CN106047249A - Composite nano-magnesia filling modified composite epoxy pouring sealant for LED displays - Google Patents

Composite nano-magnesia filling modified composite epoxy pouring sealant for LED displays Download PDF

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Publication number
CN106047249A
CN106047249A CN201610402061.XA CN201610402061A CN106047249A CN 106047249 A CN106047249 A CN 106047249A CN 201610402061 A CN201610402061 A CN 201610402061A CN 106047249 A CN106047249 A CN 106047249A
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China
Prior art keywords
nano
composite
modified
rare earth
magnesia
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Pending
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CN201610402061.XA
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Chinese (zh)
Inventor
肖宪书
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Bengbu Gaohua Resolution Technology Co Ltd
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Bengbu Gaohua Resolution Technology Co Ltd
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Priority to CN201610402061.XA priority Critical patent/CN106047249A/en
Publication of CN106047249A publication Critical patent/CN106047249A/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
    • C08G18/40—High-molecular-weight compounds
    • C08G18/48—Polyethers
    • 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
    • C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72—Polyisocyanates or polyisothiocyanates
    • C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
    • C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
    • C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
    • C08G18/7671—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group
    • 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
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • C08K5/098—Metal salts of carboxylic acids
    • 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
    • C08K9/02—Ingredients treated with inorganic 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
    • 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
    • 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)
  • Led Device Packages (AREA)

Abstract

The invention discloses a composite nano-magnesia filling modified composite epoxy pouring sealant for LED displays. According to the pouring sealant, nano-magnesia with high heat conduction is subjected to surface coupling pretreatment with a rare earth oxide-titanium aluminum complex coupling agent; then nano-magnesia is mixed and reacted with a polyurethane prepolymer; finally, composite filler integrating combination properties of inorganic matters and organic matters is obtained, has good dispersity and combination performance, overcomes the defect of proneness to agglomeration of traditional nano-filler, has excellent compounding effect with epoxy resin and efficiently improves the heat-conducting property and mechanical properties of materials; the prepared pouring sealant has good flowability, film layers are uniformly and stably distributed, LED chips packaged with the composite epoxy pouring sealant have long service life and show good application prospect in packaging of high-power LED displays.

Description

The composite epoxy filling that a kind of LED display composite Nano magnesium oxide is filling-modified Sealing
Technical field
The present invention relates to LED casting glue technical field, particularly relate to a kind of LED display composite Nano magnesium oxide and fill 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 display composite Nano aoxidizes The composite epoxy casting glue that magnesium is filling-modified.
The present invention is achieved by the following technical solutions:
The composite epoxy casting glue that a kind of LED display composite Nano magnesium oxide is filling-modified, 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 magnesium oxide 30- 50, zinc stearate 1-2, diluent CYH-277 5-15, firming agent 20-80, antioxidant 0.1-0.5, UV light stabilizing agent 0.01- 0.05, UV absorbers 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 magnesia 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 magnesia 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 magnesia.
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 Magnesium, zinc stearate, diluent, antioxidant, UV light stabilizing agent, UV absorbers mixing and stirring, add solid subsequently Agent, stirring while adding, after interpolation, mixed material is heated to 60-80 DEG C, and gained glue injects after vacuum defoamation processes In LED die to be packaged, take out pre-packaged LED after natural precuring 2-3h, be placed in vacuum drying oven, be heated to 80- 100 DEG C, after isothermal curing 3-4h, i.e. obtain the LED that embedding is good.
The present invention by the nano magnesia of high heat conduction through rare earth oxide-titanium aluminum composite coupler surface coupling pretreatment, Again by itself and base polyurethane prepolymer for use as hybrid reaction, finally give the compounded mix having inorganic matter concurrently with Organic substance combination property, its There is good dispersibility and associativity, improve the defect that Conventional nano filler is easily reunited, and compound effect with epoxy resin Good, improve heat conductivility and the mechanical property of material efficiently, the casting glue good fluidity of preparation, film layer is evenly distributed surely Fixed, the LED chip with the encapsulation of this composite epoxy resin glue is long for service life, shows in terms of high-power LED display screen encapsulation Go out good application prospect.
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 magnesium oxide 40, zinc stearate 1.5, diluent CYH-277 10, methyl hexahydrophthalic anhydride 40, antioxidant 0.2, purple Outer 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 magnesia 45, aluminate coupling agent 1.5, titanate coupling agent 1, 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 7h 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 130 DEG C, hybrid reaction 4h, and products therefrom mixes dispersion and grinds 2h with nano magnesia, is put into subsequently In step (1) reaction vessel, reduction system temperature, to 60-70 DEG C, adds dibutyl tin dilaurate, after mixed grinding reaction 2h Dropping diethanolamine, continues cooling discharge after griding reaction 1h, obtains described rare earth-base polyurethane prepolymer for use as modified Nano oxidation Magnesium.
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 Magnesium, zinc stearate, diluent, antioxidant, UV light stabilizing agent, UV absorbers mixing and stirring, add solid subsequently Agent, stirring while adding, after interpolation, mixed material is heated to 60-80 DEG C, and gained glue injects after vacuum defoamation processes In LED die to be packaged, take out pre-packaged LED after natural precuring 2.5h, be placed in vacuum drying oven, be heated to 90- 100 DEG C, after isothermal curing 3.5h, 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) 0.52
Elongation at break (%) 25.8
Hot strength (MPa) 8.5
Thermal coefficient of expansion 0.62
Water absorption rate 0.28

Claims (4)

1. the composite epoxy casting glue that a LED display composite Nano magnesium oxide is filling-modified, it is characterised in that this encapsulation Glue is 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 magnesium oxide 30-50, zinc stearate 1-2, diluent CYH-277 5-15, firming agent 20-80, antioxidant 0.1-0.5, UV light stabilizing agent 0.01-0.05, UV absorbers 0.01-0.05.
The composite epoxy casting glue that a kind of LED display composite Nano magnesium oxide the most as claimed in claim 1 is filling-modified, It is characterized in that, 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 are appropriate, nano magnesia 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 magnesia 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 magnesia.
The composite epoxy casting glue that a kind of LED display composite Nano magnesium oxide the most as claimed in claim 1 is filling-modified, It is characterized in that, described firming agent is the one in methyl hexahydrophthalic anhydride, methyl tetrahydro phthalic anhydride.
The composite epoxy casting glue that a kind of LED display composite Nano magnesium oxide the most as claimed in claim 1 is filling-modified Using method be: first by bisphenol A epoxide resin, rare earth-base polyurethane prepolymer for use as modified Nano magnesium oxide, zinc stearate, dilution Agent, antioxidant, UV light stabilizing agent, UV absorbers mixing and stirring, add firming agent subsequently, stirring while adding, After interpolation, mixed material is heated to 60-80 DEG C, and gained glue injects LED die to be packaged after vacuum defoamation processes In, take out pre-packaged LED after natural precuring 2-3h, be placed in vacuum drying oven, be heated to 80-100 DEG C, isothermal curing 3- The LED that embedding is good is i.e. obtained after 4h.
CN201610402061.XA 2016-06-08 2016-06-08 Composite nano-magnesia filling modified composite epoxy pouring sealant for LED displays Pending CN106047249A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108864582A (en) * 2018-07-20 2018-11-23 王迅 A kind of wear-resistant rubber liner
CN115819794A (en) * 2022-12-23 2023-03-21 长春永固科技有限公司 Modified epoxy resin, preparation method thereof and UV epoxy resin pouring sealant

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
CN104130736A (en) * 2014-07-28 2014-11-05 宁国市裕华电器有限公司 Encapsulating compound for thin-film capacitor
CN104448701A (en) * 2013-09-17 2015-03-25 明和化成株式会社 Epoxy resin composition, purpose of same, and fillings for epoxy resin composition

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
CN104448701A (en) * 2013-09-17 2015-03-25 明和化成株式会社 Epoxy resin composition, purpose of same, and fillings for epoxy resin composition
CN104130736A (en) * 2014-07-28 2014-11-05 宁国市裕华电器有限公司 Encapsulating compound for thin-film capacitor

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
吴玉光 等: "《化肥使用指南》", 31 July 2001, 中国农业出版社 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108864582A (en) * 2018-07-20 2018-11-23 王迅 A kind of wear-resistant rubber liner
CN115819794A (en) * 2022-12-23 2023-03-21 长春永固科技有限公司 Modified epoxy resin, preparation method thereof and UV epoxy resin pouring sealant

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Application publication date: 20161026

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