CN105969278A - Naleic anhydride toughened and modified composite heat-conduction epoxy pouring sealant for LED display screen - Google Patents
Naleic anhydride toughened and modified composite heat-conduction epoxy pouring sealant for LED display screen Download PDFInfo
- Publication number
- CN105969278A CN105969278A CN201610402049.9A CN201610402049A CN105969278A CN 105969278 A CN105969278 A CN 105969278A CN 201610402049 A CN201610402049 A CN 201610402049A CN 105969278 A CN105969278 A CN 105969278A
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- CN
- China
- Prior art keywords
- pouring sealant
- led display
- rare earth
- composite heat
- maleic anhydride
- 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.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
- Led Device Packages (AREA)
Abstract
The invention discloses a naleic anhydride toughened and modified composite heat-conduction epoxy pouring sealant for an LED display screen. According to the pouring sealant, high-heat-conduction nanometer aluminium oxide is subjected to surface coupling pretreatment with a rare earth oxide-titanium aluminum composite coupling agent and then subjected to a mixed reaction with polyurethane prepolymer, finally composite heat-conduction filler having comprehensive performance of inorganic matter and organic matter is obtained, the defect that traditional nanofiller is prone to clustering is overcome, the mixed effect with epoxy resin is good, added maleic anhydride improves toughness of composite resin, finally pouring resin sealant having high heat conduction and a good mechanical property is obtained, use performance of an LED module filled with the pouring sealant is promoted, and the composite heat-conduction epoxy pouring sealant has good application prospect on the aspect of LED display screen packaging.
Description
Technical field
The present invention relates to LED casting glue technical field, particularly relate to a kind of LED display maleic anhydride toughening modifying
Composite heat-conducting epoxy pouring sealant.
Background technology
LED display is by assembling by light emitting diode, constitutes lattice module, thus realizes large-area display merit
Can, it is widely used in daily life.LED display is progressively to more high brightness, more long-life, preferably luminescence at present
Uniformity and the development of stability aspect, this requires integrated chip, high power undoubtedly, increasingly mature along with chip technology,
The performance of chip can substantially meet use demand, and the requirement of encapsulation technology corresponding with this is more and more higher.It is known that encapsulation
Effect directly influences serviceability and the life-span of LED chip, and the development in market proposes requirements at the higher level to encapsulation technology.
Casting glue be usually used in electronic component heat conduction, bonding, seal, embedding and coating protection etc., primarily serve protection against the tide,
Dust-proof, anticorrosion, shockproof and improve effect such as stability of module.At present application more for epoxy resin casting glue, ring
The oxygen class casting glue defect maximum when application is exactly that poor thermal conductivity, viscosity are big, reduces the service life of device.In order to be suitable for
Market demand, necessary be modified traditional epoxy resin embedding adhesive processes, and encapsulates effect satisfactorily to obtaining
Really." research of LED epoxy resin embedding adhesive " literary composition is using bisphenol A epoxide resin as material of main part, with polyurethane as increasing
Tough dose, use low viscous mixing amine curing agent and epoxy active diluent, prepared that viscosity is little, light transmission good, power
Learn the product of excellent performance, but this kind of modified epoxy class casting glue heat-conducting effect is poor, inadequate environmental protection；" ZnO is at Al2O3/ heat conduction ring
Applied research in epoxy resin embedding glue " literary composition utilize heat conduction inorganic filler epoxy resin is modified process, in certain journey
Improving the heat conductivity of epoxy resin on degree, but its mechanical property but has downward trend, viscosity becomes big.
Summary of the invention
The object of the invention is contemplated to make up the defect of prior art, it is provided that a kind of LED display maleic anhydride is toughness reinforcing
Modified composite heat-conducting epoxy pouring sealant.
The present invention is achieved by the following technical solutions:
A kind of composite heat-conducting epoxy pouring sealant of LED display maleic anhydride toughening modifying, it is characterised in that this packaging plastic by
The raw material of following weight portion prepares: bisphenol A epoxide resin 40-60, rare earth-base polyurethane prepolymer for use as modified nano-alumina 30-50,
Maleic anhydride 2-5, trioctyl phosphate 4-5, diluent CYH-277 5-15, firming agent 20-80, antioxidant 0.1-0.5, ultraviolet light
Stabilizer 0.01-0.05, UV absorbers 0.01-0.05.
Described rare earth-base polyurethane prepolymer for use as modified nano-alumina is prepared by following raw material: polyether polyol 10-
20, methyl diphenylene diisocyanate 5-10, diethanolamine be appropriate, nano aluminium oxide 40-50, aluminate coupling agent 1-2, metatitanic acid
Ester coupling agent 1-1.5, rare earth oxide 0.5-0.6, dibutyl tin dilaurate 0.1-0.2.
Preparation method is:
(1) putting in reaction vessel by polyether polyol, heating removing moisture, is subsequently added diphenyl methane under nitrogen atmosphere
Diisocyanate, hybrid reaction 6-8h under the conditions of 80-90 DEG C.
(2) aluminate coupling agent, titanate coupling agent, rare earth oxide are added in reaction vessel together, stirring mixing
Uniformly post-heating is to 120-130 DEG C, hybrid reaction 4-5h, and products therefrom mixes dispersion and grinds 2-3h, subsequently with nano aluminium oxide
Being put in step (1) reaction vessel, reduction system temperature, to 60-70 DEG C, adds dibutyl tin dilaurate, mixed grinding
Drip diethanolamine after reaction 2-3h, continue cooling discharge after griding reaction 1-1.5h, obtain described rare earth-polyurethane prepolymer
Modifies nano aluminium oxide.
Described firming agent is the one in methyl hexahydrophthalic anhydride, methyl tetrahydro phthalic anhydride.
The using method of this casting glue is: first by bisphenol A epoxide resin, rare earth-base polyurethane prepolymer for use as modified Nano oxidation
Aluminum, maleic anhydride, trioctyl phosphate, diluent, antioxidant, UV light stabilizing agent, UV absorbers mixing and stirring, with
After add firming agent, stirring while adding, after interpolation, mixed material is heated to 60-80 DEG C, and gained glue is through vacuum defoamation
Inject in LED die to be packaged after process, take out pre-packaged LED after natural precuring 2-3h, be placed in vacuum drying oven,
The LED that embedding is good is i.e. obtained after isothermal curing 6-8h under the conditions of 70-80 DEG C.
The present invention by the nano aluminium oxide of high heat conduction after rare earth oxide-titanium aluminum composite coupler surface coupling pretreatment
With base polyurethane prepolymer for use as hybrid reaction, finally give the composite heat-conducting filler having inorganic matter concurrently with Organic substance combination property, improve
The defect that Conventional nano filler is easily reunited, to compound effect good with epoxy resin, and the maleic anhydride of addition improves composite resin
Toughness, is finally obtained the sealing resin glue having high heat conduction and excellent mechanical performances concurrently, with the LED module serviceability of its embedding
Obtaining and promote, it demonstrates good application prospect in terms of LED display encapsulation.
Detailed description of the invention
The casting glue of this embodiment is prepared by the raw material of following weight portion: bisphenol A epoxide resin 50, rare earth-polyurethane are pre-
Aggressiveness modified nano-alumina 40, maleic anhydride 4, trioctyl phosphate 4, diluent CYH-277 12, firming agent 60, antioxidant
0.3, UV light stabilizing agent 0.02, UV absorbers 0.03.
Its middle rare earth-base polyurethane prepolymer for use as modified nano-alumina is prepared by following raw material: polyether polyol 15, two
Methylenebis phenyl isocyanate 8, diethanolamine are appropriate, nano aluminium oxide 45, aluminate coupling agent 1.5, titanate coupling agent
1.2, rare earth oxide 0.5, dibutyl tin dilaurate 0.1.
Preparation method is:
(1) putting in reaction vessel by polyether polyol, heating removing moisture, is subsequently added diphenyl methane under nitrogen atmosphere
Diisocyanate, hybrid reaction 7.5h under the conditions of 80-90 DEG C.
(2) aluminate coupling agent, titanate coupling agent, rare earth oxide are added in reaction vessel together, stirring mixing
Uniformly post-heating is to 120-130 DEG C, hybrid reaction 4.5h, and products therefrom mixes dispersion and grinds 2.5h, subsequently with nano aluminium oxide
Being put in step (1) reaction vessel, reduction system temperature, to 60-70 DEG C, adds dibutyl tin dilaurate, mixed grinding
Drip diethanolamine after reaction 2.5h, continue cooling discharge after griding reaction 1.5h, obtain described rare earth-base polyurethane prepolymer for use as
Modified nano-alumina.
Described firming agent is the one in methyl hexahydrophthalic anhydride, methyl tetrahydro phthalic anhydride.
The using method of this casting glue is: first by bisphenol A epoxide resin, rare earth-base polyurethane prepolymer for use as modified Nano oxidation
Aluminum, maleic anhydride, trioctyl phosphate, diluent, antioxidant, UV light stabilizing agent, UV absorbers mixing and stirring, with
After add firming agent, stirring while adding, after interpolation, mixed material is heated to 70-80 DEG C, and gained glue is through vacuum defoamation
Inject in LED die to be packaged after process, take out pre-packaged LED after natural precuring 2.5h, be placed in vacuum drying oven,
The LED that embedding is good is i.e. obtained after isothermal curing 7.5h under the conditions of 70-80 DEG C.
The performance test results of this casting glue is as follows:
| Detection project | Testing result |
| Thermal conductivity (W.m-1.k-1) | 0.56 |
| Elongation at break (%) | 18.2 |
| Hot strength (MPa) | 6.6 |
| Thermal coefficient of expansion | 0.45 |
| Water absorption rate | 0.30 |
Claims (4)
1. the LED display composite heat-conducting epoxy pouring sealant of maleic anhydride toughening modifying, it is characterised in that this packaging plastic
Prepared by the raw material of following weight portion: bisphenol A epoxide resin 40-60, rare earth-base polyurethane prepolymer for use as modified nano-alumina 30-
50, maleic anhydride 2-5, trioctyl phosphate 4-5, diluent CYH-277 5-15, firming agent 20-80, antioxidant 0.1-0.5, purple
Outer light stabilizer 0.01-0.05, UV absorbers 0.01-0.05.
The composite heat-conducting epoxy pouring sealant of a kind of LED display maleic anhydride toughening modifying the most as claimed in claim 1, its
Being characterised by, described rare earth-base polyurethane prepolymer for use as modified nano-alumina is prepared by following raw material: polyether polyol
10-20, methyl diphenylene diisocyanate 5-10, diethanolamine are appropriate, nano aluminium oxide 40-50, aluminate coupling agent 1-2,
Titanate coupling agent 1-1.5, rare earth oxide 0.5-0.6, dibutyl tin dilaurate 0.1-0.2；
Preparation method is:
(1) putting in reaction vessel by polyether polyol, heating removing moisture, is subsequently added diphenyl methane under nitrogen atmosphere
Diisocyanate, hybrid reaction 6-8h under the conditions of 80-90 DEG C；
(2) aluminate coupling agent, titanate coupling agent, rare earth oxide are added in reaction vessel together, be uniformly mixed
Post-heating is to 120-130 DEG C, and hybrid reaction 4-5h, products therefrom mixes dispersion and grinds 2-3h, subsequently by it with nano aluminium oxide
Putting in step (1) reaction vessel, reduction system temperature, to 60-70 DEG C, adds dibutyl tin dilaurate, and mixed grinding reacts
Drip diethanolamine after 2-3h, continue cooling discharge after griding reaction 1-1.5h, obtain described rare earth-polyurethane prepolymer structural reform
Property nano aluminium oxide.
The composite heat-conducting epoxy pouring sealant of a kind of LED display maleic anhydride toughening modifying the most as claimed in claim 1, its
Being characterised by, described firming agent is the one in methyl hexahydrophthalic anhydride, methyl tetrahydro phthalic anhydride.
The composite heat-conducting epoxy pouring sealant of a kind of LED display maleic anhydride toughening modifying the most as claimed in claim 1
Using method is: first by bisphenol A epoxide resin, rare earth-base polyurethane prepolymer for use as modified nano-alumina, maleic anhydride, tricresyl phosphate
Monooctyl ester, diluent, antioxidant, UV light stabilizing agent, UV absorbers mixing and stirring, add firming agent, limit subsequently
Edged stirs, and after interpolation, mixed material is heated to 60-80 DEG C, and gained glue injects to be packaged after vacuum defoamation processes
In LED die, take out pre-packaged LED after natural precuring 2-3h, be placed in vacuum drying oven, permanent under the conditions of 70-80 DEG C
I.e. obtain, after temperature solidification 6-8h, the LED that embedding is good.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610402049.9A CN105969278A (en) | 2016-06-08 | 2016-06-08 | Naleic anhydride toughened and modified composite heat-conduction epoxy pouring sealant for LED display screen |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610402049.9A CN105969278A (en) | 2016-06-08 | 2016-06-08 | Naleic anhydride toughened and modified composite heat-conduction epoxy pouring sealant for LED display screen |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105969278A true CN105969278A (en) | 2016-09-28 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610402049.9A Pending CN105969278A (en) | 2016-06-08 | 2016-06-08 | Naleic anhydride toughened and modified composite heat-conduction epoxy pouring sealant for LED display screen |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107325768A (en) * | 2017-05-19 | 2017-11-07 | 合肥市惠科精密模具有限公司 | A kind of composite epoxy casting glue of LED display nano-silicon nitride toughening modifying |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101580686A (en) * | 2009-05-07 | 2009-11-18 | 中国工程物理研究院化工材料研究所 | Epoxide resin pouring sealant with low density and high impact resistance and preparation method thereof |
| CN104178076A (en) * | 2014-09-11 | 2014-12-03 | 黎明化工研究设计院有限责任公司 | Heat-conducting electric-insulating epoxy resin potting adhesive and preparation method thereof |
-
2016
- 2016-06-08 CN CN201610402049.9A patent/CN105969278A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101580686A (en) * | 2009-05-07 | 2009-11-18 | 中国工程物理研究院化工材料研究所 | Epoxide resin pouring sealant with low density and high impact resistance and preparation method thereof |
| CN104178076A (en) * | 2014-09-11 | 2014-12-03 | 黎明化工研究设计院有限责任公司 | Heat-conducting electric-insulating epoxy resin potting adhesive and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107325768A (en) * | 2017-05-19 | 2017-11-07 | 合肥市惠科精密模具有限公司 | A kind of composite epoxy casting glue of LED display nano-silicon nitride toughening modifying |
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Application publication date: 20160928 |