CN108395699A - A kind of LED encapsulation material and preparation process - Google Patents
A kind of LED encapsulation material and preparation process Download PDFInfo
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- CN108395699A CN108395699A CN201810279566.0A CN201810279566A CN108395699A CN 108395699 A CN108395699 A CN 108395699A CN 201810279566 A CN201810279566 A CN 201810279566A CN 108395699 A CN108395699 A CN 108395699A
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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
- C08L83/00—Compositions of 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; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0812—Aluminium
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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
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses a kind of LED encapsulation material and preparation process, raw material and shared mass percent are used in the LED encapsulation material：35 parts of 20 30 parts of organic siliconresin, 10 30 parts of polyphenylene sulfide, 5 15 parts of polyvinyl chloride, 5 10 parts of methyl hexahydrophthalic anhydride, 5 10 parts of kh560 coupling agents, 5 10 parts of triethylamine, 38 parts of benzotriazole, 5 10 parts of Graphene powder, 13 parts of silica flour, 13 parts of aluminium powder, 13 parts of glass fibre and containing hydrogen silicone oil.The present invention improves the anti-ultraviolet ageing ability of LED encapsulation material, extends service life by adding benzotriazole material using its material characteristic of itself, and present invention process is simple, and equipment requirement is low, and operability is strong, has good society generalization application.
Description
Technical field
The present invention relates to LED production technical fields, more particularly to a kind of LED encapsulation material and preparation process.
Background technology
Light emitting diode（English：Light-Emitting Diode, abbreviation LED）It is that a kind of can convert electrical energy into light
The semiconductor electronic component of energy.This electronic component occurred early in 1962, can only send out the feux rouges of low luminosity, Zhi Houfa in early days
Other monochromatic versions are put on display, the light that can be sent out even to this day has spread visible light, infrared ray and ultraviolet light, and luminosity also improves
To comparable luminosity.And purposes also by being used as indicator light, display board etc. at the beginning；With being constantly progressive for technology, light emitting diode
It has been widely used in display, television set daylighting decoration and illumination.
Currently, limitation of the LED encapsulation material due to its own material property, leads to its heat resistance, electric conductivity, expansion system
The parameters such as number, refractive index and hardness cannot reach the relationship of a balance, can encounter performance in a certain respect mostly when in use
Missing or bad its service life of influence.
Therefore, it invents a kind of LED encapsulation material and preparation process is necessary to solve the above problems.
Invention content
The purpose of the present invention is to provide a kind of LED encapsulation material and preparation processes, to solve to carry in above-mentioned background technology
The problem of going out.
To achieve the above object, the present invention provides the following technical solutions：A kind of LED encapsulation material, the LED encapsulation material
Used raw material and shared mass percent are：20-30 parts of organic siliconresin, 10-30 parts of polyphenylene sulfide, polyvinyl chloride 5-
15 parts, 5-10 parts of methyl hexahydrophthalic anhydride, 5-10 parts of kh560 coupling agents, 5-10 parts of triethylamine, 3-8 parts of benzotriazole, Graphene powder
3-5 parts of 5-10 parts, 1-3 parts of silica flour, 1-3 parts of aluminium powder, 1-3 parts of glass fibre and containing hydrogen silicone oil.
Preferably, the particle diameter of the silica flour and aluminium powder is less than 400nm, and the glass fibre is staple fiber.
Preferably, the containing hydrogen silicone oil is in the environment of room temperature is 25 DEG C, index of refraction 1.400, viscosity 30-40.
Preferably, when in use, the mass ratio with melt is 1 to the benzotriazole:1000,
The present invention also provides a kind of preparation processes of LED encapsulation material, specifically comprise the following steps：
Step 1：5-15 parts of 20-30 parts of organic siliconresin, 10-30 parts of polyphenylene sulfide and polyvinyl chloride is taken to be added in kneading machine
It is kneaded, melting temperature is set as 150-200 DEG C, in mixing process, 5-10 parts of triethylamine is added, continues to be kneaded, the time
It is 20-30 minutes, obtains the first mixture；
Step 2 puts into primary mix in reaction kettle, and 5-10 parts of methyl hexahydrophthalic anhydride, 5-10 parts of kh560 coupling agents is added
With 3-5 parts of containing hydrogen silicone oil, start reaction kettle and be stirred, open simultaneously temp control switch, is 100-150 by temperature setting
DEG C, obtain the second mixture；
Second mixture is positioned over room temperature to carry out cooling and standings under 0-5 DEG C of environment, and on the second mixture surface by step 3
Graphene powder is smeared, it is made uniformly to be layed in the second mixture surface；
Step 4, by the second mixture after standing continue input in reaction kettle, be added 1-3 parts of silica flour, 1-3 parts of aluminium powder and
1-3 parts of glass fibre takes 3-8 parts of benzotriazole, by it with water into mixing, quality 1:1000, then by mixed solution
It is poured into reaction kettle, reactor temperature is set as 200-250 DEG C, the agitating device started in reaction kettle stirs it
It mixes, time 40-60min；
After waiting for the stirring in reaction kettle, the cooling device of reaction kettle is started for step 5, cold to the raw material progress in kettle,
When its temperature being made to be cooled to 20-30 DEG C, the raw material in reaction kettle is taken out, is placed into mold and carries out pressing and forming, obtain finished product.
Preferably, in the step 2, the speed of agitator of reaction kettle is 200 revs/min.
Preferably, in the step 3, the laying depth of graphene is 0.5-1.5mm.
Preferably, in the step 4, the speed of agitator of reaction kettle is 300 revs/min.
The technique effect and advantage of the present invention：The present invention by the mixing of raw material be added silica flour, aluminium powder and
Glass fibre improves heat resistance, heat conductivility and coefficient of thermal expansion that LED seals material so that LED encapsulation material can be with
A relatively good working performance is kept under various severe working environments, by adding containing hydrogen silicone oil when curing stirring,
The refractive index and structural rigidity of LED encapsulation material after moulding are improved, and under the working environment in dust content not
Dust suction improves the aesthetics of LED product, and LED is improved using its material characteristic of itself by adding benzotriazole material
The anti-ultraviolet ageing ability of encapsulating material, extends service life.
Present invention process is simple, and equipment requirement is low, and operability is strong, has good society generalization application.
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
The every 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 LED encapsulation material and preparation process, include the following steps：A kind of LED encapsulation material, the LED encapsulation material institute
The raw material and shared mass percent used be：20 parts of organic siliconresin, 10 parts of polyphenylene sulfide, 5 parts of polyvinyl chloride, methyl six
5 parts of hydrogen phthalic anhydride, 5 parts of kh560 coupling agents, 5 parts of triethylamine, 3 parts of benzotriazole, 5 parts of Graphene powder, 1 part of silica flour, 1 part of aluminium powder,
The particle diameter of 3 parts of 1 part of glass fibre and containing hydrogen silicone oil, the silica flour and aluminium powder is less than 400nm, and the glass fibre is short
Fiber, the containing hydrogen silicone oil is in the environment of room temperature is 25 DEG C, index of refraction 1.400, viscosity 30, and the benzotriazole makes
Used time, the mass ratio with melt are 1:1000.
The present invention also provides a kind of preparation processes of LED encapsulation material, specifically comprise the following steps：
Step 1：5 parts of 20 parts of organic siliconresin, 10 parts of polyphenylene sulfide and polyvinyl chloride is taken to be added in kneading machine and be kneaded,
Melting temperature is set as 150 DEG C, in mixing process, 5 parts of triethylamine is added, continues to be kneaded, the time is 20 minutes, obtains first
Mixture；
Primary mix is put into reaction kettle, 5 parts of methyl hexahydrophthalic anhydride, 5 parts of kh560 coupling agents and hydrogeneous is added by step 2
3 parts of silicone oil starts reaction kettle and is stirred, and the speed of agitator of reaction kettle is 200 revs/min, opens simultaneously temp control switch, will
Temperature setting is 100 DEG C, obtains the second mixture；
Step 3, it is cooling and standings to be carried out under 0 DEG C of environment, and apply on the second mixture surface that the second mixture, which is positioned over room temperature,
Graphene powder is smeared, it is made uniformly to be layed in the second mixture surface, laying depth 0.5mm；
Step 4 continues the second mixture after standing in input to reaction kettle, and 1 part of silica flour, 1 part of aluminium powder and glass is added
1 part of fiber takes 3 parts of benzotriazole, by it with water into mixing, quality 1:1000, then mixed solution is poured into instead
It answers in kettle, then reactor temperature is set as 200 DEG C, the agitating device started in reaction kettle is stirred it, reaction kettle
Speed of agitator be 300 revs/min, time 40min；
After waiting for the stirring in reaction kettle, the cooling device of reaction kettle is started for step 5, cold to the raw material progress in kettle,
When its temperature being made to be cooled to 20 DEG C, the raw material in reaction kettle is taken out, is placed into mold and carries out pressing and forming, obtain finished product.
Embodiment 2
A kind of LED encapsulation material and preparation process, include the following steps：A kind of LED encapsulation material, the LED encapsulation material institute
The raw material and shared mass percent used be：30 parts of organic siliconresin, 30 parts of polyphenylene sulfide, 15 parts of polyvinyl chloride, methyl
10 parts of hexahydrophthalic anhydride, 10 parts of kh560 coupling agents, 10 parts of triethylamine, 8 parts of benzotriazole, 10 parts of Graphene powder, 3 parts of silica flour, aluminium
The particle diameter of 5 parts of 3 parts of powder, 3 parts of glass fibre and containing hydrogen silicone oil, the silica flour and aluminium powder is less than 400nm, the glass fibers
Dimension is staple fiber, and the containing hydrogen silicone oil is in the environment of room temperature is 25 DEG C, index of refraction 1.400, viscosity 40, the benzo three
When in use, the mass ratio with melt is 1 to azoles:1000.
The present invention also provides a kind of preparation processes of LED encapsulation material, specifically comprise the following steps：
Step 1：15 parts of 30 parts of organic siliconresin, 30 parts of polyphenylene sulfide and polyvinyl chloride is taken to be added in kneading machine and be kneaded,
Melting temperature is set as 200 DEG C, in mixing process, 10 parts of triethylamine is added, continues to be kneaded, and the time is 30 minutes, obtains the
One mixture；
Step 2 puts into primary mix in reaction kettle, and 10 parts of methyl hexahydrophthalic anhydride, 10 parts of kh560 coupling agents is added and contains
5 parts of hydrogen silicone oil starts reaction kettle and is stirred, and the speed of agitator of reaction kettle is 200 revs/min, opens simultaneously temp control switch,
It is 150 DEG C by temperature setting, obtains the second mixture；
Step 3, it is cooling and standings to be carried out under 5 DEG C of environment, and apply on the second mixture surface that the second mixture, which is positioned over room temperature,
Graphene powder is smeared, it is made uniformly to be layed in the second mixture surface, laying depth 0.1.5mm；
Step 4 continues the second mixture after standing in input to reaction kettle, and 3 parts of silica flour, 3 parts of aluminium powder and glass is added
3 parts of fiber takes 8 parts of benzotriazole, by it with water into mixing, quality 1:1000, then mixed solution is poured into instead
It answers in kettle, then reactor temperature is set as 250 DEG C, the agitating device started in reaction kettle is stirred it, reaction kettle
Speed of agitator be 300 revs/min, time 60min；
After waiting for the stirring in reaction kettle, the cooling device of reaction kettle is started for step 5, cold to the raw material progress in kettle,
When its temperature being made to be cooled to 30 DEG C, the raw material in reaction kettle is taken out, is placed into mold and carries out pressing and forming, obtain finished product.
Embodiment 3
A kind of LED encapsulation material and preparation process, include the following steps：A kind of LED encapsulation material, the LED encapsulation material institute
The raw material and shared mass percent used be：25 parts of organic siliconresin, 20 parts of polyphenylene sulfide, 10 parts of polyvinyl chloride, methyl
8 parts of hexahydrophthalic anhydride, 8 parts of kh560 coupling agents, 8 parts of triethylamine, 5 parts of benzotriazole, 8 parts of Graphene powder, 2 parts of silica flour, aluminium powder 2
The particle diameter of 4 parts of part, 2 parts of glass fibre and containing hydrogen silicone oil, the silica flour and aluminium powder is less than 400nm, the glass fibre
For staple fiber, the containing hydrogen silicone oil is in the environment of room temperature is 25 DEG C, index of refraction 1.400, viscosity 35, the benzotriazole
When in use, it is 1 with the mass ratio of melt:1000.
The present invention also provides a kind of preparation processes of LED encapsulation material, specifically comprise the following steps：
Step 1：10 parts of 25 parts of organic siliconresin, 20 parts of polyphenylene sulfide and polyvinyl chloride is taken to be added in kneading machine and be kneaded,
Melting temperature is set as 180 DEG C, in mixing process, 8 parts of triethylamine is added, continues to be kneaded, the time is 25 minutes, obtains first
Mixture；
Primary mix is put into reaction kettle, 8 parts of methyl hexahydrophthalic anhydride, 8 parts of kh560 coupling agents and hydrogeneous is added by step 2
4 parts of silicone oil starts reaction kettle and is stirred, and the speed of agitator of reaction kettle is 200 revs/min, opens simultaneously temp control switch, will
Temperature setting is 125 DEG C, obtains the second mixture；
Step 3, it is cooling and standings to be carried out under 3 DEG C of environment, and apply on the second mixture surface that the second mixture, which is positioned over room temperature,
Graphene powder is smeared, it is made uniformly to be layed in the second mixture surface, laying depth 1mm；
Step 4 continues the second mixture after standing in input to reaction kettle, and 2 parts of silica flour, 2 parts of aluminium powder and glass is added
2 parts of fiber takes 5 parts of benzotriazole, by it with water into mixing, quality 1:1000, then mixed solution is poured into instead
It answers in kettle, then reactor temperature is set as 230 DEG C, the agitating device started in reaction kettle is stirred it, reaction kettle
Speed of agitator be 300 revs/min, time 50min；
After waiting for the stirring in reaction kettle, the cooling device of reaction kettle is started for step 5, cold to the raw material progress in kettle,
When its temperature being made to be cooled to 25 DEG C, the raw material in reaction kettle is taken out, is placed into mold and carries out pressing and forming, obtain finished product.
Three kinds of LED encapsulation materials can be obtained by above three groups of embodiments, these three LED encapsulation materials are carried out respectively
The test of heat resistance, electric conductivity and anti-ultraviolet property, then carried out accordingly with the LED encapsulation material Jing Guo common process
Test, and its data is acquired comparison, as a result obtain heat resistance, the conduction of the LED encapsulation material in three groups of embodiments
Performance and anti-ultraviolet property have different improvement, the heat resistance of LED encapsulation material, electric conductivity wherein in embodiment 3
It is best with anti-ultraviolet property, it is worth highest, the present invention in the mixing of raw material by being added silica flour, aluminium powder and glass
Fiber improves heat resistance, heat conductivility and coefficient of thermal expansion that LED seals material so that LED encapsulation material can be each
A relatively good working performance is kept under the severe working environment of kind, by adding containing hydrogen silicone oil when curing stirring, is improved
The refractive index and structural rigidity of LED encapsulation material after moulding, and not dust suction under the working environment in dust content,
The aesthetics for improving LED product improves LED package materials by adding benzotriazole material using its material characteristic of itself
The anti-ultraviolet ageing ability of material, extends service life.
Finally it should be noted that：The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
With technical scheme described in the above embodiments is modified or equivalent replacement of some of the technical features,
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in the present invention's
Within protection domain.
Claims (8)
1. a kind of LED encapsulation material, which is characterized in that raw material used in the LED encapsulation material and shared quality percentage
Than for：20-30 parts of organic siliconresin, 10-30 parts of polyphenylene sulfide, 5-15 parts of polyvinyl chloride, 5-10 parts of methyl hexahydrophthalic anhydride,
5-10 parts of kh560 coupling agents, 5-10 parts of triethylamine, 3-8 parts of benzotriazole, 5-10 parts of Graphene powder, 1-3 parts of silica flour, aluminium powder
3-5 parts of 1-3 parts, 1-3 parts of glass fibre and containing hydrogen silicone oil.
2. a kind of LED encapsulation material according to claim 1, it is characterised in that：The particle of the silica flour and aluminium powder is straight
Diameter is less than 400nm, and the glass fibre is staple fiber.
3. a kind of LED encapsulation material according to claim 1, it is characterised in that：The containing hydrogen silicone oil is 25 DEG C in room temperature
In the environment of, index of refraction 1.400, viscosity 30-40.
4. a kind of LED encapsulation material according to claim 1, it is characterised in that：The benzotriazole is when in use, and molten
The mass ratio of liquid is 1:1000.
5. a kind of preparation process of LED encapsulation material, specifically comprises the following steps：
Step 1：5-15 parts of 20-30 parts of organic siliconresin, 10-30 parts of polyphenylene sulfide and polyvinyl chloride is taken to be added in kneading machine
It is kneaded, melting temperature is set as 150-200 DEG C, in mixing process, 5-10 parts of triethylamine is added, continues to be kneaded, the time
It is 20-30 minutes, obtains the first mixture；
Step 2 puts into primary mix in reaction kettle, and 5-10 parts of methyl hexahydrophthalic anhydride, 5-10 parts of kh560 coupling agents is added
With 3-5 parts of containing hydrogen silicone oil, start reaction kettle and be stirred, open simultaneously temp control switch, is 100-150 by temperature setting
DEG C, obtain the second mixture；
Second mixture is positioned over room temperature to carry out cooling and standings under 0-5 DEG C of environment, and on the second mixture surface by step 3
Graphene powder is smeared, it is made uniformly to be layed in the second mixture surface；
Step 4, by the second mixture after standing continue input in reaction kettle, be added 1-3 parts of silica flour, 1-3 parts of aluminium powder and
1-3 parts of glass fibre takes 3-8 parts of benzotriazole, by it with water into mixing, quality 1:1000, then by mixed solution
It is poured into reaction kettle, then reactor temperature is set as 200-250 DEG C, the agitating device started in reaction kettle carries out it
Stirring, time 40-60min；
After waiting for the stirring in reaction kettle, the cooling device of reaction kettle is started for step 5, cold to the raw material progress in kettle,
When its temperature being made to be cooled to 20-30 DEG C, the raw material in reaction kettle is taken out, is placed into mold and carries out pressing and forming, obtain finished product.
6. a kind of preparation process of LED encapsulation material according to claim 5, it is characterised in that：In the step 2, instead
It is 200 revs/min to answer the speed of agitator of kettle.
7. a kind of preparation process of LED encapsulation material according to claim 5, it is characterised in that：In the step 3, stone
The laying depth of black alkene is 0.5-1.5mm.
8. a kind of preparation process of LED encapsulation material according to claim 5, it is characterised in that：In the step 4, instead
It is 300 revs/min to answer the speed of agitator of kettle.
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2018
- 2018-04-01 CN CN201810279566.0A patent/CN108395699A/en active Pending
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| US6506828B1 (en) * | 1999-11-22 | 2003-01-14 | Kyowa Chemical Industry Co., Ltd. | Resin composition, molded article therefrom, and utilization thereof |
| KR20150136292A (en) * | 2014-05-27 | 2015-12-07 | 주식회사 대신테크젠 | Highly thermally conductive inorganic-polymer complex composition for applying lighting lamp LED that contains expanded graphite and manufacturing method thereof |
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Application publication date: 20180814 |