CN109880561A - A kind of epoxy resin embedding adhesive composition and preparation method thereof - Google Patents
A kind of epoxy resin embedding adhesive composition and preparation method thereof Download PDFInfo
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- CN109880561A CN109880561A CN201711274516.5A CN201711274516A CN109880561A CN 109880561 A CN109880561 A CN 109880561A CN 201711274516 A CN201711274516 A CN 201711274516A CN 109880561 A CN109880561 A CN 109880561A
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- epoxy resin
- adhesive composition
- embedding adhesive
- resin embedding
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Abstract
The invention discloses a kind of organic Silaoxacyclen epoxy resin embedding adhesives, the epoxy resin embedding adhesive composition, it include: 50~80 parts of organic Silaoxacyclen epoxy resin, 20~50 parts of bisphenol A type epoxy resins, 50~80 parts of anhydride curing agents, 0.3~1.2 part of promotor, 0.3~1.2 part of auxiliary agent of resistance to UV, 0.3~1.2 part of silane coupling agent, the present invention combines the advantage of both organic siliconresin and epoxy resin, the uv-resistance energy and the good adhesive property of epoxy resin of organic siliconresin are remained, while also making product that there is preferable ageing-resistant performance.
Description
Technical field
The present invention relates to a kind of epoxy resin embedding adhesive compositions and preparation method thereof, belong to LED screen casting glue field.
Background technique
Under the overall background of global energy shortage, LED is as a kind of efficient new type light source, and luminous efficiency is up to 80%
~90%, there are the advantages such as energy-saving and environmental protection and service life length, therefore, performance and application also receive the extensive concern of people.And it is high
The LED product of brightness low light attenuation also becomes hot spot concerned by people as following main product.Currently on the market using most
Be exactly organic silicon potting adhesive, epoxy resin embedding adhesive.
The casting glue of organosilicon uses it since the associativity with metallic support does not have the bond strength of epoxy resin high
The LED product of preparation will appear combination interface failure in use, and LED screen is caused to there is the shortcomings that blacking, discoloration.And ring
Oxygen resin have it is high with metallic support bond strength, it is identical as the epoxy crystal-bonding adhesive chemical species that die bonding uses, have more
Good compatibility makes LED screen and encapsulates the next-generation material used.Meanwhile compared with organic siliconresin, epoxy resin
The disadvantage of oneself is its water imbibition with higher, and uv-resistance can be poor.
Summary of the invention
For the defects in the prior art, the object of the present invention is to provide a kind of epoxy resin embedding adhesive composition and its systems
Preparation Method.
Epoxy resin embedding adhesive composition of the present invention is grouped as by the group of following parts by weight:
Preferred the composition is grouped as by the group of following parts by weight:
Preferred the composition is grouped as by the group of following parts by weight:
Preferred the composition is grouped as by the group of following parts by weight:
Preferred the composition is grouped as by the group of following parts by weight:
Ordinary epoxy resin of the present invention is preferably the epoxy resin, bisphenol f type epoxy resin, hydrogenation of bisphenol A-type
At least one of bisphenol A type epoxy resin, cycloaliphatic epoxy resin, phenolic resin.
Anhydride curing agent of the present invention is preferably first methyl hexahydro O-phthalic phthalic anhydride, methyl tetrahydro O-phthalic benzene
At least one of acid anhydride, trimellitic anhydride glyceride, poly sebacic polyanhydride.
Curing accelerator of the present invention be preferably imidazoles, tertiary amines, DBU, transition metal salt, in phosphoric acid salt
At least one；The imidazoles include 2-ethyl-4-methylimidazole；The tertiary amines include 2,4,6- tri- (dimethylamino first
Base) phenol.
The auxiliary agent of resistance to UV of the present invention is preferably the mixture of nano inorganic UV absorbent and phosphoric acid ester UV absorbent,
The weight ratio of the nano inorganic UV absorbent and phosphoric acid ester UV absorbent is 1:2~2:1.
The silane coupling agent of the present invention be preferably 3- glycidylpropyl trimethoxy silane, 3- shrink it is sweet
Oily ether oxygen propyl triethoxysilane, vinyltriethoxysilane, in N- aminoethyl-γ-aminopropyltrimethoxysilane
It is at least one.
Organic Silaoxacyclen epoxy resin structural of the present invention is as shown in Formulas I (SiMEP) or Formula II (SiPEP)
Compound
The present invention also provides a kind of preparation methods of organic Silaoxacyclen epoxy resin, method includes the following steps: with
NaOH makees catalyst, and hydroxy-end capped dimethyldimethoxysil,ne and epoxy group dimethoxysilane are added to 250ml's
In three-necked flask, under the conditions of 150~180 DEG C after being balanced reaction, neutralized with organosilicon phosphonate ester, removed under reduced pressure low boiling
Colorless and transparent product is made to get organic Silaoxacyclen epoxy resin in object.
The present invention also provides the preparation method of the epoxy resin embedding adhesive composition, include the following steps: organosilicon
Oxygen heterocyclic epoxy resin and ordinary epoxy resin mix, and the auxiliary agent of resistance to UV is dissolved in resin system；Then curing agent is added, consolidates
Change promotor and silane coupling agent, 0.5~1h is mixed to get organic Silaoxacyclen epoxy resin embedding adhesive.
Epoxy resin embedding adhesive composition of the present invention can be used for LED screen encapsulation.
Compared with prior art, the present invention have it is following the utility model has the advantages that
1, LED encapsulating epoxy resin casting glue of the invention have better water resistance and resistance to UV characteristic, water absorption rate <
0.5%, resistance to UV test > 2000h；
2,200% is improved than organic siliconresin to the bonding force of metallic support, room temperature metallic support shear strength > 5kgf/
Die (1 × 1mm), 250 DEG C of metallic support shear strengths > 2.5kgf/die (1 × 1mm),
3, in terms of ageing-resistant performance, double 85 test 500h, PCT have been passed through and have tested 120h；
4, with excellent uv-resistance energy and adhesive property, while also making product that there is preferable ageing-resistant performance.
Detailed description of the invention
Fig. 1: for the infrared figure of methylsiloxane oxygen heterocyclic epoxy resin.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
Examples 1 to 4
The preparation of organic Silaoxacyclen epoxy resin: making catalyst with NaOH, by hydroxy-end capped dimethylformamide dimethyl oxygroup
Silane and epoxy group dimethoxysilane are added in the three-necked flask of 250ml, being balanced under the conditions of 150~180 DEG C
It after reaction, is neutralized with organosilicon phosphonate ester, colorless and transparent product is made to get organic Silaoxacyclen ring in removed under reduced pressure low-boiling-point substance
Oxygen resin (SiMEP).
By shown in table 1, first organic Silaoxacyclen epoxy resin and bisphenol A type epoxy resin are uniformly mixed, resistance to UV is helped
Agent is dissolved in resin system；Then curing agent, curing accelerator and silane coupling agent is added, be mixed 0.5~1h to get
Epoxy resin embedding adhesive.
The component of the epoxy resin embedding adhesive of 1 Examples 1 to 4 of table
Using 4000 thrust machine of DAGA, organic Silaoxacyclen epoxy resin embedding adhesive that Examples 1 to 4 obtains is carried out
Test, the results are shown in Table 2:
The performance of the epoxy resin embedding adhesive of 2 Examples 1 to 4 of table preparation
By the result of table 2 as it can be seen that the resistance to UV of the LED screen epoxy resin embedding adhesive prepared using the method for Examples 1 to 4
Test is 2090~2120h, and 1 × 1mm chip thrust is 5.5~5.8kgf (25 DEG C), 2.6~2.8kgf (250 DEG C), and double 85 survey
Examination is 520~525h, and PCT test is 125~129h.
Embodiment 5~8
By shown in table 3, first organic Silaoxacyclen epoxy resin and bisphenol A type epoxy resin are uniformly mixed, resistance to UV is helped
Agent is dissolved in resin system；Then curing agent, curing accelerator and silane coupling agent is added, be mixed 0.5~1h to get
Epoxy resin embedding adhesive.
The component of the epoxy resin embedding adhesive of 3 embodiment 5~8 of table
Using 4000 thrust machine of DAGA, organic Silaoxacyclen epoxy resin embedding adhesive that embodiment 5~8 obtains is carried out
Test, the results are shown in Table 4:
By the result of table 4 as it can be seen that the resistance to UV of the LED screen epoxy resin embedding adhesive prepared using the method for embodiment 5~8
Test is 2150~2200h, and 1 × 1mm chip thrust is 5.5~5.9kgf (25 DEG C), 2.6~2.9kgf (250 DEG C), and double 85 survey
Examination is 525~529h, and PCT test is 126~129h.
The performance of the epoxy resin embedding adhesive of 4 embodiment 5~8 of table preparation
Embodiment 9~12
By shown in table 5, first two kinds of organic Silaoxacyclen epoxy resin are uniformly mixed, the auxiliary agent of resistance to UV is dissolved in resinite
In system；Then curing agent, curing accelerator and silane coupling agent is added, 0.5~1h is mixed to get organic Silaoxacyclen ring
Epoxy resin embedding glue.
The component of the epoxy resin embedding adhesive of 5 embodiment 9~12 of table
Using 4000 thrust machine of DAGA, organic Silaoxacyclen epoxy resin embedding adhesive that embodiment 9~12 obtains is carried out
Test, the results are shown in Table 6:
By the result of table 6 as it can be seen that using embodiment 9~12 method prepare LED screen epoxy resin embedding adhesive it is resistance to
UV test be 2090~2120h, 1 × 1mm chip thrust be 5.4~5.8kgf (25 DEG C), 2.5~2.8kgf (250 DEG C), double 85
Test is 520~524h, and PCT test is 126~129h.
The performance of the epoxy resin embedding adhesive of 6 embodiment 9~12 of table preparation
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring substantive content of the invention.
Claims (15)
1. a kind of epoxy resin embedding adhesive composition, which is characterized in that the composition is grouped as by the group of following parts by weight:
2. epoxy resin embedding adhesive composition according to claim 1, which is characterized in that the composition is by following parts by weight
Group be grouped as:
3. epoxy resin embedding adhesive composition according to claim 1, which is characterized in that the composition is by following parts by weight
Group be grouped as:
4. epoxy resin embedding adhesive composition according to claim 1, which is characterized in that the composition is by following parts by weight
Group be grouped as:
5. epoxy resin embedding adhesive composition according to claim 1, which is characterized in that the composition is by following parts by weight
Group be grouped as:
6. epoxy resin embedding adhesive composition according to claim 1-5, which is characterized in that the common epoxy
Resin can be bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol-A epoxy resin, cycloaliphatic epoxy resin,
At least one of phenolic resin.
7. epoxy resin embedding adhesive composition according to claim 1-5, which is characterized in that the anhydride-cured
Agent is methyl hexahydro O-phthalic phthalic anhydride, in methyl tetrahydro O-phthalic phthalic anhydride, trimellitic anhydride glyceride, poly sebacic polyanhydride
At least one.
8. epoxy resin embedding adhesive composition according to claim 1-5, which is characterized in that the solidification promotes
Agent is at least one of imidazoles, tertiary amines, DBU, transition metal salt, phosphoric acid salt；The imidazoles include 2- ethyl-
4-methylimidazole；The tertiary amines include 2,4,6- tri- (dimethylamino methyl) phenol.
9. epoxy resin embedding adhesive composition according to claim 1-5, which is characterized in that the auxiliary agent of resistance to UV
For the mixture of nano inorganic UV absorbent and phosphoric acid ester UV absorbent.
10. epoxy resin embedding adhesive composition according to claim 1-5, feature exist, the nano inorganic
The weight ratio of UV absorbent and phosphoric acid ester UV absorbent is 1:2~2:1.
11. epoxy resin embedding adhesive composition according to claim 1-5, which is characterized in that the silane is even
Connection agent is 3- glycidylpropyl trimethoxy silane, 3- glycidoxypropyltrietandysilane andysilane, three second of vinyl
At least one of oxysilane, N- aminoethyl-γ-aminopropyltrimethoxysilane.
12. epoxy resin embedding adhesive composition according to claim 1-5, which is characterized in that the organosilicon
Oxa- ring epoxy resin structural is such as Formulas I or Formula II compound represented
13. the preparation method of organic Silaoxacyclen epoxy resin described in -5 any one, feature exist according to claim 1
In method includes the following steps: making catalyst with NaOH, by hydroxy-end capped dimethyldimethoxysil,ne and epoxy group two
Methoxy silane is added in the three-necked flask of 250ml, under the conditions of 150~180 DEG C after being balanced reaction, uses organosilicon
Phosphonate ester neutralizes, and colorless and transparent product is made to get organic Silaoxacyclen epoxy resin in removed under reduced pressure low-boiling-point substance.
14. the preparation method of epoxy resin embedding adhesive composition described in -5 any one, feature exist according to claim 1
In including the following steps: to mix organic Silaoxacyclen epoxy resin and ordinary epoxy resin, the auxiliary agent of resistance to UV be dissolved in resin
In system；Then curing agent, curing accelerator and silane coupling agent is added, 0.5~1h is mixed to get organic Silaoxacyclen
Epoxy resin embedding adhesive.
15. application of the epoxy resin embedding adhesive composition described in -5 any one in LED screen encapsulation according to claim 1.
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| CN201711274516.5A CN109880561A (en) | 2017-12-06 | 2017-12-06 | A kind of epoxy resin embedding adhesive composition and preparation method thereof |
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| CN201711274516.5A CN109880561A (en) | 2017-12-06 | 2017-12-06 | A kind of epoxy resin embedding adhesive composition and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112759765A (en) * | 2020-12-30 | 2021-05-07 | 广州市白云化工实业有限公司 | Organic silicon prepolymer, organic silicon modified epoxy resin, adhesive, colloid and preparation method thereof |
| CN116120875A (en) * | 2022-12-28 | 2023-05-16 | 烟台德邦科技股份有限公司 | High-strength high-toughness silane modified sealant and preparation method thereof |
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| CN112759765A (en) * | 2020-12-30 | 2021-05-07 | 广州市白云化工实业有限公司 | Organic silicon prepolymer, organic silicon modified epoxy resin, adhesive, colloid and preparation method thereof |
| CN116120875A (en) * | 2022-12-28 | 2023-05-16 | 烟台德邦科技股份有限公司 | High-strength high-toughness silane modified sealant and preparation method thereof |
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