CN109355059A - A kind of the add-on type LED filament packaging silicon rubber and preparation method of high thixotropic - Google Patents
A kind of the add-on type LED filament packaging silicon rubber and preparation method of high thixotropic Download PDFInfo
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- CN109355059A CN109355059A CN201811176900.6A CN201811176900A CN109355059A CN 109355059 A CN109355059 A CN 109355059A CN 201811176900 A CN201811176900 A CN 201811176900A CN 109355059 A CN109355059 A CN 109355059A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- 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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a kind of high thixotropic add-on type LED filament packaging silicon rubber and preparation methods, consist of the following compositions: vinyl polysiloxane, vinyl silicone oil, hydrogeneous crosslinking agent, hydrophobic type gas phase silica, constitution controller, tackifier, platinum catalyst, inhibitor.High thixotropic add-on type LED filament packaging silicon rubber of the present invention has high thixotropic, high transparency, high temperature tolerance.After colloid solidification, there is good mechanical performance, elasticity is good, tear-proof, tensile strength and elongation at break are high.
Description
Technical field
The present invention relates to LED encapsulation fields, in particular to a kind of high thixotropic add-on type LED filament packaging silicon rubber
And preparation method.
Background technique
High thixotropic add-on type LED filament packaging silicon rubber is different from typical LED packages silica gel.Thixotropy silica gel has good
Good thixotropy, only with mechanical force (shaking etc.), being not required to heating can make gel become colloidal sol；It is not required to cool down, need to only stand one
It fixes time, and gel is become from colloidal sol.High thixotropic can be such that particle is steadily scattered in medium and be not easy aggregation sedimentation, also
Colloid can be made to automatically form certain shape, not flow, do not collapse, high-temperature baking is undeformed after dispensing.
High thixotropic add-on type LED filament packaging silicon rubber, is mainly used for the encapsulation of LED filament, is equally applicable to simultaneously:
The encapsulation of MCOB type LED lamp bead, COB lamp bead the multiple uses such as box dam.
LED filament lamps and lanterns have outstanding performance, realize 360 ° of complete cycle luminescent balls bubble, have the similar form of incandescent lamp and
Distribution curve flux is truly instead of the vehement optimal light source of white light.LED filament realizes three-dimensional light source, brings preceding institute not
The advantages of some lighting experiences have both environmental protection and energy saving simultaneously.
LED filament encapsulation is formed immediately after requiring dispensing, and 60-80 DEG C of prebake conditions undeformed, up to completion of cure is kept
Initial dispensing Form Factor.The encapsulation glue for meeting this requirement is presented as high thixotropic (Thixotropy) in materialogy,
It can be flowed as common fluid (when dispensing) when i.e. high shear force applies, and shear and withdraw rear (dispensing completion) immediately as solid
Body equally stops flowing.Material circle generally obtains thixotropy using thixotropic agent (thixotropic filler) is added in common glue
Energy.Thixotropic property (TI value) and high molecular material mobile performance, the additive amount of thixotropic agent, the particle size of thixotropic agent, thixotropic agent
Degree of scatter in glue is related, and homogeneity and consistency are to prepare the difficult point of thixotropic materials control.In addition, LED encapsulation is answered
With require encapsulation glue cannot excessively lose light transmittance because adding thixotropic filler, general light transmittance requirement be maintained at 80% with
On.
The high thixotropic for realizing LED filament packaging silicon rubber glue, need in colloid be added thixotropic agent (thixotropy is filled out
Material).Since LED light silk gum is a kind of optics organosilicon encapsulating material, also need to consider to add material sheet after thixotropic agent
The light transmittance of body.Hydrophobic type gas phase silica can be used as the thixotropic agent of LED filament packaging silicon rubber.But due to normal agitation mistake
The dispersion efficiency of journey is low, and after the thixotropic agent for adding 15% or more mass fraction, colloid transmitance is often reduced to 70% or less.
But additive amount is inadequate, the effect of demand is not achieved in thixotropic property.
In order to realize the high thixotropic of LED filament packaging silicon rubber glue.Constitution controller can be added in formula, can make
The adding proportion of thixotropic agent is reduced to 3% or so by 15%.While realizing high thixotropic, reservation 90% or more it is saturating
Light rate.
Due to being in a relatively closed ball bubble, although some light bulbs can be filled with nitrogen thermally conductive drop when filament work
Temperature, but temperature is still very high when filament work, is influenced by high temperature, packaging silicon rubber has some volatile substances and is precipitated, mist of oil shape
Volatile matter be attached in ball steep that wall, will affect illumination perception, reduce luminous efficiency.
Summary of the invention
The present invention is directed to solve one of above-mentioned technical problem in the related technology at least to a certain extent.For this purpose, this hair
It is bright to propose a kind of high thixotropic add-on type LED filament packaging silicon rubber and preparation method, it is therefore intended that current LED filament is overcome to seal
Fill some FAQs of silica gel: 1. synthesizing end side containing hydrogen silicone oil can more rise as crosslinking agent compared to common crosslinking agent
To the effect of chain extension.The toughness of colloid is greatly improved, is easy to split when packaging silicon rubber can be effectively prevent to work at high temperature
The problem of glue；2. by the hydrophobic type gas phase silica of addition proper ratio as thixotropic agent, and introducing hydroxy-end capped side
Vinyl silicone oil reinforces thixotropic effects as constitution controller and reaches good while retaining LED packaging silicon rubber high transparency
Good thixotropic effects.Also avoid common constitution controller can not access system, volatilization the problem of hazing at high temperature. ③
Correlative is handled using a kind of high vacuum short-path distillation technique, the volatile matter of correlative is reduced, overcomes filament lamp
The problem of hot operation hazes.Another object of the present invention is to provide the high thixotropic add-on type LED filament packaging silicon rubbers
Purposes in electronic package material.
To achieve the above object, technical scheme is as follows: a kind of high thixotropic add-on type LED filament encapsulation silicon
Glue.It is characterized by: including vinyl polysiloxane, hydrogeneous crosslinking agent, vinyl silicone oil, hydrophobic type gas phase silica, structure
Controlling agent, tackifier, platinum catalyst, inhibitor.As of the present invention: a kind of high thixotropic add-on type LED filament encapsulation
The preferred embodiment of silica gel, each component content of the high thixotropic add-on type LED filament packaging silicon rubber are as follows:
Said components high speed dispersion is sufficiently mixed uniformly to get a kind of high thixotropic add-on type LED of the present invention
Filament packaging silicon rubber.
Vinyl polysiloxane and vinyl silicone oil containing vinyl and contain hydrogen-based under the action of platinum catalyst
Hydrogeneous crosslinking agent occur addition reaction and be crosslinked, solidify.
The beneficial effects of the present invention are: the present invention compared with prior art, has the advantage that (1) present invention with MQ
Silicone resin is main base Chu material, and vinyl silicone oil and hydrogeneous crosslinking agent is cooperated to use.Silicon rubber after crosslinking curing has
Good physical property and mechanical performance and good chemical stability.Elasticity is good for colloid, tear-proof, cold-and-heat resistent impact,
Heat-resisting, radiation hardness, resistance to atmospheric aging.(2) hydrogeneous crosslinking agent of the present invention is homemade end side containing hydrogen silicone oil, with market
The side containing hydrogen silicone oil of upper common methyl blocking is different.End side containing hydrogen silicone oil use 1,1,3,3- tetramethyl disiloxane as
End-capping reagent makes the both ends of strand introduce the hydrogen-based that can be reacted with vinyl.During heating cure, end side containing hydrogen silicone oil
In addition to also acting as the effect of chain extension as crosslinking agent, so that colloid has bigger molecular weight, better flexibility after solidifying
With better performance resistant to high temperature.(3) present invention introduces hydroxy-end capped side vinyl silicone oil as structure control in formula
Agent can make the additive amount of hydrophobic type gas phase silica be reduced to 3% or so by 15%, maintain good thixotroping effect
Fruit, product light transmittance reach 90% or more.With the structure controls such as the common hydroxy silicon oil of organosilicon industry, diphenyl silanediol
Agent is compared, the hydroxy-end capped side vinyl silicone oil of addition have can reactive group vinyl, can be in material heating cure
In the process, addition reaction occurs with hydrogeneous crosslinking agent, is linked into system, form the macromolecular that can not be volatilized.So that package material
Expect the case where the later period is in use, volatile substance greatly reduces, and light bulb is avoided to haze.(4) instant-forming after dispensing, preliminary drying
Roasting 60~80 DEG C undeformed, until completion of cure keeps initial dispensing form factor.Thixotropic effects are significant and stable and consistent.
Specific embodiment
The embodiment of the present invention is described below in detail, it is intended to be used to explain the present invention, and should not be understood as to of the invention
Limitation.
The advantages of purpose in order to better illustrate the present invention, technical solution, below by specific embodiment to the present invention
It is described further.
The distillation of material is handled: by the liquid material in need used, comprising: vinyl polysiloxane, hydrogeneous crosslinking
Agent, vinyl silicone oil, constitution controller, tackifier, platinum catalyst, inhibitor are separately added into short distance molecule evaporimeter,
It is heated to 150-200 DEG C, is distilled under the vacuum degree of -90~-99KPa.Various material fugitive constituent≤0.1% after treatment,
Can be used for following embodiment 1-4 matches glue.
Embodiment 1
47 parts of vinyl polysiloxane, 35 parts of vinyl silicone oil, 8 parts of hydrogeneous crosslinking agent, 6 parts of hydrophobic type gas phase silica,
2 parts of constitution controller, 1.5 parts of tackifier, 0.45 part of platinum catalyst, 0.05 part of inhibitor.
Embodiment 2
48 parts of vinyl polysiloxane, 35 parts of vinyl silicone oil, 8 parts of hydrogeneous crosslinking agent, 5 parts of hydrophobic type gas phase silica,
2 parts of constitution controller, 1.5 parts of tackifier, 0.45 part of platinum catalyst, 0.05 part of inhibitor.
Embodiment 3
49 parts of vinyl polysiloxane, 35 parts of vinyl silicone oil, 8 parts of hydrogeneous crosslinking agent, 4 parts of hydrophobic type gas phase silica,
2 parts of constitution controller, 1.5 parts of tackifier, 0.45 part of platinum catalyst, 0.05 part of inhibitor
Embodiment 4
50 parts of vinyl polysiloxane, 35 parts of vinyl silicone oil, 8 parts of hydrogeneous crosslinking agent, 3 parts of hydrophobic type gas phase silica,
2 parts of constitution controller, 1.5 parts of tackifier, 0.45 part of platinum catalyst, 0.05 part of inhibitor
Comparative example 1
45 parts of vinyl polysiloxane, 30 parts of vinyl silicone oil, 8 parts of hydrogeneous crosslinking agent, hydrophobic type gas phase silica 15
Part, 0 part of constitution controller, 1.5 parts of tackifier, 0.45 part of platinum catalyst, 0.05 part of inhibitor
Following table is the comparison of above-described embodiment 1-4 and comparative example various aspects of performance:
Embodiment 1-4 and comparative example 1 reach instant-forming after dispensing, and 60~80 DEG C of prebake conditions undeformed, until solidification
Initial dispensing form factor is kept completely.Thixotropic effects are significant and stable and consistent.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, modifies, replacement and variant.
Claims (10)
1. a kind of add-on type LED filament packaging silicon rubber of high thixotropic, it is characterised in that: include vinyl polysiloxane, hydrogeneous friendship
Join agent, vinyl silicone oil, hydrophobic type gas phase silica, constitution controller, tackifier, platinum catalyst, inhibitor.
2. a kind of add-on type LED filament packaging silicon rubber of high thixotropic according to claim 1, it is characterised in that: described
High thixotropic add-on type LED filament packaging silicon rubber each ingredient content it is as follows:
3. a kind of add-on type LED filament packaging silicon rubber of high thixotropic according to any one of claims 1 or 2, special
Sign is: the viscosity of the vinyl polysiloxane is 5000-100000cps, contents of ethylene 1-5%.
4. a kind of add-on type LED filament packaging silicon rubber of high thixotropic according to any one of claims 1 or 2, special
Sign is: the viscosity of the vinyl silicone oil is 5000-100000cps, contents of ethylene 0.01-2%.
5. a kind of add-on type LED filament packaging silicon rubber of high thixotropic according to any one of claims 1 or 2, special
Sign is: the hydrogeneous crosslinking agent is the end side containing hydrogen silicone oil of hydrogen content 0.5-1.6%, by octamethylcy-clotetrasiloxane, 1,
3,5,7- tetramethyl-ring tetrasiloxanes, 1,1,3,3- tetramethyl disiloxane, under the catalysis of strong acid or strong acid cation resin
Copolymerization obtains.
6. a kind of add-on type LED filament packaging silicon rubber of high thixotropic according to any one of claims 1 or 2, special
Sign is: hydrophobic type gas phase silica gained after active silane is handled by conventional gas phase silica surface.
7. a kind of add-on type LED filament packaging silicon rubber of high thixotropic according to any one of claims 1 or 2, special
Sign is: the constitution controller is hydroxy-end capped side vinyl silicone oil, and wherein hydroxy radical content is 1-6.6%, and vinyl contains
Measure 1-6.5%.
8. a kind of add-on type LED filament packaging silicon rubber of high thixotropic according to any one of claims 1 or 2, special
Sign is: the tackifier are the silane coupling agent monomer that different functional groups and different degrees of functionality may be selected, acid water-soluble
The small molecule silane coupling agent polymer being copolymerized under the catalysis of liquid or strong acid cation resin.
9. a kind of add-on type LED filament packaging silicon rubber of high thixotropic according to any one of claims 1 or 2, special
Sign is: the inhibitor is the ethynylcyclohexanol of purity >=99.5%.
10. a kind of preparation method of the add-on type LED filament packaging silicon rubber of high thixotropic, it is characterised in that: the following steps are included:
1) synthesis of hydrogeneous crosslinking agent: being separately added by a certain percentage in a kettle as octamethylcy-clotetrasiloxane, 1,3,5,
7- tetramethyl-ring tetrasiloxane, 1,1,3,3- tetramethyl disiloxane add the strong acid sun of afore-mentioned materials total amount 0.1%-5%
Ion exchange resin, is warming up to 65 DEG C of -80 DEG C of insulation reactions 5-20 hours under the conditions of anhydrous.Clear oily matter is obtained after filtering
Matter.Oily mater is added in reaction kettle, 180 DEG C is warming up to, removes low molecule under vacuum, it is hydrogeneous to obtain colorless and transparent end side
Silicone oil.
2) a certain proportion of vinyltrimethoxysilane, γ-(methyl-prop respectively the synthesis of tackifier: are added in a kettle
Alkene acyl-oxygen) propyl trimethoxy silicane, 3- glycydoxy methyldiethoxysilane, deionized water, it adds
The strong acid cation resin of afore-mentioned materials total amount 0.1%-5%, is warming up to 65 DEG C of -80 DEG C of insulation reactions 5-20 hours；Reaction knot
Shu Houzai is warming up to 120 DEG C, and moisture and low molecule are removed under vacuum.The transparent tackifier of clear, colorless are obtained after filtering.
3) correlative short-path distillation:
By the liquid material in need used, comprising: vinyl polysiloxane, hydrogeneous crosslinking agent, vinyl silicone oil, structure control
Preparation, tackifier, platinum catalyst, inhibitor are separately added into short distance molecule evaporimeter, are heated to 150-200 DEG C ,-
It is distilled under the vacuum degree of 90--99KPa.Various material fugitive constituent≤0.1% after treatment.
4) preparation of high thixotropic add-on type LED filament packaging silicon rubber:
The high thixotropic add-on type LED filament packaging silicon rubber includes 2 component of A glue and B glue, and the A glue and B glue weight ratio are 4:
1, the A glue and B glue mixing after each component parts by weight content it is as follows:
Wherein:
A glue is formulated as follows:
A) vinyl polysiloxane that will pass through distillation processing is added in component A compounding kettle by inventory, and by component A, remaining passes through whole
The material of stream process is added in compounding kettle by inventory, is heated to 150-200 DEG C, is sufficiently stirred after being uniformly dispersed under vacuum state
Filtering；
B glue is formulated as follows:
B) will by distillation processing vinyl silicone oil by inventory be added B component compounding kettle in, by B component remaining through over commutation
The material of processing is added in compounding kettle by inventory, is heated to 150-200 DEG C, mistake after being uniformly dispersed is sufficiently stirred under vacuum state
Filter；
Before use, A glue and B glue are proportionally uniformly mixed, 3-5H is toasted under the conditions of 150 DEG C can reach optimal use
Energy.
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| CN201811176900.6A CN109355059A (en) | 2018-10-10 | 2018-10-10 | A kind of the add-on type LED filament packaging silicon rubber and preparation method of high thixotropic |
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| CN201811176900.6A CN109355059A (en) | 2018-10-10 | 2018-10-10 | A kind of the add-on type LED filament packaging silicon rubber and preparation method of high thixotropic |
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Cited By (5)
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| CN113234416A (en) * | 2021-05-17 | 2021-08-10 | 湖北三选科技有限公司 | Packaging adhesive for MEMS |
| CN113355046A (en) * | 2021-05-31 | 2021-09-07 | 湖北三选科技有限公司 | Packaging adhesive for electronic packaging, preparation method and packaging structure |
| CN113861930A (en) * | 2021-09-18 | 2021-12-31 | 杭州之江新材料有限公司 | Silicone adhesive for corner nails and preparation method thereof |
| CN115850709A (en) * | 2022-12-23 | 2023-03-28 | 杭州之江有机硅化工有限公司 | High-temperature-resistant auxiliary agent, preparation method and application thereof, and prepared silica gel |
| CN116239992A (en) * | 2023-03-17 | 2023-06-09 | 嘉兴金门量子材料科技有限公司 | Bending-resistant organic silicon OCA optical adhesive and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115850709A (en) * | 2022-12-23 | 2023-03-28 | 杭州之江有机硅化工有限公司 | High-temperature-resistant auxiliary agent, preparation method and application thereof, and prepared silica gel |
| CN116239992A (en) * | 2023-03-17 | 2023-06-09 | 嘉兴金门量子材料科技有限公司 | Bending-resistant organic silicon OCA optical adhesive and preparation method thereof |
| CN116239992B (en) * | 2023-03-17 | 2023-11-03 | 嘉兴金门量子材料科技有限公司 | Bending-resistant organic silicon OCA optical adhesive and preparation method thereof |
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Application publication date: 20190219 |