CN101397486A - Bi-component epoxide-resin adhesive and preparation method thereof - Google Patents
Bi-component epoxide-resin adhesive and preparation method thereof Download PDFInfo
- Publication number
- CN101397486A CN101397486A CNA2008102017641A CN200810201764A CN101397486A CN 101397486 A CN101397486 A CN 101397486A CN A2008102017641 A CNA2008102017641 A CN A2008102017641A CN 200810201764 A CN200810201764 A CN 200810201764A CN 101397486 A CN101397486 A CN 101397486A
- Authority
- CN
- China
- Prior art keywords
- component
- epoxy resin
- benzene
- resin
- resin adhesive
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Adhesives Or Adhesive Processes (AREA)
- Epoxy Resins (AREA)
Abstract
The invention relates to a two-component epoxy resin adhesive, including the following components: novolac epoxy resin, lipid ring type epoxy resin and terminal carboxylic acrylonitrile butadiene rubber in component A, and 1, 4-di-benzene (2, 4-diaminobenzene oxygen) in component B, wherein, the mass percentage of the lipid ring type epoxy resin is 20-35 percent of the novolac epoxy resin, the mass percentage of the terminal carboxylic acrylonitrile butadiene rubber CTBN is 12 percent of the novolac epoxy resin and the mass percentage of the 1, 4-di-benzene (2, 4-diaminobenzene oxygen) is 15-20 percent of the novolac epoxy resin; and the preparation of the two-component epoxy resin adhesive includes the step of evenly mixing the component A and the component B for use. The two-component epoxy resin adhesive used for conductive adhesive has good heat resistance, average stretching and shearing strength of 21.28MPa, simple preparation process and operation without solvent, and plays the role of protecting environment.
Description
Technical field
The invention belongs to the preparation field of organic adhesion agent, particularly relate to a kind of bi-component epoxide-resin adhesive and preparation method thereof.
Background technology
Conductive resin is that conductive particle and additive are scattered in a kind of electro-conductive material that forms in the resin equably, and along with the development of electronic industry, the use range of conductive resin is more and more wider.Along with development of high-tech, to the requirement of the resistance toheat of conductive resin more and more higher (long-time heat-resisting more than 200 ℃, moment is heat-resisting at 250 ℃), especially at aspects such as Aeronautics and Astronautics, military project, electronics, electric power, automobile, machineries.Conductive resin mainly is made up of resin matrix and conducting particles, and wherein resin matrix is given the conductive resin physical and mechanical property, so the selection of resin matrix is just very important.Novolac epoxy is because outstanding adhesive property and good chemical resistance and ageing resistance obtain extensive concern, alicyclic type epoxy resin has the good heat endurance energy equally as the thinner of regulation system viscosity, Resins, epoxy must just have practical value with solidifying agent reaction generation 3-D solid structure simultaneously, that is to say that solidifying agent also is the important component part of resin matrix, its performance has determined the quality of matrix resin to a certain extent.
At present, domestic research to high-temperature resistance adhesive is a lot, but is not a lot of but can reach the tackiness agent that high strength of joint can reach the ideal resistance toheat again simultaneously.People such as the Zhao Sheng of Beijing Inst. of Aeronautical Materials dragon, Liu Qingfang have introduced by high functionality Resins, epoxy AG-80 and bisphenol A type epoxy resin on the volume supplementary issue in October, 2003 " aeronautical material journal " the 23rd and have mixed, adopt and mix amine curing agent, that has made self-vulcanizing can heat-resisting 200 ℃ tackiness agent, but this kind tackiness agent tensile shear strength at high temperature is not ideal, only is 3MPa.People such as Wang Chao, Zhang Bin has introduced a kind of Resins, epoxy of solvent-free and high temperature-resistant on " Chinese tackiness agent " 1998 the 8th the 3rd phases of volume, adopt bismaleimides as matrix resin, with 4,4 '
-Diaminodiphenylmethane is as solidifying agent, and shearing resistance is up to 10MPa in the time of 250 ℃, but its curing process complexity is unfavorable for construction.
Summary of the invention
Technical problem to be solved by this invention provides a kind of bi-component epoxide-resin adhesive and preparation method thereof; conductive resin of the present invention is good with the bi-component epoxide-resin adhesive resistance toheat; tensile shear strength on average can reach 21.28MPa; this preparation process is simple; use solvent-free operation, played the effect of protection environment.
A kind of bi-component epoxide-resin adhesive of the present invention, its component comprises: A component novolac epoxy, alicyclic type epoxy resin and nbr carboxyl terminal, B component 1,4-two (2, the 4-diamino phenoxy) benzene, wherein the mass percent of alicyclic type epoxy resin is the 20-35% of phenol aldehyde type epoxy resin, the mass percent of nbr carboxyl terminal CTBN is 12% of a phenol aldehyde type epoxy resin, 1, the mass percent of two (2, the 4-diamino phenoxy) benzene of 4-is the 15-20% of novolac epoxy.
Described 1, the preparation method of two (2, the 4-diamino phenoxy) benzene of 4-, key step comprises: 1, and two (2, the 4-2,4-dinitrophenoxy base) benzene of 4-, at palladium/charcoal, hydrazine hydrate solution and alcohol solvent in 70 ℃ of-85 ℃ of temperature range internal reactions after 1～5 hour, filtered while hot, cooling mother liquor, separate out crystalline product, filter, vacuum-drying obtains 1, two (2, the 4-diamino phenoxy) the benzene crystal powders of 4-.
The oxirane value of described novolac epoxy is 0.526-0.588;
Described alicyclic type epoxy resin is 3,4-epoxy group(ing) heptanaphthenic acid-3 ', 4 '-epoxy group(ing) hexamethylene methyl esters;
Described nbr carboxyl terminal is that Shanghai EMST Electron Material Co., Ltd produces.
The preparation of a kind of bi-component epoxide-resin adhesive of the present invention comprises: component A and B component normal temperature are mixed down, and stirring gets final product.
Bi-component epoxide-resin adhesive of the present invention has the good heat endurance energy, these characteristics depend on the novolac epoxy as resin matrix, the cycloaliphatic epoxy resin (3 of reactive thinner, 4-epoxy group(ing) heptanaphthenic acid-3 ', 4 '-epoxy group(ing) hexamethylene methyl esters) and as 1 of solidifying agent, two (2, the 4-diamino phenoxy) benzene of 4-, these components help the raising of resistance toheat for the tackiness agent after solidifying provides the inflexible skeleton.
Bi-component epoxide-resin adhesive of the present invention is with respect to traditional conductive resin, its tensile shear strength has tangible improvement, polynary arylamine structure is depended in this change, it makes cured article have higher cross-linking density, and the diether linkage structure that links to each other with phenyl ring has simultaneously improved the snappiness of structure.
Beneficial effect
(1) conductive resin bi-component epoxide-resin adhesive of the present invention, resistance toheat is good, and tensile shear strength on average can reach 21.28MPa.
(2) this preparation process is simple, uses solvent-free operation, has played the effect of protection environment.
Description of drawings
Fig. 1 is the thermogravimetric curve of bi-component epoxide-resin adhesive
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Pressing novolac epoxy weight 100 calculates for unit
A B component component
Novolac epoxy 100 1, two (2, the 4-diamino phenoxy) benzene 20 of 4-
CTBN 12
Alicyclic type epoxy resin 24
Treating that the time spent mixes two kinds of components gets final product, and its performance test is as shown in table 1.Find that by thermogravimetic analysis (TGA) the product behind this kind adhesive solidification only is 1.51% at 200 ℃ of thermal weight losses.
As can be seen from Figure 1, embodiment 1 cured product has the good heat endurance energy, and 200 ℃ of thermal weight losses only are that 1.51%, 300 ℃ thermal weight loss only is 4.49%.
The comparative example 1
Pressing novolac epoxy weight 100 calculates for unit
Novolac epoxy 100
CTBN 12
Thinner 24
Dyhard RU 100 20
Treating that each composition mixes gets final product, and its performance test is as shown in table 1.
Table 1 embodiment 1 and comparative example's 1 tensile shear strength test
| |
Comparative example's 1 tensile shear strength (MPa) |
| 21.28 | 14.77 |
As can be seen from Table 1, the tensile shear strength of embodiment 1 is obviously greater than the comparative example, and 1, two (2, the 4-diamino phenoxy) benzene of 4-are as solidifying agent, and the bonding strength of resin system is had clear improvement, and tensile shear strength on average can reach 21.28MPa.
Embodiment 2
Pressing novolac epoxy weight 100 calculates for unit
A B component component
Novolac epoxy 100 1, two (2, the 4-diamino phenoxy) benzene 20 of 4-
CTBN 12
Alicyclic type epoxy resin 30
Treating that the time spent mixes two kinds of components gets final product.
Embodiment 3
Pressing novolac epoxy weight 100 calculates for unit
A B component component
Novolac epoxy 100 1, two (2, the 4-diamino phenoxy) benzene 20 of 4-
CTBN 12
Alicyclic type epoxy resin 35
Treating that the time spent mixes two kinds of components gets final product.
Pressing novolac epoxy weight 100 calculates for unit
A B component component
Novolac epoxy 100 1, two (2, the 4-diamino phenoxy) benzene 15 of 4-
CTBN 12
Alicyclic type epoxy resin 24
Treating that the time spent mixes two kinds of components gets final product.
Claims (5)
1. bi-component epoxide-resin adhesive, its component comprises: A component novolac epoxy, alicyclic type epoxy resin and nbr carboxyl terminal, B component 1, two (2, the 4-diamino phenoxy) benzene of 4-, wherein the mass percent of alicyclic type epoxy resin is the 20-35% of phenol aldehyde type epoxy resin, the mass percent of nbr carboxyl terminal CTBN is 12% of a phenol aldehyde type epoxy resin, 1, the mass percent of two (2, the 4-diamino phenoxy) benzene of 4-is the 15-20% of novolac epoxy.
2. a kind of bi-component epoxide-resin adhesive according to claim 1, it is characterized in that: described 1,4-two (2, the 4-diamino phenoxy) preparation method of benzene, key step comprises: 1, two (2, the 4-2,4-dinitrophenoxy base) benzene of 4-, in palladium/charcoal, hydrazine hydrate solution and alcohol solvent system in 70 ℃ of-85 ℃ of temperature range internal reactions after 1～5 hour, filtered while hot, the cooling mother liquor is separated out crystalline product, filters, vacuum-drying, obtain 1, two (2, the 4-diamino phenoxy) the benzene crystal powders of 4-.
3. a kind of bi-component epoxide-resin adhesive according to claim 1 is characterized in that: the oxirane value of described novolac epoxy is 0.526-0.588.
4. a kind of bi-component epoxide-resin adhesive according to claim 1 is characterized in that: described alicyclic type epoxy resin is 3,4-epoxy group(ing) heptanaphthenic acid-3 ', 4 '-epoxy group(ing) hexamethylene methyl esters.
5. the preparation of a bi-component epoxide-resin adhesive comprises: component A and B component are mixed at normal temperatures, and stirring gets final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102017641A CN101397486B (en) | 2008-10-24 | 2008-10-24 | Bi-component epoxide-resin adhesive and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102017641A CN101397486B (en) | 2008-10-24 | 2008-10-24 | Bi-component epoxide-resin adhesive and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101397486A true CN101397486A (en) | 2009-04-01 |
| CN101397486B CN101397486B (en) | 2012-01-04 |
Family
ID=40516335
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008102017641A Expired - Fee Related CN101397486B (en) | 2008-10-24 | 2008-10-24 | Bi-component epoxide-resin adhesive and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101397486B (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102031082A (en) * | 2010-12-10 | 2011-04-27 | 东华大学 | Benzimidazole diamine curing type epoxy adhesive and preparation method thereof |
| CN101602926B (en) * | 2009-07-16 | 2012-05-02 | 常熟市江南粘合剂有限公司 | Room temperature curing epoxy adhesive and preparation method thereof |
| CN101544879B (en) * | 2009-04-30 | 2012-06-13 | 东华大学 | Preparation method for high strength solventless epoxy adhesive |
| CN102732201A (en) * | 2012-06-25 | 2012-10-17 | 烟台开发区泰盛精化新材料有限公司 | Wear-resistant and weather-resistant epoxy resin coating adhesive and its preparation method |
| CN103214793A (en) * | 2013-04-22 | 2013-07-24 | 东华大学 | Advanced composite material matrix resin and preparation method thereof |
| CN104293270A (en) * | 2014-10-31 | 2015-01-21 | 浙江红高梁木业有限公司 | Epoxy resin adhesive used for wood floor and preparation method of epoxy resin adhesive |
| CN105331305A (en) * | 2015-12-16 | 2016-02-17 | 太仓康盛化工有限公司 | Fast-curing epoxy resin adhesive |
| CN112280247A (en) * | 2020-10-29 | 2021-01-29 | 西安永兴科技发展有限公司 | High-temperature-resistant high-humidity-heat-resistant fiber-reinforced composite material and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6265469B1 (en) * | 1999-09-02 | 2001-07-24 | Du Pont Wirex Ltd | Epoxy resin adhesive for flexible printed circuits |
| CN101130679B (en) * | 2006-08-25 | 2011-11-16 | 比亚迪股份有限公司 | Adhesion agent and method of manufacturing the same |
-
2008
- 2008-10-24 CN CN2008102017641A patent/CN101397486B/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101544879B (en) * | 2009-04-30 | 2012-06-13 | 东华大学 | Preparation method for high strength solventless epoxy adhesive |
| CN101602926B (en) * | 2009-07-16 | 2012-05-02 | 常熟市江南粘合剂有限公司 | Room temperature curing epoxy adhesive and preparation method thereof |
| CN102031082A (en) * | 2010-12-10 | 2011-04-27 | 东华大学 | Benzimidazole diamine curing type epoxy adhesive and preparation method thereof |
| CN102031082B (en) * | 2010-12-10 | 2013-04-03 | 东华大学 | Benzimidazole diamine curing type epoxy adhesive and preparation method thereof |
| CN102732201A (en) * | 2012-06-25 | 2012-10-17 | 烟台开发区泰盛精化新材料有限公司 | Wear-resistant and weather-resistant epoxy resin coating adhesive and its preparation method |
| CN102732201B (en) * | 2012-06-25 | 2014-04-09 | 烟台开发区泰盛精化新材料有限公司 | Wear-resistant and weather-resistant epoxy resin coating adhesive and its preparation method |
| CN103214793A (en) * | 2013-04-22 | 2013-07-24 | 东华大学 | Advanced composite material matrix resin and preparation method thereof |
| CN104293270A (en) * | 2014-10-31 | 2015-01-21 | 浙江红高梁木业有限公司 | Epoxy resin adhesive used for wood floor and preparation method of epoxy resin adhesive |
| CN104293270B (en) * | 2014-10-31 | 2015-11-04 | 浙江红高梁木业有限公司 | A kind of epoxyn for timber floor and preparation method thereof |
| CN105331305A (en) * | 2015-12-16 | 2016-02-17 | 太仓康盛化工有限公司 | Fast-curing epoxy resin adhesive |
| CN112280247A (en) * | 2020-10-29 | 2021-01-29 | 西安永兴科技发展有限公司 | High-temperature-resistant high-humidity-heat-resistant fiber-reinforced composite material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101397486B (en) | 2012-01-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101397486B (en) | Bi-component epoxide-resin adhesive and preparation method thereof | |
| CN110128982B (en) | Normal-temperature fast-curing structural adhesive and preparation method thereof | |
| CN105694790B (en) | It is a kind of can the epoxy adhesive of rapid disassembling and its preparation and disassembling method | |
| CN102702743B (en) | High-toughness high-heat-conduction epoxy-imine resin system and preparation method and application thereof | |
| CN111154442B (en) | Environment-friendly high-temperature-resistant modified epoxy resin adhesive and preparation method thereof | |
| CN107779147B (en) | High-strength epoxy honeycomb adhesive and preparation method thereof | |
| CN102618200B (en) | Organosilicone-epoxy-polyimide adhesive and preparation method thereof | |
| CN101818037A (en) | Room-temperature curing epoxy structural adhesive composition and preparation method thereof | |
| CN101781540A (en) | High-performance conducting resin and preparation method thereof | |
| CN102020961A (en) | High-heat-conduction flexible aluminum base copper-clad plate for LED heat radiating substrate | |
| CN104693684A (en) | Adhesive, organic ceramic plate and preparation method of organic ceramic plate | |
| CN103160229B (en) | Glue liquor for environment-friendly light laminated board, laminated board and preparation method of glue liquor | |
| CN105176081A (en) | Preparation method for flame-retardant heat-resistant antenna radome base material | |
| CN103963378A (en) | High thermal conductivity type metal-based copper clad laminate and preparation method thereof | |
| CN105061764B (en) | A kind of thermoset polyimide resin and its composite laminate and their preparation method and application | |
| CN114410260A (en) | Modified epoxy resin adhesive and preparation method thereof | |
| JP2021050329A (en) | Recyclable led packaging conductive adhesive composition and method for manufacturing the same | |
| CN114752335A (en) | Preparation method of high-temperature-resistant high-adhesion conductive silver adhesive | |
| CN101845143B (en) | Modified bismaleimide resin as well as preparation method and application thereof | |
| CN105001825A (en) | Low temperature resisting epoxy resin adhesive and preparation method thereof | |
| CN101503608B (en) | Phenolic epoxy resin system conductive adhesive and preparation thereof | |
| CN111334233A (en) | Adhesive for conductive cloth adhesive tape, preparation method and application thereof | |
| CN116751531A (en) | Heat-conducting insulating adhesive film and preparation method and application thereof | |
| CN103963381B (en) | Metal-based copper-clad plate and preparation method thereof | |
| CN114752314B (en) | High-durability high-temperature cured epoxy structural adhesive film and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120104 Termination date: 20181024 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |