CN103450835B - Epoxy resin adhesive and preparation method thereof - Google Patents
Epoxy resin adhesive and preparation method thereof Download PDFInfo
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Abstract
The invention provides an epoxy resin adhesive comprising a component A and a component B. The component A comprises 70-85 parts by weight of bisphenol A epoxy resin, 15-30 parts by weight of toughness modified bisphenol A epoxy resin and 20-40 parts by weight of a first filler; and the component B comprises 40-70 parts by weight of a polymercaptan curing agent, 30-60 parts by weight of a modified amine curing agent and 15-30 parts by weight of a second filler. According to the two-component epoxy resin adhesive provided by the invention, introduction of the toughness modified bisphenol A epoxy resin into the component A and compound of the modified amine curing agent and polymercaptan curing agent in the component B improve toughness of the epoxy resin adhesive, and the epoxy resin adhesive can be quickly cured at room temperature.
Description
Technical field
The present invention relates to field of adhesive technology, particularly relate to a kind of epoxyn and preparation method thereof.
Background technology
Along with the aggravation of environmental pollution, environmental problem is subject to increasing attention, and traditional fossil energy can not meet the growing energy demand of people.Along with the development of science and technology, photovoltaic industry instead of the partial function of fossil energy gradually.Maximum raw materials is adopted to be polysilicon chip and monocrystalline silicon piece in photovoltaic industry.And the cutting of monocrystalline silicon piece and polysilicon chip, to produce be an important link in whole industrial chain.Crystal silicon chip is in cutting process, and need the fixing brilliant holder of tackiness agent and glass, glass and crystal bar, therefore tackiness agent is crystal silicon chip indispensable auxiliary material in cutting process.In order to not affect working efficiency, needing the intensity reached within the time short as far as possible during tackiness agent self-vulcanizing needed for cutting, then having higher performance requriements to the tackiness agent being applied to bonding crystal bar and glass.
At present, the tackiness agent being applied to photovoltaic industry is mainly epoxy resin solidifying system, and epoxy resin solidifying system forms primarily of epoxy resin, solidifying agent and subsidiary material.Epoxy resin is the general name of the macromolecular compound containing two or more epoxide group in a molecule, and it can not be used alone, and only has and could become thermosetting resin by curing cross-linked with after solidifying agent mixing, play cohesive action.The System Curing At Room Temperature that epoxy resin solidifying system is comparatively commonly used has the system of epoxy resin and aliphatic polyamine and the system of epoxy resin and polymeric amide.The system of epoxy resin and aliphatic polyamine, product poor toughness, during operation, toxicity is comparatively large, and pungency is strong; Although and the system good toughness of epoxy resin and polymeric amide, toxicity is also lower, and gel time is relatively long, and under the condition of 25 DEG C, gel time reaches 5h, and usually solidification just can reach certain solidification intensity after 7 days.For the present situation of cold curing adhesive, contriver considers a kind of novel room temperature curing epoxy adhesive.
Summary of the invention
The technical problem that the present invention solves is to provide one to have higher toughness and the fireballing epoxyn of self-vulcanizing.
In view of this, the invention provides a kind of epoxyn, comprise component A and B component, described component A comprises: the bisphenol A type epoxy resin of 70 ~ 85 weight parts, the toughness modified bisphenol A type epoxy resin of 15 ~ 30 weight parts, the first filler of 20 ~ 40 weight parts; Described B component comprises: the polythiol class solidifying agent of 40 ~ 70 weight parts, the modified amine curing agent of 30 ~ 60 weight parts, the second filler of 15 ~ 30 weight parts.
Preferably, described B component also comprises: the thixotropic agent of 0.5 ~ 3 weight part, the coupling agent of 1 ~ 3 weight part, or the pigment of 0.05 ~ 0.2 weight part.
Preferably, described bisphenol A type epoxy resin is one or more in E51 epoxy resin, E44 epoxy resin, 128 epoxy resin and 127 epoxy resin.
Preferably, described toughness modified bisphenol A type epoxy resin is liquid nitrile rubber modified bisphenol A type epoxy resin or thiorubber modified bisphenol A type epoxy resin.
Preferably, described first filler is titanium dioxide, silicon powder, aluminum oxide powder, magnesia powder, aluminium hydrate powder or calcium carbonate.
Preferably, described polythiol class solidifying agent is the polythiol class solidifying agent through taste masking process.
Preferably, described thixotropic agent is hydrophobic fumed silica or hydrogenated castor oil.
Preferably, described coupling agent is silane coupling agent.
Preferably, described second filler is titanium dioxide, silicon powder, aluminum oxide powder, magnesia powder, aluminium hydrate powder or calcium carbonate.
Present invention also offers a kind of preparation method of epoxyn, comprise the following steps:
A) by the toughness modified bisphenol A type epoxy resin of the bisphenol A type epoxy resin of 70 ~ 85 weight parts and 15 ~ 30 weight parts, under the rate of dispersion of the stirring velocitys of 50 ~ 80 revs/min and 500 ~ 800 revs/min, dispersed with stirring 5 ~ 20min, then the first filler of 20 ~ 40 weight parts is added, dispersed with stirring 10 ~ 30min under the rate of dispersion of the stirring velocitys of 50 ~ 80 revs/min and 700 ~ 1000 revs/min, under the stirring velocity of 10 ~ 30 revs/min, stir 3 ~ 5min, obtain component A;
B) by the polythiol class solidifying agent of 40 ~ 70 weight parts and the modified amine curing agent of 30 ~ 60 weight parts, under the rate of dispersion of the stirring velocitys of 50 ~ 80 revs/min and 100 ~ 300 revs/min, dispersed with stirring 5 ~ 20min, then the second filler of 15 ~ 30 weight parts is added, dispersed with stirring 20 ~ 40min under the rate of dispersion of the stirring velocitys of 50 ~ 80 revs/min and 1000 ~ 1800 revs/min, under the stirring velocity of 10 ~ 30 revs/min, stir 3 ~ 5min, obtain B component;
C) described component A and described B component are uniformly mixed, obtain epoxyn;
The not successively restriction of described step a) and step b) order.
Compared with prior art, the invention provides a kind of epoxyn, comprise component A and B component, above-mentioned epoxyn introduces toughness modified bisphenol A type epoxy resin in component A, toughness modified bisphenol A type epoxy resin is when epoxy adhesive cures, play toughening effect, improve the toughness of tackiness agent; Polythiol class solidifying agent in B component, during solidification, thermal discharge is large, but self-vulcanizing speed is fast, and modified amine curing agent can at room temperature solidify, but the time of primary solidification is slower, therefore select modified amine curing agent and polythiol class solidifying agent to carry out composite, make tackiness agent at room temperature fast setting, and reduce the thermal discharge produced when being used alone Polymercaptan curing agent.Two-component epoxy resin adhesive provided by the invention, by introducing toughness modified bisphenol A type epoxy resin in component A, in B component, modified amine curing agent and polythiol class solidifying agent is composite, the toughness of the epoxyn of raising, and at room temperature can fast setting.
Embodiment
In order to understand the present invention further, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these describe just for further illustrating the features and advantages of the present invention, instead of limiting to the claimed invention.
The embodiment of the invention discloses a kind of epoxyn, comprise component A and B component, described component A comprises: the bisphenol A type epoxy resin of 70 ~ 85 weight parts, the toughness modified bisphenol A type epoxy resin of 15 ~ 30 weight parts, the first filler of 20 ~ 40 weight parts; Described B component comprises: the polythiol class solidifying agent of 40 ~ 70 weight parts, the modified amine curing agent of 30 ~ 60 weight parts, the second filler of 15 ~ 30 weight parts.
Bisphenol A type epoxy resin described in component A is preferably one or more in E51 epoxy resin, E44 epoxy resin, 128 epoxy resin and 127 epoxy resin.Described toughness modified bisphenol A type epoxy resin is preferably liquid nitrile rubber modified bisphenol A type epoxy resin or polythiol rubber bisphenol A type epoxy resin, is more preferably liquid nitrile rubber modified bisphenol A type epoxy resin.Respond the end carboxyl liquid nitrile rubber (CTBN) of active group in liquid nitrile rubber, there is active function groups carboxyl at CTBN molecular chain two ends, at high temperature can with epoxy reaction, rubber flexible segment is introduced in cross linking of epoxy resin structure, thus make modified bisphenol A type epoxy resin roughening, there is good toughness.Described first filler is preferably the filler of powder class, and described first filler is preferably titanium dioxide, silicon powder, aluminum oxide powder, magnesia powder, aluminium hydrate powder or calcium carbonate, is more preferably titanium dioxide.In described component A, bisphenol A type epoxy resin is 70 ~ 85 weight parts, be preferably 75 ~ 80 weight parts, described toughness modified bisphenol A type epoxy resin is 15 ~ 30 weight parts, is preferably 20 ~ 25 weight parts, described first filler is 20 ~ 40 weight parts, is preferably 25 ~ 35 weight parts.
Polythiol in B component be a kind of can the solidifying agent of cured epoxy resin at low temperatures, polythiol has larger irritating smell, and the present invention preferably adopts the Polymercaptan curing agent by taste masking process, with meet the requirement of environmental protection.Aliphatic modified amine curing agent, smell is low, also can at room temperature cured epoxy resin, but in adhesive cures process, the time of primary solidification is slower.Therefore have employed polythiol in B component and modified amine is carried out composite, when solidifying agent is mixed with epoxy resin, can room temperature fast-curing be realized.Described second filler is preferably the filler of powder class, and described second filler is preferably titanium dioxide, silicon powder, aluminum oxide powder, magnesia powder, aluminium hydrate powder or calcium carbonate, is more preferably silicon powder.In described B component, polythiol class solidifying agent is 40 ~ 70 weight parts, and be preferably 50 ~ 60 weight parts, described modified amine curing agent is 30 ~ 60 weight parts, and be preferably 40 ~ 50 weight parts, described second filler is 15 ~ 30 weight parts, is preferably 20 ~ 25 weight parts.
Preferably, the pigment of the thixotropic agent of 0.5 ~ 3 weight part, the coupling agent of 1 ~ 3 weight part or 0.05 ~ 0.2 weight part is also comprised in B component, described thixotropic agent is preferably 1 ~ 2 weight part, and described coupling agent is preferably 2 ~ 2.5 weight parts, and described pigment optimization is 0.1 ~ 0.15 weight part.Described thixotropic agent makes binder component have certain mobility, and can keep certain form when solidifying, also can solve the problem of filling settlement in the epoxyn shelf lives, described thixotropic agent is preferably hydrophobic fumed silica or hydrogenated castor oil.Described coupling agent makes organic phase, mineral filler and can more firmly be bonded together between framework material surface and contacted organic phase, makes epoxyn have better cohesive strength.Described coupling agent is preferably silane coupling agent, is more preferably KH550 and KH560.For ensureing A, B component are easy to distinguish whether mix, preferably add pigment in B component when mixing, and described pigment optimization is titanium ultramarine.
Raw material needed for epoxyn provided by the invention is commercially available.Preparation method the present invention of component A and B component is not particularly limited, as long as ensure that component A and B component can fully mix, component A specifically can be prepared by the following method: by the toughness modified bisphenol A type epoxy resin of the bisphenol A type epoxy resin of 70 ~ 85 weight parts and 15 ~ 30 weight parts, dispersed with stirring 5 ~ 20min under the rate of dispersion of the stirring velocitys of 50 ~ 80 revs/min and 500 ~ 800 revs/min, then the first filler of 20 ~ 40 weight parts is added, dispersed with stirring 10 ~ 30min under the rate of dispersion of the stirring velocitys of 50 ~ 80 revs/min and 700 ~ 1000 revs/min, vacuumize limit below the stirring velocitys of 10 ~ 30 revs/min and stir 3 ~ 5min, obtain component A.
B component specifically can be prepared by the following method: by the polythiol class solidifying agent of 40 ~ 70 weight parts and the modified amine curing agent of 30 ~ 60 weight parts, under the rate of dispersion of the stirring velocitys of 50 ~ 80 revs/min and 100 ~ 300 revs/min, dispersed with stirring 5 ~ 20min, then the second filler of 15 ~ 30 weight parts is added, dispersed with stirring 20 ~ 40min under the rate of dispersion of the stirring velocitys of 50 ~ 80 revs/min and 1000 ~ 1800 revs/min, under the stirring velocity of 10 ~ 30 revs/min, stir 3 ~ 5min, obtain B component.Component A and B component have been prepared and to have been stored respectively afterwards, before epoxyn uses, mixed by component A, namely obtain epoxyn with B component.Preparation component A and the condition optimization of B component are room temperature or 40 ~ 70 DEG C.The temperature that said components A mixes with B component is preferably 20 ~ 26 DEG C.Mass ratio when component A mixes with B component is preferably 1:0.9 ~ 1.2.Tackiness agent outward appearance provided by the invention is thick slurry, not containing any volatile solvent.At room temperature viscosity is at 40000 ~ 120000cps.
In order to understand the present invention further, describe in detail to epoxyn provided by the invention below in conjunction with embodiment, protection scope of the present invention is not limited by the following examples.
Embodiment 1
Component A: bisphenol A type epoxy resin: 80 weight parts, nbr carboxyl terminal modified bisphenol A type epoxy resin: 20 weight parts, titanium dioxide: 30 weight parts;
B component: Polymercaptan curing agent (the 3380s polythiol that Shenzhen Jia Dida provides): 70 weight parts, modified amine curing agent (5408 modified amine curing agents that Shenzhen Jia Dida provides): 30 weight parts, hydrophobic fumed silica: 2 weight parts, KH-550:3 weight part, silicon powder: 30 weight parts, phthalocyanine blue: 0.1 weight part;
Take 128 resin 1600g by weight, nbr carboxyl terminal modified epoxy 400g adds in the blending apparatus with vacuum unit, stir with the intensification limit, stirring velocity limit of 60 revs/min, after being warming up to 60 DEG C, open dispersion, vacuumize limit dispersed with stirring 15min below at the rate of dispersion of the stirring velocitys of 60 revs/min and 800 revs/min.Machine is out of service, 600g titanium dioxide is added in material, under the rotating speed of 15 revs/min, powder is soaked, then dispersed with stirring 30min under the rate of dispersion of the stirring velocity of mixing speed to 60 rev/min and 1000 revs/min is adjusted, finally, vacuumize limit below the stirring velocitys of 20 revs/min and stir 5min, then encapsulation is preserved and is namely obtained component A.
Take 3380s Polymercaptan curing agent 1400g by weight, 5408 modified amine curing agent 600g, KH550 silane coupling agent 60g adds in the blending apparatus with vacuum unit, under the condition of 45 DEG C, vacuumizes while stir 20min with the stirring velocity of 60 revs/min.Machine is out of service, 40g aerosil is added in material, 2g phthalocyanine blue pigment, 600g silicon powder, under the rotating speed of 15 revs/min, powder is soaked, then adjust dispersed with stirring 30min under the rate of dispersion of the stirring velocity of mixing speed to 60 rev/min and 1200 revs/min, finally, vacuumize limit below the stirring velocitys of 20 revs/min and stir 5min, then encapsulation is preserved and is namely obtained B component.
During use, above-mentioned component A and B component are at room temperature mixed can use with the ratio of mass ratio 1:1.Mixing 30g, operable time is 5 ~ 6min, and bonding steel-steel print, tests with universal testing machine, self-vulcanizing 8h, and shearing resistance can reach 19MPa, and tensile strength can reach 20MPa.
Embodiment 2
Component A: bisphenol A type epoxy resin: 70 weight parts, nbr carboxyl terminal modified bisphenol A type epoxy resin: 15 weight parts, titanium dioxide: 20 weight parts;
B component: Polymercaptan curing agent (the 3380s polythiol that Shenzhen Jia Dida provides): 40 weight parts, modified amine curing agent (5408 modified amine curing agents that Shenzhen Jia Dida provides): 60 weight parts, hydrophobic fumed silica: 3 weight parts, KH-560:1 weight part, silicon powder: 15 weight parts, phthalocyanine blue: 0.05 weight part;
Take E44 resin 1400g by weight, nbr carboxyl terminal modified epoxy 300g adds in the blending apparatus with vacuum unit, stir with the intensification limit, stirring velocity limit of 50 revs/min, after being warming up to 70 DEG C, open dispersion, vacuumize limit dispersed with stirring 10min below at the rate of dispersion of the stirring velocitys of 50 revs/min and 500 revs/min.Machine is out of service, 400g titanium dioxide is added in material, under the rotating speed of 10 revs/min, powder is soaked, then dispersed with stirring 10min under the rate of dispersion of the stirring velocity of mixing speed to 50 rev/min and 700 revs/min is adjusted, finally, vacuumize limit below the stirring velocitys of 10 revs/min and stir 3min, then encapsulation is preserved and is namely obtained component A.
Take 3380s Polymercaptan curing agent 800g by weight, 5408 modified amine curing agent 1200g, KH-560 silane coupling agent 20g adds in the blending apparatus with vacuum unit, under the condition of 40 DEG C, vacuumizes while stir 10min with the stirring velocity of 50 revs/min.Machine is out of service, 60g aerosil is added in material, 1g phthalocyanine blue pigment, 300g silicon powder, under the rotating speed of 15 revs/min, powder is soaked, then adjust dispersed with stirring 20min under the rate of dispersion of the stirring velocity of mixing speed to 50 rev/min and 1000 revs/min, finally, vacuumize limit below the stirring velocitys of 10 revs/min and stir 5min, then encapsulation is preserved and is namely obtained B component.
During use, above-mentioned component A and B component are at room temperature mixed can use with the ratio of mass ratio 1:0.9.Mixing 30g, operable time is 9 ~ 11min, and bonding steel-steel print, tests with universal testing machine, self-vulcanizing 6h, and shearing resistance can reach 19MPa, and tensile strength can reach 20MPa.
Embodiment 3
Component A: bisphenol A type epoxy resin: 85 weight parts, nbr carboxyl terminal modified bisphenol A type epoxy resin: 30 weight parts, titanium dioxide: 40 weight parts;
B component: Polymercaptan curing agent (the 3380s polythiol that Shenzhen Jia Dida provides): 60 weight parts, modified amine curing agent (5408 modified amine curing agents that Shenzhen Jia Dida provides): 40 weight parts, hydrophobic fumed silica: 0.5 weight part, KH-560:2 weight part, silicon powder: 20 weight parts, phthalocyanine blue: 0.2 weight part;
Take E51 resin 1700g by weight, nbr carboxyl terminal modified epoxy 600g adds in the blending apparatus with vacuum unit, stir with the intensification limit, stirring velocity limit of 80 revs/min, after being warming up to 50 DEG C, open dispersion, vacuumize limit dispersed with stirring 20min below at the rate of dispersion of the stirring velocitys of 80 revs/min and 600 revs/min.Machine is out of service, 800g titanium dioxide is added in material, under the rotating speed of 15 revs/min, powder is soaked, then dispersed with stirring 20min under the rate of dispersion of the stirring velocity of mixing speed to 80 rev/min and 800 revs/min is adjusted, finally, vacuumize limit below the stirring velocitys of 30 revs/min and stir 4min, then encapsulation is preserved and is namely obtained component A.
Take 3380s Polymercaptan curing agent 1200g by weight, 5408 modified amine curing agent 800g, KH-560 silane coupling agent 10g adds in the blending apparatus with vacuum unit, under the condition of 60 DEG C, vacuumizes while stir 5min with the stirring velocity of 80 revs/min.Machine is out of service, 40g aerosil is added in material, 4g phthalocyanine blue pigment, 400g silicon powder, under the rotating speed of 20 revs/min, powder is soaked, then adjust dispersed with stirring 40min under the rate of dispersion of the stirring velocity of mixing speed to 80 rev/min and 1800 revs/min, finally, vacuumize limit below the stirring velocitys of 30 revs/min and stir 5min, then encapsulation is preserved and is namely obtained B component.
During use, above-mentioned component A and B component are at room temperature mixed can use with the ratio of mass ratio 1:1.2.Mixing 30g, operable time is 7 ~ 8min, and bonding steel-steel print, tests with universal testing machine, self-vulcanizing 6h, and shearing resistance can reach 21MPa, and tensile strength can reach 20MPa.
The explanation of above embodiment just understands method of the present invention and core concept thereof for helping.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 carry out some improvement and modification to the present invention, these improve and modify and also fall in the protection domain of the claims in the present invention.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (10)
1. an epoxyn, is characterized in that, comprises component A and B component, and described component A comprises: the bisphenol A type epoxy resin of 70 ~ 85 weight parts, the toughness modified bisphenol A type epoxy resin of 15 ~ 30 weight parts, the first filler of 20 ~ 40 weight parts; Described B component comprises: the polythiol class solidifying agent of 40 ~ 70 weight parts, the modified amine curing agent of 30 ~ 60 weight parts, the second filler of 15 ~ 30 weight parts; Described modified amine curing agent is 5408 modified amine curing agents.
2. epoxyn according to claim 1, is characterized in that, described B component also comprises: the thixotropic agent of 0.5 ~ 3 weight part, the coupling agent of 1 ~ 3 weight part, or the pigment of 0.05 ~ 0.2 weight part.
3. epoxyn according to claim 1, is characterized in that, described bisphenol A type epoxy resin is one or more in E51 epoxy resin, E44 epoxy resin, 128 epoxy resin and 127 epoxy resin.
4. epoxyn according to claim 1, is characterized in that, described toughness modified bisphenol A type epoxy resin is liquid nitrile rubber modified bisphenol A type epoxy resin or thiorubber modified bisphenol A type epoxy resin.
5. epoxyn according to claim 1, is characterized in that, described first filler is titanium dioxide, silicon powder, aluminum oxide powder, magnesia powder, aluminium hydrate powder or calcium carbonate.
6. epoxyn according to claim 1, is characterized in that, described polythiol class solidifying agent is the polythiol class solidifying agent through taste masking process.
7. epoxyn according to claim 2, is characterized in that, described thixotropic agent is hydrophobic fumed silica or hydrogenated castor oil.
8. epoxyn according to claim 2, is characterized in that, described coupling agent is silane coupling agent.
9. epoxyn according to claim 1, is characterized in that, described second filler is titanium dioxide, silicon powder, aluminum oxide powder, magnesia powder, aluminium hydrate powder or calcium carbonate.
10. a preparation method for epoxyn, is characterized in that, comprises the following steps:
A) by the toughness modified bisphenol A type epoxy resin of the bisphenol A type epoxy resin of 70 ~ 85 weight parts and 15 ~ 30 weight parts, under the rate of dispersion of the stirring velocitys of 50 ~ 80 revs/min and 500 ~ 800 revs/min, dispersed with stirring 5 ~ 20min, then the first filler of 20 ~ 40 weight parts is added, dispersed with stirring 10 ~ 30min under the rate of dispersion of the stirring velocitys of 50 ~ 80 revs/min and 700 ~ 1000 revs/min, under the stirring velocity of 10 ~ 30 revs/min, stir 3 ~ 5min, obtain component A;
B) by the polythiol class solidifying agent of 40 ~ 70 weight parts and the modified amine curing agent of 30 ~ 60 weight parts, under the rate of dispersion of the stirring velocitys of 50 ~ 80 revs/min and 100 ~ 300 revs/min, dispersed with stirring 5 ~ 20min, then the second filler of 15 ~ 30 weight parts is added, dispersed with stirring 20 ~ 40min under the rate of dispersion of the stirring velocitys of 50 ~ 80 revs/min and 1000 ~ 1800 revs/min, under the stirring velocity of 10 ~ 30 revs/min, stir 3 ~ 5min, obtain B component;
C) described component A and described B component are uniformly mixed, obtain epoxyn;
Described step a) and step b) order not successively restriction;
Described modified amine curing agent is 5408 modified amine curing agents.
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| CN1546590A (en) * | 2003-12-04 | 2004-11-17 | 四川大学 | Preparation method of room temperature cured high temperature tolerant flexible epoxy adhesive |
| CN101818037A (en) * | 2009-02-27 | 2010-09-01 | 汉高（中国）投资有限公司 | Room-temperature curing epoxy structural adhesive composition and preparation method thereof |
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