CN106085344A - Ultraviolet leds lamp bead encapsulation glue and preparation method thereof - Google Patents
Ultraviolet leds lamp bead encapsulation glue and preparation method thereof Download PDFInfo
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- CN106085344A CN106085344A CN201610550566.0A CN201610550566A CN106085344A CN 106085344 A CN106085344 A CN 106085344A CN 201610550566 A CN201610550566 A CN 201610550566A CN 106085344 A CN106085344 A CN 106085344A
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- China
- Prior art keywords
- parts
- lamp bead
- encapsulation glue
- ultraviolet leds
- leds lamp
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- 239000003292 glue Substances 0.000 title claims abstract description 57
- 239000011324 bead Substances 0.000 title claims abstract description 56
- 238000005538 encapsulation Methods 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 62
- -1 methyl hydrogen Chemical compound 0.000 claims abstract description 52
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 25
- 239000001257 hydrogen Substances 0.000 claims abstract description 22
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 22
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 21
- 239000003054 catalyst Substances 0.000 claims abstract description 20
- 239000003112 inhibitor Substances 0.000 claims abstract description 18
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical group C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims abstract description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 36
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 5
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 239000004593 Epoxy Substances 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 230000000903 blocking effect Effects 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 3
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Natural products OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 238000010025 steaming Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- 238000002454 metastable transfer emission spectrometry Methods 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims 1
- 238000002834 transmittance Methods 0.000 abstract description 16
- 230000032683 aging Effects 0.000 abstract description 11
- 230000008901 benefit Effects 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- 230000004048 modification Effects 0.000 description 9
- 238000012986 modification Methods 0.000 description 9
- 239000000203 mixture Substances 0.000 description 8
- 125000002769 thiazolinyl group Chemical group 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 230000007423 decrease Effects 0.000 description 3
- 239000002562 thickening agent Substances 0.000 description 3
- 230000007812 deficiency Effects 0.000 description 2
- LLVWLCAZSOLOTF-UHFFFAOYSA-N 1-methyl-4-[1,4,4-tris(4-methylphenyl)buta-1,3-dienyl]benzene Chemical compound C1=CC(C)=CC=C1C(C=1C=CC(C)=CC=1)=CC=C(C=1C=CC(C)=CC=1)C1=CC=C(C)C=C1 LLVWLCAZSOLOTF-UHFFFAOYSA-N 0.000 description 1
- 241000208340 Araliaceae Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-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
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- 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
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a kind of ultraviolet leds lamp bead encapsulation glue and preparation method thereof, it includes following component: end-vinyl organopolysiloxane, liquid ethylene base MQ silicones, linear methyl hydrogen polysiloxanes, platinum complex catalyst, inhibitor and viscosifier.The formula of the ultraviolet leds lamp bead encapsulation glue that the present invention provides is reasonable, and the siliconoxygen bond bond energy of silicone backbone is the highest, and the UV light being amenable to high energy irradiates and do not ruptures, and bond effect is good；The advantages such as and organosilicon can keep higher light transmittance in the widest wave-length coverage, having high-low temperature resistant, ageing-resistant, transparency is high, good moldability, caking property is good, and condition of cure is gentle, combination property is good；The preparation method that the present invention provides can quickly make ultraviolet leds lamp bead encapsulation glue goods, and processing step is succinct, it is easy to accomplish, productivity ratio is high.
Description
Technical field
The present invention relates to LED lamp bead encapsulation glue technical field, be specifically related to a kind of ultraviolet leds lamp bead encapsulation glue and
Its preparation method.
Background technology
Ultraviolet source (UV) has fluorescent effect, biological effect, Photochemical effects and photoelectric effect, in industry, agricultural, state
The fields such as anti-and medical treatment are used widely.And the tradition UV light fixture heavy metal such as have service life short, mercurous not environmentally, response
The shortcoming of time length, it is long that LED UV light source has service life, and response time is fast, and heat is low, the advantage of energy-conserving and environment-protective.Along with state
The requirement of family's 12 energy-conserving and environment-protective and the progress of science and technology, LED UV chip is the most full-fledged, and therefore exploitation one is used
Extremely urgent in the glue of LED UV light-source encapsulation.
Summary of the invention
For above-mentioned deficiency, an object of the present invention is, it is provided that a kind of formula is reasonable, and adhesive property is good, is amenable to
The UV light of high energy irradiates and does not ruptures, and the ultraviolet leds lamp bead encapsulation glue that light transmittance is good.
The two of the purpose of the present invention are, for above-mentioned deficiency, it is provided that a kind of energy quick Fabrication go out above-mentioned ultraviolet leds lamp
The preparation method of bead seal dress glue.
For achieving the above object, technical scheme provided by the present invention is: a kind of ultraviolet leds lamp bead encapsulation glue, presses
Following component is included according to parts by weight:
End-vinyl organopolysiloxane 10 ~ 50 parts,
Liquid ethylene base MQ silicones 50 ~ 80 parts,
Linear methyl hydrogen polysiloxanes 2 ~ 30 parts,
Platinum complex catalyst 0.1 ~ 1 part,
Inhibitor 0.03 ~ 0.3 part,
Viscosifier 1 ~ 5 part.
As a modification of the present invention, described end-vinyl organopolysiloxane is two ends ethenyl blocking in molecule
Straight chain organopolysiloxane, viscosity is 1000 ~ 50000mpa.s/25 DEG C.
As a modification of the present invention, described linear methyl hydrogen polysiloxanes is former containing the hydrogen of more than 2 in molecule
The straight-chain methyl hydrogen polysiloxanes of son.
As a modification of the present invention, described platinum complex catalyst is Karst platinum catalyst.
As a modification of the present invention, described inhibitor is the one or many in alkynol class or many vinylsiloxanes
Kind.
As a modification of the present invention, described viscosifier be γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane,
γ-methacryloxypropyl trimethoxy silane, γ-methacryloxypropyl trimethoxy silane, 1,3-diene
One or more in propyl group list shrink isocyanuric acid ester.
A kind of preparation method of above-mentioned ultraviolet leds lamp bead encapsulation glue, it comprises the following steps:
(1) raw material of following ratio of weight and number is weighed: 10 ~ 50 parts of end-vinyl organopolysiloxanes, 50 ~ 80 parts of liquid ethylene bases
MQ silicones, 2 ~ 30 parts of linear methyl hydrogen polysiloxanes, 0.1 ~ 1 part of platinum complex catalyst, 0.03 ~ 0.3 part of inhibitor, 1 ~ 5
Part viscosifier；
(2) by end-vinyl organopolysiloxane, liquid ethylene base MQ silicones, linear methyl hydrogen polysiloxanes, platinum complex
Catalyst, inhibitor and viscosifier add in power mixer, are 15 ~ 35HZ at revolution speed, and rotational velocity is 15 ~ 35HZ's
Under the conditions of disperse stirring 15 ~ 60 minutes, then evacuation is after 15 ~ 30 minutes, prepares ultraviolet leds lamp bead encapsulation glue.
As a modification of the present invention, described liquid ethylene base MQ silicones uses following methods to prepare: first by 50 ~
The dehydrated alcohol of 100 parts, the pure water of the concentrated hydrochloric acid of 10 ~ 20 parts and 50 ~ 100 parts is put in four-hole boiling flask, then drip 50 ~
The mixed liquor that 100 parts of methyl closure agents and 30 ~ 80 parts of vinyl closure agents mix mutually, reacts 0.5 ~ 1.5 hour at 30 ~ 80 DEG C；
Then the dropping tetraethyl orthosilicate of 100 ~ 200 parts or the dimethyldiethoxysilane of 50 ~ 150 parts or the poly-methyl of 50 ~ 150 parts
Triethoxysilane, temperature during dropping controls between 30 ~ 80 DEG C, reacts at such a temperature 3 ~ 6 hours, reacted after dripping off
The toluene extraction of rear addition 100 ~ 200 parts, then stands separatory, then cleans toluene layer with the pure water of 100 ~ 200 parts, be washed till PH
Value is in neutrality, and the end-vinyl organopolysiloxane then adding 50 ~ 150 parts is miscible, after mixing between 120 ~ 170 DEG C often
Pressure steams toluene, and reduce pressure after substantially steaming toluene distillation 1 ~ 2 hour again, is cooled to room temperature, i.e. prepares described liquid after having steamed
State Vinyl MQ silicon resin.
As a modification of the present invention, ultraviolet leds lamp bead encapsulation glue is injected mould, toast 30 at 80 ~ 100 DEG C
~ 90 minutes, then toast 2 ~ 5 hours at 150 ~ 170 DEG C, obtain test specimens.
As a modification of the present invention, described mould uses polytetrafluoroethylmaterial material to make.
The invention have the benefit that the formula of the ultraviolet leds lamp bead encapsulation glue that the present invention provides is reasonable, organosilicon
The siliconoxygen bond bond energy of main chain is the highest, and the UV light being amenable to high energy irradiates and do not ruptures, and bond effect is good；And organosilicon is the widest
Wave-length coverage in can keep higher light transmittance, there is high-low temperature resistant, ageing-resistant, transparency is high, good moldability, caking property
Good, the advantages such as condition of cure is gentle, combination property is good；The preparation method that the present invention provides can quickly make ultraviolet leds lamp bead
Glue goods are used in encapsulation, and processing step is succinct, it is easy to accomplish, productivity ratio is high.
Below in conjunction with the accompanying drawings with embodiment, the present invention is further described.
Accompanying drawing explanation
Fig. 1 is ultraviolet leds lamp bead encapsulation glue of the present invention light transmittance at different wavelengths.
Fig. 2 is ultraviolet leds lamp bead encapsulation glue of the present invention light transmittance variation diagram at different wavelengths.
Fig. 3 is traditional LED lamp bead seal dress glue light transmittance at different wavelengths.
Fig. 4 is traditional LED lamp bead seal dress glue light transmittance variation diagram at different wavelengths.
Fig. 5 is ultraviolet leds lamp bead encapsulation glue of the present invention to decline aging data in the 365nm time.
Fig. 6 is ultraviolet leds lamp bead encapsulation glue of the present invention to decline aging data in the 310nm time.
Fig. 7 is ultraviolet leds lamp bead encapsulation glue mechanical property aging data when 365nm of the present invention.
Fig. 8 is ultraviolet leds lamp bead encapsulation glue mechanics aging data when 310nm of the present invention.
Detailed description of the invention
Embodiment 1, a kind of ultraviolet leds lamp bead encapsulation glue that the present embodiment provides, include as follows according to parts by weight
Component: end-vinyl organopolysiloxane 10 parts, liquid ethylene base MQ silicones 60 parts, linear methyl hydrogen polysiloxanes 10 parts,
Platinum complex catalyst 0.5 part, inhibitor 0.2 part, viscosifier 2 parts.
It is also preferred that the left described end-vinyl organopolysiloxane to be preferably the straight chain of two ends ethenyl blocking in molecule organic
Polysiloxanes, viscosity is 1000 ~ 50000mpa.s/25 DEG C.Described linear methyl hydrogen polysiloxanes is preferably in molecule containing 2
The straight-chain methyl hydrogen polysiloxanes of above hydrogen atom.Described platinum complex catalyst is preferably Karst platinum catalyst.Institute
State one or more that inhibitor is preferably in alkynol class or many vinylsiloxanes.Described viscosifier are preferably γ-(2,3-
Epoxy the third oxygen) propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, γ-methacryloxypropyl
One or more in base propyl trimethoxy silicane, 1,3-diallyl list shrink isocyanuric acid ester.
A kind of preparation method of above-mentioned ultraviolet leds lamp bead encapsulation glue, it comprises the following steps:
(1) raw material of following ratio of weight and number is weighed: 10 parts of end-vinyl organopolysiloxanes, 60 parts of liquid ethylene base MQ silicon trees
Fat, 10 parts of linear methyl hydrogen polysiloxanes, 0.5 part of platinum complex catalyst, 0.2 part of inhibitor, 2 parts of viscosifier；Concrete, institute
State liquid ethylene base MQ silicones use following methods prepare: first by the dehydrated alcohol of 50 ~ 100 parts, the concentrated hydrochloric acid of 10 ~ 20 parts and
The pure water of 50 ~ 100 parts is put in four-hole boiling flask, then drips 50 ~ 100 parts of methyl closure agents and 30 ~ 80 parts of vinyl end sockets
The mixed liquor that agent mixes mutually, reacts 0.5 ~ 1.5 hour at 30 ~ 80 DEG C；Then the dropping tetraethyl orthosilicate of 100 ~ 200 parts or 50 ~
The dimethyldiethoxysilane of 150 parts or the poly-MTES of 50 ~ 150 parts, temperature during dropping controls 30 ~
Between 80 DEG C, react at such a temperature after dripping off 3 ~ 6 hours, add the toluene extraction of 100 ~ 200 parts after having reacted, then stand
Separatory, then cleans toluene layer with the pure water of 100 ~ 200 parts, and being washed till pH value is neutrality, then adds the end second of 50 ~ 150 parts
Thiazolinyl organopolysiloxane is miscible, and after mixing, between 120 ~ 170 DEG C, normal pressure steams toluene, distillation of reducing pressure again after substantially steaming
Toluene 1 ~ 2 hour, is cooled to room temperature, i.e. prepares described liquid ethylene base MQ silicones after having steamed.
(2) by end-vinyl organopolysiloxane, liquid ethylene base MQ silicones, linear methyl hydrogen polysiloxanes, platinum network
Mixture catalyst, inhibitor and viscosifier add in power mixer, are 15 ~ 35HZ at revolution speed, and rotational velocity is 15 ~
Disperseing stirring 15 ~ 60 minutes under conditions of 35HZ, then evacuation is after 15 ~ 30 minutes, prepares the encapsulation of ultraviolet leds lamp bead and uses
Glue.
(3) ultraviolet leds lamp bead encapsulation glue is injected mould, toasts 30 ~ 90 minutes at 80 ~ 100 DEG C, then 150 ~
170 DEG C are toasted 2 ~ 5 hours, obtain test specimens.It is also preferred that the left described mould uses polytetrafluoroethylmaterial material to make.
Embodiment 2, a kind of ultraviolet leds lamp bead encapsulation glue that the present embodiment provides and preparation method thereof, itself and enforcement
Example 1 is essentially identical, and distinctive points is, its composition weight number is than difference: end-vinyl organopolysiloxane 30 parts, liquid second
Thiazolinyl MQ silicones 80 parts, linear methyl hydrogen polysiloxanes 18 parts, platinum complex catalyst 0.1 part, inhibitor 0.3 part, thickening
Agent 5 parts.
Embodiment 3, a kind of ultraviolet leds lamp bead encapsulation glue that the present embodiment provides and preparation method thereof, itself and enforcement
Example 1 is essentially identical, and distinctive points is, its composition weight number is than difference: end-vinyl organopolysiloxane 50 parts, liquid second
Thiazolinyl MQ silicones 50 parts, linear methyl hydrogen polysiloxanes 2 parts, platinum complex catalyst 1 part, inhibitor 0.03 part, viscosifier 1
Part.
Embodiment 4, a kind of ultraviolet leds lamp bead encapsulation glue that the present embodiment provides and preparation method thereof, itself and enforcement
Example 1 is essentially identical, and distinctive points is, its composition weight number is than difference: end-vinyl organopolysiloxane 40 parts, liquid second
Thiazolinyl MQ silicones 55 parts, linear methyl hydrogen polysiloxanes 30 parts, platinum complex catalyst 0.8 part, inhibitor 0.25 part, thickening
Agent 3 parts.
Embodiment 5, a kind of ultraviolet leds lamp bead encapsulation glue that the present embodiment provides and preparation method thereof, itself and enforcement
Example 1 is essentially identical, and distinctive points is, its composition weight number is than difference: end-vinyl organopolysiloxane 25 parts, liquid second
Thiazolinyl MQ silicones 75 parts, linear methyl hydrogen polysiloxanes 16 parts, platinum complex catalyst 0.6 part, inhibitor 0.18 part, thickening
Agent 3.5 parts.
Embodiment 6, a kind of ultraviolet leds lamp bead encapsulation glue that the present embodiment provides and preparation method thereof, itself and embodiment 1 base
This is identical, and distinctive points is, its composition weight number is than difference: end-vinyl organopolysiloxane 38 parts, liquid ethylene base
MQ silicones 68 parts, linear methyl hydrogen polysiloxanes 23 parts, platinum complex catalyst 0.7 part, inhibitor 0.22 part, viscosifier
4.5 part.
Above-described embodiment is only the preferable embodiment of the present invention, and the present invention can not enumerate out whole embodiment party
Formula, the technical scheme of one of all employing above-described embodiments, or the equivalent variations done according to above-described embodiment, all protect in the present invention
In the range of protecting.
See the form in Fig. 1, for ultraviolet leds lamp bead encapsulation glue of the present invention light transmittance at different wavelengths.Ginseng
See Fig. 2, for ultraviolet leds lamp bead encapsulation glue of the present invention light transmittance variation diagram at different wavelengths.
See the form in Fig. 3, for traditional LED lamp bead seal dress glue light transmittance at different wavelengths.See Fig. 4, for
Traditional LED lamp bead seal dress glue light transmittance variation diagram at different wavelengths.
By Fig. 1 and Fig. 3 it can be seen that ultraviolet leds lamp bead encapsulation glue of the present invention is 280～400nm, all have relatively
High light transmittance, during 280nm, light transmittance is up to 82%, and 300nm is up to 92.9%, during 360nm 94.2%, and traditional LED lamp bead seal dress
Being 63.3% with the glue light transmittance when 280nm, the light transmittance when 300nm is 82.5%, and the light transmittance when 360nm is
89.4%。
See Fig. 5, decline aging data in the 365nm time for ultraviolet leds lamp bead encapsulation glue of the present invention.See Fig. 6, this
Invention ultraviolet leds lamp bead encapsulation glue declined aging data in the 310nm time.By Fig. 5 and Fig. 6, it can be seen that ultraviolet of the present invention
Light LED lamp bead encapsulation glue light decay when 365nm and 310nm is 0.65% and 3.69% respectively, all can reach LED UV light source
Encapsulation requirement.
See Fig. 7, for ultraviolet leds lamp bead encapsulation glue mechanical property aging data when 365nm of the present invention.See figure
8, for ultraviolet leds lamp bead encapsulation glue mechanics aging data when 310nm of the present invention.
Shown by above-mentioned data, the present invention provide ultraviolet leds lamp bead encapsulation glue have high-low temperature resistant, ageing-resistant,
The advantages such as transparency is high, good moldability, and caking property is good, and condition of cure is gentle, combination property is good, it is adaptable to the envelope of LED UV light source
Dress.
The announcement of book and teaching according to the above description, those skilled in the art in the invention can also be to above-mentioned embodiment party
Formula changes and revises.Therefore, the invention is not limited in detailed description of the invention disclosed and described above, to the present invention's
Some modifications and changes should also be as falling in the scope of the claims of the present invention.Although additionally, this specification using
Some specific terms, but these terms are merely for convenience of description, the present invention does not constitute any restriction.Such as the present invention
Described in above-described embodiment, use same or similarity method and component and other compositions of obtaining and preparation method thereof all exists
In scope.
Claims (10)
1. a ultraviolet leds lamp bead encapsulation glue, it is characterised in that include following component according to parts by weight:
End-vinyl organopolysiloxane 10 ~ 50 parts,
Liquid ethylene base MQ silicones 50 ~ 80 parts,
Linear methyl hydrogen polysiloxanes 2 ~ 30 parts,
Platinum complex catalyst 0.1 ~ 1 part,
Inhibitor 0.03 ~ 0.3 part,
Viscosifier 1 ~ 5 part.
Ultraviolet leds lamp bead encapsulation glue the most according to claim 1, it is characterised in that: described end-vinyl is organic poly-
Siloxanes is the straight chain organopolysiloxane of two ends ethenyl blocking in molecule, and viscosity is 1000 ~ 50000mpa.s/25 DEG C.
Ultraviolet leds lamp bead encapsulation glue the most according to claim 1 and 2, it is characterised in that: described linear methyl hydrogen gathers
Siloxanes is the straight-chain methyl hydrogen polysiloxanes of the hydrogen atom containing more than 2 in molecule.
Ultraviolet leds lamp bead encapsulation glue the most according to claim 1 and 2, it is characterised in that: described platinum complex is catalyzed
Agent is Karst platinum catalyst.
Ultraviolet leds lamp bead encapsulation glue the most according to claim 4, it is characterised in that: described inhibitor is alkynol class
Or one or more in many vinylsiloxanes.
Ultraviolet leds lamp bead encapsulation glue the most according to claim 4, it is characterised in that: described viscosifier be γ-(2,
3-epoxy the third oxygen) propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, γ-methacryl
One or more in epoxide propyl trimethoxy silicane, 1,3-diallyl list shrink isocyanuric acid ester.
7. the preparation method of a ultraviolet leds lamp bead encapsulation glue, it is characterised in that: it comprises the following steps:
(1) raw material of following ratio of weight and number is weighed: 10 ~ 50 parts of end-vinyl organopolysiloxanes, 50 ~ 80 parts of liquid ethylene bases
MQ silicones, 2 ~ 30 parts of linear methyl hydrogen polysiloxanes, 0.1 ~ 1 part of platinum complex catalyst, 0.03 ~ 0.3 part of inhibitor, 1 ~ 5
Part viscosifier；
(2) by end-vinyl organopolysiloxane, liquid ethylene base MQ silicones, linear methyl hydrogen polysiloxanes, platinum complex
Catalyst, inhibitor and viscosifier add in power mixer, are 15 ~ 35HZ at revolution speed, and rotational velocity is 15 ~ 35HZ's
Under the conditions of disperse stirring 15 ~ 60 minutes, then evacuation is after 15 ~ 30 minutes, prepares ultraviolet leds lamp bead encapsulation glue.
The preparation method of ultraviolet leds lamp bead encapsulation glue the most according to claim 7, it is characterised in that: described liquid
Vinyl MQ silicon resin uses following methods to prepare: first by the dehydrated alcohol of 50 ~ 100 parts, the concentrated hydrochloric acid of 10 ~ 20 parts and 50 ~ 100
The pure water of part is put in four-hole boiling flask, then drips 50 ~ 100 parts of methyl closure agents and 30 ~ 80 parts of vinyl closure agents mix mutually
The mixed liquor closed, reacts 0.5 ~ 1.5 hour at 30 ~ 80 DEG C；Then the dropping tetraethyl orthosilicate of 100 ~ 200 parts or 50 ~ 150 parts
Dimethyldiethoxysilane or the poly-MTES of 50 ~ 150 parts, temperature during dropping control 30 ~ 80 DEG C it
Between, react at such a temperature after dripping off 3 ~ 6 hours, add the toluene extraction of 100 ~ 200 parts after having reacted, then stand separatory,
Then cleaning toluene layer with the pure water of 100 ~ 200 parts, being washed till pH value is neutrality, and the end-vinyl then adding 50 ~ 150 parts has
Machine polysiloxanes is miscible, and after mixing, between 120 ~ 170 DEG C, normal pressure steams toluene, and the toluene distillation 1 of reducing pressure again after substantially steaming ~
2 hours, it is cooled to room temperature after having steamed, i.e. prepares described liquid ethylene base MQ silicones.
9. according to the preparation method of the ultraviolet leds lamp bead encapsulation glue described in claim 7 or 8, it is characterised in that: by ultraviolet
Light LED lamp bead encapsulation glue injects mould, toasts 30 ~ 90 minutes at 80 ~ 100 DEG C, then toasts 2 ~ 5 hours at 150 ~ 170 DEG C,
Obtain test specimens.
The preparation method of ultraviolet leds lamp bead encapsulation glue the most according to claim 9, it is characterised in that: described mould
Employing polytetrafluoroethylmaterial material is made.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109762167A (en) * | 2018-12-14 | 2019-05-17 | 中国科学院深圳先进技术研究院 | A kind of LED small-size chips heat conductive insulating die bond material and preparation method thereof |
| CN109825244A (en) * | 2018-12-30 | 2019-05-31 | 苏州桐力光电股份有限公司 | One kind can ultraviolet lighting and the double cured clear silicone gels of heating |
| WO2020140855A1 (en) * | 2018-12-30 | 2020-07-09 | 苏州桐力光电股份有限公司 | Printing technology for full lamination method |
| CN112054109A (en) * | 2020-09-11 | 2020-12-08 | 天津中环电子照明科技有限公司 | Ultraviolet LED packaging adhesive with high light extraction efficiency and light aging resistance and packaging structure |
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| CN102181055A (en) * | 2011-01-14 | 2011-09-14 | 仲恺农业工程学院 | Preparation method of reactive MQ silicon resin |
| CN104789186A (en) * | 2015-04-28 | 2015-07-22 | 杭州福斯特光伏材料股份有限公司 | Single-component LED (light-emitting diode) filament thixotrope without oil discharge and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102181055A (en) * | 2011-01-14 | 2011-09-14 | 仲恺农业工程学院 | Preparation method of reactive MQ silicon resin |
| CN104789186A (en) * | 2015-04-28 | 2015-07-22 | 杭州福斯特光伏材料股份有限公司 | Single-component LED (light-emitting diode) filament thixotrope without oil discharge and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109762167A (en) * | 2018-12-14 | 2019-05-17 | 中国科学院深圳先进技术研究院 | A kind of LED small-size chips heat conductive insulating die bond material and preparation method thereof |
| CN109825244A (en) * | 2018-12-30 | 2019-05-31 | 苏州桐力光电股份有限公司 | One kind can ultraviolet lighting and the double cured clear silicone gels of heating |
| WO2020140855A1 (en) * | 2018-12-30 | 2020-07-09 | 苏州桐力光电股份有限公司 | Printing technology for full lamination method |
| CN112054109A (en) * | 2020-09-11 | 2020-12-08 | 天津中环电子照明科技有限公司 | Ultraviolet LED packaging adhesive with high light extraction efficiency and light aging resistance and packaging structure |
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