CN117736678A - Low-temperature rapid-curing epoxy resin composition and preparation method thereof - Google Patents
Low-temperature rapid-curing epoxy resin composition and preparation method thereof Download PDFInfo
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- CN117736678A CN117736678A CN202310510741.3A CN202310510741A CN117736678A CN 117736678 A CN117736678 A CN 117736678A CN 202310510741 A CN202310510741 A CN 202310510741A CN 117736678 A CN117736678 A CN 117736678A
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 38
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 38
- 239000000203 mixture Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims description 14
- 239000012745 toughening agent Substances 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- 239000000945 filler Substances 0.000 claims abstract description 17
- 239000003381 stabilizer Substances 0.000 claims abstract description 11
- 239000013008 thixotropic agent Substances 0.000 claims abstract description 11
- 239000000049 pigment Substances 0.000 claims abstract description 10
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 9
- 150000001875 compounds Chemical class 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 15
- -1 imidazole compound Chemical class 0.000 claims description 14
- 238000005303 weighing Methods 0.000 claims description 13
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 9
- 239000002270 dispersing agent Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 239000004593 Epoxy Substances 0.000 claims description 7
- 239000003292 glue Substances 0.000 claims description 5
- 229920005989 resin Polymers 0.000 claims description 5
- 239000011347 resin Substances 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 150000001412 amines Chemical class 0.000 claims description 4
- 239000004408 titanium dioxide Substances 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- 230000002378 acidificating effect Effects 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 claims description 2
- 125000003396 thiol group Chemical group [H]S* 0.000 claims description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims 6
- 229910002092 carbon dioxide Inorganic materials 0.000 claims 3
- 239000001569 carbon dioxide Substances 0.000 claims 3
- 239000006096 absorbing agent Substances 0.000 claims 2
- 230000002401 inhibitory effect Effects 0.000 claims 2
- 230000003213 activating effect Effects 0.000 claims 1
- 230000032683 aging Effects 0.000 claims 1
- 235000012239 silicon dioxide Nutrition 0.000 claims 1
- 239000000377 silicon dioxide Substances 0.000 claims 1
- 238000010276 construction Methods 0.000 abstract description 2
- 238000004134 energy conservation Methods 0.000 abstract 1
- 238000001723 curing Methods 0.000 description 25
- 230000001070 adhesive effect Effects 0.000 description 8
- 239000000853 adhesive Substances 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 238000004806 packaging method and process Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 241000276425 Xiphophorus maculatus Species 0.000 description 4
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 4
- 239000000498 cooling water Substances 0.000 description 4
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 4
- 229910021485 fumed silica Inorganic materials 0.000 description 4
- 230000009974 thixotropic effect Effects 0.000 description 4
- 229910002012 Aerosil® Inorganic materials 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 238000007790 scraping Methods 0.000 description 3
- 229920000459 Nitrile rubber Polymers 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- HNYOPLTXPVRDBG-UHFFFAOYSA-N barbituric acid Chemical compound O=C1CC(=O)NC(=O)N1 HNYOPLTXPVRDBG-UHFFFAOYSA-N 0.000 description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical class OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 239000000539 dimer Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229920006332 epoxy adhesive Polymers 0.000 description 2
- 229920006335 epoxy glue Polymers 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 2
- 239000004926 polymethyl methacrylate Substances 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 238000004904 shortening Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- AJSTXXYNEIHPMD-UHFFFAOYSA-N triethyl borate Chemical compound CCOB(OCC)OCC AJSTXXYNEIHPMD-UHFFFAOYSA-N 0.000 description 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 2
- IMQFZQVZKBIPCQ-UHFFFAOYSA-N 2,2-bis(3-sulfanylpropanoyloxymethyl)butyl 3-sulfanylpropanoate Chemical compound SCCC(=O)OCC(CC)(COC(=O)CCS)COC(=O)CCS IMQFZQVZKBIPCQ-UHFFFAOYSA-N 0.000 description 1
- OWMNWOXJAXJCJI-UHFFFAOYSA-N 2-(oxiran-2-ylmethoxymethyl)oxirane;phenol Chemical compound OC1=CC=CC=C1.OC1=CC=CC=C1.C1OC1COCC1CO1 OWMNWOXJAXJCJI-UHFFFAOYSA-N 0.000 description 1
- JJSYPAGPNHFLML-UHFFFAOYSA-N 2-ethyl-2-(hydroxymethyl)propane-1,3-diol;3-sulfanylpropanoic acid Chemical compound OC(=O)CCS.OC(=O)CCS.OC(=O)CCS.CCC(CO)(CO)CO JJSYPAGPNHFLML-UHFFFAOYSA-N 0.000 description 1
- VSZSIEBALNXIFG-UHFFFAOYSA-N 2-hydroxyethyl 2,2-bis(sulfanyl)acetate Chemical compound OCCOC(=O)C(S)S VSZSIEBALNXIFG-UHFFFAOYSA-N 0.000 description 1
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 1
- IISBACLAFKSPIT-UHFFFAOYSA-N Bisphenol A Natural products C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 1
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 1
- VTLHIRNKQSFSJS-UHFFFAOYSA-N [3-(3-sulfanylbutanoyloxy)-2,2-bis(3-sulfanylbutanoyloxymethyl)propyl] 3-sulfanylbutanoate Chemical compound CC(S)CC(=O)OCC(COC(=O)CC(C)S)(COC(=O)CC(C)S)COC(=O)CC(C)S VTLHIRNKQSFSJS-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 125000002723 alicyclic group Chemical group 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- YQGOWXYZDLJBFL-UHFFFAOYSA-N dimethoxysilane Chemical compound CO[SiH2]OC YQGOWXYZDLJBFL-UHFFFAOYSA-N 0.000 description 1
- UBHZUDXTHNMNLD-UHFFFAOYSA-N dimethylsilane Chemical compound C[SiH2]C UBHZUDXTHNMNLD-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Substances OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 1
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000013035 low temperature curing Methods 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920006295 polythiol Polymers 0.000 description 1
- 150000004053 quinones Chemical class 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Epoxy Resins (AREA)
Abstract
The low-temperature rapid-curing epoxy resin composition comprises the following components in parts by weight: 20-40 parts of epoxy resin, 5-10 parts of toughening agent, 20-30 parts of curing agent, 5-10 parts of accelerator, 0.1-1 part of stabilizer, 10-15 parts of filler, 2-10 parts of pigment, 1-5 parts of thixotropic agent and 0.1-1 part of auxiliary agent. The composition has the advantages of quick curing, good stability, excellent moisture and heat resistance, shortened curing time, energy conservation and shortened construction period.
Description
Technical Field
The invention belongs to the technical field of adhesives, and particularly relates to a specific single-component epoxy resin composition and a preparation method thereof, wherein the application field is the industries of lighting industry, integrated circuits, circuit boards and the like which need a low-temperature curing bonding mode.
Background
LED lighting technology has been a mainstream lighting method in recent years because of its energy saving, environmental protection, long life, flexible use shape and scene, and the like, and has largely replaced conventional lighting methods. The LED light bar is adhered by using an aluminum substrate as an assembly circuit board, using a patch LED for assembly, adopting a fixed mode of adhesive dispensing and adhering, and having the advantages of thin thickness and no space occupation. The application is becoming more and more widespread.
At present, the main flow of bonding of the LED light bars adopts the full-automatic processes of machine dispensing, bonding and curing, and mainly adopts two bonding modes of UV (ultraviolet) glue and low-temperature epoxy glue. The UV adhesive is a mainstream use trend, and is mainly characterized by quick curing time, no need of heating curing, no need of mixing and the like compared with the epoxy adhesive. However, the UV adhesive has an unsatisfactory adhesion to some materials, and is not suitable for outdoor environments with extreme weather resistance. Compared with UV glue, epoxy glue has the advantages of strong weather resistance, chemical reagent resistance, high bonding strength to metal and plastic, solidification only by heating and the like, and is increasingly favored in the market. However, most products on the market have long curing time, usually 10-20 minutes, which affects the production efficiency of the production line and is difficult to meet the production requirement. And the commonly used single-component quick-curing epoxy system has the characteristics of lower strength and general wet heat resistance, and the commercial products can not meet the requirements of the LED industry on the comprehensive performance of the products gradually.
Disclosure of Invention
The invention aims to solve the defect that the traditional single-component epoxy adhesive is difficult to cure rapidly and has high stability, overcome the defect that a mercaptan system is poor in humidity resistance and heat resistance, and provide a single-component low-temperature rapid-curing epoxy resin composition aiming at the bonding requirement of the lighting industry and a preparation method thereof. Has excellent adhesive property to common materials in the electronic industry such as metal, plastic and the like. The method has the advantages of greatly shortening the curing time, improving the efficiency of the LED light source preparation assembly line, saving energy and shortening the construction period. The specific properties of the composition are as follows: the curing speed is below 3min at 80 ℃, the initial shear strength (bonded with the aluminum substrate) is greater than 25MPa, and the shear strength is kept above 20MPa after double-eighth-fifth-aging for 168 h.
The present inventors have made a series of studies in order to solve the above-mentioned problems, and as a result, have found that the above-mentioned objects are achieved by a series of resin compositions. The method comprises the following steps: 20-40 parts of epoxy resin, 8-15 parts of toughening agent, 20-30 parts of curing agent, 2-8 parts of accelerator, 0.2-1 part of stabilizer, 10-15 parts of filler, 2-10 parts of pigment, 1-5 parts of thixotropic agent and 0.1-1 part of auxiliary agent.
The epoxy resin is a compound containing two or more epoxy groups per molecule, and contains glycidyl ether bisphenol A, bisphenol F type epoxy resin, glycidyl esters, glycidyl amines, alicyclic epoxy resin, hydrogenated epoxy resin, phenolic epoxy resin and the like. Bisphenol a and bisphenol F type epoxy resins are preferable from the viewpoint of general versatility.
Still further preferred embodiments are mixtures of one or more of Epikote 828El, NERF-170, hansen, epikote 862, korea Kelong KF-8100, DY128 from Shandong, shell.
The toughening agent is a mixture of modified epoxy resin and other substances capable of increasing toughness of epoxy resin compounds and epoxy resin, and comprises a mixture formed by dispersing nitrile rubber core-shell particles in the epoxy resin, polyurethane, dimer acid modified epoxy resin and the like.
In a further preferred embodiment, the toughening agent is one or more of core-shell toughening type Japanese KaNEKA-MX 125, polyurethane modified epoxy Dow chemical DER-791, carboxyl terminated liquid nitrile rubber complexed with high new CTBN1300 x 8, silicone modified epoxy modified Albiflex297, dimer acid modified epoxy resin complexed with high new EPD 172.
The curing agent is a polythiol compound, which refers to a compound with more than two thiol groups in the molecule. For example: trimethylolpropane tris (3-mercaptopropionate), pentaerythritol tetrakis (3-mercaptobutyrate), 3-mercaptopropionate- [2,4, 6-trioxo-1, 3, 5-triazine-1, 3,5 (2H, 4H, 6H) -yl ] tris-2, 1-ethylene glycol, ethylene glycol dimercaptoethanate, trimethylolpropane tris (beta-mercaptopropionate), and the like.
Still further preferred embodiments are mixtures of one or more of Karenz PE1, SC organic chemistry Lecad803, lecad806, thiocure 331 of Bruno Bock, germany, of Showa.
The accelerator is a compound which can activate and release an alkaline substance under a curing temperature condition, is generally inactive or less active at room temperature, and can inhibit activity at a low temperature, such as an imidazole compound, an acid anhydride compound, an amine adduct, a urea compound, an amine imide compound, or the like. Imidazole and amine accelerators are preferred from the viewpoint of curing temperature and curing system.
Still more preferably, the accelerator is one or more of Fujicure FXR1020, japanese-taste essence AjicurePN-H, japanese-taste essence AjicurePN-23J, japanese-taste essence AjicureMY-24.
The stabilizer is a compound capable of releasing an acidic substance in the resin mixture to effectively inhibit the occurrence of the resin curing reaction, and is usually a compound having Lewis acidity, and is usually a solid organic acid. Including carboxylic acid group containing compounds, quinone compounds, phenol compounds, enol compounds, barbituric acid, boric acid compounds, and the like. From the viewpoint of accelerator selection, barbituric acid, boric acid compounds are preferable.
Still further preferred is that the accelerator is HSCHEM 3200, triethyl borate in the chemical industry.
The filler is one or a mixture of more of nano calcium carbonate, silicon micropowder, platy talcum powder and mica powder.
Still more preferably, the filler is a mixture of one or more of nano calcium carbonate CCR-S10 of Japanese white stone, viscoexcel30HV, viscolite-OS, platy talcum powder HY-TA06 of sea-borne powder, platy talcum powder HY-TM1 of sea-borne powder, platy talcum powder AG-609 of U.S. Specialty Minerals and silicon micropowder NQ1050 of Jiangsu-associated new material.
The pigment is titanium dioxide. Preferably DuPont Ti-Pure R706.
The thixotropic agent is hydrophobic fumed silica, preferably fumed silica obtained by treatment with dimethoxysilane, dimethylsilane or hexamethylsilane. Fumed silica having a specific surface area of 50 to 200 is preferable from the viewpoints of viscosity increase and thixotropic property.
Still further preferred embodiments are those wherein the fumed silica is a mixture of one or more of AEROSIL R202, wak HDK H20.
The auxiliary agent is other components capable of improving the resin compound, such as a coupling agent, a defoaming agent, a dispersing agent, a water absorbent and the like.
Still more preferably, the auxiliary agent is a mixture of one or more of KBM-403, KBM-503, X-12-967C, X-12-1290, X-12-1287A, BYK4511, pick chemical, germany.
The invention also provides a preparation method of the epoxy compound, which comprises the following steps:
and 1, weighing the epoxy resin and the toughening agent according to the weight, and heating the epoxy resin and the toughening agent to 50 ℃ if the viscosity of the toughening agent is too high to weigh.
Step 2: the epoxy resin and the toughening agent are added into a small-sized 1L dynamic mixer which can be pumped by cooling water and can be vacuumized, stirred and dispersed for 30 minutes, and wall scraping is carried out for a plurality of times until the materials are uniform.
Step 3: the filler and pigment are weighed according to the weight, added into a dynamic mixer, rapidly stirred for 2-3 hours at a high speed of 2000rpm, and scraped for a plurality of times until the powder is uniformly dispersed.
Step 4: weighing stabilizer and curing agent according to weight, adding into a dynamic mixer, and dispersing at high speed and low speed for 1 hour.
Step 5: and (3) opening cooling water to keep the temperature of the glue solution at 15-25 ℃, weighing the accelerator according to weight, adding the accelerator into a dynamic mixer, and stirring for 1 hour.
Step 6: the thixotropic agent is weighed according to the weight, added into a dynamic mixer, slowly stirred until the mixture is completely mixed, then vacuum is opened, and slowly stirred for 1 hour under vacuum for complete defoaming.
Detailed Description
The invention is further illustrated below in connection with specific examples.
Comparative example 1 preparation method:
the following components were weighed according to the following table:
| comparative example 1 | ||
| Description of the invention | Brand/substance name | Parts by weight |
| Epoxy resin | NERF-170 | 40 |
| Toughening agent | 102C-4L | 8 |
| Curing agent | Lecad803 | 30 |
| Stabilizing agent | HSCHEM 3200 | 0.2 |
| Accelerating agent | Fujicure FXR1020 | 8 |
| Filler 1 | NQ1050 | 6 |
| Filler 2 | CCR-S10 | 3.5 |
| Filler 3 | Viscoexcel 30HV | 3.5 |
| Pigment | Ti-Pure R706 | 5 |
| Thixotropic agent | Aerosil R202 | 2 |
| Auxiliary agent | KBM-403 | 1 |
According to the preparation method of the epoxy compound, the method comprises the following steps: step 1: the epoxy resin and the toughening agent are weighed according to the weight, and if the viscosity of the toughening agent is too high to be weighed, the toughening agent is heated to 50 ℃ for weighing. Step 2: the epoxy resin and the toughening agent are added into a small-sized 1L dynamic mixer which can be pumped by cooling water and can be vacuumized, stirred and dispersed for 30 minutes, and wall scraping is carried out for a plurality of times until the materials are uniform. Step 3: weighing filler and pigment according to weight, adding into a dynamic mixer, rapidly reading and stirring at high speed of 2000rpm for 2-3 hours, scraping the wall for several times until the powder is uniformly dispersed. Step 4: weighing stabilizer and curing agent according to weight, adding into a dynamic mixer, and dispersing at high speed and low speed for 1 hour. Step 5: and (3) opening cooling water to keep the temperature of the glue solution at 15-25 ℃, weighing the accelerator according to weight, adding the accelerator into a dynamic mixer, and stirring for 1 hour. Step 6: weighing thixotropic agent according to weight, adding into a dynamic mixer, slowly stirring until complete mixing, then opening vacuum, slowly stirring under vacuum for 1 hour to sufficiently defoam, and packaging after uniform bubble-free.
Mixing according to the preparation method, dispersing at high speed, cooling, stirring, vacuum defoaming until the mixture is uniform and has no bubbles, and sub-packaging to obtain the product.
| Example 2 | ||
| Description of the invention | Brand/substance name | Parts by weight |
| Epoxy resin | Epikote 828El | 25 |
| Toughening agent | MX125 | 15 |
| Curing agent | Karenz PE1 | 30 |
| Stabilizing agent | Boric acid triethyl ester | 0.2 |
| Accelerating agent | AjicurePN-H | 5 |
| Filler 1 | NQ1050 | 6 |
| Filler 2 | Viscoexcel 30HV | 3.5 |
| Filler 3 | AG-609 | 3.5 |
| Pigment | Ti-Pure R706 | 2 |
| Thixotropic agent | Aerosil R202 | 5 |
| Auxiliary agent | X-12-967C | 0.1 |
Mixing according to the preparation method, dispersing at high speed, cooling, stirring, vacuum defoaming until the mixture is uniform and has no bubbles, and sub-packaging to obtain the product.
| Example 3 | ||
| Description of the invention | Brand/substance name | Parts by weight |
| Epoxy resin | AG-80 | 20 |
| Toughening agent | AG-609 | 15 |
| Curing agent | Lecad803 | 28 |
| Stabilizing agent | HSCHEM 3200 | 1 |
| Accelerating agent | Ajicure PN-23 | 3 |
| Filler 1 | NQ1050 | 8 |
| Filler 2 | CCR-S10 | 3.5 |
| Filler 3 | HY-TM1 | 3.5 |
| Pigment | Ti-Pure R706 | 10 |
| Thixotropic agent | HDK H20 | 1 |
| Auxiliary agent | X-12-1287A | 1 |
Mixing according to the preparation method, dispersing at high speed, cooling, stirring, vacuum defoaming until the mixture is uniform and has no bubbles, and sub-packaging to obtain the product.
Mixing according to the preparation method, dispersing at high speed, cooling, stirring, vacuum defoaming until the mixture is uniform and has no bubbles, and sub-packaging to obtain the product.
Mixing according to the preparation method, dispersing at high speed, cooling, stirring, vacuum defoaming until the mixture is uniform and has no bubbles, and sub-packaging to obtain the product.
The adhesive samples prepared in the above 1 comparative example and 5 examples were subjected to performance tests, mainly to test the viscosity, thixotropic property, curing speed, stability, shear strength, resistance to heat and humidity, etc.
The specific test method is as follows:
viscosity/thixotropic: an Dongpa rheometer MCR72 rheometer, viscosity was measured at 25 ℃,2rpm and 20 rpm. The viscosity at 2rpm divided by the viscosity at 20rpm calculated thixotropic.
Curing speed: A TA DSC25 differential scanning calorimeter, procedure for 30min at constant temperature of 80℃and curing was completed when 98% of peak area was reached.
Stability: the gum sample was stored at 40℃for 7 days to measure the viscosity at 2rpm, and the lack of doubling of the viscosity indicated stable storage.
Shear strength: the adhesive was tested for shear strength on aluminum and PMMA specimens using a universal tensile machine.
Wet heat resistance: the shear strength was measured again after the above shear samples were stored in a double-eight-five environmental box for 168 hours.
Various performance test tables for the products prepared in the examples of the invention:
* 1.2. All test PMMA samples were broken.
From a comparison of comparative example 1 and example 1, it is understood that the present invention can satisfy the advantage of better stability while the curing speed is faster. The comparative example 1 and examples 2 to 5 show that the moisture and heat resistance of the invention are improved remarkably. As shown by the performance test results, the invention has the performance of simultaneously meeting the requirements of quick curing and excellent stability, and simultaneously overcomes the defect of poor moisture and heat resistance. The adhesive force is strong, most of lighting industry standards in the market are met, and the product has excellent applicability and excellent performance.
Claims (3)
1. The low-temperature rapid-curing epoxy resin composition is characterized by comprising the following components in parts by weight: 20-40 parts of epoxy resin, 8-15 parts of toughening agent, 20-30 parts of curing agent, 2-8 parts of accelerator, 0.2-1 part of stabilizer, 10-15 parts of filler, 2-10 parts of pigment, 1-5 parts of thixotropic agent and 0.1-1 part of auxiliary agent, wherein the epoxy resin is a mixture of modified epoxy resin and other substances capable of increasing toughness of the epoxy resin compound and the epoxy resin, the curing agent is a compound with more than two thiol groups in the molecule, the compound comprises an imidazole compound, an anhydride compound, an amine adduct, a urea compound or an amine imide compound, the accelerator is a compound capable of activating and releasing alkaline substances under the condition of curing temperature, the compound is generally inactive or lower in activity at room temperature, the auxiliary agent is a compound capable of inhibiting activity at low temperature, the compound comprises an imidazole compound, an anhydride compound, an amine adduct, a urea compound or an amine imide compound, the stabilizer is a compound capable of releasing acidic substances in the resin mixture, thereby effectively inhibiting the resin reaction, the curing agent is a plate-shaped compound, the epoxy resin is a dispersing agent is a silicon dioxide, the mixture is a dispersing agent, the titanium dioxide is a water-absorbing agent, the titanium dioxide powder is a water-absorbing agent, the mixture is a plurality of silicon dioxide powder, the dispersing agent is a silicon dioxide powder, the dispersing agent is the titanium dioxide powder, the dispersing agent is the carbon dioxide powder is the dispersing agent is the carbon dioxide, the dispersing agent is the carbon dioxide.
2. A method of preparing the epoxy resin composition of claim 1, comprising: respectively weighing epoxy resin and a toughening agent according to weight, adding the epoxy resin and the toughening agent into a dynamic mixer, stirring for 30 minutes, weighing filler according to weight, adding pigment into the dynamic mixer, stirring for 2-3 hours, weighing a stabilizing agent according to weight, adding a curing agent into the dynamic mixer, stirring for 1 hour, keeping the temperature of a glue solution at 15-25 ℃, weighing an accelerating agent according to weight, adding the accelerating agent into the dynamic mixer, stirring for 1 hour, weighing a thixotropic agent according to weight, adding the thixotropic agent into the dynamic mixer, and stirring for 1 hour under vacuum to complete the preparation of the epoxy resin composition.
3. The one-part epoxy composition of claim 1, wherein the one-part epoxy composition has the following properties for bonding in the lighting industry: the curing speed is below 3min at 80 ℃, the aluminum substrate can be stably stored for 168h at 40 ℃, the initial shear strength is larger than 25MPa, and the shear strength is kept above 20MPa after double-eighth-fifth aging for 168 h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310510741.3A CN117736678A (en) | 2023-05-08 | 2023-05-08 | Low-temperature rapid-curing epoxy resin composition and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310510741.3A CN117736678A (en) | 2023-05-08 | 2023-05-08 | Low-temperature rapid-curing epoxy resin composition and preparation method thereof |
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| Publication Number | Publication Date |
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| CN117736678A true CN117736678A (en) | 2024-03-22 |
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| CN202310510741.3A Pending CN117736678A (en) | 2023-05-08 | 2023-05-08 | Low-temperature rapid-curing epoxy resin composition and preparation method thereof |
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| Country | Link |
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| CN (1) | CN117736678A (en) |
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- 2023-05-08 CN CN202310510741.3A patent/CN117736678A/en active Pending
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