CN104745132B - A kind of outdoor paster lamp bead epoxide-resin glue and preparation method thereof - Google Patents
A kind of outdoor paster lamp bead epoxide-resin glue and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of epoxide-resin glue, and in particular to a kind of outdoor paster lamp bead epoxide-resin glue and preparation method thereof.The outdoor paster lamp bead epoxide-resin glue of the present invention, the glue is made up of two kinds of components of A, B, it is characterized in that, wherein A glue is made up of epoxy resin, antioxidant, light stabilizer and coupling agent；B glue is made up of curing agent, accelerator, polyalcohol, blue agent.The present invention is the epoxide-resin glue for outdoor paster lamp bead.Have that bonding force is strong, thermal oxidative aging is strong, moisture resistance is good, the advantages of ultraviolet-resistent property is strong.Outdoor paster lamp bead encapsulation glue is especially suitable for, is adapted to industrialized production.
Description
Technical field
The present invention relates to a kind of epoxide-resin glue, and in particular to a kind of outdoor paster lamp bead epoxide-resin glue and its preparation
Method.
Background technology
Due to LED have electric light transformation efficiency height, environmental protection, long lifespan, low operating voltage, small volume, generate heat less, brightness
The advantages of high, light beam concentrates stable, therefore it is widely used in the fields such as radiating light source, illumination and display.Used to reduce LED
During light because of scattering loss, that is, to chip carry out mechanical protection, it need to be packaged.Because it makes in open air for a long time
Must possess higher light transmittance, refractive index with, LED encapsulation material, excellent resistant of high or low temperature and protection against the tide, solvent resistant, color inhibition,
Ultraviolet aging resistance and other optics, chemical property.
Current LED pasters encapsulating material mainly uses organic siliconresin, but the high refractive index organic silicon resin of domestic production
Cementability and stability are poor, therefore domestic market is occupied by Dow corning and Japanese SHIN-ETSU HANTOTAI etc. always.Common bisphenol type epoxy
Resin high temperature resistant, color inhibition and ultra-violet resistance are poor, therefore are less applied to LED and encapsulate.
Country someone studied the envelope that silane coupler modified cycloaliphatic epoxy resin is used as high-powered LED lamp at present
Glue is filled, the CN102703008A patent applications as disclosed in Chinese patent disclose a kind of packaging plastic for great power LED,
But, the glue has the shortcomings that production cost is high, viscosity is high, anti-moisture performance is not good, is not suitable for outdoor paster lamp bead.
The content of the invention
The present invention new is used for outdoor SMD lamp to solve the above-mentioned problems in the prior art there is provided a kind of
Epoxide-resin glue of pearl and preparation method thereof.
The outdoor paster lamp bead epoxide-resin glue of the present invention, the glue is made up of two kinds of components of A, B, and wherein component A is by ring
Oxygen tree fat, antioxidant, light stabilizer and coupling agent composition；B component is made up of curing agent, accelerator, polyalcohol, blue agent.
The preferred scheme of the present invention is that the weight ratio of component A and B component is 1:0.9-1.0, and component A is by by weight
The following material composition of part ratio：Organic-silicon-modified cycloaliphatic epoxy resin 10-15
Preferably, B component by ratio by weight following material composition：
Organic-silicon-modified cycloaliphatic epoxy resin of the present invention is POSS structure silsesquioxane resins；It is preferred that by following
Method is made：By aminomethyl phenyl dimethoxysilane, phenyltrimethoxysila,e, 2- (3,4- 7-oxa-bicyclo[4.1.0s base) ethyl front three
The aqueous hydrochloric acid solution of TMOS 0.1% is put into reactor in proportion, is warming up to 90-120 DEG C of reaction backflow 4-5h, is warming up to
The accessory substance that 120-130 DEG C of vacuum distillation elimination reaction is produced, produces organic-silicon-modified cycloaliphatic epoxy resin.
The preferred scheme of the present invention is that described cycloaliphatic epoxy resin is double (2,3 epoxy cyclopentyl) ether, 3,4- ring
Epoxide -6- methylcyclohexyls formic acid -3 ', 4 '-epoxy radicals -6 '-methylcyclohexyl methyl esters, vinyl cyclic ethylene diepoxide,
3,4- expoxycyclohexyl formic acid -3 ', 4 '-expoxycyclohexyl methyl esters, diisoamyl diene diepoxide, adipic acid two (3,
4- epoxy radicals -6- methylcyclohexyls methyl esters), the one or more in bicyclopentadiene diepoxide.
The preferred scheme of the present invention is that the antioxidant is 2,6- di-tert-butyl-4-methy phenols, four [β-(3,5- bis-
Tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester,
One or more in the double Lauryl Alcohol esters of triphenyl phosphite, the monooctyl ester of phosphorous acid three, thio-2 acid.
The preferred scheme of the present invention is that the light stabilizer is Methyl Salicylate, the 2- (2 ˊ-ˊ of hydroxyl-5-methyl
Phenyl) BTA, the one or more in 2-hydroxy-4-n-octoxybenzophenone.
The preferred scheme of the present invention is that the coupling agent is glycidol ether alkoxy silane.
The preferred scheme of the present invention is that the curing agent is methylhexahydrophthalic anhydride, methyl hexahydro O-phthalic
In acid anhydrides and methyl tetrahydrophthalic anhydride mixture, methylhexahydrophthalic anhydride and methylnadic anhydride mixture
One or more.
The present invention preferred scheme be, the accelerator be tetramethyl amine bromide, tetraethylammonium bromide, 2-methylimidazole,
One or more in 2-ethyl-4-methylimidazole, aluminium acetylacetonate, boron trifluoride amine complex.
The preferred scheme of the present invention is, the polyalcohol is glycerine, 1,6- hexylene glycols, neopentyl glycol, polyethylene glycol, poly-
One or more in propane diols.
The present invention also provides the preparation method of outdoor paster lamp bead epoxide-resin glue, comprises the steps：
1) preparation of component A：Be 10-15 organic-silicon-modified cycloaliphatic epoxy resin by weight, 40-45 fat
Ring race epoxy resin, 40-45 bisphenol-A epoxy resins, 0.1-3 antioxidant, 0.1-3 light stabilizer, 0.5-4
Coupling agent is put into reactor in proportion, and 1-2h, froth breaking, encapsulation are stirred in 80-100 DEG C；
2) preparation of B component：Be 92-96 curing agent by weight, 0.1-3 accelerator, 0.5-3 it is polynary
Alcohol, 0.001-0.01 tune blue agent are proportionally added into reactor, and 1-2h, froth breaking, encapsulation are stirred in 70-90 DEG C.
3) it is 1 according to weight ratio by component A and B component:0.9-1.0 proportioning, it is well mixed to be solidified, wherein in
125-130 DEG C first solidifies 0.5-1.5 hours, solidifies 3~5 hours after 130-150 DEG C, produces outdoor paster lamp bead asphalt mixtures modified by epoxy resin
Fat glue.
The present invention carries out modification by copolymerization to epoxy resin, a kind of modifying epoxy resin by organosilicon is synthesized, by being aggregated in ring
In oxygen resin backbone after embedded Si-O-Si keys, the epoxy resin cure after organic-silicon-modified, with bonding force is strong, heat resistanceheat resistant oxygen
Aging is strong, moisture resistance is good, the advantages of ultraviolet-resistent property is strong.Outdoor paster lamp bead encapsulation glue is especially suitable for, is adapted to industry metaplasia
Production.
Embodiment
The invention will be described further by the following examples, of the invention to help understanding, but the protection model of the present invention
Enclose and be not limited in these embodiments.
Embodiment one
(1) organic-silicon-modified cycloaliphatic epoxy resin is prepared：By 15% aminomethyl phenyl dimethoxysilane, 10% benzene
Base trimethoxy silane, 60% 2- (3,4- 7-oxa-bicyclo[4.1.0s base) ethyl trimethoxy silanes and 15% 0.1% hydrochloric acid
The aqueous solution is put into reactor in proportion, is warming up to 90-120 DEG C of reaction backflow 4-5h, is warming up to 120-130 DEG C of vacuum distillation
The accessory substance that elimination reaction is produced.
(2) preparation of component A：By weight than the organic-silicon-modified cycloaliphatic epoxy resin for 13%, 44% adipic acid
Two (3,4- epoxy radicals -6- methylcyclohexyls methyl esters), 40% bisphenol-A epoxy resin, 1% 2,6- di-t-butyls -4-
Methylphenol, 1% Methyl Salicylate, 1% γ-(oxygen of 2,3- epoxies third) propyl trimethoxy silicane is in proportion
Put into reactor, 1-2h, froth breaking are stirred in 80-100 DEG C.
(3) preparation of B component：By weight than methyl hexahydrophthalic anhydride for 96%, 1% 2-methylimidazole, 2.99%
Polyethylene glycol, 0.01% tune blue agent are proportionally added into reactor, and 1-2h, froth breaking are stirred in 70-90.
(4) component of A, B two presses 1：0.94 it is well mixed solidified, wherein in 125-130 DEG C first solidification 0.5-1.5 it is small
When, solidify 3~5 hours after 130-150 DEG C, produce outdoor paster lamp bead epoxide-resin glue.
Embodiment two
(1) organic-silicon-modified cycloaliphatic epoxy resin is prepared：By 15% aminomethyl phenyl dimethoxysilane, 10% benzene
Base trimethoxy silane, 60% 2- (3,4- 7-oxa-bicyclo[4.1.0s base) ethyl trimethoxy silanes and 15% 0.1% hydrochloric acid
The aqueous solution is put into reactor in proportion, is warming up to 90-120 DEG C of reaction backflow 4-5h, is warming up to 120-130 DEG C of vacuum distillation and takes off
The accessory substance produced except reaction.
(2) preparation of component A：By weight than organic-silicon-modified cycloaliphatic epoxy resin, the 45% 3,4- rings for 12%
Epoxide hexahydrobenzoid acid -3 ', 4 '-expoxycyclohexyl methyl esters, 40% bisphenol-A epoxy resin, the four of 1% [β-(3,5-
Di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, 1% 2-hydroxy-4-n-octoxybenzophenone, 1% γ-
(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is put into reactor in proportion, and 1-2h, froth breaking are stirred in 80-100 DEG C.
(3) preparation of B component：By weight than the methyl hexahydrophthalic anhydride for 96%, 1% 4 bromide, 2.99%
Polypropylene glycol, 0.01% tune blue agent be proportionally added into reactor, in 70-90 stir 1-2h, froth breaking.
(4) component of A, B two presses 1：0.96 it is well mixed solidified, wherein in 125-130 DEG C first solidification 0.5-1.5 it is small
When, solidify 3~5 hours after 130-150 DEG C, produce outdoor paster lamp bead epoxide-resin glue.
Embodiment three
(1) organic-silicon-modified cycloaliphatic epoxy resin is prepared：By 15% aminomethyl phenyl dimethoxysilane, 10% benzene
Base trimethoxy silane, 60% 2- (3,4- 7-oxa-bicyclo[4.1.0s base) ethyl trimethoxy silanes and 15% 0.1% hydrochloric acid
The aqueous solution is put into reactor in proportion, is warming up to 90-120 DEG C of reaction backflow 4-5h, is warming up to 120-130 DEG C of vacuum distillation and takes off
The accessory substance produced except reaction.
(2) preparation of component A：By weight for 10% organic-silicon-modified cycloaliphatic epoxy resin, the 3 of 45%,
4- expoxycyclohexyls formic acid -3 ', 4 '-expoxycyclohexyl methyl esters, 40.8% bisphenol-A epoxy resin, 0.1% β -
(3,5- di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester, 0.1% 2-hydroxy-4-n-octoxybenzophenone, 4%
Glycidol ether alkoxy silane put into proportion in reactor, in 80-100 DEG C stir 1-2h, froth breaking, encapsulation；
(3) preparation of B component：By weight for 96% methylhexahydrophthalic anhydride, 3% 2- ethyls-
4-methylimidazole, 0.999% 1,6- hexylene glycols, 0.001% tune blue agent are proportionally added into reactor, in 70-90
DEG C stirring 1-2h, froth breaking, encapsulation.
(4) it is 1 according to weight ratio by component A and B component:0.9 proportioning, it is well mixed to be solidified, wherein in 125-
130 DEG C first solidify 0.5-1.5 hours, solidify 3~5 hours after 130-150 DEG C, produce outdoor paster lamp bead epoxy resin
Glue.
Example IV
(1) organic-silicon-modified cycloaliphatic epoxy resin is prepared：By 15% aminomethyl phenyl dimethoxysilane, 10% benzene
Base trimethoxy silane, 60% 2- (3,4- 7-oxa-bicyclo[4.1.0s base) ethyl trimethoxy silanes and 15% 0.1% hydrochloric acid
The aqueous solution is put into reactor in proportion, is warming up to 90-120 DEG C of reaction backflow 4-5h, is warming up to 120-130 DEG C of vacuum distillation and takes off
The accessory substance produced except reaction
(2) preparation of component A：By weight than organic-silicon-modified cycloaliphatic epoxy resin, the 42% 3,4- rings for 15%
Epoxide hexahydrobenzoid acid -3 ', 4 '-expoxycyclohexyl methyl esters, 40% bisphenol-A epoxy resin, the four of 1% [β-(3,5-
Di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, 1% 2-hydroxy-4-n-octoxybenzophenone, 1% γ-
(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is put into reactor in proportion, and 1-2h, froth breaking are stirred in 80-100 DEG C.
(3) preparation of B component：By weight than the methyl hexahydrophthalic anhydride for 96%, 1% 4 bromide, 2.99%
Polypropylene glycol, 0.01% tune blue agent be proportionally added into reactor, in 70-90 stir 1-2h, froth breaking.
(4) component of A, B two presses 1：0.95 proportioning, it is well mixed to be solidified, wherein first solidifying 0.5- in 125-130 DEG C
1.5 hours, solidify 3~5 hours after 130-150 DEG C, produce outdoor paster lamp bead epoxide-resin glue.
Embodiment five
(1) organic-silicon-modified cycloaliphatic epoxy resin is prepared：By 15% aminomethyl phenyl dimethoxysilane, 10% benzene
Base trimethoxy silane, 60% 2- (3,4- 7-oxa-bicyclo[4.1.0s base) ethyl trimethoxy silanes and 15% 0.1% hydrochloric acid
The aqueous solution is put into reactor in proportion, is warming up to 90-120 DEG C of reaction backflow 4-5h, is warming up to 120-130 DEG C of vacuum distillation and takes off
The accessory substance produced except reaction.
(2) preparation of component A：By weight part ratio for 12 parts organic-silicon-modified cycloaliphatic epoxy resin, 42 parts it is double (2,
3 epoxy cyclopentyls) ether, 40 parts of bisphenol-A epoxy resins, 0.2 part of 2,6 di tert butyl 4 methyl phenol, 3 parts
Methyl Salicylate, 4 parts of γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane are put into reactor in proportion,
1-2h, froth breaking, encapsulation are stirred in 80-100 DEG C；
(3) preparation of B component：Methylhexahydrophthalic anhydride, 0.9 part of tetraethyl by weight for 95 parts
Ammonium bromide, 2.2 parts of neopentyl glycol, 0.005 part of tune blue agent are proportionally added into reactor, and 1- is stirred in 70-90 DEG C
2h, froth breaking, encapsulation.
(4) it is 1 according to weight ratio by component A and B component:0.9 proportioning, it is well mixed to be solidified, wherein in 125-
130 DEG C first solidify 0.5-1.5 hours, solidify 3~5 hours after 130-150 DEG C, produce outdoor paster lamp bead epoxy resin
Glue.
Embodiment six
(1) organic-silicon-modified cycloaliphatic epoxy resin is prepared：By 15% aminomethyl phenyl dimethoxysilane, 10% benzene
Base trimethoxy silane, 60% 2- (3,4- 7-oxa-bicyclo[4.1.0s base) ethyl trimethoxy silanes and 15% 0.1% hydrochloric acid
The aqueous solution is put into reactor in proportion, is warming up to 90-120 DEG C of reaction backflow 4-5h, is warming up to 120-130 DEG C of vacuum distillation
The accessory substance that elimination reaction is produced
(2) preparation of component A：Organic-silicon-modified cycloaliphatic epoxy resin, oneself of 41 parts by weight for 15 parts
Diacid two (3,4- epoxy radicals -6- methylcyclohexyls methyl esters), 44 parts of bisphenol-A epoxy resins, 1.7 parts of phosphorous acid three are pungent
Ester, 1.6 parts of 2-hydroxy-4-n-octoxybenzophenone, 2.6 parts of γ-(oxygen of 2,3- epoxies third) propyl trimethoxy silicane
Put into proportion in reactor, 1-2h, froth breaking, encapsulation are stirred in 80-100 DEG C；
(3) preparation of B component：Methylhexahydrophthalic anhydride, 1.4 parts of acetyl by weight for 94.6 parts
Acetone aluminium, 2.5 parts of glycerine, 0.009 part of tune blue agent are proportionally added into reactor, and 1-2h is stirred in 70-90 DEG C,
Froth breaking, encapsulation.
(4) it is 1 according to weight ratio by component A and B component:1 proportioning, it is well mixed to be solidified, wherein in 125-130
DEG C first solidify 0.5-1.5 hour, after 130-150 DEG C of solidification 3~5 hours, produce outdoor paster lamp bead epoxide-resin glue.
The product of the embodiment of the present invention, after testing：1. outward appearance is transparency liquid, no isolation, gel and particle, each component face
Aberration is different substantially；2. existing phenyl polysiloxane structure in the organic-silicon-modified cycloaliphatic epoxy resin synthesized, molecular structure, also has
Alicyclic epoxy structural, solidfied material has good high-low temperature resistant and UVResistant effect；3. impact strength is more than 12.8KJ/m2,
Bending strength is more than 14J；4. glass transition temperature is more than 423.15K；5. -40 DEG C (30min) → 100 DEG C (30min) circulations 600
Secondary, thermal shock is unchanged；6. three Reflow Solderings (260 DEG C of peak temperature, time 10s) packaging plastic is crossed without coming off and xanthochromia is existing
As；7. it is hot and humid：70 DEG C, 90% relative humidity, 100 DEG C of digestion 1h of red ink or soak at room temperature 30 days, no infiltration.
Above-described embodiment is preferably embodiment, but embodiments of the present invention are not by above-described embodiment of the invention
Limitation, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, it is simple
Change, should be equivalent substitute mode, be included within protection scope of the present invention.
Claims (1)
1. a kind of outdoor paster lamp bead epoxide-resin glue, the glue is made up of two kinds of components of A, B, it is characterized in that, wherein component A by
Epoxy resin, antioxidant, light stabilizer and coupling agent composition；B component is by curing agent, accelerator, polyalcohol, blue agent group
Into, it is characterized in that, it is made up of following steps：
(1) organic-silicon-modified cycloaliphatic epoxy resin is prepared：By 15% aminomethyl phenyl dimethoxysilane, 10% phenyl three
Methoxy silane, 60% 2- (3,4- 7-oxa-bicyclo[4.1.0s base) ethyl trimethoxy silanes and 15% 0.1% hydrochloric acid are water-soluble
Liquid is put into reactor in proportion, is warming up to 90-120 DEG C of reaction backflow 4-5h, is warming up to 120-130 DEG C of vacuum distillation removing anti-
The accessory substance that should be produced；
(2) preparation of component A：Organic-silicon-modified cycloaliphatic epoxy resin, 41 parts of adipic acid by weight for 15 parts
Two (3,4- epoxy radicals -6- methylcyclohexyls methyl esters), 44 parts of bisphenol-A epoxy resins, 1.7 parts of the monooctyl ester of phosphorous acid three,
1.6 parts of 2-hydroxy-4-n-octoxybenzophenone, 2.6 parts of γ-(oxygen of 2,3- epoxies third) propyl trimethoxy silicane are pressed
Ratio is put into reactor, and 1-2h, froth breaking, encapsulation are stirred in 80-100 DEG C；
(3) preparation of B component：Methylhexahydrophthalic anhydride, 1.4 parts of acetylacetone,2,4-pentanedione by weight for 94.6 parts
Aluminium, 2.5 parts of glycerine, 0.009 part of tune blue agent are proportionally added into reactor, are stirred 1-2h in 70-90 DEG C, are disappeared
Bubble, encapsulation；
(4) it is 1 according to weight ratio by component A and B component:1 proportioning, it is well mixed to be solidified, wherein in 125-130 DEG C of elder generation
Solidification 0.5-1.5 hours, solidifies 3~5 hours after 130-150 DEG C, produces outdoor paster lamp bead epoxide-resin glue.
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| CN105461902B (en) * | 2015-11-11 | 2017-06-30 | 吴江市莘塔前进五金厂 | A kind of use for electronic products thin-film material and preparation method thereof |
| CN105238315B (en) * | 2015-11-20 | 2018-02-06 | 烟台德邦先进硅材料有限公司 | A kind of silicon-modified epoxy packaging plastic |
| CN105384914A (en) * | 2015-12-18 | 2016-03-09 | 无锡创达新材料股份有限公司 | High-temperature-resistant ultraviolet-resistant epoxy resin prepolymer and preparation method thereof |
| BR112019025061B1 (en) | 2017-06-09 | 2023-03-14 | Hexion Inc | COMPOSITE EPOXY RESIN SYSTEM AND METHOD FOR MANUFACTURING A COMPOSITE |
| CN109825232A (en) * | 2019-02-27 | 2019-05-31 | 华南理工大学 | A kind of epoxy packages glue and preparation method thereof for LED |
| CN110746918A (en) * | 2019-10-30 | 2020-02-04 | 惠州市鑫惠利光电材料有限公司 | Low-light-attenuation LED epoxy packaging adhesive |
| CN111334247A (en) * | 2020-04-17 | 2020-06-26 | 南京智聚科技咨询有限公司 | Packaging adhesive for full-spectrum LED lamp |
| CN111334232A (en) * | 2020-04-28 | 2020-06-26 | 东莞市恒尔朗实业有限公司 | Weather-resistant intermediate-temperature curing epoxy resin adhesive and preparation method thereof |
| CN115368857A (en) * | 2022-08-23 | 2022-11-22 | 书香门地集团股份有限公司 | Anti-cracking low-halogen low-transparency epoxy resin sealant |
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| CN1331870C (en) * | 2004-10-27 | 2007-08-15 | 西北工业大学 | Epoxy-silsesquioxanes preparation method |
| CN101654509A (en) * | 2009-09-25 | 2010-02-24 | 上海大学 | Preparation method of epoxy silsesquioxane/epoxy resin hybrid material for packaging large-power LED |
| CN101974227A (en) * | 2010-05-20 | 2011-02-16 | 复旦大学 | Low-stress epoxy/organic silicon/POSS nano hybrid material, and preparation method and application thereof |
| CN101921571B (en) * | 2010-08-13 | 2014-11-05 | 王行柱 | High-temperature resistant packaging adhesive for high-power LED lamp and preparation method thereof |
| CN102807676B (en) * | 2012-08-16 | 2014-07-09 | 方舟(佛冈)化学材料有限公司 | Phenyl modified epoxy organic silicon resin and preparation method thereof, organic silicon packaging adhesive and LED lamp |
| CN103265923B (en) * | 2013-05-15 | 2014-10-29 | 陕西煤业化工技术研究院有限责任公司 | Epoxy resin composite for high-power LED (light-emitting diode) encapsulation and preparation method thereof |
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