CN103265925B - High-durability epoxy resin adhesive and preparation method thereof - Google Patents
High-durability epoxy resin adhesive and preparation method thereof Download PDFInfo
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- CN103265925B CN103265925B CN201310206338.8A CN201310206338A CN103265925B CN 103265925 B CN103265925 B CN 103265925B CN 201310206338 A CN201310206338 A CN 201310206338A CN 103265925 B CN103265925 B CN 103265925B
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Abstract
The invention relates to an epoxy resin and a preparation method thereof, and in particular relates to a high-durability modified epoxy resin and a preparation method thereof, aiming at solving the problems that an existing epoxy resin adhesive for bonding metal and nonmetal, which are not subjected to strict surface treatment, is poor in adhesive property and durability. The high-durability modified epoxy resin is prepared from epoxy resin, carboxyl nitrile butadiene rubber latex and polyacrylate rubber latex. The preparation method comprises the following steps of: firstly, carrying out demulsification on the carboxyl nitrile butadiene rubber latex, drying, and adding the dried carboxyl nitrile butadiene rubber latex into the epoxy resin for reaction; and after the reaction, carrying out demulsification on the polyacrylate rubber latex, drying, and adding the dried polyacrylate rubber latex into the epoxy resin for reaction to obtain the high-durability modified epoxy resin. When the high-durability epoxy resin adhesive is used for bonding LY2CZ aluminium alloy polished by abrasive paper, the shear strength of the bonded aluminium alloy subjected to hygrothermal aging at 55 DEG C and with relative humidity (RH) of 98%-100% for 1000h can reach 22.11MPa, and the shear strength of the bonded aluminium alloy subjected to salt mist aging at 90 DEG C for 300h can reach 22.13MPa. The high-durability epoxy resin adhesive is good in durability, and the preparation method is simple and is applied to the field of adhesives.
Description
Technical field
The present invention relates to epoxy resin and preparation method thereof.
Background technology
Current high-performance modified epoxy resin adhesive is bonding through strict surface-treated metal with nonmetally all have good bonding strength and an endurance quality, but bonding is without strict surface-treated metal and nonmetal, not only bonding strength is low, and endurance quality is poor.
Polyurethane-modified E51 epoxy resin is matrix resin, sizing agent prepared by 200# polyamide curing agent, there is good bonding intensity and endurance quality, the LY2CZ aluminium alloy that bonding phosphoric acid is processed, normal temperature shearing resistance can reach 43MPa, 55 degree RH98-100% hydrothermal agings 1000 hours and the shearing resistance of 90 degree salt fogs after aging 300 hours still can remain unchanged, even also increase, and excellent in durability.But the LY2CZ that bonding sand papering is processed, normal temperature shearing resistance only has 20.21MPa, and the shearing resistance of 55 degree RH98-100% hydrothermal agings after 1000 hours only has 7.43MPa, and the shearing resistance of 90 degree salt fogs after aging 300 hours only has 4.13MPa.
And another conventional high-performance epoxy resin sizing agent: CTBN modification E51 epoxy resin is matrix resin, sizing agent prepared by 200# polyamide curing agent, also there is good bonding intensity and endurance quality, the LY2CZ aluminium alloy that bonding phosphoric acid is processed, normal temperature shearing resistance can reach 37MPa, the adhesive property that 55 degree RH98-100% hydrothermal agings 1000 hours are compared under normal temperature with the shearing resistance of 90 degree salt fogs after aging 300 hours also increases, excellent in durability.But the LY2CZ that bonding sand papering is processed, normal temperature shearing resistance only has 19.23MPa, and 55 degree RH98-100% hydrothermal agings 1000 hours and the shearing resistance of 90 degree salt fogs after aging 300 hours are almost nil.
At present domestic also do not have a kind of sizing agent for without strict surface-treated metal with nonmetally have good bonding intensity and an endurance quality.
Summary of the invention
The present invention for solve with existing bonding without strict surface-treated metal and nonmetallic epoxy resin adhesive adhesiveproperties poor with the poor problem of endurance quality, and provide a kind of high-durability energy modified epoxy and preparation method thereof.
A kind of high-durability energy epoxy resin adhesive of the present invention is made by the epoxy resin of 90～110 parts, 3.75～22.5 parts of carboxyl butadiene acrylonitrile rubber breasts and 1.25～7.5 parts of polyacrylic ester latexs by mass fraction; And described carboxyl butadiene acrylonitrile rubber breast is 3:1 with the mass ratio of polyacrylic ester latex.
The preparation method of a kind of high-durability energy epoxy resin adhesive of the present invention carries out according to the following steps:
One, by mass fraction, take the epoxy resin of 90～110 parts, 3.75～22.5 parts of carboxyl butadiene acrylonitrile rubber breasts and 1.25～7.5 parts of polyacrylic ester latexs, wherein said carboxyl butadiene acrylonitrile rubber breast is 3:1 with the mass ratio of polyacrylic ester latex;
Two,, after carboxyl butadiene acrylonitrile rubber breast breakdown of emulsion step 1 being taken, dry, standby;
Three,, after polyacrylic ester latex breakdown of emulsion step 1 being taken, dry, standby;
Four, the carboxyl butadiene acrylonitrile rubber breast after step 2 is joined in the epoxy resin that step 1 takes, in temperature, be to react 1h～3h under the condition of 110～130 ℃, add again the polyacrylic ester latex after step 3, in temperature, be to react 0.5h～1.5h under the condition of 110～130 ℃, obtain under normal temperature is the modified epoxy of thick liquid, i.e. high-durability energy epoxy resin adhesive.
Method of the present invention is by rationally controlling the proportioning between each reactant, rationally control reaction conditions and prepare a kind of high-durability energy epoxy resin adhesive, after solidifying as solidifying agent by 200# polymeric amide, after the LY2CZ aluminium alloy that bonding sand papering is processed, carry out the detection of shearing resistance, obtaining high-durability energy epoxy resin adhesive normal temperature down cut intensity of the present invention is 18.32MPa～22.23MPa, the shearing resistance of 55 degree RH98-100% hydrothermal agings after 1000 hours is 18.11MPa～22.11MPa, the shearing resistance of 90 degree salt fogs after aging 300 hours is 17.87MPa～22.13MPa, adhesiveproperties is good, excellent in durability, and preparation method is simple, be applicable to suitability for industrialized production, compared with other epoxy resin adhesives, compare, bonding without strict surface-treated metal with nonmetally all there is good adhesiveproperties and endurance quality, can be applicable to sizing agent field.
Embodiment
Embodiment one: a kind of high-durability energy epoxy resin adhesive of present embodiment is made by the epoxy resin of 90～110 parts, 3.75～22.5 parts of carboxyl butadiene acrylonitrile rubber breasts and 1.25～7.5 parts of polyacrylic ester latexs by mass fraction; And described carboxyl butadiene acrylonitrile rubber breast is 3:1 with the mass ratio of polyacrylic ester latex.
A kind of high-durability energy epoxy resin adhesive of present embodiment, after solidifying as solidifying agent by 200# polymeric amide, after the LY2CZ aluminium alloy that bonding sand papering is processed, carry out the detection of shearing resistance, obtaining high-durability energy epoxy resin adhesive normal temperature down cut intensity of the present invention is 18.32MPa～22.23MPa, the shearing resistance of 55 degree RH98-100% hydrothermal agings after 1000 hours is 18.11MPa～22.11MPa, the shearing resistance of 90 degree salt fogs after aging 300 hours is 17.87MPa～22.13MPa, adhesiveproperties is good, excellent in durability, compared with other epoxy resin adhesives, compare, bonding without strict surface-treated metal with nonmetally all there is good adhesiveproperties and endurance quality, can be applicable to sizing agent field.
Embodiment two: present embodiment is different from embodiment one: a kind of high-durability energy epoxy resin adhesive is made by the epoxy resin of 100 parts, 15 parts of carboxyl butadiene acrylonitrile rubber breasts and 5 parts of polyacrylic ester latexs by mass fraction.Other step and parameter are identical with embodiment one.
Embodiment three: the preparation method of a kind of high-durability energy epoxy resin adhesive of present embodiment carries out according to the following steps:
One, by mass fraction, take the epoxy resin of 90～110 parts, 3.75～22.5 parts of carboxyl butadiene acrylonitrile rubber breasts and 1.25～7.5 parts of polyacrylic ester latexs, wherein said carboxyl butadiene acrylonitrile rubber breast is 3:1 with the mass ratio of polyacrylic ester latex;
Two,, after carboxyl butadiene acrylonitrile rubber breast breakdown of emulsion step 1 being taken, dry, standby;
Three,, after polyacrylic ester latex breakdown of emulsion step 1 being taken, dry, standby;
Four, the carboxyl butadiene acrylonitrile rubber breast after step 2 is joined in the epoxy resin that step 1 takes, in temperature, be to react 1h～3h under the condition of 110～130 ℃, add again the polyacrylic ester latex after step 3, in temperature, be to react 0.5h～1.5h under the condition of 110～130 ℃, obtain under normal temperature is the modified epoxy of thick liquid, i.e. high-durability energy epoxy resin adhesive.
The method of present embodiment is by rationally controlling the proportioning between each reactant, rationally control reaction conditions and prepare a kind of high-durability energy epoxy resin adhesive, after solidifying as solidifying agent by 200# polymeric amide, after the LY2CZ aluminium alloy that bonding sand papering is processed, carry out the detection of shearing resistance, obtaining high-durability energy epoxy resin adhesive normal temperature down cut intensity of the present invention is 18.32MPa～22.23MPa, the shearing resistance of 55 degree RH98-100% hydrothermal agings after 1000 hours is 18.11MPa～22.11MPa, the shearing resistance of 90 degree salt fogs after aging 300 hours is 17.87MPa～22.13MPa, adhesiveproperties is good, excellent in durability, and preparation method is simple, be applicable to suitability for industrialized production, compared with other epoxy resin adhesives, compare, bonding without strict surface-treated metal with nonmetally all there is good adhesiveproperties and endurance quality, can be applicable to sizing agent field.
Embodiment four: present embodiment is different from embodiment three: take the epoxy resin of 100 parts, 15 parts of carboxyl butadiene acrylonitrile rubber breasts and 5 parts of polyacrylic ester latexs by mass fraction in step 1.Other step and parameter are identical with embodiment three.
Embodiment five: present embodiment is different from embodiment three or four: the carboxyl butadiene acrylonitrile rubber breast after step 2 joins in the epoxy resin that step 1 takes is to react 2h under the condition of 120 ℃ in temperature.Other step and parameter are identical with embodiment three or four.
Embodiment six: present embodiment is different from one of embodiment three to five: adding the polyacrylic ester latex after step 3 in step 4, is to react 1h under the condition of 120 ℃ in temperature again.Other step and parameter are identical with one of embodiment three to five.
Embodiment 1: a kind of preparation method of high-durability energy epoxy resin adhesive carries out according to the following steps:
One, by mass fraction, take the epoxy resin of 100 parts, 3.75 parts of carboxyl butadiene acrylonitrile rubber breasts and 1.25 parts of polyacrylic ester latexs;
Two,, after carboxyl butadiene acrylonitrile rubber breast breakdown of emulsion step 1 being taken, dry, standby;
Three,, after polyacrylic ester latex breakdown of emulsion step 1 being taken, dry, standby;
Four, the carboxyl butadiene acrylonitrile rubber breast after step 2 is joined in the epoxy resin that step 1 takes, in temperature, be to react 2h under the condition of 120 ℃, add again the polyacrylic ester latex after step 3, in temperature, be to react 1h under the condition of 120 ℃, obtain under normal temperature is the modified epoxy of thick liquid, i.e. high-durability energy epoxy resin adhesive.
Epoxy resin in the present embodiment, carboxyl butadiene acrylonitrile rubber breast and polyacrylic ester latex are commercially available prod.
Embodiment 2: a kind of preparation method of high-durability energy epoxy resin adhesive carries out according to the following steps:
One, by mass fraction, take 7.5 parts of carboxyl butadiene acrylonitrile rubber breasts of epoxy resin and 2.5 parts of polyacrylic ester latexs of 100 parts;
Two,, after carboxyl butadiene acrylonitrile rubber breast breakdown of emulsion step 1 being taken, dry, standby;
Three,, after polyacrylic ester latex breakdown of emulsion step 1 being taken, dry, standby;
Four, the carboxyl butadiene acrylonitrile rubber breast after step 2 is joined in the epoxy resin that step 1 takes, in temperature, be to react 2h under the condition of 120 ℃, add again the polyacrylic ester latex after step 3, in temperature, be to react 1h under the condition of 120 ℃, obtain under normal temperature is the modified epoxy of thick liquid, i.e. high-durability energy epoxy resin adhesive.
Epoxy resin in the present embodiment, carboxyl butadiene acrylonitrile rubber breast and polyacrylic ester latex are commercially available prod.
Embodiment 3: a kind of preparation method of high-durability energy epoxy resin adhesive carries out according to the following steps:
One, by mass fraction, take 11.25 parts of carboxyl butadiene acrylonitrile rubber breasts of epoxy resin and 3.75 parts of polyacrylic ester latexs of 100 parts;
Two,, after carboxyl butadiene acrylonitrile rubber breast breakdown of emulsion step 1 being taken, dry, standby;
Three,, after polyacrylic ester latex breakdown of emulsion step 1 being taken, dry, standby;
Four, the carboxyl butadiene acrylonitrile rubber breast after step 2 is joined in the epoxy resin that step 1 takes, in temperature, be to react 2h under the condition of 120 ℃, add again the polyacrylic ester latex after step 3, in temperature, be to react 1h under the condition of 120 ℃, obtain under normal temperature is the modified epoxy of thick liquid, i.e. high-durability energy epoxy resin adhesive.
Epoxy resin in the present embodiment, carboxyl butadiene acrylonitrile rubber breast and polyacrylic ester latex are commercially available prod.
Embodiment 4: a kind of preparation method of high-durability energy epoxy resin adhesive carries out according to the following steps:
One, by mass fraction, take 15 parts of carboxyl butadiene acrylonitrile rubber breasts of epoxy resin and 5 parts of polyacrylic ester latexs of 100 parts;
Two,, after carboxyl butadiene acrylonitrile rubber breast breakdown of emulsion step 1 being taken, dry, standby;
Three,, after polyacrylic ester latex breakdown of emulsion step 1 being taken, dry, standby;
Four, the carboxyl butadiene acrylonitrile rubber breast after step 2 is joined in the epoxy resin that step 1 takes, in temperature, be to react 2h under the condition of 120 ℃, add again the polyacrylic ester latex after step 3, in temperature, be to react 1h under the condition of 120 ℃, obtain under normal temperature is the modified epoxy of thick liquid, i.e. high-durability energy epoxy resin adhesive.
Epoxy resin in the present embodiment, carboxyl butadiene acrylonitrile rubber breast and polyacrylic ester latex are commercially available prod.
Embodiment 5: a kind of preparation method of high-durability energy epoxy resin adhesive carries out according to the following steps:
One, by mass fraction, take 18.75 parts of carboxyl butadiene acrylonitrile rubber breasts of epoxy resin and 6.25 parts of polyacrylic ester latexs of 100 parts;
Two,, after carboxyl butadiene acrylonitrile rubber breast breakdown of emulsion step 1 being taken, dry, standby;
Three,, after polyacrylic ester latex breakdown of emulsion step 1 being taken, dry, standby;
Four, the carboxyl butadiene acrylonitrile rubber breast after step 2 is joined in the epoxy resin that step 1 takes, in temperature, be to react 2h under the condition of 120 ℃, add again the polyacrylic ester latex after step 3, in temperature, be to react 1h under the condition of 120 ℃, obtain under normal temperature is the modified epoxy of thick liquid, i.e. high-durability energy epoxy resin adhesive.
Epoxy resin in the present embodiment, carboxyl butadiene acrylonitrile rubber breast and polyacrylic ester latex are commercially available prod.
Embodiment 6: a kind of preparation method of high-durability energy epoxy resin adhesive carries out according to the following steps:
One, by mass fraction, take 22.5 parts of carboxyl butadiene acrylonitrile rubber breasts of epoxy resin and 7.5 parts of polyacrylic ester latexs of 100 parts;
Two,, after carboxyl butadiene acrylonitrile rubber breast breakdown of emulsion step 1 being taken, dry, standby;
Three,, after polyacrylic ester latex breakdown of emulsion step 1 being taken, dry, standby;
Four, the carboxyl butadiene acrylonitrile rubber breast after step 2 is joined in the epoxy resin that step 1 takes, in temperature, be to react 2h under the condition of 120 ℃, add again the polyacrylic ester latex after step 3, in temperature, be to react 1h under the condition of 120 ℃, obtain under normal temperature is the modified epoxy of thick liquid, i.e. high-durability energy epoxy resin adhesive.
Epoxy resin in the present embodiment, carboxyl butadiene acrylonitrile rubber breast and polyacrylic ester latex are commercially available prod.
Test one, high-durability energy epoxy resin adhesive prepared by embodiment 1～6 carry out shear strength test, and process of the test is as follows:
After adopting 200# polymeric amide as solidifying agent, the high-durability energy epoxy resin adhesive of embodiment 1～6 preparation to be solidified, be coated in the LY2CZ aluminium alloy test piece of sand papering processing, close up test piece, pressurization 0.01MPa, ambient cure 24 hours, with existing universal epoxy resin sizing agent: 200# polyamide curing agent solidifies E51 epoxy resin as a control group, carries out simultaneous test;
Now according to GB7124, sizing agent bonded metal material shearing resistance experimental technique, with INSTRON4467 type electronic tension tester, above-mentioned test piece is carried out to shear strength test, obtains result as shown in table 1:
Table 1: sizing agent shearing resistance contrast table
Claims (6)
1. a high-durability energy modified epoxy, is characterized in that a kind of high-durability energy modified epoxy made by the epoxy resin of 90～110 parts, 3.75～22.5 parts of carboxylic acrylonitrile butadiene rubber latexs and 1.25～7.5 parts of polyacrylic ester latexs by mass fraction; And described carboxylic acrylonitrile butadiene rubber latex and the mass ratio of polyacrylic ester latex are 3:1;
Described a kind of high-durability energy modified epoxy is prepared from according to the following steps:
One, by after carboxylic acrylonitrile butadiene rubber latex breakdown of emulsion, dry, standby;
Two, by after polyacrylic ester latex breakdown of emulsion, dry, standby;
Three, the carboxylic acrylonitrile butadiene rubber latex after step 1 is joined in epoxy resin, in temperature, be to react 1h～3h under the condition of 110～130 ℃, add again the polyacrylic ester latex after step 2, in temperature, be to react 0.5h～1.5h under the condition of 110～130 ℃, obtaining under normal temperature is the modified epoxy of thick liquid.
2. a kind of high-durability energy modified epoxy according to claim 1, is characterized in that a kind of high-durability energy modified epoxy made by the epoxy resin of 100 parts, 15 parts of carboxylic acrylonitrile butadiene rubber latexs and 5 parts of polyacrylic ester latexs by mass fraction.
3. prepare the method for a kind of high-durability energy modified epoxy as claimed in claim 1, it is characterized in that a kind of preparation method of high-durability energy modified epoxy carries out according to the following steps:
One, by mass fraction, take the epoxy resin of 90～110 parts, 3.75～22.5 parts of carboxylic acrylonitrile butadiene rubber latexs and 1.25～7.5 parts of polyacrylic ester latexs, the mass ratio of wherein said carboxylic acrylonitrile butadiene rubber latex and polyacrylic ester latex is 3:1;
Two,, after carboxylic acrylonitrile butadiene rubber latex breakdown of emulsion step 1 being taken, dry, standby;
Three,, after polyacrylic ester latex breakdown of emulsion step 1 being taken, dry, standby;
Four, the carboxylic acrylonitrile butadiene rubber latex after step 2 is joined in the epoxy resin that step 1 takes, in temperature, be to react 1h～3h under the condition of 110～130 ℃, add again the polyacrylic ester latex after step 3, in temperature, be to react 0.5h～1.5h under the condition of 110～130 ℃, obtaining under normal temperature is the modified epoxy of thick liquid.
4. the preparation method of a kind of high-durability energy modified epoxy according to claim 3, is characterized in that by mass fraction, taking the epoxy resin of 100 parts, 15 parts of carboxylic acrylonitrile butadiene rubber latexs and 5 parts of polyacrylic ester latexs in step 1.
5. according to the preparation method of a kind of high-durability energy modified epoxy described in claim 3 or 4, it is characterized in that in step 4, the carboxylic acrylonitrile butadiene rubber latex after step 2 being joined in the epoxy resin that step 1 takes, is to react 2h under the condition of 120 ℃ in temperature.
6. the preparation method of a kind of high-durability energy modified epoxy according to claim 5, is characterized in that adding the polyacrylic ester latex after step 3 in step 4 again, is to react 1h under the condition of 120 ℃ in temperature.
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| US11492525B2 (en) * | 2017-09-12 | 2022-11-08 | Ddp Specialty Electronic Materials Us, Llc | Adhesive formulation |
| US10581016B2 (en) | 2017-11-10 | 2020-03-03 | Wuhan China Star Optoelectronics Semiconductor Display Technology Co., Ltd. | Package structure, packaging method and electronic device |
| CN107799666B (en) * | 2017-11-10 | 2019-04-23 | 武汉华星光电半导体显示技术有限公司 | Encapsulating structure, packaging method and electronic device |
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