CN108300408A - A kind of high lux maintenance LED organosilicon material for packaging - Google Patents
A kind of high lux maintenance LED organosilicon material for packaging Download PDFInfo
- Publication number
- CN108300408A CN108300408A CN201711396294.4A CN201711396294A CN108300408A CN 108300408 A CN108300408 A CN 108300408A CN 201711396294 A CN201711396294 A CN 201711396294A CN 108300408 A CN108300408 A CN 108300408A
- Authority
- CN
- China
- Prior art keywords
- parts
- vinyl
- component
- silica gel
- organosilicon material
- 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.)
- Granted
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- 239000000463 material Substances 0.000 title claims abstract description 59
- 238000012423 maintenance Methods 0.000 title claims abstract description 17
- 238000004806 packaging method and process Methods 0.000 title claims abstract description 16
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 68
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 49
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000000741 silica gel Substances 0.000 claims abstract description 48
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 48
- -1 polymethylphenylsiloxane Polymers 0.000 claims abstract description 36
- 239000000843 powder Substances 0.000 claims abstract description 27
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000003054 catalyst Substances 0.000 claims abstract description 17
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 16
- 230000000694 effects Effects 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 229920001577 copolymer Polymers 0.000 claims abstract description 13
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000001257 hydrogen Substances 0.000 claims abstract description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 11
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 11
- 229910000077 silane Inorganic materials 0.000 claims abstract description 11
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 8
- 229920005989 resin Polymers 0.000 claims abstract description 8
- 239000011347 resin Substances 0.000 claims abstract description 8
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Substances C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 230000008878 coupling Effects 0.000 claims abstract description 7
- 238000010168 coupling process Methods 0.000 claims abstract description 7
- 238000005859 coupling reaction Methods 0.000 claims abstract description 7
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 7
- 229920001921 poly-methyl-phenyl-siloxane Polymers 0.000 claims abstract description 7
- 229920005573 silicon-containing polymer Polymers 0.000 claims abstract description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 66
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 42
- 229960001866 silicon dioxide Drugs 0.000 claims description 42
- 238000006243 chemical reaction Methods 0.000 claims description 41
- 229920000734 polysilsesquioxane polymer Polymers 0.000 claims description 40
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 30
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 24
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 23
- 229910052757 nitrogen Inorganic materials 0.000 claims description 21
- 238000002360 preparation method Methods 0.000 claims description 16
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 10
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 10
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 9
- 125000000746 allylic group Chemical group 0.000 claims description 9
- 230000031709 bromination Effects 0.000 claims description 9
- 238000005893 bromination reaction Methods 0.000 claims description 9
- 239000012044 organic layer Substances 0.000 claims description 9
- 239000000047 product Substances 0.000 claims description 9
- 238000000926 separation method Methods 0.000 claims description 9
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 9
- HDYFAPRLDWYIBU-UHFFFAOYSA-N 1-silylprop-2-en-1-one Chemical class [SiH3]C(=O)C=C HDYFAPRLDWYIBU-UHFFFAOYSA-N 0.000 claims description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 8
- 239000011777 magnesium Substances 0.000 claims description 8
- 229910052749 magnesium Inorganic materials 0.000 claims description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical class [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 5
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 5
- 239000000292 calcium oxide Substances 0.000 claims description 5
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 5
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical class CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 5
- IUYHWZFSGMZEOG-UHFFFAOYSA-M magnesium;propane;chloride Chemical group [Mg+2].[Cl-].C[CH-]C IUYHWZFSGMZEOG-UHFFFAOYSA-M 0.000 claims description 5
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 230000006837 decompression Effects 0.000 claims description 4
- YQGOWXYZDLJBFL-UHFFFAOYSA-N dimethoxysilane Chemical compound CO[SiH2]OC YQGOWXYZDLJBFL-UHFFFAOYSA-N 0.000 claims description 4
- 239000003292 glue Substances 0.000 claims description 4
- 239000000178 monomer Substances 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 229910000085 borane Inorganic materials 0.000 claims description 3
- 150000001721 carbon Chemical class 0.000 claims description 3
- 238000006116 polymerization reaction Methods 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- UORVGPXVDQYIDP-UHFFFAOYSA-N trihydridoboron Substances B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 claims description 3
- 238000005292 vacuum distillation Methods 0.000 claims description 3
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical class OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 2
- 229920001843 polymethylhydrosiloxane Polymers 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims 1
- 239000004327 boric acid Substances 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- 238000007711 solidification Methods 0.000 claims 1
- 230000008023 solidification Effects 0.000 claims 1
- 230000004907 flux Effects 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 4
- 239000005977 Ethylene Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000005538 encapsulation Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 238000006459 hydrosilylation reaction Methods 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- WRECIMRULFAWHA-UHFFFAOYSA-N trimethyl borate Chemical class COB(OC)OC WRECIMRULFAWHA-UHFFFAOYSA-N 0.000 description 2
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- 241001062009 Indigofera Species 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 239000005083 Zinc sulfide Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000004494 ethyl ester group Chemical group 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 229920003216 poly(methylphenylsiloxane) Polymers 0.000 description 1
- 229920006380 polyphenylene oxide Polymers 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
Classifications
-
- 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
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/52—Encapsulations
- H01L33/56—Materials, e.g. epoxy or silicone resin
-
- 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
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
-
- 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
-
- 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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Silicon Polymers (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of high lux maintenance LED organosilicon material for packaging, the organosilicon material includes organic silica gel component A, organic silica gel B component, nano magnesia, fluorescent powder and acrylate copolymer；Wherein organic silica gel component A composition is as follows：0.05 0.5 parts of 5 15 parts of dimethyl silicone polymer, organic 38 parts of the borosilicate tackifier of activity, 10 25 parts of end-vinyl ultra-branching organic siliconresin and the platinum catalyst that end group is 60 85 parts of the polymethylphenylsiloxane of vinyl, end group is vinyl；Organic silica gel B component composition is as follows：End group is 5 15 parts of 45 55 parts of 35 45 parts of polymethyl-benzene base vinylsiloxane, polymethyl hydrogen siloxane, the MQ resins of vinyl, 172 38 parts of silane coupling A；Machine silica gel component A in organosilicon material, organic silica gel B component, nano magnesia, fluorescent powder and acrylate copolymer quality parts ratio be 100:100:2.5‑18:3‑8:1‑3.The present invention has the advantages that：（1）Resistance to environment hot and cold alternation；（2）It will not xanthochromia；（3）High light flux.
Description
Technical field
The present invention relates to a kind of LED encapsulation materials, more particularly, to a kind of high lux maintenance LED encapsulation organosilicon material
Material.
Background technology
LED, that is, light emitting diode is a kind of high-performance solid light source, with the advantage in terms of energy conservation and environmental protection, and uses the longevity
It orders long.Currently, LED is commonly applied in daily life and work, its application principle is by indigo plant
Light LED is irradiated fluorescent material, generates the yellow light with blue light complementation, and then obtain white light.
Energy Star standard requires the LED light of 25000 hour longevity conjunction to exist in 6000 hours when requirement lux maintenances
91.8%, and if have lamp-type be oriented lamp, highest test environment temperature up to 55 DEG C ± 5 DEG C, want by the quite high standard of proposition
It asks.
Such as a kind of a kind of encapsulating material of LED filament disclosed in Chinese patent literature, application publication number CN
105542693 A, including red fluorescence powder and the glue crosslinking agent that is mixed with；Glue crosslinking agent is prepared by the raw material of following parts by weight
It arrives：72 parts of epoxy resin, 18-22 parts of polyphenylene oxide powder, 4 parts of methyl phenyl silicone oil, nano-zinc sulfide 0.2-0.4, mass concentration
In nano-ceramic powder transparency liquid 6-8, nano-titanium dioxide 4-5, benzoyl peroxide 0.1-0.2, the maleic anhydride of 30-40%
0.4-0.5, silane coupling agent 0.1-0.2,0.01-0.02 parts of chloroform antioxidant, 20-25 parts of curing agent.The present invention overcomes existing
There is the angle of emergence present in technology small, the low technological deficiency of light emission rate provides a kind of envelope improving transmissivity and luminous intensity
Package material.But there is also many shortcomings, such as the material of main part used in its formula is epoxy resin, quality
It is often more crisp, the possibility of fragmentation may be faced in hot and cold alternation, xanthochromia may occurs in it in use in addition,
The luminous efficiency and luminous flux of vivid final LED light.
Invention content
The present invention be in order to overcome in the prior art encapsulating material intolerant to hot and cold alternation, may exist xanthochromia possibility,
And the problem that luminous flux is relatively low, one kind is provided and can be resistant to environment hot and cold alternation, will not xanthochromia, a kind of bloom of high light flux it is logical
Sustainment rate LED organosilicon material for packaging.
To achieve the goals above, the present invention uses following technical scheme：
A kind of high lux maintenance LED organosilicon material for packaging, the organosilicon material include organic silica gel component A, have
Machine silica gel B component, nano magnesia, fluorescent powder and acrylate copolymer；
The organic silica gel component A composition is as follows：End group is 60-85 parts of the polymethylphenylsiloxane of vinyl, end group is
5-15 parts of dimethyl silicone polymer, organic 3-8 parts of the borosilicate tackifier of activity, the end-vinyl ultra-branching organic siliconresin of vinyl
10-25 parts and 0.05-0.5 parts of platinum catalyst；
The organosilicon B component composition is as follows：End group is 35-45 parts of the polymethyl-benzene base vinylsiloxane of vinyl, gathers
45-55 parts of methyl hydrogen siloxane, 5-15 parts of MQ resins, silane coupling A -172；
Machine silica gel component A, organic silica gel B component, nano magnesia, fluorescent powder and acroleic acid polymerization in the organosilicon material
The quality parts ratio of object is 100:100:2.5-18:3-8:1-3.
The material of main part used in the present invention is organosilicon material, by containing vinyl component and silicon in organosilicon AB glue
Under the action of platinum catalyst hydrosilylation occurs for hydrogen ingredient, and to be solidified into one, it is organic that activity is added wherein
Borosilicate tackifier and end-vinyl ultra-branching organic siliconresin can effectively adjust the viscosity and form of whole resin so that its
Suitable for the requirement of encapsulation, while active group is increased again, to be formed by curing more tie points, to meet package material
Expect the requirement to mechanical property.The luminous flux of encapsulating material can effectively be increased by adding nano oxidized magnesium component in the material.
And the addition of acrylate copolymer, although the light transmittance of LED lamp bead can be made to decline 5-10%, in 6000 hours mistakes of lighting
In journey acrylate copolymer gradually become by milky do it is colourless, to step up light light emission rate 5-10%.It is mended during lighting
It repays and maintains the stabilization of luminous flux since luminous flux declines.
Preferably, the preparation method of the organic borosilicate tackifier of activity is as follows：Under nitrogen protection according to quality
100 parts of number meter polymethyl hydrogen siloxane, 100 parts of toluene, three（Pentafluorophenyl group）0.02 part of borine drips thereto after stirring evenly
15 parts of hydroxy-ethyl acrylates are added to be dissolved in the solution of 10 parts of toluene, control temperature is to 30 DEG C after being added dropwise to complete, reaction 30 minutes, then
4 parts of trimethylborates are added dropwise thereto again and are dissolved in the solution of 10 parts of toluene, increasing temperature, the reaction was continued 2 hours to 50 DEG C, reduces
Temperature is added 2 parts of activated carbon stirring and adsorbings and filters to take filtrate after 0.5 hour, decompression steams toluene and obtained with low-boiling-point substance to room temperature
The organic borosilicate tackifier of activity.
The organic borosilicate tackifier of addition activity can adjust the viscosity of overall package material so that it is suitable as package material
Material.In addition wherein also contain acrylic acid structure, terrible addition reaction of hydrogen easily occurs with silicon hydrogen, increases reaction forming point, contributes to
The increase of its mechanical strength.
Preferably, the preparation method of the end-vinyl ultra-branching organic siliconresin is as follows：
（a）The preparation of monomer：Under -20 DEG C and nitrogen protection atmosphere, trichlorine is added in a kettle according to mass fraction meter
10 parts of silane and 100 parts dry of ether, then thereto the allylic bromination magnesium that 1.0 mol/L are added dropwise while stirring
190-200 parts of diethyl ether solution, the reaction was continued 30 minutes after being added dropwise, and then heats to 20 DEG C, and the reaction was continued 1.5-3 hours,
The dilute hydrochloric acid 100ml for stopping reacting addition 1mol/L thereto is stirred 30 minutes, is stood liquid separation and is taken upper organic layer, with saturated carbon
Acid sodium solution is washed to neutrality, product through being evaporated under reduced pressure, cross silicagel column, finally obtain three pure acrylsilanes；
（b）Under nitrogen protection atmosphere, step is taken（a）In obtained 150 parts of 100 parts of three acrylsilanes, toluene and platiniferous
2% catalyst 0.1-0.5 parts of Karst is added in reaction kettle, and temperature is increased after stirring evenly to 90 DEG C, is reacted 4-8 hours,
Vacuum distillation removes toluene and oligomer, obtains end-vinyl ultra-branching organic siliconresin.
Dissaving polymer is the tree form modification of highly branched three-D space structure, contains the end that can be largely modified
Base has many advantages, such as that intermolecular less entanglement, dissolubility is good, viscosity is low, easy film forming and reactivity are high.End-vinyl ultra-branching
The one kind of organic siliconresin as dissaving polymer not only has all properties of dissaving polymer, simultaneously as structure
A large amount of vinyl is contained in outer end, and reactivity is high, can be good at participating in hydrosilylation.
Preferably, also containing 16 vinyl polysilsesquioxanes in the organosilicon material.
Preferably, the preparation method of the 16 vinyl polysilsesquioxanes is as follows：
1）Under nitrogen protection, meter takes 10 parts of 60 parts of tetramethylammonium hydroxide and calcium oxide to be dissolved in methanol 80 in parts by weight
It is added in reaction kettle in part, the solution that 20 parts of vinyltrimethoxysilanes are dissolved in 60 parts of methanol is then added dropwise thereto, often
It is stirred to react under temperature 12-18 hours, then increases temperature to flowing back, be evaporated under reduced pressure after the reaction was continued 24 hours, obtain white powder
End, white powder passes through water respectively and the n-hexane of boiling cleans 3 times, obtains eight vinyl polysilsesquioxanes；
2）Step 1 is taken according to mass fraction meter）In 50 parts of eight vinyl polysilsesquioxane, 100 parts of tetrahydrofuran, methyl two
80-85 parts of methoxy silane and 0.5 part of the Karst catalyst of platiniferous 2%, are stirred to react 24 hours at a reflux temperature, react
After be added 2 parts of activated carbons, stirring 30 minutes after.It filters to get filtrate, it is complete with unreacted to be evaporated under reduced pressure away tetrahydrofuran
Methyl dimethoxysilane obtains the polysilsesquioxane containing 16 methoxyl groups；
3）Under nitrogen protection, meter takes step 2 in parts by weight）In 15 parts of the polysilsesquioxane containing 16 methoxyl groups be dissolved in
In 100 parts of tetrahydrofurans, then thereto the allylic bromination magnesium diethyl ether solution that 1.0 mol/L are added dropwise while stirring
180ml, 30 DEG C are reacted 2 hours, are then increased temperature and after the reaction was continued 30 minutes, are stopped reaction to 50 DEG C and being added thereto
The dilute hydrochloric acid 100ml of 1mol/L is stirred 30 minutes, is stood liquid separation and is taken upper organic layer, in being washed to saturated sodium carbonate solution
Property, product through being evaporated under reduced pressure, cross silicagel column, finally obtain 16 pure vinyl polysilsesquioxanes.
Preferably, machine silica gel component A, organic silica gel B component and 16 vinyl are poly- again in the organosilicon material
The 100 of half siloxanes:100:3.
Polysilsesquioxane is a kind of unique cage structure organo-silicon compound, due to the silicon containing rigidity in its structure
Oxygen cage structure, therefore the heat-resisting and mechanical property of its molecule is very excellent, adding it in encapsulating material can be effective
Reinforcing material heat-resisting and mechanical property, be added to the refractive index as material can also be improved in encapsulating material in addition,
Be conducive to the luminous efficiency of LED light.
Preferably, after the organosilicon material is according to the good each component of recipe configuration, it is packaged using dispenser, so
It is placed at 85-105 DEG C and carries out baking-curing.
Therefore, the present invention has the advantages that：（1）Resistance to environment hot and cold alternation；（2）It will not xanthochromia；（3）Bloom is logical
Amount.
Specific implementation mode
Technical scheme of the present invention is made to further describe explanation below by specific embodiment.
If saying the raw material that the raw material of use is commonly used in the art without specified otherwise, in the embodiment of the present invention, implement
Method employed in example, is the conventional method of this field.
Embodiment 1
A kind of high lux maintenance LED organosilicon material for packaging, the organosilicon material include organic silica gel component A, have
Machine silica gel B component, nano magnesia, fluorescent powder and acrylate copolymer；
The organic silica gel component A composition is as follows：End group is 60 parts of the polymethylphenylsiloxane of vinyl, end group is ethylene
5 parts of the dimethyl silicone polymer of base, organic 3 parts of the borosilicate tackifier of activity, 10 parts of end-vinyl ultra-branching organic siliconresin and
0.05 part of platinum catalyst；
The organosilicon B component composition is as follows：End group is 35 parts of polymethyl-benzene base vinylsiloxane, the poly- methyl of vinyl
45 parts of hydrogen siloxane, 5 parts of MQ resins, 3 parts of silane coupling A -172；
Machine silica gel component A, organic silica gel B component, nano magnesia, fluorescent powder and acroleic acid polymerization in the organosilicon material
The quality parts ratio of object is 100:100:2.5:3:1.
After the organosilicon material is according to the good each component of recipe configuration, it is packaged using dispenser, is subsequently placed in 85
Baking-curing is carried out at DEG C.
Then the LED light after will be packaged carries out thang-kng rate test at 55 DEG C, and the thang-kng rate after 6000 hours is
95.6%, refractive index 1.52.
Embodiment 2
A kind of high lux maintenance LED organosilicon material for packaging, the organosilicon material include organic silica gel component A, have
Machine silica gel B component, 16 vinyl polysilsesquioxanes, nano magnesia, fluorescent powder and acrylate copolymer；
The organic silica gel component A composition is as follows：End group is 85 parts of the polymethylphenylsiloxane of vinyl, end group is ethylene
15 parts of the dimethyl silicone polymer of base, organic 8 parts of the borosilicate tackifier of activity, 25 parts of end-vinyl ultra-branching organic siliconresin and
0.5 part of platinum catalyst；
The organosilicon B component composition is as follows：End group is 45 parts of polymethyl-benzene base vinylsiloxane, the poly- methyl of vinyl
55 parts of hydrogen siloxane, 15 parts of MQ resins, 8 parts of silane coupling A -172；
Machine silica gel component A, organic silica gel B component, 16 vinyl polysilsesquioxanes, nano oxygen in the organosilicon material
The quality parts ratio for changing magnesium, fluorescent powder and acrylate copolymer is 100:100:3: 18: 8: 3.
After the organosilicon material is according to the good each component of recipe configuration, it is packaged using dispenser, is subsequently placed in 100
Baking-curing is carried out at DEG C.
Then the LED light after will be packaged carries out thang-kng rate test at 55 DEG C, and the thang-kng rate after 6000 hours is
96.2%, refractive index 1.56.
Embodiment 3
A kind of high lux maintenance LED organosilicon material for packaging, the organosilicon material include organic silica gel component A, have
Machine silica gel B component, 16 vinyl polysilsesquioxanes, nano magnesia, fluorescent powder and acrylate copolymer；
The organic silica gel component A composition is as follows：End group is 75 parts of the polymethylphenylsiloxane of vinyl, end group is ethylene
8 parts of the dimethyl silicone polymer of base, organic 5 parts of the borosilicate tackifier of activity, 18 parts of end-vinyl ultra-branching organic siliconresin and
0.2 part of platinum catalyst；
The organosilicon B component composition is as follows：End group is 40 parts of polymethyl-benzene base vinylsiloxane, the poly- methyl of vinyl
50 parts of hydrogen siloxane, 8 parts of MQ resins, 5 parts of silane coupling A -172；
Machine silica gel component A, organic silica gel B component, 16 vinyl polysilsesquioxanes, nano oxygen in the organosilicon material
The quality parts ratio for changing magnesium, fluorescent powder and acrylate copolymer is 100:100:3:10:5:2.
After the organosilicon material is according to the good each component of recipe configuration, it is packaged using dispenser, is subsequently placed in 105
Baking-curing is carried out at DEG C.
Then the LED light after will be packaged carries out thang-kng rate test at 55 DEG C, and the thang-kng rate after 6000 hours is
95.9%, refractive index 1.55.
Embodiment 4
A kind of high lux maintenance LED organosilicon material for packaging, the organosilicon material include organic silica gel component A, have
Machine silica gel B component, 16 vinyl polysilsesquioxanes, nano magnesia, fluorescent powder and acrylate copolymer；
The organic silica gel component A composition is as follows：End group is 65 parts of the polymethylphenylsiloxane of vinyl, end group is ethylene
12 parts of the dimethyl silicone polymer of base, organic 4 parts of the borosilicate tackifier of activity, 20 parts of end-vinyl ultra-branching organic siliconresin and
0.4 part of platinum catalyst；
The organosilicon B component composition is as follows：End group is 40 parts of polymethyl-benzene base vinylsiloxane, the poly- methyl of vinyl
42 parts of hydrogen siloxane, 13 parts of MQ resins, 7 parts of silane coupling A -172；
Machine silica gel component A, organic silica gel B component, 16 vinyl polysilsesquioxanes, nano oxygen in the organosilicon material
The quality parts ratio for changing magnesium, fluorescent powder and acrylate copolymer is 100:100:3:12:7:1.
After the organosilicon material is according to the good each component of recipe configuration, it is packaged using dispenser, is subsequently placed in 95
Baking-curing is carried out at DEG C.
Then the LED light after will be packaged carries out thang-kng rate test at 55 DEG C, and the thang-kng rate after 6000 hours is
95.1%, refractive index 1.59.
Embodiment 5
The preparation method of the organic borosilicate tackifier of activity is as follows：Under nitrogen protection according to the poly- methyl hydrogen of mass fraction meter
100 parts of siloxanes, 100 parts of toluene, three（Pentafluorophenyl group）15 parts of acrylic acid hydroxyls are added dropwise in 0.02 part of borine thereto after stirring evenly
Ethyl ester is dissolved in the solution of 10 parts of toluene, and temperature is controlled after being added dropwise to complete to 30 DEG C, reacts 30 minutes, is then added dropwise 4 thereto again
Part trimethylborate is dissolved in the solution of 10 parts of toluene, and increasing temperature, the reaction was continued 2 hours to 50 DEG C, reduces temperature to room temperature, adds
Enter 2 parts of activated carbon stirring and adsorbings and filter to take filtrate after 0.5 hour, decompression steams toluene and obtains the organic borosilicate increasing of activity with low-boiling-point substance
Stick.
Embodiment 6
The preparation method of the end-vinyl ultra-branching organic siliconresin is as follows：
（a）The preparation of monomer：Under -20 DEG C and nitrogen protection atmosphere, trichlorine is added in a kettle according to mass fraction meter
10 parts of silane and 100 parts dry of ether, then thereto the allylic bromination magnesium that 1.0 mol/L are added dropwise while stirring
190 parts of diethyl ether solution, the reaction was continued 30 minutes after being added dropwise, and then heats to 20 DEG C, and the reaction was continued 1.5-3 hours, stops
The dilute hydrochloric acid 100ml that 1mol/L is added in reaction thereto is stirred 30 minutes, is stood liquid separation and is taken upper organic layer, with saturated sodium carbonate
Solution is washed to neutrality, product through being evaporated under reduced pressure, cross silicagel column, finally obtain three pure acrylsilanes；
（b）Under nitrogen protection atmosphere, step is taken（a）In obtained 150 parts of 100 parts of three acrylsilanes, toluene and platiniferous
2% 0.1 part of Karst catalyst is added in reaction kettle, and temperature is increased after stirring evenly to 90 DEG C, is reacted 4-8 hours, decompression
Distillation removes toluene and oligomer, obtains end-vinyl ultra-branching organic siliconresin.
The end-vinyl ultra-branching organic siliconresin is tested by GPC, and using toluene as mobile phase, polystyrene is mark
Quasi- sample, relative molecular weight 12863.
Embodiment 7
The preparation method of the end-vinyl ultra-branching organic siliconresin is as follows：
（a）The preparation of monomer：Under -20 DEG C and nitrogen protection atmosphere, trichlorine is added in a kettle according to mass fraction meter
10 parts of silane and 100 parts dry of ether, then thereto the allylic bromination magnesium that 1.0 mol/L are added dropwise while stirring
190-200 parts of diethyl ether solution, the reaction was continued 30 minutes after being added dropwise, and then heats to 20 DEG C, and the reaction was continued 1.5-3 hours,
The dilute hydrochloric acid 100ml for stopping reacting addition 1mol/L thereto is stirred 30 minutes, is stood liquid separation and is taken upper organic layer, with saturated carbon
Acid sodium solution is washed to neutrality, product through being evaporated under reduced pressure, cross silicagel column, finally obtain three pure acrylsilanes；
（b）Under nitrogen protection atmosphere, step is taken（a）In obtained 150 parts of 100 parts of three acrylsilanes, toluene and platiniferous
2% catalyst 0.1-0.5 parts of Karst is added in reaction kettle, and temperature is increased after stirring evenly to 90 DEG C, is reacted 4-8 hours,
Vacuum distillation removes toluene and oligomer, obtains end-vinyl ultra-branching organic siliconresin.
The end-vinyl ultra-branching organic siliconresin is tested by GPC, and using toluene as mobile phase, polystyrene is mark
Quasi- sample, relative molecular weight 14580.
Embodiment 8
The preparation method of the 16 vinyl polysilsesquioxanes is as follows：
1）Under nitrogen protection, meter takes 10 parts of 60 parts of tetramethylammonium hydroxide and calcium oxide to be dissolved in methanol 80 in parts by weight
It is added in reaction kettle in part, the solution that 20 parts of vinyltrimethoxysilanes are dissolved in 60 parts of methanol is then added dropwise thereto, often
It is stirred to react under temperature 12 hours, then increases temperature to flowing back, be evaporated under reduced pressure after the reaction was continued 24 hours, obtain white powder,
White powder passes through water respectively and the n-hexane of boiling cleans 3 times, obtains eight vinyl polysilsesquioxanes；
2）Step 1 is taken according to weight fraction meter）In 50 parts of eight vinyl polysilsesquioxane, 100 parts of tetrahydrofuran, methyl two
80 parts of methoxy silane and 0.5 part of the Karst catalyst of platiniferous 2%, are stirred to react 24 hours, reaction terminates at a reflux temperature
2 parts of activated carbons are added afterwards, after stirring 30 minutes.It filters to get filtrate, is evaporated under reduced pressure away tetrahydrofuran and the complete methyl of unreacted
Dimethoxysilane obtains the polysilsesquioxane containing 16 methoxyl groups；
3）Under nitrogen protection, meter takes step 2 in parts by weight）In 15 parts of the polysilsesquioxane containing 16 methoxyl groups be dissolved in
In 100 parts of tetrahydrofurans, then thereto the allylic bromination magnesium diethyl ether solution that 1.0 mol/L are added dropwise while stirring
180ml, 30 DEG C are reacted 2 hours, are then increased temperature and after the reaction was continued 30 minutes, are stopped reaction to 50 DEG C and being added thereto
The dilute hydrochloric acid 100ml of 1mol/L is stirred 30 minutes, is stood liquid separation and is taken upper organic layer, in being washed to saturated sodium carbonate solution
Property, product through being evaporated under reduced pressure, cross silicagel column, finally obtain 16 pure vinyl polysilsesquioxanes.
Embodiment 9
The preparation method of the 16 vinyl polysilsesquioxanes is as follows：
1）Under nitrogen protection, meter takes 10 parts of 60 parts of tetramethylammonium hydroxide and calcium oxide to be dissolved in methanol 80 in parts by weight
It is added in reaction kettle in part, the solution that 20 parts of vinyltrimethoxysilanes are dissolved in 60 parts of methanol is then added dropwise thereto, often
It is stirred to react under temperature 18 hours, then increases temperature to flowing back, be evaporated under reduced pressure after the reaction was continued 24 hours, obtain white powder,
White powder passes through water respectively and the n-hexane of boiling cleans 3 times, obtains eight vinyl polysilsesquioxanes；
2）Step 1 is taken according to weight fraction meter）In 50 parts of eight vinyl polysilsesquioxane, 100 parts of tetrahydrofuran, methyl two
85 parts of methoxy silane and 0.5 part of the Karst catalyst of platiniferous 2%, are stirred to react 24 hours, reaction terminates at a reflux temperature
2 parts of activated carbons are added afterwards, after stirring 30 minutes.It filters to get filtrate, is evaporated under reduced pressure away tetrahydrofuran and the complete methyl of unreacted
Dimethoxysilane obtains the polysilsesquioxane containing 16 methoxyl groups；
3）Under nitrogen protection, meter takes step 2 in parts by weight）In 15 parts of the polysilsesquioxane containing 16 methoxyl groups be dissolved in
In 100 parts of tetrahydrofurans, then thereto the allylic bromination magnesium diethyl ether solution that 1.0 mol/L are added dropwise while stirring
180ml, 30 DEG C are reacted 2 hours, are then increased temperature and after the reaction was continued 30 minutes, are stopped reaction to 50 DEG C and being added thereto
The dilute hydrochloric acid 100ml of 1mol/L is stirred 30 minutes, is stood liquid separation and is taken upper organic layer, in being washed to saturated sodium carbonate solution
Property, product through being evaporated under reduced pressure, cross silicagel column, finally obtain 16 pure vinyl polysilsesquioxanes.
Embodiment 10
The preparation method of the 16 vinyl polysilsesquioxanes is as follows：
1）Under nitrogen protection, meter takes 10 parts of 60 parts of tetramethylammonium hydroxide and calcium oxide to be dissolved in methanol 80 in parts by weight
It is added in reaction kettle in part, the solution that 20 parts of vinyltrimethoxysilanes are dissolved in 60 parts of methanol is then added dropwise thereto, often
It is stirred to react under temperature 15 hours, then increases temperature to flowing back, be evaporated under reduced pressure after the reaction was continued 24 hours, obtain white powder,
White powder passes through water respectively and the n-hexane of boiling cleans 3 times, obtains eight vinyl polysilsesquioxanes；
2）Step 1 is taken according to weight fraction meter）In 50 parts of eight vinyl polysilsesquioxane, 100 parts of tetrahydrofuran, methyl two
82 parts of methoxy silane and 0.5 part of the Karst catalyst of platiniferous 2%, are stirred to react 24 hours, reaction terminates at a reflux temperature
2 parts of activated carbons are added afterwards, after stirring 30 minutes.It filters to get filtrate, is evaporated under reduced pressure away tetrahydrofuran and the complete methyl of unreacted
Dimethoxysilane obtains the polysilsesquioxane containing 16 methoxyl groups；
3）Under nitrogen protection, meter takes step 2 in parts by weight）In 15 parts of the polysilsesquioxane containing 16 methoxyl groups be dissolved in
In 100 parts of tetrahydrofurans, then thereto the allylic bromination magnesium diethyl ether solution that 1.0 mol/L are added dropwise while stirring
180ml, 30 DEG C are reacted 2 hours, are then increased temperature and after the reaction was continued 30 minutes, are stopped reaction to 50 DEG C and being added thereto
The dilute hydrochloric acid 100ml of 1mol/L is stirred 30 minutes, is stood liquid separation and is taken upper organic layer, in being washed to saturated sodium carbonate solution
Property, product through being evaporated under reduced pressure, cross silicagel column, finally obtain 16 pure vinyl polysilsesquioxanes.
Claims (7)
1. a kind of high lux maintenance LED organosilicon material for packaging, characterized in that the organosilicon material includes organosilicon
Glue component A, organic silica gel B component, nano magnesia, fluorescent powder and acrylate copolymer；
The organic silica gel component A composition is as follows：End group is 60-85 parts of the polymethylphenylsiloxane of vinyl, end group is
5-15 parts of dimethyl silicone polymer, organic 3-8 parts of the borosilicate tackifier of activity, the end-vinyl ultra-branching organic siliconresin of vinyl
10-25 parts and 0.05-0.5 parts of platinum catalyst；
The organosilicon B component composition is as follows：End group is 35-45 parts of the polymethyl-benzene base vinylsiloxane of vinyl, gathers
45-55 parts of methyl hydrogen siloxane, 5-15 parts of MQ resins, -172 3-8 parts of silane coupling A；
Machine silica gel component A, organic silica gel B component, nano magnesia, fluorescent powder and acroleic acid polymerization in the organosilicon material
The quality parts ratio of object is 100:100:2.5-18:3-8:1-3.
2. a kind of high lux maintenance LED organosilicon material for packaging according to claim 1, characterized in that described
The preparation method of the organic borosilicate tackifier of activity is as follows：Under nitrogen protection according to mass fraction meter polymethyl hydrogen siloxane 100
Part, 100 parts of toluene, three（Pentafluorophenyl group）0.02 part of borine is added dropwise 15 parts of hydroxy-ethyl acrylates and is dissolved in 10 thereto after stirring evenly
The solution of part toluene controls temperature to 30 DEG C, reacts 30 minutes, 4 parts of boric acid front threes are then added dropwise thereto again after being added dropwise to complete
Ester is dissolved in the solution of 10 parts of toluene, and increasing temperature, the reaction was continued 2 hours to 50 DEG C, reduces temperature to room temperature, 2 parts of activated carbons are added
Stirring and adsorbing filters to take filtrate after 0.5 hour, decompression steams toluene and obtains the organic borosilicate tackifier of activity with low-boiling-point substance.
3. a kind of high lux maintenance LED organosilicon material for packaging according to claim 1, characterized in that described
The preparation method of end-vinyl ultra-branching organic siliconresin is as follows：
（a）The preparation of monomer：Under -20 DEG C and nitrogen protection atmosphere, trichlorine is added in a kettle according to mass fraction meter
10 parts of silane and 100 parts dry of ether, then thereto the allylic bromination magnesium that 1.0 mol/L are added dropwise while stirring
190-200 parts of diethyl ether solution, the reaction was continued 30 minutes after being added dropwise, and then heats to 20 DEG C, and the reaction was continued 1.5-3 hours,
The dilute hydrochloric acid 100ml for stopping reacting addition 1mol/L thereto is stirred 30 minutes, is stood liquid separation and is taken upper organic layer, with saturated carbon
Acid sodium solution is washed to neutrality, product through being evaporated under reduced pressure, cross silicagel column, finally obtain three pure acrylsilanes；
（b）Under nitrogen protection atmosphere, step is taken（a）In obtained 150 parts of 100 parts of three acrylsilanes, toluene and platiniferous
2% catalyst 0.1-0.5 parts of Karst is added in reaction kettle, and temperature is increased after stirring evenly to 90 DEG C, is reacted 4-8 hours,
Vacuum distillation removes toluene and oligomer, obtains end-vinyl ultra-branching organic siliconresin.
4. a kind of high lux maintenance LED organosilicon material for packaging according to claim 1, characterized in that described
Also contain 16 vinyl polysilsesquioxanes in organosilicon material.
5. a kind of high lux maintenance LED organosilicon material for packaging according to claim 4, characterized in that described
The preparation method of 16 vinyl polysilsesquioxanes is as follows：
1）Under nitrogen protection, meter takes 10 parts of 60 parts of tetramethylammonium hydroxide and calcium oxide to be dissolved in methanol 80 in parts by weight
It is added in reaction kettle in part, the solution that 20 parts of vinyltrimethoxysilanes are dissolved in 60 parts of methanol is then added dropwise thereto, often
It is stirred to react under temperature 12-18 hours, then increases temperature to flowing back, be evaporated under reduced pressure after the reaction was continued 24 hours, obtain white powder
End, white powder passes through water respectively and the n-hexane of boiling cleans 3 times, obtains eight vinyl polysilsesquioxanes；
2）Step 1 is taken according to mass fraction meter）In 50 parts of eight vinyl polysilsesquioxane, 100 parts of tetrahydrofuran, methyl two
80-85 parts of methoxy silane and 0.5 part of the Karst catalyst of platiniferous 2%, are stirred to react 24 hours at a reflux temperature, react
After be added 2 parts of activated carbons, stirring 30 minutes after filter to get filtrate, be evaporated under reduced pressure away tetrahydrofuran and the complete first of unreacted
Base dimethoxysilane obtains the polysilsesquioxane containing 16 methoxyl groups；
3）Under nitrogen protection, meter takes step 2 in parts by weight）In 15 parts of the polysilsesquioxane containing 16 methoxyl groups be dissolved in
In 100 parts of tetrahydrofurans, then thereto the allylic bromination magnesium diethyl ether solution that 1.0 mol/L are added dropwise while stirring
180ml, 30 DEG C are reacted 2 hours, are then increased temperature and after the reaction was continued 30 minutes, are stopped reaction to 50 DEG C and being added thereto
The dilute hydrochloric acid 100ml of 1mol/L is stirred 30 minutes, is stood liquid separation and is taken upper organic layer, in being washed to saturated sodium carbonate solution
Property, product through being evaporated under reduced pressure, cross silicagel column, finally obtain 16 pure vinyl polysilsesquioxanes.
6. a kind of high lux maintenance LED organosilicon material for packaging according to claim 1 or 4 or 5, characterized in that
Machine silica gel component A, organic silica gel B component and the 100 of 16 vinyl polysilsesquioxanes in the organosilicon material:100:
3。
7. a kind of high lux maintenance LED organosilicon material for packaging according to claim 1, characterized in that described
It after organosilicon material is according to the good each component of recipe configuration, is packaged using dispenser, is subsequently placed at 85-105 DEG C and is dried
Roasting solidification.
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| WO2021109730A1 (en) * | 2019-12-02 | 2021-06-10 | 苏州太湖电工新材料股份有限公司 | Two-component organosilicon potting sealant and application method therefor |
| CN112370577A (en) * | 2020-10-15 | 2021-02-19 | 浙江省肿瘤医院 | Portable fistula protection drainage mechanism |
| CN112370577B (en) * | 2020-10-15 | 2022-12-16 | 浙江省肿瘤医院 | Portable fistula protection drainage mechanism |
| CN115232476A (en) * | 2022-07-11 | 2022-10-25 | 浙江葆润应用材料有限公司 | Material for liquid cooling pipe sleeve and preparation method and application thereof |
| CN115232476B (en) * | 2022-07-11 | 2024-03-22 | 浙江葆润应用材料有限公司 | Material for liquid cooling pipe sleeve and preparation method and application thereof |
| CN115505268A (en) * | 2022-09-30 | 2022-12-23 | 江苏至昕新材料有限公司 | Organic silicon insulating gel for packaging semiconductor module and preparation process thereof |
| CN115505268B (en) * | 2022-09-30 | 2024-02-06 | 江苏至昕新材料有限公司 | Organic silicon insulating gel for packaging semiconductor module and preparation process thereof |
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