CN109679292A - A kind of high durable agent of low hygroscopicity LED encapsulation material and preparation method thereof - Google Patents
A kind of high durable agent of low hygroscopicity LED encapsulation material and preparation method thereof Download PDFInfo
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- CN109679292A CN109679292A CN201910028937.2A CN201910028937A CN109679292A CN 109679292 A CN109679292 A CN 109679292A CN 201910028937 A CN201910028937 A CN 201910028937A CN 109679292 A CN109679292 A CN 109679292A
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- led encapsulation
- epoxy resin
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- 239000000463 material Substances 0.000 title claims abstract description 55
- 238000005538 encapsulation Methods 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- -1 amino silane modified bisphenol Chemical class 0.000 claims abstract description 68
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 33
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 32
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 32
- 239000003822 epoxy resin Substances 0.000 claims abstract description 30
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 30
- 239000002994 raw material Substances 0.000 claims abstract description 23
- CCJAYIGMMRQRAO-UHFFFAOYSA-N 2-[4-[(2-hydroxyphenyl)methylideneamino]butyliminomethyl]phenol Chemical compound OC1=CC=CC=C1C=NCCCCN=CC1=CC=CC=C1O CCJAYIGMMRQRAO-UHFFFAOYSA-N 0.000 claims abstract description 22
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 17
- 235000010215 titanium dioxide Nutrition 0.000 claims abstract description 17
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 15
- 239000010703 silicon Substances 0.000 claims abstract description 15
- 230000000740 bleeding effect Effects 0.000 claims abstract description 14
- OUPZKGBUJRBPGC-UHFFFAOYSA-N 1,3,5-tris(oxiran-2-ylmethyl)-1,3,5-triazinane-2,4,6-trione Chemical compound O=C1N(CC2OC2)C(=O)N(CC2OC2)C(=O)N1CC1CO1 OUPZKGBUJRBPGC-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000005038 ethylene vinyl acetate Substances 0.000 claims abstract description 12
- GLDOVTGHNKAZLK-UHFFFAOYSA-N n-octadecyl alcohol Natural products CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims abstract description 12
- 239000001257 hydrogen Substances 0.000 claims abstract description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 11
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 10
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 10
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims abstract description 9
- 235000019260 propionic acid Nutrition 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims description 30
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 17
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 16
- 238000007872 degassing Methods 0.000 claims description 11
- 229930185605 Bisphenol Natural products 0.000 claims description 9
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 claims description 6
- 125000005456 glyceride group Chemical group 0.000 claims description 6
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical class [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 claims description 6
- 238000007711 solidification Methods 0.000 claims description 6
- 230000008023 solidification Effects 0.000 claims description 6
- 229920013822 aminosilicone Polymers 0.000 claims description 4
- YBRVSVVVWCFQMG-UHFFFAOYSA-N 4,4'-diaminodiphenylmethane Chemical compound C1=CC(N)=CC=C1CC1=CC=C(N)C=C1 YBRVSVVVWCFQMG-UHFFFAOYSA-N 0.000 claims description 3
- ZFOZVQLOBQUTQQ-UHFFFAOYSA-N Citronensaeure-tributylester Natural products CCCCOC(=O)CC(O)(C(=O)OCCCC)CC(=O)OCCCC ZFOZVQLOBQUTQQ-UHFFFAOYSA-N 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- 229920001038 ethylene copolymer Polymers 0.000 claims description 3
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 2
- 235000009508 confectionery Nutrition 0.000 claims description 2
- 239000004519 grease Substances 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 2
- QZCLKYGREBVARF-UHFFFAOYSA-N Acetyl tributyl citrate Chemical compound CCCCOC(=O)CC(C(=O)OCCCC)(OC(C)=O)CC(=O)OCCCC QZCLKYGREBVARF-UHFFFAOYSA-N 0.000 claims 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims 1
- 239000005977 Ethylene Substances 0.000 claims 1
- 150000001335 aliphatic alkanes Chemical class 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- YQGOWXYZDLJBFL-UHFFFAOYSA-N dimethoxysilane Chemical compound CO[SiH2]OC YQGOWXYZDLJBFL-UHFFFAOYSA-N 0.000 claims 1
- 230000008595 infiltration Effects 0.000 claims 1
- 238000001764 infiltration Methods 0.000 claims 1
- 229910000077 silane Inorganic materials 0.000 claims 1
- 239000000052 vinegar Substances 0.000 claims 1
- PESZCXUNMKAYME-UHFFFAOYSA-N Citroflex A-4 Chemical compound CCCCOC(=O)CC(O)(C(=O)OCCCC)C(C(C)=O)C(=O)OCCCC PESZCXUNMKAYME-UHFFFAOYSA-N 0.000 abstract description 5
- 230000000052 comparative effect Effects 0.000 description 8
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- 229910003978 SiClx Inorganic materials 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 3
- QMMBZOSZCYBCDC-UHFFFAOYSA-N NCCNCCC[SiH](OC(OCC)(OCC)OCC)OC Chemical compound NCCNCCC[SiH](OC(OCC)(OCC)OCC)OC QMMBZOSZCYBCDC-UHFFFAOYSA-N 0.000 description 2
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- JBGDSVVIBTXYJD-UHFFFAOYSA-N 2-hydroxy-4-oxopentane-1,2,3-tricarboxylic acid Chemical compound CC(=O)C(C(O)=O)C(O)(C(O)=O)CC(O)=O JBGDSVVIBTXYJD-UHFFFAOYSA-N 0.000 description 1
- 244000248349 Citrus limon Species 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 239000011469 building brick Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 210000002615 epidermis Anatomy 0.000 description 1
- HDERJYVLTPVNRI-UHFFFAOYSA-N ethene;ethenyl acetate Chemical compound C=C.CC(=O)OC=C HDERJYVLTPVNRI-UHFFFAOYSA-N 0.000 description 1
- BFMKFCLXZSUVPI-UHFFFAOYSA-N ethyl but-3-enoate Chemical compound CCOC(=O)CC=C BFMKFCLXZSUVPI-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000010358 mechanical oscillation Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 125000005487 naphthalate group Chemical group 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 150000003151 propanoic acid esters Chemical class 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
-
- 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
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The present invention provides a kind of high durable agent of low hygroscopicity LED encapsulation materials and preparation method thereof, it is prepared by the raw material of following parts by weight: 20-40 parts of amino silane modified bisphenol f type epoxy resin, 15-25 parts of polytetrafluoroethylene (PTFE), 10-18 parts of ethylene-vinyl acetate copolymer, 6-13 parts of polypropylene terephthalate, 6-12 parts of polyvinyl alcohol, 4-9 parts of N hydroxymethyl acrylamide, 3-7 parts of tributyl 2-acetylcitrate, 5-10 parts of rutile type titanium white, 2-5 parts of silicon boride, 6-10 parts of graphene oxide, 4-8 parts of propionic acid n-octadecyl alcohol ester, 8-14 parts of vinyltrimethoxysilane, 7-15 parts of polymethyl hydrogen siloxane, 3-6 parts of bleeding agent, 5-9 parts of triglycidyl isocyanurate.LED encapsulation material produced by the present invention has good thermal conductivity, lower hygroscopicity and good mechanical strength, is with a wide range of applications as LED encapsulation material.
Description
Technical field
The invention belongs to encapsulating material technical fields, and in particular to a kind of high durable agent of low hygroscopicity LED encapsulation material and its
Preparation method.
Background technique
LED is made of chip, metal wire, bracket, conducting resinl, encapsulating material etc., and encapsulating material therein primarily serves
Sealing and protection chip work normally, and avoid it by the influence of humidity in ambient enviroment and temperature；Fixed and support conducting wire, prevents
Only electronic building brick is generated variation that is damaged and causing component parameter by mechanical oscillation, impact；It reduces between LED chip and air
The gap of refractive index is to increase light output and effectively by hot the effects of being discharged of inside generation.Therefore, for encapsulating material,
It will have excellent leakproofness, translucency, caking property, dielectric properties and mechanical performance.
Encapsulating material used at present includes epoxy resin, polycarbonate, polymethyl methacrylate, glass, organic
The high transparency material such as silicon, however, with the brightness of LED and the continuous improvement of power and the development of white light LEDs, to LED's
Encapsulating material is also put forward higher requirements, such as more high refractive index, high transparency, high-termal conductivity, resistance to ultraviolet and heat ageing energy
Power and low thermal expansion coefficient, ion concentration and stress etc..And hygroscopicity, easy to aging, poor heat resistance, height existing for epoxy itself
The defects of mild short wavelength light is easy to change under shining, cured internal stress is big, largely effects on and shortens the service life of LED component.Cause
This, it is necessary to it is further improved on the basis of existing LED encapsulation material, to improve the comprehensive performance of LED encapsulation material.
Summary of the invention
For the above problem of the existing technology, the purpose of the present invention is to provide a kind of high durable agent of low hygroscopicity LED
Encapsulating material and preparation method thereof.
To achieve the goals above, the present invention the following technical schemes are provided:
A kind of high durable agent of low hygroscopicity LED encapsulation material, is prepared: amino silane modified by the raw material of following parts by weight
20-40 parts of bisphenol f type epoxy resin, 15-25 parts of polytetrafluoroethylene (PTFE), 10-18 parts of ethylene-vinyl acetate copolymer, poly- to benzene
6-13 parts of naphthalate, 6-12 parts of polyvinyl alcohol, 4-9 parts of N hydroxymethyl acrylamide, tributyl 2-acetylcitrate 3-7
Part, 5-10 parts of rutile type titanium white, 2-5 parts of silicon boride, 6-10 parts of graphene oxide, 4-8 parts of propionic acid n-octadecyl alcohol ester, second
8-14 parts of alkenyl trimethoxy silane, 7-15 parts of polymethyl hydrogen siloxane, 3-6 parts of bleeding agent, triglycidyl isocyanurate
5-9 parts.
Further, it is (1-3): 1 aerosol-OT salt and isooctanol that the bleeding agent, which is mass ratio,
Polyoxyethylene ether.Preferably, a kind of high durable agent of low hygroscopicity LED encapsulation material of the present invention, by the original of following parts by weight
Material is prepared: 30 parts modified of bisphenol A type epoxy resin of amino silicones, 20 parts of polytetrafluoroethylene (PTFE), ethene-vinyl acetate
4 parts of copolymer 1,10 parts of polypropylene terephthalate, 9 parts of polyvinyl alcohol, 7 parts of N hydroxymethyl acrylamide, acetyl lemon
5 parts of sour tributyl, 7.5 parts of rutile type titanium white, 3.5 parts of silicon boride, 8 parts of graphene oxide, propionic acid n-octadecyl alcohol ester 6
Part, 11 parts of vinyltrimethoxysilane, 11 parts of polymethyl hydrogen siloxane, 4.5 parts of bleeding agent, triglycidyl isocyanurate
7 parts.
Further, amino silane modified bisphenol f type epoxy resin of the present invention the preparation method is as follows: by bis-phenol
F type epoxy resin and N- (β-aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane are mixed with the weight ratio of 10:1,
90-100 DEG C is raised the temperature in the state of stirring, and 4,4'- diaminodiphenylmethane is then added and continues to be stirred to react
Reaction system is cooled to room temperature up to amino silane modified bisphenol f type epoxy resin by 40min.
The preparation method of LED encapsulation material of the present invention, comprising the following steps:
(1) weigh each raw material by corresponding parts by weight, by amino silane modified bisphenol f type epoxy resin, polytetrafluoroethylene (PTFE),
Ethylene-vinyl acetate copolymer and polypropylene terephthalate are placed in reaction kettle, under the revolving speed of 300-500r/min
It stirs and is to slowly warm up to 90-100 DEG C, after keeping this temperature mixing 10-20min, reaction temperature is down to 50-70 DEG C, it will be golden
Red stone-type titanium dioxide, silicon boride, graphene oxide are pre-mixed uniformly, are added into reaction kettle while stirring, after
Continue after being stirred 30-50min, mixture A is made；
(2) it will be mixed except each raw material of remaining of N hydroxymethyl acrylamide and triglycidyl isocyanurate, in 200-
It is stirred 15-30min under the revolving speed of 400r/min, mixture B is made；
(3) mixture A and mixture B are mixed, N hydroxymethyl acrylamide is then added and isocyanuric acid three contracts
Water glyceride, raises the temperature to 70-90 DEG C while stirring, continues to be de-gassed after being stirred to react 1-2h, takes off
The gas disposal time is 40-60min；
(4) mixture after degassing process is poured into mold, up to LED encapsulation material after solidification.
The utility model has the advantages that the present invention provides a kind of high durable agent of low hygroscopicity LED encapsulation material and preparation method thereof, the present invention
One kind using amino silane modified bisphenol f type epoxy resin as matrix resin, the modulus drop of the epoxy resin after modification
Low, silane group has lower surface tension and flexibility, solution can be promoted to penetrate into inside material epidermis through stomata, pole
The earth increases the permeability of polymeric system, so that flexibility is greatly improved, while improving the superficiality of resin
Energy；Amino silane modified bisphenol f type epoxy resin and polytetrafluoroethylene (PTFE), ethylene-vinyl acetate copolymer, poly terephthalic acid
Propylene glycol ester interworking plays an important role the performances such as resistant of high or low temperature, water resistance, the high tenacity for improving material.Rutile
Type titanium dioxide, silicon boride, graphene oxide can be improved the heat-conductive characteristic of material, and thermal shock resistance properties at high temperature is good
It is good, improve the weatherability of material.Polyvinyl alcohol provides the good film forming of material system；N hydroxymethyl acrylamide promotes raw material
Between cementation；Tributyl 2-acetylcitrate plays an important role the hardness for improving material；The positive octadecanol of propionic acid
Ester can be improved the photo and thermal stability of material；The addition of triglycidyl isocyanurate promotes the work of the crosslinking between raw material
With；The addition of vinyltrimethoxysilane, polymethyl hydrogen siloxane greatly improves the agent of low hygroscopicity energy of material.
It is obtained from test result, LED encapsulation material produced by the present invention has good thermal conductivity, lower moisture pick-up properties
With good mechanical strength, therefore encapsulating material produced by the present invention have stronger weatherability and agent of low hygroscopicity energy, conduct
LED encapsulation material is with a wide range of applications.
Specific embodiment
The invention will now be further described with reference to specific embodiments, but examples are merely exemplary, not to this hair
Bright range constitutes any restrictions.It will be understood by those skilled in the art that without departing from the spirit and scope of the invention
Can with the details and forms of the technical scheme of the invention are modified or replaced, but these modification and replacement each fall within it is of the invention
In protection scope.
The preparation method of amino silane modified bisphenol f type epoxy resin described in following embodiment and comparative example is such as
Under: by bisphenol f type epoxy resin and N- (β-aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane with the weight ratio of 10:1 into
Row mixing, raises the temperature to 90-100 DEG C while stirring, 4,4'- diaminodiphenylmethane is then added and continues to stir
40min is reacted, reaction system is cooled to room temperature up to amino silane modified bisphenol f type epoxy resin.
Embodiment 1
A kind of high durable agent of low hygroscopicity LED encapsulation material, is prepared by the raw material of following parts by weight: by following parts by weight
Raw material be prepared: 30 parts modified of bisphenol A type epoxy resin of amino silicones, 20 parts of polytetrafluoroethylene (PTFE), ethyl vinyl acetate
14 parts of ethylene copolymer, 10 parts of polypropylene terephthalate, 9 parts of polyvinyl alcohol, 7 parts of N hydroxymethyl acrylamide, acetyl
5 parts of tributyl citrate, 7.5 parts of rutile type titanium white, 3.5 parts of silicon boride, 8 parts of graphene oxide, the positive octadecanol of propionic acid
6 parts of ester, 11 parts of vinyltrimethoxysilane, 11 parts of polymethyl hydrogen siloxane, 4.5 parts of bleeding agent, isocyanuric acid three shrink sweet
7 parts of grease.The bleeding agent is the aerosol-OT salt and isooctanol polyethoxylate that mass ratio is 2:1.
The preparation method of LED encapsulation material of the present invention, comprising the following steps:
(1) weigh each raw material by corresponding parts by weight, by amino silane modified bisphenol f type epoxy resin, polytetrafluoroethylene (PTFE),
Ethylene-vinyl acetate copolymer and polypropylene terephthalate are placed in reaction kettle, are stirred under the revolving speed of 400r/min
And 95 DEG C are to slowly warm up to, after keeping this temperature mixing 15min, reaction temperature is down to 60 DEG C, by rutile type titanium white, boron
SiClx, graphene oxide are pre-mixed uniformly, are added into reaction kettle while stirring, continue to be stirred 40min
Afterwards, mixture A is made；
(2) it will be mixed except each raw material of remaining of N hydroxymethyl acrylamide and triglycidyl isocyanurate, in 300r/
It is stirred 23min under the revolving speed of min, mixture B is made；
(3) mixture A and mixture B are mixed, N hydroxymethyl acrylamide is then added and isocyanuric acid three contracts
Water glyceride raises the temperature to 80 DEG C while stirring, continues to be de-gassed after being stirred to react 1.5h, at degassing
The reason time is 50min；
(4) mixture after degassing process is poured into mold, up to LED encapsulation material after solidification.
Embodiment 2
A kind of high durable agent of low hygroscopicity LED encapsulation material, is prepared: amino silane modified by the raw material of following parts by weight
20 parts of bisphenol f type epoxy resin, 15 parts of polytetrafluoroethylene (PTFE), 10 parts of ethylene-vinyl acetate copolymer, poly terephthalic acid the third two
6 parts of alcohol ester, 6 parts of polyvinyl alcohol, 4 parts of N hydroxymethyl acrylamide, 3 parts of tributyl 2-acetylcitrate, rutile type titanium white 5
Part, 2 parts of silicon boride, 6 parts of graphene oxide, 4 parts of propionic acid n-octadecyl alcohol ester, 8 parts of vinyltrimethoxysilane, poly- methyl hydrogen
7 parts of siloxanes, 3 parts of bleeding agent, 5 parts of triglycidyl isocyanurate.
The bleeding agent is the aerosol-OT salt and isooctanol polyethoxylate that mass ratio is 1:1.
The preparation method of LED encapsulation material of the present invention, comprising the following steps:
(1) weigh each raw material by corresponding parts by weight, by amino silane modified bisphenol f type epoxy resin, polytetrafluoroethylene (PTFE),
Ethylene-vinyl acetate copolymer and polypropylene terephthalate are placed in reaction kettle, are stirred under the revolving speed of 300r/min
And 90 DEG C are to slowly warm up to, after keeping this temperature mixing 10min, reaction temperature is down to 50 DEG C, by rutile type titanium white, boron
SiClx, graphene oxide are pre-mixed uniformly, are added into reaction kettle while stirring, continue to be stirred 30min
Afterwards, mixture A is made；
(2) it will be mixed except each raw material of remaining of N hydroxymethyl acrylamide and triglycidyl isocyanurate, in 200r/
It is stirred 15min under the revolving speed of min, mixture B is made；
(3) mixture A and mixture B are mixed, N hydroxymethyl acrylamide is then added and isocyanuric acid three contracts
Water glyceride raises the temperature to 70 DEG C while stirring, continues to be de-gassed after being stirred to react 1h, degassing process
Time is 40min；
(4) mixture after degassing process is poured into mold, up to LED encapsulation material after solidification.
Embodiment 3
A kind of high durable agent of low hygroscopicity LED encapsulation material, is prepared: amino silane modified by the raw material of following parts by weight
25 parts of bisphenol f type epoxy resin, 18 parts of polytetrafluoroethylene (PTFE), 12 parts of ethylene-vinyl acetate copolymer, poly terephthalic acid the third two
8 parts of alcohol ester, 8 parts of polyvinyl alcohol, 6 parts of N hydroxymethyl acrylamide, 4 parts of tributyl 2-acetylcitrate, rutile type titanium white 7
Part, 3 parts of silicon boride, 7 parts of graphene oxide, 5 parts of propionic acid n-octadecyl alcohol ester, 10 parts of vinyltrimethoxysilane, poly- methyl
9 parts of hydrogen siloxane, 4 parts of bleeding agent, 6 parts of triglycidyl isocyanurate.
The bleeding agent is the aerosol-OT salt and isooctanol polyethoxylate that mass ratio is 1.5:1.
The preparation method of LED encapsulation material of the present invention, comprising the following steps:
(1) weigh each raw material by corresponding parts by weight, by amino silane modified bisphenol f type epoxy resin, polytetrafluoroethylene (PTFE),
Ethylene-vinyl acetate copolymer and polypropylene terephthalate are placed in reaction kettle, are stirred under the revolving speed of 350r/min
And 92 DEG C are to slowly warm up to, after keeping this temperature mixing 13min, reaction temperature is down to 55 DEG C, by rutile type titanium white, boron
SiClx, graphene oxide are pre-mixed uniformly, are added into reaction kettle while stirring, continue to be stirred 35min
Afterwards, mixture A is made；
(2) it will be mixed except each raw material of remaining of N hydroxymethyl acrylamide and triglycidyl isocyanurate, in 250r/
It is stirred 20min under the revolving speed of min, mixture B is made；
(3) mixture A and mixture B are mixed, N hydroxymethyl acrylamide is then added and isocyanuric acid three contracts
Water glyceride raises the temperature to 75 DEG C while stirring, continues to be de-gassed after being stirred to react 1.2h, at degassing
The reason time is 45min；
(4) mixture after degassing process is poured into mold, up to LED encapsulation material after solidification.
Embodiment 4
A kind of high durable agent of low hygroscopicity LED encapsulation material, is prepared: amino silane modified by the raw material of following parts by weight
40 parts of bisphenol f type epoxy resin, 25 parts of polytetrafluoroethylene (PTFE), 18 parts of ethylene-vinyl acetate copolymer, poly terephthalic acid the third two
13 parts of alcohol ester, 12 parts of polyvinyl alcohol, 9 parts of N hydroxymethyl acrylamide, 7 parts of tributyl 2-acetylcitrate, rutile type titanium white
10 parts, 5 parts of silicon boride, 10 parts of graphene oxide, 8 parts of propionic acid n-octadecyl alcohol ester, 14 parts of vinyltrimethoxysilane, poly- first
15 parts of base hydrogen siloxane, 6 parts of bleeding agent, 9 parts of triglycidyl isocyanurate.
The bleeding agent is the aerosol-OT salt and isooctanol polyethoxylate that mass ratio is 3:1.
The preparation method of LED encapsulation material of the present invention, comprising the following steps:
(1) weigh each raw material by corresponding parts by weight, by amino silane modified bisphenol f type epoxy resin, polytetrafluoroethylene (PTFE),
Ethylene-vinyl acetate copolymer and polypropylene terephthalate are placed in reaction kettle, are stirred under the revolving speed of 500r/min
And be to slowly warm up to 100 DEG C, after keeping this temperature mixing 20min, reaction temperature is down to 70 DEG C, by rutile type titanium white,
Silicon boride, graphene oxide are pre-mixed uniformly, are added into reaction kettle while stirring, continue to be stirred
After 50min, mixture A is made；
(2) it will be mixed except each raw material of remaining of N hydroxymethyl acrylamide and triglycidyl isocyanurate, in 400r/
It is stirred 30min under the revolving speed of min, mixture B is made；
(3) mixture A and mixture B are mixed, N hydroxymethyl acrylamide is then added and isocyanuric acid three contracts
Water glyceride raises the temperature to 90 DEG C while stirring, continues to be de-gassed after being stirred to react 2h, degassing process
Time is 60min；
(4) mixture after degassing process is poured into mold, up to LED encapsulation material after solidification.
Comparative example 1
Comparative example 1 the difference from embodiment 1 is that, amino silane modified bisphenol f type epoxy resin is replaced in comparative example 1
Change bisphenol f type epoxy resin into.
Comparative example 2
Comparative example 2 the difference from embodiment 1 is that, rutile type titanium white and poly- methyl hydrogen silicon are not added in comparative example 2
Oxygen alkane.
LED encapsulation material made from embodiment 1-4 and comparative example 1-2 is subjected to following performance test, test result is such as
Shown in table 1, obtained from table 1, LED encapsulation material produced by the present invention have good thermal conductivity, lower moisture pick-up properties and
Good mechanical strength, therefore encapsulating material produced by the present invention has stronger weatherability and agent of low hygroscopicity energy, is used as LED
Encapsulating material is with a wide range of applications.
Table 1
Claims (5)
1. a kind of high durable agent of low hygroscopicity LED encapsulation material, which is characterized in that be prepared by the raw material of following parts by weight: ammonia
20-40 parts modified of bisphenol f type epoxy resin of base silane, 15-25 parts of polytetrafluoroethylene (PTFE), ethylene-vinyl acetate copolymer 10-18
Part, 6-13 parts of polypropylene terephthalate, 6-12 parts of polyvinyl alcohol, 4-9 parts of N hydroxymethyl acrylamide, acetyl tributyl citrate
3-7 parts of tributyl, 5-10 parts of rutile type titanium white, 2-5 parts of silicon boride, 6-10 parts of graphene oxide, the positive octadecanol of propionic acid
4-8 parts of ester, 8-14 parts of vinyltrimethoxysilane, 7-15 parts of polymethyl hydrogen siloxane, 3-6 parts of bleeding agent, isocyanuric acid three
5-9 parts of ethylene oxidic ester.
2. a kind of high durable agent of low hygroscopicity LED encapsulation material according to claim 1, which is characterized in that the infiltration
Agent is that mass ratio is (1-3): 1 aerosol-OT salt and isooctanol polyethoxylate.
3. a kind of high durable agent of low hygroscopicity LED encapsulation material according to claim 1, which is characterized in that by following weight
The raw material of part is prepared: 30 parts modified of bisphenol A type epoxy resin of amino silicones, 20 parts of polytetrafluoroethylene (PTFE), ethylene-vinegar
14 parts of sour ethylene copolymer, 10 parts of polypropylene terephthalate, 9 parts of polyvinyl alcohol, 7 parts of N hydroxymethyl acrylamide, second
5 parts of acyl tributyl citrate, 7.5 parts of rutile type titanium white, 3.5 parts of silicon boride, 8 parts of graphene oxide, positive 18 carbon of propionic acid
6 parts of alcohol ester, 11 parts of vinyltrimethoxysilane, 11 parts of polymethyl hydrogen siloxane, 4.5 parts of bleeding agent, isocyanuric acid three shrink
7 parts of glyceride.
4. a kind of high durable agent of low hygroscopicity LED encapsulation material according to claim 1, which is characterized in that the amino silicone
The modified bisphenol f type epoxy resin of alkane the preparation method is as follows: by bisphenol f type epoxy resin and N- (β-aminoethyl)-γ-ammonia third
Ylmethyl dimethoxysilane is mixed with the weight ratio of 10:1, raises the temperature to 90-100 DEG C while stirring,
Then 4,4'- diaminodiphenylmethane is added to continue to be stirred to react 40min, reaction system is cooled to room temperature up to amino silane
Modified bisphenol f type epoxy resin.
5. the preparation method of the described in any item LED encapsulation materials of claim 1-4, which comprises the following steps:
(1) each raw material is weighed by corresponding parts by weight, by amino silane modified bisphenol f type epoxy resin, polytetrafluoroethylene (PTFE), second
Alkene-acetate ethylene copolymer and polypropylene terephthalate are placed in reaction kettle, are stirred under the revolving speed of 300-500r/min
It mixes and is to slowly warm up to 90-100 DEG C, after keeping this temperature mixing 10-20min, reaction temperature is down to 50-70 DEG C, by golden red
Stone-type titanium dioxide, silicon boride, graphene oxide are pre-mixed uniformly, are added into reaction kettle while stirring, are continued
After being stirred 30-50min, mixture A is made；
(2) it will be mixed except each raw material of remaining of N hydroxymethyl acrylamide and triglycidyl isocyanurate, in 200-400r/
It is stirred 15-30min under the revolving speed of min, mixture B is made；
(3) mixture A and mixture B are mixed, then addition N hydroxymethyl acrylamide and isocyanuric acid three shrink sweet
Grease raises the temperature to 70-90 DEG C while stirring, continues to be de-gassed after being stirred to react 1-2h, at degassing
The reason time is 40-60min；
(4) mixture after degassing process is poured into mold, up to LED encapsulation material after solidification.
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| CN113529201A (en) * | 2021-06-29 | 2021-10-22 | 吉祥三宝高科纺织有限公司 | Composite fabric combining moisture absorption, heat release and phase change temperature adjustment and preparation method thereof |
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