CN106047253A - Nanometer aluminum oxide modified composite epoxy pouring sealant for LED streetlamp display screen - Google Patents

Nanometer aluminum oxide modified composite epoxy pouring sealant for LED streetlamp display screen Download PDF

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Publication number
CN106047253A
CN106047253A CN201610409977.8A CN201610409977A CN106047253A CN 106047253 A CN106047253 A CN 106047253A CN 201610409977 A CN201610409977 A CN 201610409977A CN 106047253 A CN106047253 A CN 106047253A
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CN
China
Prior art keywords
display screen
aluminum oxide
alumina
led
composite epoxy
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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.)
Pending
Application number
CN201610409977.8A
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Chinese (zh)
Inventor
闫亚洲
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Anhui Fuyuan Photoelectric Technology Co Ltd
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Anhui Fuyuan Photoelectric Technology Co Ltd
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Priority to CN201610409977.8A priority Critical patent/CN106047253A/en
Publication of CN106047253A publication Critical patent/CN106047253A/en
Pending legal-status Critical Current

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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
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6666—Compounds of group C08G18/48 or C08G18/52
    • C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
    • C08G18/6681—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38
    • C08G18/6688—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3271
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets
    • C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Led Device Packages (AREA)

Abstract

The invention discloses a nanometer aluminum oxide modified composite epoxy pouring sealant for an LED streetlamp display screen. The nanometer aluminum oxide modified composite epoxy pouring sealant has the advantages that during the preparation of the sealant, surface treatment is performed on nanometer aluminum oxide through a silane coupling agent, the treated nanometer aluminum oxide is allowed to react with polyurethane prepolymer to obtain silicon-containing polyurethane prepolymer modified nanometer aluminum oxide; the modified nanometer aluminum oxide filler has good dispersity and combinability, and effects of strengthening, toughness increasing and thermal conductivity increasing are achieved; a cured sealant film is good in stability and excellent in electric performance, has an even heat conduction effect and is promising in application prospect in LED display screen encapsulation.

Description

A kind of LED street lamp display screen is with nanometer alumina modified composite epoxy casting glue
Technical field
The present invention relates to LED casting glue technical field, particularly relate to a kind of LED street lamp display screen with nanometer alumina modified Composite epoxy casting glue.
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 street lamp display screen is with nano oxidized The composite epoxy casting glue that aluminum is modified.
The present invention is achieved by the following technical solutions:
A kind of LED street lamp display screen is with nanometer alumina modified composite epoxy casting glue, it is characterised in that this packaging plastic Prepared by the raw material of following weight portion: bisphenol A epoxide resin 30-60, silicon-based polyurethane performed polymer modified nano-alumina 40- 50, diluent CYH-277 5-15, firming agent 20-80, antioxidant 0.1-0.5, UV light stabilizing agent 0.01-0.05, ultraviolet light Absorbent 0.01-0.05.
Described silicon-based polyurethane performed polymer 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, silane coupler 2-3, dibutyl Tin dilaurate stannum 0.1-0.2.
Preparation method is:
(1) putting in reaction vessel by polyether polyol, heating removing moisture, is subsequently added diphenyl under nitrogen atmosphere Methane diisocyanate, hybrid reaction 6-8h under the conditions of 80-90 DEG C.
(2) nano aluminium oxide is disperseed 1-1.5h with silane coupler mixed grinding, put into step (1) reaction subsequently In container, reduction system temperature, to 60-70 DEG C, adds dibutyl tin dilaurate, drips diethyl after mixed grinding reaction 2-3h Hydramine, continues cooling discharge after griding reaction 1-1.5h, obtains described silicon-based polyurethane performed polymer 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, the oxidation of silicon-based polyurethane performed polymer modified Nano Aluminum, diluent, antioxidant, UV light stabilizing agent, UV absorbers mixing and stirring, add firming agent, Bian Jia subsequently Limit is stirred, and after interpolation, mixed material is heated to 90-100 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, be heated to 110-130 DEG C, permanent I.e. obtain, after temperature solidification 3-4h, the LED that embedding is good.
The present invention by nano aluminium oxide after silane coupler surface processes with polyurethane prepolymer precursor reactant, obtain siliceous poly- Urethane performed polymer modified nano-alumina, this modified nano alumina filters has good dispersion in the epoxy Property and associativity, reach strengthen, toughness reinforcing, improve heat conductivity effect, the packaging adhesive film good stability after solidification, electrical property is excellent Good, there is uniform heat-conducting effect, have broad application prospects in LED display encapsulates.
Detailed description of the invention
The casting glue of this embodiment is prepared by the raw material stirring mix homogeneously of following weight portion: bisphenol A epoxide resin 40, contain Silicon polyurethane performed polymer modified nano-alumina 40, diluent CYH-277 10, methyl hexahydrophthalic anhydride 50, antioxidant 0.2, ultraviolet Light stabilizer 0.02, UV absorbers 0.02.
Wherein silicon-based polyurethane performed polymer modified nano-alumina is prepared by following raw material: polyether polyol 15, two Methylenebis phenyl isocyanate 8, diethanolamine are appropriate, nano aluminium oxide 45, silane coupler 2.5, dibutyl tin dilaurate 0.1。
Preparation method is:
(1) putting in reaction vessel by polyether polyol, heating removing moisture, is subsequently added diphenyl under nitrogen atmosphere Methane diisocyanate, hybrid reaction 6h under the conditions of 85 DEG C.
(2) nano aluminium oxide is disperseed 1h with silane coupler mixed grinding, put into step (1) reaction vessel subsequently In, reduction system temperature, to 60 DEG C, adds dibutyl tin dilaurate, drips diethanolamine, continue after mixed grinding reaction 2.5h Cooling discharge after continuous griding reaction 1.2h, obtains described silicon-based polyurethane performed polymer modified nano-alumina.
The using method of this casting glue is: first by bisphenol A epoxide resin, the oxidation of silicon-based polyurethane performed polymer modified Nano Aluminum, diluent, antioxidant, UV light stabilizing agent, UV absorbers mixing and stirring, add firming agent, Bian Jia subsequently Limit is stirred, and after interpolation, mixed material is heated to 90 DEG C, and gained glue injects LED mould to be packaged after vacuum defoamation processes In tool, take out pre-packaged LED after natural precuring 3h, be placed in vacuum drying oven, be heated to 120 DEG C, isothermal curing 3.5h After i.e. obtain the LED that embedding is good.
The performance test results of this casting glue is as follows:
Detection project Testing result
Thermal conductivity (W.m-1.k-1) 0.55
Elongation at break (%) 26.5
Hot strength (MPa) 10.4
Thermal coefficient of expansion 0.58
Water absorption rate 0.18

Claims (4)

1. a LED street lamp display screen is with nanometer alumina modified composite epoxy casting glue, it is characterised in that this packaging plastic by The raw material of following weight portion prepare: bisphenol A epoxide resin 30-60, silicon-based polyurethane performed polymer modified nano-alumina 40-50, Diluent CYH-277 5-15, firming agent 20-80, antioxidant 0.1-0.5, UV light stabilizing agent 0.01-0.05, UV Absorption Agent 0.01-0.05.
A kind of LED street lamp display screen the most as claimed in claim 1 is with nanometer alumina modified composite epoxy casting glue, and it is special Levying and be, described silicon-based polyurethane performed polymer 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, silane coupler 2-3, dibutyl Tin dilaurate stannum 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) nano aluminium oxide is disperseed 1-1.5h with silane coupler mixed grinding, put into step (1) reaction vessel subsequently In, reduction system temperature, to 60-70 DEG C, adds dibutyl tin dilaurate, drips diethanolamine after mixed grinding reaction 2-3h, Continue cooling discharge after griding reaction 1-1.5h, obtain described silicon-based polyurethane performed polymer modified nano-alumina.
A kind of LED street lamp display screen the most as claimed in claim 1 is with nanometer alumina modified composite epoxy casting glue, and it is special Levying and be, described firming agent is the one in methyl hexahydrophthalic anhydride, methyl tetrahydro phthalic anhydride.
A kind of LED street lamp display screen making with nanometer alumina modified composite epoxy casting glue the most as claimed in claim 1 By method it is: first by bisphenol A epoxide resin, silicon-based polyurethane performed polymer modified nano-alumina, diluent, antioxidant, ultraviolet Light stabilizer, UV absorbers mixing and stirring, add firming agent subsequently, stirring while adding, mixes after interpolation Material is heated to 90-100 DEG C, and gained glue injects in LED die to be packaged after vacuum defoamation processes, natural precuring 2- Take out pre-packaged LED after 3h, be placed in vacuum drying oven, be heated to 110-130 DEG C, i.e. obtain embedding after isothermal curing 3-4h good LED.
CN201610409977.8A 2016-06-03 2016-06-03 Nanometer aluminum oxide modified composite epoxy pouring sealant for LED streetlamp display screen Pending CN106047253A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106753128A (en) * 2016-12-16 2017-05-31 安徽中威光电材料有限公司 Anti-corrosion type epoxy resin composite material that a kind of LED tack coats are modified with expanded vermiculite powder and preparation method thereof
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 (3)

* Cited by examiner, † Cited by third party
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 Low-density high-impact-resistance epoxy resin pouring sealant and preparation method thereof
CN103087665A (en) * 2013-01-31 2013-05-08 合肥工业大学 High-heat-conductivity insulation low-viscosity epoxy resin pouring sealant and preparation method thereof
CN104263299A (en) * 2014-09-01 2015-01-07 上海三思电子工程有限公司 Single-component epoxy thermal conductive adhesive and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
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 Low-density high-impact-resistance epoxy resin pouring sealant and preparation method thereof
CN103087665A (en) * 2013-01-31 2013-05-08 合肥工业大学 High-heat-conductivity insulation low-viscosity epoxy resin pouring sealant and preparation method thereof
CN104263299A (en) * 2014-09-01 2015-01-07 上海三思电子工程有限公司 Single-component epoxy thermal conductive adhesive and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106753128A (en) * 2016-12-16 2017-05-31 安徽中威光电材料有限公司 Anti-corrosion type epoxy resin composite material that a kind of LED tack coats are modified with expanded vermiculite powder and preparation method thereof
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: 20161026