CN105567146A - Epoxy single-component electronic adhesive and preparation method thereof - Google Patents
Epoxy single-component electronic adhesive and preparation method thereof Download PDFInfo
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- CN105567146A CN105567146A CN201610169654.6A CN201610169654A CN105567146A CN 105567146 A CN105567146 A CN 105567146A CN 201610169654 A CN201610169654 A CN 201610169654A CN 105567146 A CN105567146 A CN 105567146A
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- epoxy
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- electronics glue
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses an epoxy single-component electronic adhesive and a preparation method thereof. The epoxy single-component electronic adhesive comprises the following components in percentage by mass: a bisphenol A epoxy resin, a modified epoxy resin, a simple function diluter, a latent curing agent, a filler and a functional aid. The modified epoxy resin comprises the following components in percentage by mass: a novolac epoxy resin, a polyfunctional diluter, elacostearic anhydride and an imidazole curing agent. The epoxy single-component electronic adhesive has high bonding power and high impact resistance, and can be well applied to electronic components.
Description
Technical field
The present invention relates to Material Field, particularly relate to a kind of epoxy single-component electronics glue paste and preparation method thereof.
Background technology
Be applied to the single-component epoxy glue of electronic devices and components as VCM motor now, the common problem existed is that the toughness of glue is inadequate, show as bonding force and shock resistance is not up to standard, particularly along with newcooperative medical system and the miniaturization of electronic devices and components structure, bond area reduces, and this problem seems particularly outstanding.Although conventional toughner can increase the snappiness of system as polyurethane-modified or modified rubber glue etc., improvement be there is no to bonding force.Therefore a kind of electronics glue paste having bonds well power and shock resistance is needed badly.
Summary of the invention
Based on this, be necessary for the problems referred to above, a kind of epoxy single-component electronics glue paste and preparation method thereof is provided.
Concrete technical scheme is as follows:
A kind of epoxy single-component electronics glue paste, by percentage to the quality, comprises following component:
Wherein, described modified epoxy by percentage to the quality, comprises following component:
Wherein in some embodiments, above-mentioned epoxy single component electronics glue paste by percentage to the quality, comprises following component:
Wherein, described modified epoxy by percentage to the quality, comprises following component:
Wherein in some embodiments, described monofunctional diluent is one or more in benzyl glycidyl ether, glycidyl neodecanoate, phenyl glycidyl ether.
Wherein in some embodiments, described imidazole curing agent is one or more in glyoxal ethyline, 1-cyanoethyl-2-ethyl-4-methylimidazole, 1-cyanoethyl-2-phenylimidazole.
Wherein in some embodiments, described multifunctional thinner is one or more in 1,6-hexanediol diglycidyl ether, BDDE, polypropylene glycol diglycidyl ether.
Wherein in some embodiments, described latent curing agent is modified polyamine type solidifying agent.
Wherein in some embodiments, described filler is one or both in calcium carbonate, silicon powder.
Wherein in some embodiments, described functional aid is defoamer and coupling agent, and both proportionings are 1:3.
The present invention also provides a kind of preparation method of above-mentioned epoxy single-component electronics glue paste, comprises the following steps:
(1) mixture of described novolac epoxy and multifunctional thinner is added reactor, be warming up to 85 ~ 95 DEG C, after at the uniform velocity drip the mixture of tung oil acid anhydride and imidazole curing agent, be warming up to 95 ~ 105 DEG C after dropwising and keep 1.8 ~ 2.2h, finally be warming up to 110 ~ 120 DEG C and keep 1.8 ~ 2.2h, period keeps stirring, and is then cooled to 55 ~ 65 DEG C of dischargings, obtains modified epoxy;
(2) by described bisphenol A type epoxy resin, modified epoxy, monofunctional diluent, latent curing agent, filler and functional aid 15 ~ 30 DEG C of mixing and stirring, grinding, filters, filling, to obtain final product.
Wherein in some embodiments, the preparation method of above-mentioned epoxy single-component electronics glue paste comprises the following steps:
(1) mixture of described novolac epoxy and multifunctional thinner is added reactor at normal temperatures, be warming up to 85 ~ 95 DEG C, after at the uniform velocity drip the mixture of tung oil acid anhydride and imidazole curing agent, be warming up to 95 ~ 105 DEG C after dropwising and keep 1.8 ~ 2.2h, finally be warming up to 110 ~ 120 DEG C and keep 1.8 ~ 2.2h, period keeps the stirring velocity of 350 ~ 450rpm to stir, and is then cooled to 55 ~ 65 DEG C of dischargings, obtains modified epoxy;
(2) by described bisphenol A type epoxy resin, modified epoxy, monofunctional diluent, latent curing agent, filler and functional aid 15 ~ 30 DEG C of mixing and stirring, grind with three-roller afterwards, it is 15 ~ 30 DEG C that process of lapping controls material temperature degree, guarantee fineness be less than 25 μm after discharging, filter, filling, to obtain final product.
The present invention compared to the advantage of prior art and beneficial effect is:
(1) the present inventor team is for the cohesive force existing for the existing single-component electronics glue paste being applied to electronic component and shock resistance shortcoming not up to standard, by large quantifier elimination, draw and adopt tung oil acid anhydride to carry out toughening modifying to epoxy resin, selected epoxy resin is elite multifunctional novolac epoxy and multifunctional thinner, and coordinate optimum proportioning (as the addition of tung oil acid anhydride, the proportioning etc. of novolac epoxy and multifunctional thinner), obtain the epoxy single component electronics glue paste of high bonding force and high impact properties.
(2) preparation method of the present invention is by the processing condition of setting optimum, as carried out in the temperature-rise period in toughening modifying at tung oil acid anhydride to epoxy resin, take interim intensification, can guarantee tung oil acid anhydride only with the part functional group reactions on multifunctional novolac epoxy and multifunctional thinner, thus remaining epoxide group can react performance to reach high bonding force and shock resistance with latent curing agent when glue paste solidifies on most molecular structure.
Embodiment
Below with reference to specific embodiment, the present invention will be further described.
The raw material that the embodiment of the present invention adopts is commercially available convenient source, wherein:
Bisphenol A type epoxy resin E51 is purchased from Changchun, Taiwan chemical industry or Yang Nongjin lake, Jiangsu chemical industry;
Novolac epoxy F44 and F51 is purchased from Changchun, Taiwan chemical industry or blue star new chemical materials;
Benzyl glycidyl ether, glycidyl neodecanoate, 1,6-hexanediol diglycidyl ether, polypropylene glycol diglycidyl ether are purchased from New far Chemical Industry Co., Ltd. of Anhui;
Latent curing agent EH-5031S is purchased from Ai Dike (Shanghai) trade Co., Ltd;
Defoamer BYK066N, coupling agent Z-6040 are respectively purchased from BYK and DOW CORNING;
Tung oil acid anhydride is purchased from synthetic materials good in Yangzhou;
1-cyanoethyl-2-ethyl-4-methylimidazole, 1-cyanoethyl-2-phenylimidazole are purchased from Japanese aginomoto.
Embodiment 1
A kind of epoxy single component electronics glue paste, by percentage to the quality, comprises following component:
(the defoamer BYK066N in above-mentioned functions auxiliary agent and the proportioning of coupling agent Z-6040 are 1:3)
Wherein, described modified epoxy by percentage to the quality, comprises following component:
Preparation method comprises the following steps:
(1) mixture of described novolac epoxy and multifunctional thinner is added reactor at normal temperatures, be warming up to 85 ~ 95 DEG C, after at the uniform velocity drip the mixture of tung oil acid anhydride and imidazole curing agent, be warming up to 95 ~ 105 DEG C after dropwising and keep 2h, finally be warming up to 110 ~ 120 DEG C and keep 2h, period keeps the stirring velocity of 350 ~ 450rpm to stir, and is then cooled to 55 ~ 65 DEG C of dischargings, obtains modified epoxy;
(2) by described bisphenol A type epoxy resin, modified epoxy, monofunctional diluent, latent curing agent, filler and functional aid 15 ~ 30 DEG C of mixing and stirring, grind with three-roller afterwards, it is 15 ~ 30 DEG C that process of lapping controls material temperature degree, guarantee fineness be less than 25 μm after discharging, filter, filling, to obtain final product.
Embodiment 2
A kind of epoxy single component electronics glue paste, by percentage to the quality, comprises following component:
(the defoamer BYK066N in above-mentioned functions auxiliary agent and the proportioning of coupling agent Z-6040 are 1:3)
Wherein, described modified epoxy by percentage to the quality, comprises following component:
Preparation method is with embodiment 1.
Embodiment 3
A kind of epoxy single component electronics glue paste, by percentage to the quality, comprises following component:
(proportioning of the BYK066N in above-mentioned functions auxiliary agent and coupling agent Z-6040 is 1:3)
Wherein, described modified epoxy by percentage to the quality, comprises following component:
Preparation method is with embodiment 1.
Embodiment 4
A kind of epoxy single component electronics glue paste, by percentage to the quality, comprises following component:
(the defoamer BYK066N in above-mentioned functions auxiliary agent and the proportioning of coupling agent Z-6040 are 1:3)
Wherein, described modified epoxy by percentage to the quality, comprises following component:
Preparation method is with embodiment 1.
Comparative example 1
Electronics glue paste in this comparative example is substantially identical with the epoxy single component electronics glue paste in embodiment 1, and difference is: the modified epoxy in this comparative example polyurethane modified epoxy resin equivalent replace embodiment 1.
Electronics glue paste in this comparative example prepares with reference to method in embodiment 1.
Comparative example 2
Electronics glue paste in this comparative example is substantially identical with the epoxy single component electronics glue paste in embodiment 1, and difference is: with bisphenol A type epoxy resin equivalent replace novolac epoxy in the modified epoxy part of this comparative example.
Electronics glue paste in this comparative example prepares with reference to method in embodiment 1.
Comparative example 3
Electronics glue paste in this comparative example is substantially identical with the epoxy single component electronics glue paste in embodiment 1, and difference is: with the multifunctional thinner of monofunctional diluent equivalent replace in the modified epoxy part of this comparative example.
Electronics glue paste in this comparative example prepares with reference to method in embodiment 1.
Comparative example 4
Electronics glue paste in this comparative example is substantially identical with the epoxy single component electronics glue paste in embodiment 1, and difference is that its preparation method comprises the following steps:
(1) mixture of described novolac epoxy and multifunctional thinner is added reactor at normal temperatures, be warming up to 85 ~ 95 DEG C, after at the uniform velocity drip the mixture of tung oil acid anhydride and imidazole curing agent, dropwise rear constant temperature 85 ~ 95 DEG C and keep 1.8-2.2h, period keeps the stirring velocity of 350 ~ 450rpm to stir, then be cooled to 55 ~ 65 DEG C of dischargings, obtain modified epoxy;
(2) by described bisphenol A type epoxy resin, modified epoxy, monofunctional diluent, latent curing agent, filler and functional aid mixing and stirring at lower than 30 DEG C, grind with three-roller afterwards, process of lapping controls material temperature degree and is no more than 30 DEG C, guarantee fineness be less than 25 μm after discharging, filter, filling, to obtain final product.
The electronics glue paste prepare above-described embodiment 1 ~ 4 and comparative example 1 ~ 4 and VCM motor carry out performance test, and wherein, bonding force is tested with pull and push dynamometer,
Conventional VCM motor adopts point gum machine to fit afterwards at four some point glue (putting the glue paste of embodiment 1 ~ 4 and comparative example 1 ~ 4 gained respectively), again after 80 DEG C of * 40min solidify, obtain VCM motor A, B, C, D, E, F, G, H respectively, carry out performance test.
(new texture VCM motor is less based on glue paste bond area conventional VCM motor to new texture VCM motor, the novel VCM motor that glue consumption is less) adopt point gum machine to fit afterwards at four some point glue (putting the glue paste of embodiment 1 ~ 4 and comparative example 1 ~ 4 gained respectively), again after 80 DEG C of * 40min solidify, obtain VCM motor A1, B1, C1, D1, E1, F1, G1, H1 respectively, carry out performance test.
Bonding force testing method: the numerical value adopting thrustmeter test bonding force, the better numerical value of bonding force is larger, and it is qualified that bonding force is greater than 4kg.
Drop test testing method: load 4 VCM motors (preparation of same glue paste) in particular device, carry out falling of specified altitude and number of times, each VCM motor has 4 adhesive spots, whether rear observation 16 adhesive spots there is cracking or crackle. there are cracking or crackle to be all judged to be defective, without any bad be qualified, require that falling of same number of times is carried out respectively in 6 faces of VCM motor, falling height is the drop number of 1.6 ± 0.1m is that every face amounts to 18 times for 3 times, requires that 16 points are all qualified in cracking.
Carry out micro-drop test again after 1.6m drop test passes through, then do not proceed micro-drop test by 1.6m drop test.Micro-drop test method is: falling height is micro-drop number of 10cm is that every face amounts to 4.2 ten thousand times for 7,000 times, requires that maximum 2 of 16 points have crackle to be qualified.
Detected result asks for an interview following table 1,2
Table 1 embodiment 1 ~ 4 and comparative example 1 ~ 4 gained glue paste performance (conventional VCM motor)
Table 2 embodiment 1 ~ 4 and comparative example 1 ~ 4 gained glue paste performance (new texture VCM motor)
As can be seen from the above results, the epoxy single-component electronics glue paste that embodiment 1 and 4 prepares has larger and stable bonding force, by the strictest drop test; The epoxy single-component electronics glue paste of embodiment 2 ~ 3, its performance is slightly inferior compared with embodiment 1 and 4, but also good than comparative example 1 ~ 4.
The electronics glue paste of comparative example 1 ~ 4 gained, because modified epoxy does not use specific tung oil acid anhydride modification (comparative example 1), or the epoxy resin that modified epoxy adopts not is novolac epoxy (comparative example 2), or the thinner not multifunctional thinner (comparative example 3) that modified epoxy adopts, or preparation method is prepared according to constant temperature technique, fail intensification segmentation modification (comparative example 4), the bonding force of the electronics glue paste finally obtained and anti-dropping capability are all not good.
Each technical characteristic of the above embodiment can combine arbitrarily, for making description succinct, the all possible combination of each technical characteristic in above-described embodiment is not all described, but, as long as the combination of these technical characteristics does not exist contradiction, be all considered to be the scope that this specification sheets is recorded.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be construed as limiting the scope of the patent.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. an epoxy single-component electronics glue paste, is characterized in that, by percentage to the quality, comprises following component:
Wherein, described modified epoxy by percentage to the quality, comprises following component:
2. epoxy single-component electronics glue paste according to claim 1, is characterized in that, by percentage to the quality, comprise following component:
Wherein, described modified epoxy by percentage to the quality, comprises following component:
3. epoxy single-component electronics glue paste according to claim 1 and 2, it is characterized in that, described monofunctional diluent is one or more in benzyl glycidyl ether, glycidyl neodecanoate, phenyl glycidyl ether.
4. epoxy single-component electronics glue paste according to claim 1 and 2, is characterized in that, described imidazole curing agent is one or more in glyoxal ethyline, 1-cyanoethyl-2-ethyl-4-methylimidazole, 1-cyanoethyl-2-phenylimidazole.
5. epoxy single-component electronics glue paste according to claim 1 and 2, is characterized in that, described multifunctional thinner is one or more in 1,6-hexanediol diglycidyl ether, BDDE, polypropylene glycol diglycidyl ether.
6. epoxy single-component electronics glue paste according to claim 1 and 2, is characterized in that, described latent curing agent is modified polyamine type solidifying agent.
7. epoxy single-component electronics glue paste according to claim 1 and 2, is characterized in that, described filler is one or both in calcium carbonate, silicon powder.
8. epoxy single-component electronics glue paste according to claim 1 and 2, it is characterized in that, described functional aid is defoamer and coupling agent, and both proportionings are 1:3.
9. a preparation method for the epoxy single-component electronics glue paste described in any one of claim 1 ~ 8, is characterized in that, comprise the following steps:
(1) mixture of described novolac epoxy and multifunctional thinner is added reactor, be warming up to 85 ~ 95 DEG C, after at the uniform velocity drip the mixture of tung oil acid anhydride and imidazole curing agent, be warming up to 95 ~ 105 DEG C after dropwising and keep 1.8 ~ 2.2h, finally be warming up to 110 ~ 120 DEG C and keep 1.8 ~ 2.2h, period keeps stirring, and is then cooled to 55 ~ 65 DEG C of dischargings, obtains modified epoxy;
(2) by described bisphenol A type epoxy resin, modified epoxy, monofunctional diluent, latent curing agent, filler and functional aid 15 ~ 30 DEG C of mixing and stirring, grinding, filters, filling, to obtain final product.
10. the preparation method of epoxy single-component electronics glue paste according to claim 9, is characterized in that, comprise the following steps:
(1) mixture of described novolac epoxy and multifunctional thinner is added reactor at normal temperatures, be warming up to 85 ~ 95 DEG C, after at the uniform velocity drip the mixture of tung oil acid anhydride and imidazole curing agent, be warming up to 95 ~ 105 DEG C after dropwising and keep 1.8 ~ 2.2h, finally be warming up to 110 ~ 120 DEG C and keep 1.8 ~ 2.2h, period keeps the stirring velocity of 350 ~ 450rpm to stir, and is then cooled to 55 ~ 65 DEG C of dischargings, obtains modified epoxy;
(2) by described bisphenol A type epoxy resin, modified epoxy, monofunctional diluent, latent curing agent, filler and functional aid 15 ~ 30 DEG C of mixing and stirring, grind with three-roller afterwards, it is 15 ~ 30 DEG C that process of lapping controls material temperature degree, guarantee fineness be less than 25 μm after discharging, filter, filling, to obtain final product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610169654.6A CN105567146B (en) | 2016-03-22 | 2016-03-22 | Epoxy one-component electronics adhesive and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610169654.6A CN105567146B (en) | 2016-03-22 | 2016-03-22 | Epoxy one-component electronics adhesive and preparation method thereof |
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| CN105567146A true CN105567146A (en) | 2016-05-11 |
| CN105567146B CN105567146B (en) | 2018-03-02 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106928892A (en) * | 2017-04-14 | 2017-07-07 | 广州日高新材料科技有限公司 | Single-component epoxy electronic pastes and its preparation method and application |
| CN111478527A (en) * | 2020-05-06 | 2020-07-31 | 东莞市畅科电机有限公司 | Manufacturing method of coreless motor |
| CN112831281A (en) * | 2021-01-29 | 2021-05-25 | 东莞市新懿电子材料技术有限公司 | Adhesive for adhering and filling LCP (liquid Crystal display) base and nickel-plated iron sheet of VCM (Voice coil Motor) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1651542A (en) * | 2005-01-07 | 2005-08-10 | 武汉理工大学 | Epoxy resin binding agent for sand paper and its preparation method |
| US20070293603A1 (en) * | 2006-06-19 | 2007-12-20 | Ashland Licensing And Intellectual Property Llc | Epoxy adhesive composition and use thereof |
| CN101104784A (en) * | 2007-08-03 | 2008-01-16 | 江苏科技大学 | Composite laminated board high-temperature resistant adhesive and preparation method thereof |
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2016
- 2016-03-22 CN CN201610169654.6A patent/CN105567146B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1651542A (en) * | 2005-01-07 | 2005-08-10 | 武汉理工大学 | Epoxy resin binding agent for sand paper and its preparation method |
| US20070293603A1 (en) * | 2006-06-19 | 2007-12-20 | Ashland Licensing And Intellectual Property Llc | Epoxy adhesive composition and use thereof |
| CN101104784A (en) * | 2007-08-03 | 2008-01-16 | 江苏科技大学 | Composite laminated board high-temperature resistant adhesive and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106928892A (en) * | 2017-04-14 | 2017-07-07 | 广州日高新材料科技有限公司 | Single-component epoxy electronic pastes and its preparation method and application |
| CN111478527A (en) * | 2020-05-06 | 2020-07-31 | 东莞市畅科电机有限公司 | Manufacturing method of coreless motor |
| CN112831281A (en) * | 2021-01-29 | 2021-05-25 | 东莞市新懿电子材料技术有限公司 | Adhesive for adhering and filling LCP (liquid Crystal display) base and nickel-plated iron sheet of VCM (Voice coil Motor) |
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| CN105567146B (en) | 2018-03-02 |
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