CN101928539A - High-temperature resistant single-component epoxy structure glue, preparation method and using method thereof - Google Patents
High-temperature resistant single-component epoxy structure glue, preparation method and using method thereof Download PDFInfo
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- CN101928539A CN101928539A CN 201010278347 CN201010278347A CN101928539A CN 101928539 A CN101928539 A CN 101928539A CN 201010278347 CN201010278347 CN 201010278347 CN 201010278347 A CN201010278347 A CN 201010278347A CN 101928539 A CN101928539 A CN 101928539A
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Abstract
The invention relates to a high-temperature resistant single-component epoxy structure glue, a preparation method and a using method thereof. The epoxy structure glue is prepared by raw materials based on parts by weight: 100 parts of epoxy resin, 10-25 parts of toughening agent, 20-40 parts of filler, 1-5 parts of coupling agent, 5-10 parts of curing agent and 3-8 parts of thixotropic agent. The high-temperature resistant single-component epoxy structure glue has certain properties in the aspects of metal and nonmetal, thus not only having the adhesive bonding function, but also being used for filling gaps; and due to the low coefficient of thermal expansion, the cured product can be used for a long time at higher temperature and does not crack by internal stress.
Description
Technical field
The present invention relates to a kind of epoxy structural rubber and preparation method thereof and using method, relate in particular to a kind of high-temperature resistant single-component epoxy structure glue and preparation method thereof and using method, belong to adhesive area.
Background technology
Epoxyn has good adhesiveproperties, is widely used in bonding occasion.In some adhesive applications occasions, one side be metal such as aluminium, be nonmetal simultaneously such as resol, the good heat conductivity of metal, and nonmetal heat conductivility is relatively poor, and metal and nonmetal between bigger gap is arranged, add epoxy structural rubber with regard to needs and carry out bonding.The ordinary epoxy resin thermal conductivity is relatively poor, causes epoxy adhesive and nonmetal binding face overheated easily, thereby produces internal stress, influences quality product.
Summary of the invention
It is relatively poor to the present invention is directed to the ordinary epoxy resin thermal conductivity, cause epoxy adhesive and nonmetal binding face overheated easily, thereby generation internal stress, influence the deficiency of quality product, a kind of high-temperature resistant single-component epoxy structure glue and preparation method thereof and using method are provided, this high-temperature resistant single-component epoxy structure glue had both had the characteristic of certain connection metal, the characteristic that has nonmetal aspect again, can play bonding effect, can play the effect of blind again, the product after little thermal expansivity make to solidify can be under higher temperature life-time service and be unlikely to ftracture because of internal stress.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of high-temperature resistant single-component epoxy structure glue is made by the raw material of following parts by weight: 100 parts Resins, epoxy, 10 parts～25 parts toughner, 20 parts～40 parts filler, 1 part～5 parts coupling agent, 5 parts～10 parts solidifying agent and 3 parts～8 parts thixotropic agent.
The invention has the beneficial effects as follows: the present invention adopts a large amount of metallic aluminium powders of adding and aluminum oxide powder to improve the heat conductivility of Resins, epoxy; Resin adopts novolac epoxy to combine with ordinary epoxy resin, makes exothermic heat of reaction mild, and the heat of generation can in time be derived; In addition, add a large amount of metallic aluminium powders and aluminum oxide powder and silicon powder and make that the thermal expansivity of system is very little, glue-line has metal and nonmetallic performance concurrently, therefore can eliminate interfacial stress significantly, can repair the following gap of 5mm; Adopt a large amount of special ball aluminum powder of interpolation to influence bonding strength hardly, bonding force is strong, shearing resistance 〉=30MPa.Range of viscosities is adjustable, and viscosity is big, and thixotropy can be constructed good operability by facade well.
On the basis of technique scheme, the present invention can also do following improvement.
Further, described Resins, epoxy is the mixture of F-51 novolac epoxy and E-51 Resins, epoxy or the mixture of F-51 novolac epoxy and E-44 Resins, epoxy.
Further, described toughner is the polyfunctional group block macromolecular prepolymer with distant pawl type molecular structure, solidifies with Resins, epoxy and can play active dilution and chemical toughness reinforcing dual-use function.
In the present invention, described toughner is the KH-07A of Dalian triumphant magnificent new technology Engineering Co., Ltd, KH-07B, wherein a kind of or several mixture arbitrarily of KH-07C, KH-07D.
Further, described filler is the mixture of ball aluminum powder, aluminum oxide powder and silicon powder.
Further, described ball aluminum powder particle diameter is 5 microns～15 microns, and the order number of described aluminum oxide powder is 400 orders, and the order number of described silicon powder is 1250 orders.
Further, described coupling agent is γ-amine propyl-triethoxysilicane.
Further, described solidifying agent is a Toluene-2,4-diisocyanate, the mixture of 4-two [N, N-dimethylamino] third urea and Dyhard RU 100.
Further, described thixotropic agent is a gas-phase silicon.
The present invention also provides a kind of technical scheme that solves the problems of the technologies described above as follows: a kind of preparation method of high temperature single-component epoxy structure glue comprises: at first, with the raw material of following parts by weight is that 100 parts Resins, epoxy, 10 parts～25 parts toughner and 1 part～5 parts coupling agent add in the mixing kettle, stirring at normal temperature 1 hour～2 hours, the rotating speed of mixing kettle is 100rpm～180rpm; Then, the filler that in mixing kettle, adds 20 parts～40 parts, stirring at normal temperature 20 minutes～40 minutes, the rotating speed of mixing kettle is 1000rpm～1200rpm, after uniform mixture to be mixed is reduced to normal temperature, the solidifying agent that adds 5 parts～10 parts again, stirring at normal temperature 30 minutes, the rotating speed of mixing kettle is 100rpm～180rpm; At last, add 20 parts～40 parts filler in mixing kettle, stirring at normal temperature 20 minutes～40 minutes is regulated viscosity 200～400Pas discharging and can be obtained epoxy structural rubber.
The present invention also provides a kind of technical scheme that solves the problems of the technologies described above as follows: a kind of using method of high temperature single-component epoxy structure glue comprises: at first, will treat that bonding plane cleans up; Then, epoxy structural rubber is evenly coated between two bonding planes; At last, under 120 ℃～150 ℃ temperature, solidified 30 minutes～60 minutes, can use behind the naturally cooling.
Embodiment
Below principle of the present invention and feature are described, institute gives an actual example and only is used to explain the present invention, is not to be used to limit scope of the present invention.
Embodiment 1
Pressing Resins, epoxy gross weight 100 calculates for unit
With Resins, epoxy E-51 50g, F-51 50g and toughner KH-07A 2.5g, KH-07B 2.5g, KH-07C 2.5g, KH-07D 2.5g, γ-amine propyl-triethoxysilicane 1g adds in the mixing kettle, and stirring at normal temperature 1h～2h, rotating speed are 100r～180rpm; Add aluminum oxide powder 5g, ball aluminum powder 10g, silicon powder 5g, rotating speed is that 1000r～1200rpm stirs 20 min～40min, reduces to normal temperature after mixing, and adds Dyhard RU 100 3g, Toluene-2,4-diisocyanate, 4-two [N, N-dimethylamino] the third urea 2g stirs 30min with 100r～180rpm, add gas-phase silicon 3g at last, stir 20min～40min, regulate viscosity 200～400Pas, discharging obtains epoxy structural rubber.
The comparative example 1
Implementation process is with embodiment 1, and difference is that aluminium powder is common aluminium powder, non-sphere.
Embodiment 1 and comparative example's 1 epoxy structural rubber, performance test is as follows:
The test of experiment test example 1 tensile shear strength:
This test is tested according to GB/T 7124-2008,45# steel-steel sample, and 130 ℃ solidify 30min, detect tensile shear strength behind the 24h.
Sample that table 1 embodiment 1 makes and the contrast of comparative example's The performance test results
| Sample | Embodiment 1 | The comparative example 1 |
| Shearing resistance (MPa) | 30 | 22 |
As can be seen from Table 1, add the bonding strength height of ball aluminum powder than common aluminium powder, it is bonding to be more suitable for being used for structure.
Embodiment 2
Pressing Resins, epoxy gross weight 100 calculates for unit
With Resins, epoxy E-51 70g, F-51 30g and toughner KH-07C 5g, KH-07D 20g, γ-amine propyl-triethoxysilicane 5g adds in the mixing kettle, and stirring at normal temperature 1h～2h, rotating speed are 100r～180rpm; Add aluminum oxide powder 10g, ball aluminum powder 20g, silicon powder 10g, rotating speed are that 1000r～1200rpm stirs 20 min～40min, reduce to normal temperature after mixing, add Dyhard RU 100 6g, Toluene-2,4-diisocyanate, 4-two [N, the N-dimethylamino] the third urea 4g, stir 30min with 100r～180rpm, add gas-phase silicon 8g at last and stir 20 min～40min, regulate viscosity 200～400Pas discharging and obtain epoxy structural rubber.
The comparative example 2
Implementation process is with embodiment 2, and difference is not for adding aluminum oxide powder and silicon powder.
Embodiment 2 and comparative example's 2 epoxy structural rubber, performance test is as follows:
The test of experiment test example 2 thermal expansivity
This test is carried out as follows: the control bondline thickness is 2mm, and 130 ℃ solidify 30min, adopts the thermal expansivity of TMA test sample behind the 24h.
Experiment test example 3 is filled the gap size test
This test is carried out as follows: glue-line is coated on the aluminium flake of thick 2mm, detects the situation of glue-line behind 130 ℃ of curing 30min of different thickness, see if there is overheat condition and take place.
Sample that table 2 embodiment 2 makes and the contrast of comparative example's The performance test results
As can be seen from Table 2, add appropriate amount of alumina powder and silicon powder, thermal expansivity obviously reduces; Curable adhesive layer thickness can reach 5mm, and the comparative example can only reach 3mm.
Embodiment 3
Pressing Resins, epoxy gross weight 100 calculates for unit
With Resins, epoxy E-51 20g, F-51 80g and toughner KH-07C 18g, silane coupling agent γ-amine propyl-triethoxysilicane 3g adds in the mixing kettle, and stirring at normal temperature 1 h～2h, rotating speed are 100r～180rpm; Add aluminum oxide powder 5g, ball aluminum powder 15g, silicon powder 10g, rotating speed are that 1000r～1200rpm stirs 20 min～40min, reduce to normal temperature after mixing, add Dyhard RU 100 6g, Toluene-2,4-diisocyanate, 4-two [N, the N-dimethylamino] the third urea 1g, stir 30min with 100r～180rpm, add gas-phase silicon 5g at last and stir 20 min～40min, regulate viscosity 200～400Pas discharging and obtain epoxy structural rubber.
The above only is preferred embodiment of the present invention, and is in order to restriction the present invention, within the spirit and principles in the present invention not all, any modification of being done, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. high-temperature resistant single-component epoxy structure glue, it is characterized in that described epoxy structural rubber is made by the raw material of following parts by weight: 100 parts Resins, epoxy, 10 parts～25 parts toughner, 20 parts～40 parts filler, 1 part～5 parts coupling agent, 5 parts～10 parts solidifying agent and 3 parts～8 parts thixotropic agent.
2. high-temperature resistant single-component epoxy structure glue according to claim 1 is characterized in that, described Resins, epoxy is the mixture of F-51 novolac epoxy and E-51 Resins, epoxy or the mixture of F-51 novolac epoxy and E-44 Resins, epoxy.
3. high-temperature resistant single-component epoxy structure glue according to claim 1 is characterized in that, described toughner is the polyfunctional group block macromolecular prepolymer with distant pawl type molecular structure.
4. high-temperature resistant single-component epoxy structure glue according to claim 1 is characterized in that, described filler is the mixture of ball aluminum powder, aluminum oxide powder and silicon powder.
5. high-temperature resistant single-component epoxy structure glue according to claim 4 is characterized in that, described ball aluminum powder particle diameter is 5 microns～15 microns, and the order number of described aluminum oxide powder is 400 orders, and the order number of described silicon powder is 1250 orders.
6. high-temperature resistant single-component epoxy structure glue according to claim 1 is characterized in that, described coupling agent is γ-amine propyl-triethoxysilicane.
7. high-temperature resistant single-component epoxy structure glue according to claim 1 is characterized in that, described solidifying agent is a Toluene-2,4-diisocyanate, the mixture of 4-two [N, N-dimethylamino] third urea and Dyhard RU 100.
8. high-temperature resistant single-component epoxy structure glue according to claim 1 is characterized in that, described thixotropic agent is a gas-phase silicon.
9. the preparation method of a high-temperature resistant single-component epoxy structure glue, it is characterized in that, described preparation method comprises: at first, with the raw material of following parts by weight is that 100 parts Resins, epoxy, 10 parts～25 parts toughner and 1 part～5 parts coupling agent add in the mixing kettle, stirring at normal temperature 1 hour～2 hours, the rotating speed of mixing kettle is 100rpm～180rpm; Then, the filler that in mixing kettle, adds 20 parts～40 parts, stirring at normal temperature 20 minutes～40 minutes, the rotating speed of mixing kettle is 1000rpm～1200rpm, after uniform mixture to be mixed is reduced to normal temperature, the solidifying agent that adds 5 parts～10 parts again, stirring at normal temperature 30 minutes, the rotating speed of mixing kettle is 100rpm～180rpm; At last, add 20 parts～40 parts filler in mixing kettle, stirring at normal temperature 20 minutes～40 minutes is regulated the viscosity discharging and can be obtained epoxy structural rubber.
10. the using method of a high-temperature resistant single-component epoxy structure glue is characterized in that, described using method comprises: at first, will treat that bonding plane cleans up; Then, epoxy structural rubber is evenly coated between two bonding planes; At last, under 120 ℃～150 ℃ temperature, solidified 30 minutes～60 minutes, can use behind the naturally cooling.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709983A (en) * | 2013-12-23 | 2014-04-09 | 东莞市亚聚电子材料有限公司 | High temperature resisting bottom filler glue and preparation method thereof |
| CN103740060A (en) * | 2013-12-23 | 2014-04-23 | 东莞市亚聚电子材料有限公司 | Low-halogen underfill adhesive and preparation method thereof |
| CN103756612A (en) * | 2013-12-23 | 2014-04-30 | 东莞市亚聚电子材料有限公司 | Low-temperature setting underfill adhesive and preparation method thereof |
| CN104356988A (en) * | 2014-10-31 | 2015-02-18 | 浙江同泰建设集团有限公司 | One-component epoxy resin sticky steel glue and preparation method thereof |
| CN106753112A (en) * | 2016-11-29 | 2017-05-31 | 广西大学 | A kind of epoxy construction structure glue |
| CN106753111A (en) * | 2016-11-29 | 2017-05-31 | 厦门山川材料科技有限公司 | A kind of formula and processing technology of the imitative porcelain cement of family expenses |
| CN108130042A (en) * | 2018-01-19 | 2018-06-08 | 重庆中田化工有限公司 | A kind of automobile sqtructural adhesive and preparation method thereof |
| CN113528056A (en) * | 2021-06-29 | 2021-10-22 | 深圳市金菱通达电子有限公司 | Heat-conducting structural adhesive for new energy power battery and manufacturing method thereof |
| CN113637441A (en) * | 2021-08-12 | 2021-11-12 | 长春艾德斯新材料有限公司 | Epoxy resin adhesive capable of being rapidly cured at room temperature and preparation method thereof |
| CN114032056A (en) * | 2021-11-15 | 2022-02-11 | 烟台海利泰粘合材料有限公司 | Single-component epoxy resin magnetic steel bonding structural adhesive |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103709983A (en) * | 2013-12-23 | 2014-04-09 | 东莞市亚聚电子材料有限公司 | High temperature resisting bottom filler glue and preparation method thereof |
| CN103740060A (en) * | 2013-12-23 | 2014-04-23 | 东莞市亚聚电子材料有限公司 | Low-halogen underfill adhesive and preparation method thereof |
| CN103756612A (en) * | 2013-12-23 | 2014-04-30 | 东莞市亚聚电子材料有限公司 | Low-temperature setting underfill adhesive and preparation method thereof |
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| CN103709983B (en) * | 2013-12-23 | 2015-12-30 | 东莞市亚聚电子材料有限公司 | A kind of high temperature resistant underfill and preparation method thereof |
| CN104356988A (en) * | 2014-10-31 | 2015-02-18 | 浙江同泰建设集团有限公司 | One-component epoxy resin sticky steel glue and preparation method thereof |
| CN106753112A (en) * | 2016-11-29 | 2017-05-31 | 广西大学 | A kind of epoxy construction structure glue |
| CN106753111A (en) * | 2016-11-29 | 2017-05-31 | 厦门山川材料科技有限公司 | A kind of formula and processing technology of the imitative porcelain cement of family expenses |
| CN108130042A (en) * | 2018-01-19 | 2018-06-08 | 重庆中田化工有限公司 | A kind of automobile sqtructural adhesive and preparation method thereof |
| CN113528056A (en) * | 2021-06-29 | 2021-10-22 | 深圳市金菱通达电子有限公司 | Heat-conducting structural adhesive for new energy power battery and manufacturing method thereof |
| CN113637441A (en) * | 2021-08-12 | 2021-11-12 | 长春艾德斯新材料有限公司 | Epoxy resin adhesive capable of being rapidly cured at room temperature and preparation method thereof |
| CN113637441B (en) * | 2021-08-12 | 2022-05-17 | 长春艾德斯新材料有限公司 | Epoxy resin adhesive capable of being rapidly cured at room temperature and preparation method thereof |
| CN114032056A (en) * | 2021-11-15 | 2022-02-11 | 烟台海利泰粘合材料有限公司 | Single-component epoxy resin magnetic steel bonding structural adhesive |
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Application publication date: 20101229 |