CN103305132B - Fast-curing structural adhesive and preparation method thereof - Google Patents
Fast-curing structural adhesive and preparation method thereof Download PDFInfo
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- CN103305132B CN103305132B CN201210058488.4A CN201210058488A CN103305132B CN 103305132 B CN103305132 B CN 103305132B CN 201210058488 A CN201210058488 A CN 201210058488A CN 103305132 B CN103305132 B CN 103305132B
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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 field of adhesive technology, especially a kind of fast setting sqtructural adhesive, meanwhile, the invention also discloses the preparation method of tackiness agent.
Background technology
Epoxyn has metal base bonding strength high, shrinking percentage is low, ageing-resistant performance is excellent, the plurality of advantages such as excellent electrical property, 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, low to plastic basis material bonding strength.Wherein, one-component epoxy resin adhesive needs to be heated to more than at least 80 DEG C and could solidify, and solidifying two-component epoxy resin adhesive faster also needs could locate for about at least 10 minutes.These defects and deficiency have had a strong impact on the application of epoxyn in allegro modernization industrial production.Because the component in each field such as aerospace, automobile, electronics, machinery not only comprise the metal bases such as aluminium, magnesium, stainless steel, also comprise the plastic basis material such as PC, ABS, PET, PMMA, PEI or plastic blend material.The defect of epoxyn length setting time, is difficult to adapt to modern production line balance, has a strong impact on production efficiency.
It is fast that acrylic ester adhesive has curing speed, and setting time is short, the advantage excellent to plastic basis material cementability.But have wet and heat ageing resistant poor performance, shrinking percentage is large, easily causes bond internal stress large, cause the shortcoming such as warpage, distortion.
Therefore 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 to the focus having become industry research compared with the tackiness agent of high-adhesive-strength.
Summary of the invention
In order to solve shortcomings and deficiencies of the prior art, the present invention is provided by epoxyn and acrylic ester adhesive blended can quick position, to metal, plastic basis material, there is comparatively high-adhesive-strength simultaneously, and the tackiness agent of wet and heat ageing resistant excellent property.
In order to realize foregoing invention object, the invention provides following technical scheme:
A kind of fast setting sqtructural adhesive of the present invention, comprises following component:
Wherein, described epoxy resin comprises E-51 epoxy resin, the mixture of one or more any ratios in E-44 epoxy resin or E-20 epoxy resin.
Wherein, described acrylic resin comprises urethane acrylate, polyether acrylate, the mixture of one or more any ratios in polyester acrylate or epoxy acrylate; Described acrylate monomer comprises methyl methacrylate, hydroxyethyl methylacrylate, Rocryl 410, (methyl) vinylformic acid tetrahydrofuran ester, (methyl) isobornyl acrylate, N, N DMAA, polyfunctionality (methyl) acrylate, polyethyleneglycol diacrylate, the mixture of one or more any ratios in ethoxylated bisphenol A diacrylate or (methyl) vinylformic acid.
Wherein, described latent epoxy resin curing agent comprises Dyhard RU 100 class, imidazoles, anhydrides, the mixture of one or more any ratios in borontrifluoride boron amide or polythiol.
Wherein, described single-component epoxy stablizer is barbituric acid.
Wherein, described acrylate light trigger comprises 2, 4, 6-trimethylbenzoy-dipheny 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, the mixture of one or more any ratios in 2-hydroxy-2-methyl-1-phenyl third-1-ketone or 2-benzyl-2-(dimethylamino)-1-[4-(4-morpholinyl) phenyl]-1-butanone.
Wherein, described filler comprises aerosil, calcium carbonate, the mixture of one or more any ratios in nano aluminium oxide or shell core rubber powder.Described auxiliary agent comprises silane coupling agent, defoamer, epoxy-resin systems stablizer, the mixture of one or more any ratios in curing catalyst or adhesion promoter.
Meanwhile, the invention also discloses the preparation method of above-mentioned fast setting sqtructural adhesive, comprise the steps:
(1) acrylate resin and acrylate monomer Homogeneous phase mixing even;
(2) add acrylate light trigger, intensification is stirred to acrylate light trigger and dissolves completely;
(3) add epoxy resin, single-component epoxy stablizer and auxiliary agent successively to stir;
(4), after cooling, add latent epoxy resin curing agent, high-speed stirring is to being uniformly dispersed;
(5) fillers such as aerosil are added, high-speed stirring
(6) under vacuum conditions, remove bubble, obtain finished product.
Wherein, the warming temperature described in step (2) is 30-50 DEG C.Cooling temperature described in step (4) is less than 25 DEG C.
Beneficial effect of the present invention is: the fast setting sqtructural adhesive according to component formula disclosed by the invention and preparation method thereof preparation can complete location at 5-30 under uviolizing second, and the bond behind location can move and not affect final bonding strength; Rear fast setting sqtructural adhesive completes solidification in a heated condition, and the condition be heating and curing is 80-150 DEG C, 30-120 minute.The setting time that fast setting sqtructural adhesive of the present invention efficiently solves prior art is long, defect and the deficiencies such as wet and heat ageing resistant poor performance.Fast setting sqtructural adhesive of the present invention is applicable to have at least one to be transparent substrate in two kinds of bonding base materials, and two kinds of base materials can the situation of resistance at least 80 DEG C of temperature.
Embodiment
Describe the present invention below in conjunction with specific embodiment.
Embodiment one
Get 25Kg urethane acrylate and 15Kg N, N DMAA to add in stirring tank and stir 10-30 minute, until mix; After adding 2Kg 2,4,6-trimethylbenzoy-dipheny phosphine oxide, be warming up to 40 DEG C, high-speed stirring 30-60 minute until 2,4,6-trimethylbenzoy-dipheny phosphine oxide dissolves completely; After add 35.5Kg E-51 epoxy resin successively, 1Kg barbituric acid, 0.5Kg silane coupling agent stir 10-30 minute to evenly, control whipping temp and be no more than 50 DEG C; Cool to less than 25 degrees Celsius, add 18Kg polythiol, high-speed stirring 30-60 minute, be uniformly dispersed, in whipping process, control temperature is no more than 25 DEG C; Add the fillers such as 3Kg aerosil, high-speed stirring 15-30 minute, control whipping temp not higher than 25 DEG C, vacuumize and remove bubble, control temperature is no more than 25 DEG C, obtains finished product A, canned, and finished product storing temp must not higher than 5 DEG C.
Embodiment two
Get 10Kg polyether acrylate and 30Kg (methyl) isobornyl acrylate to add in stirring tank and stir 10-30 minute, until mix; After adding the benzophenone of 5Kg benzophenone and replacement, be warming up to 30 DEG C, high-speed stirring 30-60 minute until the benzophenone of benzophenone and replacement is dissolved completely; After add 50.9KgE-44 epoxy resin successively, 0.5Kg barbituric acid, 0.1Kg epoxy-resin systems stablizer stir 10-30 minute to evenly, control whipping temp and be no more than 50 DEG C; Cool to less than 25 degrees Celsius, add the borontrifluoride boron amide of 2.5Kg, high-speed stirring 30-60 minute, is uniformly dispersed, and in whipping process, control temperature is no more than 25 DEG C; Add the fillers such as 1Kg calcium carbonate, high-speed stirring 15-30 minute, control whipping temp not higher than 25 DEG C, vacuumize and remove bubble, control temperature is no more than 25 DEG C, obtains finished product B, canned, and finished product storing temp must not higher than 5 DEG C.
Embodiment three
Get 40Kg polyester acrylate and 5Kg (methyl) vinylformic acid tetrahydrofuran ester to add in stirring tank and stir 10-30 minute, until mix; After adding 5Kg diethoxy acetophenone, be warming up to 50 DEG C, high-speed stirring 30-60 minute until diethoxy acetophenone dissolves completely; After add 36KgE-20 epoxy resin successively, 5Kg barbituric acid, 2Kg curing catalyst stir 10-30 minute to evenly, control whipping temp and be no more than 50 DEG C; Cool to less than 25 degrees Celsius, add 2Kg methylimidazole epoxy propane butyl ether affixture, high-speed stirring 30-60 minute, is uniformly dispersed, and in whipping process, control temperature is no more than 25 DEG C; Add the fillers such as 5Kg nano aluminium oxide, high-speed stirring 15-30 minute, control whipping temp not higher than 25 DEG C, vacuumize and remove bubble, control temperature is no more than 25 DEG C, obtains finished product C, canned, and finished product storing temp must not higher than 5 DEG C.
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 the product obtained by component of the present invention and method thereof in setting time, complete set time, volumetric shrinkage, the performance of the aspect such as tensile shear strength and wet and heat ageing resistant is all obviously better than prior art, effectively solves defect and the deficiency of prior art existence.
Below be only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles 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 (5)
1. a preparation method for fast setting sqtructural adhesive, is characterized in that: described tackiness agent is made up of following component,
Described single-component epoxy stablizer is barbituric acid;
Described filler comprises aerosil, calcium carbonate, the mixture of one or more any ratios in nano aluminium oxide or shell core rubber powder;
Described auxiliary agent comprises silane coupling agent, defoamer, epoxy-resin systems stablizer, the mixture of one or more any ratios in curing catalyst or adhesion promoter;
Described preparation method comprises the steps:
(1) by acrylate resin and acrylate monomer Homogeneous phase mixing even;
(2) add acrylate light trigger, intensification is stirred to acrylate light trigger and dissolves completely, and described warming temperature is 30-50 DEG C;
(3) add epoxy resin, single-component epoxy stablizer and auxiliary agent successively to stir;
(4), after cooling, add latent epoxy resin curing agent, high-speed stirring is to being uniformly dispersed, and described cooling temperature is less than 25 DEG C;
(5) described filler is added, high-speed stirring;
(6) under vacuum conditions, remove bubble, obtain finished product.
2. the preparation method of fast setting sqtructural adhesive according to claim 1, is characterized in that: described epoxy resin comprises E-51 epoxy resin, the mixture of one or more any ratios in E-44 epoxy resin or E-20 epoxy resin.
3. the preparation method of fast setting sqtructural adhesive according to claim 1, it is characterized in that: described acrylic resin comprises urethane acrylate, polyether acrylate, the mixture of one or more any ratios in polyester acrylate or epoxy acrylate; Described acrylate monomer comprises methyl methacrylate, hydroxyethyl methylacrylate, Rocryl 410, (methyl) vinylformic acid tetrahydrofuran ester, (methyl) isobornyl acrylate, the mixture of one or more any ratios in polyfunctionality (methyl) acrylate or ethoxylated bisphenol A diacrylate.
4. the preparation method of fast setting sqtructural adhesive according to claim 1, is characterized in that: described latent epoxy resin curing agent comprises Dyhard RU 100 class, the mixture of one or more any ratios in imidazoles or borontrifluoride boron amide.
5. the preparation method of fast setting sqtructural adhesive according to claim 1, is characterized in that: described acrylate light trigger is benzophenone.
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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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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| GB2562747A (en) * | 2017-05-23 | 2018-11-28 | Henkel IP & Holding GmbH | Low-viscosity photocurable adhesive compositions |
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| EP1047744B1 (en) * | 1998-01-16 | 2002-10-02 | Loctite (R & D) Limited | Curable epoxy-based compositions |
| WO2012021258A1 (en) * | 2010-08-10 | 2012-02-16 | 3M Innovative Properties Company | Epoxy structural adhesive |
| CN102127386B (en) * | 2010-12-29 | 2013-11-20 | 东莞市新懿电子材料技术有限公司 | Photocuring and thermocuring conductive adhesive and preparation method |
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| GB2562747A (en) * | 2017-05-23 | 2018-11-28 | Henkel IP & Holding GmbH | Low-viscosity photocurable adhesive compositions |
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Effective date of registration: 20200115 Address after: 200000 floor 5, building 12, No. 201, Minyi Road, Xinqiao Town, Songjiang District, Shanghai Patentee after: Taway new material technology (Shanghai) Co., Ltd Address before: 201601 Shanghai City, Jinshan District Jinshanwei town Qiushi Road No. 688 Patentee before: Shanghai UV-TECH Material Technologies Co., Ltd. |
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