyester acrylate and 5Kg (methyl) the vinylformic acid tetrahydrofuran ester adding stirring tank and stirred 10-30 minute, until mixing; After adding the 5Kg diethoxy acetophenone, be warming up to 50 ℃, dissolved fully until diethoxy acetophenone in high-speed stirring 30-60 minute; After add 36KgE-20 Resins, epoxy, 5Kg barbituric acid, 2Kg curing catalyst successively and stir 10-30 minute to evenly, the control whipping temp is no more than 50 ℃; Cool to below 25 degrees centigrade, add 2Kg methylimidazole epoxy propane butyl ether affixture, high-speed stirring 30-60 minute, be uniformly dispersed, the control temperature is no more than 25 ℃ in the whipping process; Add fillers such as 5Kg nano aluminium oxide, high-speed stirring 15-30 minute, the control whipping temp was not higher than 25 ℃, vacuumized and removed bubble, and the control temperature is no more than 25 ℃, gets finished product C, and canned, the finished product storing temp must not be higher than 5 ℃.
Table one, the comparative analysis table of product of the present invention and each technical data of prior art
As can be seen from the above table, according to component of the present invention and the prepared product of method thereof in setting time, set time fully, volumetric shrinkage, the performance of aspect such as tensile shear strength and wet and heat ageing resistant all obviously is better than prior art, has effectively solved defective and deficiency that prior art exists.
It below only is preferred implementation of the present invention; 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 make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. a fast setting sqtructural adhesive is characterized in that, comprises following component:
2. fast setting sqtructural adhesive according to claim 1, it is characterized in that: described Resins, epoxy comprises E-51 Resins, epoxy, the mixture of one or more any ratios in E-44 Resins, epoxy or the E-20 Resins, epoxy.
3. fast setting sqtructural adhesive according to claim 1, it is characterized in that: described acrylic resin comprises urethane acrylate, polyether acrylate, the mixture of any ratio of one or more in polyester acrylate or the epoxy acrylate; Described acrylate monomer comprises methyl methacrylate, hydroxyethyl methylacrylate, Rocryl 410, (methyl) vinylformic acid tetrahydrofuran ester, (methyl) isobornyl acrylate, N, the N DMAA, polyfunctionality (methyl) acrylate, polyethyleneglycol diacrylate, the mixture of one or more any ratios in ethoxyquin bisphenol a diacrylate or (methyl) vinylformic acid.
4. fast setting sqtructural adhesive according to claim 1, it is characterized in that: described latent epoxy resin curing agent comprises the Dyhard RU 100 class, imidazoles, anhydrides, the mixture of any ratio of one or more in boron trifluoride amine or the polythiol.
5. fast setting sqtructural adhesive according to claim 1, it is characterized in that: described single-component epoxy stablizer is barbituric acid.
6. fast setting sqtructural adhesive according to claim 1; it is characterized in that: described acrylate light trigger comprises 2; 4; 6-trimethylbenzoyl-diphenyl phosphine oxide; the benzophenone of benzophenone and replacement; the methyl phenyl ketone of methyl phenyl ketone and replacement; bitter almond oil camphor and alkyl ester thereof; the xanthone of xanthone and replacement; phosphine oxide, diethoxy acetophenone, benzoin methylether; ethoxybenzoin; benzoin iso-propylether, diethoxy xanthone, chloro thio-xanthene-one; N methyldiethanol amine benzophenone, 2-hydroxy-2-methyl-1-phenyl third-1-ketone or 2-benzyl-2-(dimethylamino)-1-[4-(4-morpholinyl) phenyl]-mixture of one or more any ratios in the 1-butanone.
7. fast setting sqtructural adhesive according to claim 1, it is characterized in that: described filler comprises aerosil, calcium carbonate, the mixture of one or more any ratios in nano aluminium oxide or the shell nuclear rubber powder; Described auxiliary agent comprises silane coupling agent, defoamer, epoxy-resin systems stablizer, the mixture of any ratio of one or more in curing catalyst or the adhesion promoter.
8. the preparation method of fast setting sqtructural adhesive according to claim 1 is characterized in that, comprises the steps:
(1) acrylate resin and acrylate monomer are evenly mixed;
(2) add the acrylate light trigger, intensification is stirred to the acrylate light trigger and dissolves fully;
(3) adding Resins, epoxy, single-component epoxy stablizer and auxiliary agent successively stirs;
(4) after the cooling, add the latent epoxy curing agent, high-speed stirring is to being uniformly dispersed;
(5) add filler such as aerosil, high-speed stirring
(6) under vacuum state, remove bubble, get finished product.
9. the preparation method of fast setting sqtructural adhesive according to claim 8, it is characterized in that: the intensification temperature described in the step (2) is 30-50 ℃.
10. the preparation method of fast setting sqtructural adhesive according to claim 8, it is characterized in that: the cooling temperature described in the step (4) is below 25 ℃.
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| CN201210058488.4A CN103305132B (en) | 2012-03-06 | 2012-03-06 | Fast-curing structural adhesive and preparation method thereof |
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| CN201210058488.4A CN103305132B (en) | 2012-03-06 | 2012-03-06 | Fast-curing structural adhesive and preparation method thereof |
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| CN103305132B CN103305132B (en) | 2015-03-25 |
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Cited By (22)
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| CN104312141A (en) * | 2014-11-14 | 2015-01-28 | 南京百川行远激光科技有限公司 | Photosensitive resin and preparation method thereof |
| CN104479604A (en) * | 2014-10-30 | 2015-04-01 | 田琳琳 | Adhesive for motion floor |
| CN104559887A (en) * | 2014-12-26 | 2015-04-29 | 东莞市腾威电子材料技术有限公司 | Adhesive with ultraviolet light and moisture dual-curing function as well as preparation and application of adhesive |
| CN104893636A (en) * | 2015-05-12 | 2015-09-09 | 临沂高新区晶润电子材料有限公司 | Novel low-temperature curing glue for adhering LED and preparation method thereof |
| CN105086903A (en) * | 2015-09-03 | 2015-11-25 | 侯颖 | Preparation method of adhesive for plastic |
| CN105219329A (en) * | 2015-11-19 | 2016-01-06 | 中科院广州化学有限公司南雄材料生产基地 | A kind of low halogen type intermediate temperature setting camera module group rubber and preparation method thereof and application |
| CN106010372A (en) * | 2016-08-08 | 2016-10-12 | 安田信邦（厦门）电子科技有限公司 | Aqueous eco-friendly heat insulation glue and manufacturing method thereof |
| CN106394692A (en) * | 2016-09-22 | 2017-02-15 | 浙江吉利新能源商用车有限公司 | B column structure of automobile and manufacturing method of B column structure |
| CN108276739A (en) * | 2018-01-29 | 2018-07-13 | 哈尔滨工业大学 | A kind of shape memory polymer networks formation system and preparation method thereof of controllable light and heat two-stage reaction |
| CN108485589A (en) * | 2018-04-18 | 2018-09-04 | 东莞市新懿电子材料技术有限公司 | A kind of anti-ultraviolet UV glue and preparation method thereof |
| CN108753228A (en) * | 2018-06-15 | 2018-11-06 | 浙江航通舟新材料科技有限公司 | A kind of acrylic resin modified dual cure systems syringe needle glue of epoxy resin-and preparation method thereof |
| CN108929648A (en) * | 2018-04-24 | 2018-12-04 | 无锡光群雷射科技有限公司 | UV compound adhesive bonding agent and preparation method thereof |
| CN109219635A (en) * | 2016-05-02 | 2019-01-15 | 德莎欧洲股份公司 | Curable adhesive compound and reactive adhesive tape based thereon |
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| CN110194941A (en) * | 2019-05-29 | 2019-09-03 | 厦门艾贝森电子有限公司 | A kind of dimensionally stable resting form heating curable epoxy jelly membrane and preparation method |
| CN111073526A (en) * | 2019-12-23 | 2020-04-28 | 烟台信友新材料有限公司 | Fast-positioning two-component acrylate structural adhesive and preparation and use methods thereof |
| CN111826109A (en) * | 2020-06-22 | 2020-10-27 | 上海回天新材料有限公司 | UV-curable two-component epoxy adhesive |
| WO2022155800A1 (en) * | 2021-01-20 | 2022-07-28 | Henkel Ag & Co. Kgaa | Fast-dry pre-applied adhesive composition |
| CN115074035A (en) * | 2021-08-10 | 2022-09-20 | 河南天濮环保科技有限公司 | Curing structure adhesive film with strong adhesive force and preparation method thereof |
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| CN115975516A (en) * | 2023-01-17 | 2023-04-18 | 道生天合材料科技(上海)股份有限公司 | Composite adhesive and preparation method and use method thereof |
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| CN104479604A (en) * | 2014-10-30 | 2015-04-01 | 田琳琳 | Adhesive for motion floor |
| CN104312141A (en) * | 2014-11-14 | 2015-01-28 | 南京百川行远激光科技有限公司 | Photosensitive resin and preparation method thereof |
| CN104559887A (en) * | 2014-12-26 | 2015-04-29 | 东莞市腾威电子材料技术有限公司 | Adhesive with ultraviolet light and moisture dual-curing function as well as preparation and application of adhesive |
| CN104893636A (en) * | 2015-05-12 | 2015-09-09 | 临沂高新区晶润电子材料有限公司 | Novel low-temperature curing glue for adhering LED and preparation method thereof |
| CN105086903A (en) * | 2015-09-03 | 2015-11-25 | 侯颖 | Preparation method of adhesive for plastic |
| CN105219329A (en) * | 2015-11-19 | 2016-01-06 | 中科院广州化学有限公司南雄材料生产基地 | A kind of low halogen type intermediate temperature setting camera module group rubber and preparation method thereof and application |
| CN109219635B (en) * | 2016-05-02 | 2021-03-23 | 德莎欧洲股份公司 | Curable adhesive compound and reactive adhesive tape based thereon |
| CN109219635A (en) * | 2016-05-02 | 2019-01-15 | 德莎欧洲股份公司 | Curable adhesive compound and reactive adhesive tape based thereon |
| CN106010372A (en) * | 2016-08-08 | 2016-10-12 | 安田信邦（厦门）电子科技有限公司 | Aqueous eco-friendly heat insulation glue and manufacturing method thereof |
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| CN106394692A (en) * | 2016-09-22 | 2017-02-15 | 浙江吉利新能源商用车有限公司 | B column structure of automobile and manufacturing method of B column structure |
| US11299570B2 (en) | 2017-05-23 | 2022-04-12 | Henkel Ag & Co. Kgaa | Low-viscosity photocurable adhesive compositions |
| GB2562747B (en) * | 2017-05-23 | 2019-06-26 | Henkel IP & Holding GmbH | Low-viscosity photocurable adhesive compositions |
| CN108276739B (en) * | 2018-01-29 | 2020-09-08 | 哈尔滨工业大学 | Shape memory polymer network forming system capable of controlling heat and light two-stage reaction and preparation method thereof |
| CN108276739A (en) * | 2018-01-29 | 2018-07-13 | 哈尔滨工业大学 | A kind of shape memory polymer networks formation system and preparation method thereof of controllable light and heat two-stage reaction |
| CN108485589A (en) * | 2018-04-18 | 2018-09-04 | 东莞市新懿电子材料技术有限公司 | A kind of anti-ultraviolet UV glue and preparation method thereof |
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| CN108753228A (en) * | 2018-06-15 | 2018-11-06 | 浙江航通舟新材料科技有限公司 | A kind of acrylic resin modified dual cure systems syringe needle glue of epoxy resin-and preparation method thereof |
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| CN110194941A (en) * | 2019-05-29 | 2019-09-03 | 厦门艾贝森电子有限公司 | A kind of dimensionally stable resting form heating curable epoxy jelly membrane and preparation method |
| CN111073526A (en) * | 2019-12-23 | 2020-04-28 | 烟台信友新材料有限公司 | Fast-positioning two-component acrylate structural adhesive and preparation and use methods thereof |
| CN111826109A (en) * | 2020-06-22 | 2020-10-27 | 上海回天新材料有限公司 | UV-curable two-component epoxy adhesive |
| WO2022155800A1 (en) * | 2021-01-20 | 2022-07-28 | Henkel Ag & Co. Kgaa | Fast-dry pre-applied adhesive composition |
| CN115074035A (en) * | 2021-08-10 | 2022-09-20 | 河南天濮环保科技有限公司 | Curing structure adhesive film with strong adhesive force and preparation method thereof |
| CN115074035B (en) * | 2021-08-10 | 2024-07-19 | 河南天濮环保科技有限公司 | Cured structural adhesive film with strong adhesive force and preparation method thereof |
| CN115353843A (en) * | 2022-07-29 | 2022-11-18 | 浙江国能科技有限公司 | UV adhesive for PET plastic bonding and preparation method thereof |
| CN115975516A (en) * | 2023-01-17 | 2023-04-18 | 道生天合材料科技(上海)股份有限公司 | Composite adhesive and preparation method and use method thereof |
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