CN108641672A - A kind of anti-oxidant LED packaging plastics of high transparency - Google Patents
A kind of anti-oxidant LED packaging plastics of high transparency Download PDFInfo
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- CN108641672A CN108641672A CN201810554610.4A CN201810554610A CN108641672A CN 108641672 A CN108641672 A CN 108641672A CN 201810554610 A CN201810554610 A CN 201810554610A CN 108641672 A CN108641672 A CN 108641672A
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- parts
- methyl
- high transparency
- general structure
- led packaging
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- 239000003963 antioxidant agent Substances 0.000 title claims abstract description 21
- 230000003078 antioxidant effect Effects 0.000 title claims abstract description 21
- 235000006708 antioxidants Nutrition 0.000 title claims abstract description 21
- 238000004806 packaging method and process Methods 0.000 title claims abstract description 21
- 229920003023 plastic Polymers 0.000 title claims abstract description 21
- 239000004033 plastic Substances 0.000 title claims abstract description 21
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 42
- 230000000903 blocking effect Effects 0.000 claims abstract description 34
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 claims abstract description 27
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 11
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 5
- 239000003054 catalyst Substances 0.000 claims abstract description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 27
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 24
- 239000000126 substance Substances 0.000 claims description 23
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 13
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 12
- 229910021529 ammonia Inorganic materials 0.000 claims description 12
- 239000003921 oil Substances 0.000 claims description 11
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 10
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 7
- 239000000908 ammonium hydroxide Substances 0.000 claims description 7
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical group CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- OTEKOJQFKOIXMU-UHFFFAOYSA-N 1,4-bis(trichloromethyl)benzene Chemical compound ClC(Cl)(Cl)C1=CC=C(C(Cl)(Cl)Cl)C=C1 OTEKOJQFKOIXMU-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 238000007259 addition reaction Methods 0.000 claims description 5
- 239000012295 chemical reaction liquid Substances 0.000 claims description 5
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 claims description 5
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 5
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 5
- 229910052697 platinum Inorganic materials 0.000 claims description 5
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 3
- NKLOIQIDDWPNFE-UHFFFAOYSA-N [SiH4].C(C)(C)(C)OOC(C)(C)C Chemical compound [SiH4].C(C)(C)(C)OOC(C)(C)C NKLOIQIDDWPNFE-UHFFFAOYSA-N 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims 1
- XJQIBXPDDJYFMB-UHFFFAOYSA-N [Li].C[SiH2]N[SiH3] Chemical class [Li].C[SiH2]N[SiH3] XJQIBXPDDJYFMB-UHFFFAOYSA-N 0.000 claims 1
- 125000003342 alkenyl group Chemical group 0.000 claims 1
- 239000000460 chlorine Substances 0.000 claims 1
- 229910052801 chlorine Inorganic materials 0.000 claims 1
- 125000001309 chloro group Chemical group Cl* 0.000 claims 1
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 9
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 abstract description 5
- 239000004945 silicone rubber Substances 0.000 abstract description 5
- 230000032683 aging Effects 0.000 abstract description 3
- 230000035939 shock Effects 0.000 abstract description 3
- 229920000260 silastic Polymers 0.000 abstract description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 11
- 229920002554 vinyl polymer Polymers 0.000 description 11
- 238000002834 transmittance Methods 0.000 description 6
- JVZKVVDFQLHZBY-UHFFFAOYSA-N N1[SiH2]N[SiH2]N[SiH2]N[SiH2]1 Chemical compound N1[SiH2]N[SiH2]N[SiH2]N[SiH2]1 JVZKVVDFQLHZBY-UHFFFAOYSA-N 0.000 description 4
- QQIRAVWVGBTHMJ-UHFFFAOYSA-N [dimethyl-(trimethylsilylamino)silyl]methane;lithium Chemical class [Li].C[Si](C)(C)N[Si](C)(C)C QQIRAVWVGBTHMJ-UHFFFAOYSA-N 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- SHWQWXGIWFEYTA-UHFFFAOYSA-N 2,2,4,4,6,6-hexakis-phenyl-1,3,5,2,4,6-triazatrisilinane Chemical compound N1[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)N[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)N[Si]1(C=1C=CC=CC=1)C1=CC=CC=C1 SHWQWXGIWFEYTA-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 229920001709 polysilazane Polymers 0.000 description 3
- 229920001296 polysiloxane Polymers 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- DJYUESVJHJQLMR-UHFFFAOYSA-N [N].C1(=CC=CC=C1)[Si]C Chemical compound [N].C1(=CC=CC=C1)[Si]C DJYUESVJHJQLMR-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000007142 ring opening reaction Methods 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- UGXMKSYKRKUMGY-UHFFFAOYSA-N 1,3,5,2,4,6-triazatrisilinane Chemical compound N1[SiH2]N[SiH2]N[SiH2]1 UGXMKSYKRKUMGY-UHFFFAOYSA-N 0.000 description 1
- OGNSDRMLWYNUED-UHFFFAOYSA-N 1-cyclohexyl-4-[4-[4-(4-cyclohexylcyclohexyl)cyclohexyl]cyclohexyl]cyclohexane Chemical group C1CCCCC1C1CCC(C2CCC(CC2)C2CCC(CC2)C2CCC(CC2)C2CCCCC2)CC1 OGNSDRMLWYNUED-UHFFFAOYSA-N 0.000 description 1
- 0 CN(*)C(*)(*)NC[Si](C)(C)* Chemical compound CN(*)C(*)(*)NC[Si](C)(C)* 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- OGPNXGJLKXGASM-UHFFFAOYSA-N [Si].CC=C Chemical compound [Si].CC=C OGPNXGJLKXGASM-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 230000003026 anti-oxygenic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 125000006267 biphenyl group Chemical group 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 229910052564 epsomite Inorganic materials 0.000 description 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009776 industrial production Methods 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
- 210000003739 neck Anatomy 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 1
- -1 polysiloxanes Polymers 0.000 description 1
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical group CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/60—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which all the silicon atoms are connected by linkages other than oxygen atoms
- C08G77/62—Nitrogen atoms
-
- 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
-
- 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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Computer Hardware Design (AREA)
- Health & Medical Sciences (AREA)
- Power Engineering (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Manufacturing & Machinery (AREA)
- Packages (AREA)
- Wrappers (AREA)
- Packaging Frangible Articles (AREA)
Abstract
The invention belongs to silastic material technical field, more particularly to a kind of anti-oxidant LED packaging plastics of high transparency, by weight comprising following component：100 parts of methyl vinyl silicone rubber, 40~80 parts of the poly bis phenyl methyl silazane of methyl blocking, 10~40 parts of deicer, 4~8 parts of silane coupling agent, 0.1~0.3 part of platinum group catalyst, with good heat resistance, ageing resistance, anti-time property and cold-resistant thermal shock resistance properties, it is especially suitable for LED bulb and uses.
Description
Technical field
The invention belongs to silastic material technical field, more particularly to a kind of anti-oxidant LED packaging plastics of high transparency.
Background technology
Organo-silicon compound refer to that molecular backbone contains silicon-oxygen chemical key and silicon atom is at least straight with an organic group
Connect connected a kind of organic polymer synthetic material.Wherein, it is for the polysiloxanes that main chain forms with siliceous-oxygen-chemistry of silicones key
Most, most widely used, research the is most deep a kind of product of quantity in organosilicon product, and with siliceous-nitrogen-chemistry of silicones key for main chain group
At polysilazane product also gradually develop in.
The patent document of CN103305009A discloses a kind of preparation method of High-transparency silicon rubber, by methyl ethylene silicon
Rubber raw rubber, gas-phase silica, stearic acid 1801, dimethyldimethoxysil,ne, hexamethyldisilazane and distillation washiness
It is secondary to be uniformly mixed, after sizing material is kneaded and formed heating, heat refining, be cooled to room temperature to obtain High-transparency silicon rubber, have it is higher
The transparency, the heat resistance and antioxygenic property of the product are poor, in the case where not turning yellow, are only capable of under the conditions of 60~80 DEG C
Continuous use 15 days or so.
CN103122149A discloses a kind of optical package high refractive index High-transparency silicon rubber and preparation method thereof, leads to
The component A containing phenyl, vinyl for crossing a variety of fixed proportions, containing groups such as vinyl, the B component of methyl and component Cs containing phenyl
Point mixed configuration forms, and so as to improve the mechanical performance of silicon rubber, still, multicomponent combination may lead to product synthesis obtained
Step is complicated, raw material detection, the difficulty increase of production, it is difficult to carry out preferable control to overall performance.
Invention content
The present invention to solve the above-mentioned problems, provides a kind of anti-oxidant LED packaging plastics of high transparency, has good heat-resisting
Property, ageing resistance, anti-time property and cold-resistant thermal shock resistance properties, be especially suitable for LED bulb and use.
The present invention is realized using following technical scheme：
A kind of anti-oxidant LED packaging plastics of high transparency, by weight, including following component：Methyl vinyl silicone rubber 100
Part, 40~80 parts of the poly bis phenyl methyl silazane of methyl blocking, 10~40 parts of deicer, 4~8 parts of silane coupling agent, platinum group is urged
0.1~0.3 part of agent.
Preferred scheme, the deicer are vinyltrimethoxysilane.Select vinyltrimethoxysilane conduct
On the one hand deicer is used as deicer that can prevent from generating bubble in product, ensure that product smearing is uniformly not stratified, to improve
Coating and bond effect, on the other hand, included vinyl improves vinyl accounting in high transparency organosilicon material
Than the proportioning of high transparency organosilicon material medium vinyl, phenyl and methyl can be adjusted on demand, to obtain the production of different performance
Product, the heat resistance of high transparency organosilicon material, anti-time property and tensile resistance are preferable, on the other hand, can prevent product from generating
Bubble improves coating, bond effect.
Preferred scheme, the silane coupling agent are three tert-butyl peroxide silane of vinyl, three ethoxy of 3- aminopropyls
Base silane or γ-glycidyl ether oxygen propyl trimethoxy silicane, can improve the bonding force between metal, LED support.
Preferred scheme, the platinum group catalyst are the aqueous isopropanol of chloroplatinic acid, and platinum content is 1000~10000ppm.
Preferred scheme, the poly bis phenyl methyl silazane of methyl blocking are prepared by following steps：
1 part of hexichol dichlorosilane is added into reaction kettle in terms of mass parts in S1, in 4~6 parts of addition reaction kettles of toluene, stirs
It mixes and is passed through ammonia to not absorbed, after being alkalinity with pH test paper test reaction liquid, keep being passed through ammonia under the conditions of 16~18 DEG C
Stop reaction after 1~5h of gaseity, hexaphenyl cyclotrisilazane and octaphenyl cyclotetrasilazane is made, at this temperature hexaphenyl
Up to 36%, up to 52% following reaction occurs cyclotrisilazane yield for octaphenyl cyclotetrasilazane yield,
It reacts (a)：
It reacts (b)：
Wherein, n is integer, and in terms of mass parts, 60% or more the substance accounting of 50≤n≤200, pH of the invention is represented
Phenyl；
S2 is added in ammonium hydroxide and stirring to solution and is visible by naked eyes solid, is dehydrated isolated oil phase, is added into oil phase
It after drier is carried out dehydrating, is distilled under the conditions of 330~340 DEG C of temperature, condenser pipe is used in combination to intercept 240~300 DEG C of fractions,
Wherein, in terms of mass parts, hexaphenyl cyclotrisilazane accounting 30~50%, octaphenyl cyclotetrasilazane accounting 50~70%；
S3, in terms of mass parts, into reaction kettle be added step S2 obtain 1 part of substance, be dried after toluene 3~5
Part, 0.05~0.2 part of hexamethyldisilazane lithium salts, and the ruthenium trichloride of 10~30ppm is added, in 180~200 DEG C of dry nitrogens
2~3h is reacted in gas atmosphere, it is poly- that hexaphenyl cyclotrisilazane ring-opening reaction obtains the poly- diphenyl silazane of the first methyl blocking
Object is closed, the structure of the poly- diphenyl silicon nitrogen silane copolymer of the first methyl blocking is：
Wherein, pH represents phenyl, and n is integer, and 50≤n≤200；
Octaphenyl cyclotetrasilazane ring-opening reaction obtains the poly- diphenyl silicon nitrogen silane copolymer of second of methyl blocking, and described
The structure of the poly- diphenyl silicon nitrogen silane copolymer of two kinds of methyl blockings is：
Wherein, pH represents phenyl, and n is integer, and 50≤n≤200；
S4, in terms of mass parts, into reaction kettle be added step S3 obtain 5~10 parts of 1 part of substance, methanol, the concentrated sulfuric acid 4~
6 parts, under the conditions of 115~120 DEG C 0.5~1h be obtained by the reaction meet general structure (1) and general structure (2) methyl blocking it is poly-
Double phenyl methyl silazane mixtures,
General structure (1)：
General structure (2)：
In general structure (1) and (2), pH represents phenyl, and n is integer, and 50≤n≤200, in terms of mass parts, the first
Base blocks the substance accounting 30~50% for meeting general structure (1) in poly bis phenyl methyl silazane, meets general structure (2)
Substance accounting 50~70%.
Preferred scheme, in step S2, the ammonia temperature is 18~20 DEG C.Chloride leach is anti-for heat absorption in ammonium hydroxide
It answers, the ammonia temperature of addition is only suitably above temperature of reaction system, prevents the temperature of ammonium chloride from occurring acutely to change, avoids reacting
Mixture in kettle reacts in the presence of water, and then ensures that the purity of reactant and yield reach dbjective state.
Preferred scheme, in step S2, the drier is to select magnesium sulfate, and drying capacity is strong, is generated after water suction
MgSO4·7H2O can be separated from oil phase rapidly so that industrial production efficiency effectively improves.
The beneficial effects of the invention are as follows：
1, in the anti-oxidant LED packaging plastics of high transparency of the invention, phenyl accounting about 50%, methyl accounting about 30%, ethylene
Fiduciary point ratio about 20%, phenyl, methyl and vinyl collocation are reasonable, and are free of other heteroions and functional group in being formulated so that high
Transparent anti-oxidant LED packaging plastics have good heat resistance, ageing resistance, anti-time property and cold-resistant thermal shock resistance properties, are especially suitable for
LED bulb uses.
2, on the one hand the vinyltrimethoxysilane that the present invention selects is used as deicer that can prevent from generating gas in product
Bubble ensures that product smearing is uniformly not stratified, and to improve coating and bond effect, on the other hand, included vinyl carries
High accounting of the vinyl in high transparency organosilicon material, can adjust high transparency organosilicon material medium vinyl, phenyl on demand
With the proportioning of methyl, to obtain the product of different performance, the heat resistance of high transparency organosilicon material and anti-time property are preferable, another
Aspect can prevent product from generating bubble, improve coating, bond effect.
3, in the poly bis phenyl methyl silazane mixture of methyl blocking that the method for the invention by organic synthesis obtains, benzene
Base is separately attached on silicon atom, and methyl is separately attached on a nitrogen-atoms, and forms repetitive unit, each to repeat to tie
The electron cloud of structure unit is all relatively independent, the σ keys between constitutional repeating unit and will not be superimposed between pi bond, is not interfered with
The refractive index of the poly bis phenyl methyl silazane of methyl blocking, the stable refractive index of product are reliable so that high temperature resistant LED high transparencies
Refractive index and translucency reach requirement.
4, in polysilazane molecule, with the increase of phenyl content, refractive index can improve；Phenyl and methyl can carry
The heat resistance of high polysilazane entirety, in terms of quantity ratio, benzene in the poly bis phenyl methyl silazane of methyl blocking produced by the present invention
Fiduciary point ratio is up to 65%, and methyl accounting is up to 30% so that product has good heat resistance；And the poly bis phenyl methyl of methyl blocking
Other heteroions and functional group are free of in silazane, and there is good inoxidizability.
Specific implementation mode
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
All other embodiment that technical staff is obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1
A kind of anti-oxidant LED packaging plastics of high transparency, by weight, including following component：Methyl vinyl silicone rubber 100
Part, 40 parts of the poly bis phenyl methyl silazane of methyl blocking, 10 parts of vinyltrimethoxysilane, three tert-butyl peroxide of vinyl
8 parts of silane, platinum content are 0.2 part of the aqueous isopropanol of the chloroplatinic acid of 5000ppm.
The poly bis phenyl methyl silazane of methyl blocking is prepared by following steps：
1 part of hexichol dichlorosilane is added into reaction kettle in terms of mass parts in S1, in 6 parts of addition reaction kettles of toluene, stirring
And ammonia is passed through to not absorbed, after being alkalinity with pH test paper test reaction liquid, keep being passed through ammonia state under the conditions of 18 DEG C
Stop reaction after 1h；
S2 is added in 13 DEG C of ammonium hydroxide and stirring to solution and is visible by naked eyes solid, isolated oil phase is dehydrated, into oil phase
It is added after magnesium sulfate is carried out dehydrating, is distilled under the conditions of 330 DEG C of temperature, condenser pipe is used in combination to intercept 240~300 DEG C of fractions；
S3, in terms of mass parts, into reaction kettle be added step S2 obtain 1 part of substance, be dried after 5 parts of toluene,
0.05 part of hexamethyldisilazane lithium salts, and the ruthenium trichloride of 30ppm is added, react 3h in 180 DEG C of dry nitrogen atmospheres；
4 parts of 5 parts of 1 part of substance, methanol, the concentrated sulfuric acid that step S3 is obtained are added into reaction kettle in terms of mass parts by S4,
The poly bis phenyl methyl silicon nitrogen of methyl blocking for meeting general structure (1) and general structure (2) is obtained by the reaction in 0.5h under the conditions of 120 DEG C
Alkane mixture,
General structure (1)：
General structure (2)：
In general structure (1), in terms of mass parts, the poly bis phenyl methyl silazane accounting of methyl blocking of 180≤n≤200
93%.
In general structure (2), in terms of mass parts, the poly bis phenyl methyl silazane accounting of methyl blocking of 170≤n≤190
90%.
In terms of mass parts, the substance accounting of general structure (1) is met in the poly bis phenyl methyl silazane of methyl blocking
34%, meet the substance accounting 66% of general structure (2).
By the anti-oxidant LED packaging plastics of the high transparency it is mixing cured after under the conditions of 60 DEG C 30d is stored in atmospheric environment
Afterwards, light transmittance is tested, light transmittance is 92.9% at a length of 450nm of 10mm light path cuvette medium waves.
Embodiment 2
A kind of anti-oxidant LED packaging plastics of high transparency, by weight, including following component：Methyl vinyl silicone rubber 100
Part, 80 parts of the poly bis phenyl methyl silazane of methyl blocking, 20 parts of vinyltrimethoxysilane, 3- aminopropyl triethoxysilicanes
4 parts of alkane, platinum content are 0.3 part of the aqueous isopropanol of the chloroplatinic acid of 1000ppm.
The poly bis phenyl methyl silazane of methyl blocking is prepared by following steps：
1 part of hexichol dichlorosilane is added into reaction kettle in terms of mass parts in S1, in 4 parts of addition reaction kettles of toluene, stirring
And ammonia is passed through to not absorbed, after being alkalinity with pH test paper test reaction liquid, keep being passed through ammonia state under the conditions of 16 DEG C
Stop reaction after 5h；
S2 is added in 18 DEG C of ammonium hydroxide and stirring to solution and is visible by naked eyes solid, isolated oil phase is dehydrated, into oil phase
It is added after magnesium sulfate is carried out dehydrating, is distilled under the conditions of 340 DEG C of temperature, condenser pipe is used in combination to intercept 240~300 DEG C of fractions；
S3, in terms of mass parts, into reaction kettle be added step S2 obtain 1 part of substance, be dried after 5 parts of toluene,
0.2 part of hexamethyldisilazane lithium salts, and the ruthenium trichloride of 10ppm is added, react 2h in 200 DEG C of dry nitrogen atmospheres；
6 parts of 10 parts of 1 part of substance, methanol, the concentrated sulfuric acid that step S3 is obtained are added into reaction kettle in terms of mass parts by S4,
The poly bis phenyl methyl silazane of methyl blocking for meeting general structure (1) and general structure (2) is obtained by the reaction in 1h under the conditions of 115 DEG C
Mixture,
General structure (1)：
General structure (2)：
In general structure (1), in terms of mass parts, the poly bis phenyl methyl silazane accounting of methyl blocking of 50≤n≤70
62%.
In general structure (2), in terms of mass parts, the poly bis phenyl methyl silazane accounting of methyl blocking of 50≤n≤70
65%.
In terms of mass parts, the substance accounting of general structure (1) is met in the poly bis phenyl methyl silazane of methyl blocking
48%, meet the substance accounting 52% of general structure (2).
By the anti-oxidant LED packaging plastics of the high transparency it is mixing cured after under the conditions of 60 DEG C 30d is stored in atmospheric environment
Afterwards, light transmittance is tested, light transmittance is 94.8% at a length of 450nm of 10mm light path cuvette medium waves.
Embodiment 3
A kind of anti-oxidant LED packaging plastics of high transparency, by weight, including following component：Methyl vinyl silicone rubber 100
Part, 60 parts of the poly bis phenyl methyl silazane of methyl blocking, 40 parts of vinyltrimethoxysilane, γ-glycidyl ether oxygen propyl
6 parts of trimethoxy silane, platinum content are 0.1 part of the aqueous isopropanol of the chloroplatinic acid of 10000ppm.
The poly bis phenyl methyl silazane of methyl blocking is prepared by following steps：
1 part of hexichol dichlorosilane is added into reaction kettle in terms of mass parts in S1, in 4 parts of addition reaction kettles of toluene, stirring
And ammonia is passed through to not absorbed, after being alkalinity with pH test paper test reaction liquid, keep being passed through ammonia state under the conditions of 17 DEG C
Stop reaction after 3h；
S2 is added in 19 DEG C of ammonium hydroxide and stirring to solution and is visible by naked eyes solid, isolated oil phase is dehydrated, into oil phase
It is added after magnesium sulfate is carried out dehydrating, is distilled under the conditions of 335 DEG C of temperature, condenser pipe is used in combination to intercept 240~300 DEG C of fractions；
S3, in terms of mass parts, into reaction kettle be added step S2 obtain 1 part of substance, be dried after 3 parts of toluene,
0.1 part of hexamethyldisilazane lithium salts, and the ruthenium trichloride of 20ppm is added, react 2.5h in 190 DEG C of dry nitrogen atmospheres；
5 parts of 7 parts of 1 part of substance, methanol, the concentrated sulfuric acid that step S3 is obtained are added into reaction kettle in terms of mass parts by S4,
The poly bis phenyl methyl silicon nitrogen of methyl blocking for meeting general structure (1) and general structure (2) is obtained by the reaction in 0.8h under the conditions of 118 DEG C
Alkane mixture,
General structure (1)：
General structure (2)：
In general structure (1), in terms of mass parts, the poly bis phenyl methyl silazane accounting of methyl blocking of 110≤n≤130
76%.
In general structure (2), in terms of mass parts, the poly bis phenyl methyl silazane accounting of methyl blocking of 90≤n≤110
81%.
In terms of mass parts, the substance accounting of general structure (1) is met in the poly bis phenyl methyl silazane of methyl blocking
41%, meet the substance accounting 59% of general structure (2).
By the anti-oxidant LED packaging plastics of the high transparency it is mixing cured after under the conditions of 60 DEG C 30d is stored in atmospheric environment
Afterwards, light transmittance is tested, light transmittance is 92.4% at a length of 450nm of 10mm light path cuvette medium waves.
Example the above is only the implementation of the present invention is not intended to limit the scope of the invention, every to utilize this hair
Equivalent structure or equivalent flow shift made by bright description is applied directly or indirectly in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (7)
1. a kind of anti-oxidant LED packaging plastics of high transparency, which is characterized in that by weight, including following component：Methyl ethylene
100 parts of silicon rubber, 40~80 parts of the poly bis phenyl methyl silazane of methyl blocking, 10~40 parts of deicer, silane coupling agent 4~8
Part, 0.1~0.3 part of platinum group catalyst.
2. the anti-oxidant LED packaging plastics of high transparency according to claim 1, which is characterized in that the deicer is vinyl
Trimethoxy silane.
3. the anti-oxidant LED packaging plastics of high transparency according to claim 1, which is characterized in that the silane coupling agent is second
Three tert-butyl peroxide silane of alkenyl, 3-aminopropyltriethoxysilane or γ-glycidyl ether oxygen propyl trimethoxy silicon
Alkane.
4. the anti-oxidant LED packaging plastics of high transparency according to claim 1, which is characterized in that the platinum group catalyst is chlorine
The aqueous isopropanol of platinic acid, platinum content are 1000~10000ppm.
5. the anti-oxidant LED packaging plastics of high transparency according to claim 1, which is characterized in that the poly bis benzene of methyl blocking
Ylmethyl silazane is prepared by following steps：
1 part of hexichol dichlorosilane is added into reaction kettle in terms of mass parts in S1, and in 4~6 parts of addition reaction kettles of toluene, stirring is simultaneously
Ammonia is passed through to not absorbed, after being alkalinity with pH test paper test reaction liquid, keeps being passed through ammonia shape under the conditions of 16~18 DEG C
Stop reaction after 1~5h of state；
S2 is added in ammonium hydroxide and stirring to solution and is visible by naked eyes solid, is dehydrated isolated oil phase, drying is added into oil phase
It after agent is carried out dehydrating, is distilled under the conditions of 330~340 DEG C of temperature, condenser pipe is used in combination to intercept 240~300 DEG C of fractions；
S3, in terms of mass parts, into reaction kettle be added step S2 obtain 1 part of substance, be dried after 3~5 parts of toluene, six
0.05~0.2 part of methyl disilazane lithium salts, and the ruthenium trichloride of 10~30ppm is added, in 180~200 DEG C of drying nitrogen gas
2~3h is reacted in atmosphere；
4~6 parts of 5~10 parts of 1 part of substance, methanol, the concentrated sulfuric acid that step S3 is obtained are added into reaction kettle in terms of mass parts by S4,
The poly bis benzene of methyl blocking for meeting general structure (1) and general structure (2) is obtained by the reaction in 0.5~1h under the conditions of 115~120 DEG C
Ylmethyl silazane mixture,
General structure (1)：
General structure (2)：
In general structure (1) and (2), pH represents phenyl, and n is integer, in terms of mass parts, the substance accounting 60% of 50≤n≤200
More than, the substance accounting 30~50% of general structure (1) is met in the poly bis phenyl methyl silazane of methyl blocking, meets knot
The substance accounting 50~70% of structure general formula (2).
6. the anti-oxidant LED packaging plastics of high transparency according to claim 4, which is characterized in that in step S2, the ammonium hydroxide temperature
Degree is 18~20 DEG C.
7. the anti-oxidant LED packaging plastics of high transparency according to claim 4, which is characterized in that in step S2, the drier
To select magnesium sulfate.
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| CN116515455A (en) * | 2023-06-29 | 2023-08-01 | 中山高峻照明电器有限公司 | Ultraviolet LED lamp bead bonded by silazane and preparation method thereof |
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| CN104232015B (en) * | 2014-09-16 | 2016-08-24 | 上海应用技术学院 | The list packaging organic silicon rubber packaging plastic of a kind of high-power type white light LEDs and preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116515455A (en) * | 2023-06-29 | 2023-08-01 | 中山高峻照明电器有限公司 | Ultraviolet LED lamp bead bonded by silazane and preparation method thereof |
| CN116515455B (en) * | 2023-06-29 | 2023-11-21 | 中山高峻照明电器有限公司 | Ultraviolet LED lamp bead bonded by silazane and preparation method thereof |
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