CN109054731A - A kind of cementability high refractive index additional organosilicon packaging plastic and preparation method thereof - Google Patents
A kind of cementability high refractive index additional organosilicon packaging plastic and preparation method thereof Download PDFInfo
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- CN109054731A CN109054731A CN201810879831.9A CN201810879831A CN109054731A CN 109054731 A CN109054731 A CN 109054731A CN 201810879831 A CN201810879831 A CN 201810879831A CN 109054731 A CN109054731 A CN 109054731A
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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
- C09J11/06—Non-macromolecular additives organic
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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
-
- 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
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Silicon Polymers (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The invention discloses a kind of cementability high refractive index additional organosilicon packaging plastics and preparation method thereof.This method is to be uniformly mixed phenyl vinyl polysiloxane, modified phenyl-vinyl silicon oil, phenyl hydrogen-containing silicon oil, the hydrogeneous silicone resin of phenyl, 1- acetenyl -1- cyclohexanol and Karst catalyst, remove bubble, in 100~150 DEG C of 1~4h of solidification, cementability high refractive index additional organosilicon packaging plastic is obtained.High refractive index additional organosilicon packaging plastic prepared by the present invention, adhesive property and good mechanical performance.Preparation method of the invention is simple and easy to do, and environmental protection, raw material sources are extensive, industrialized production easy to accomplish, are expected to be widely used in LED component encapsulation field.
Description
Technical field
The present invention relates to organosilicon encapsulating material technical field, in particular to cementability high refractive index additional organosilicon seals
Fill glue and preparation method thereof.
Background technique
Encapsulating material is the important component of LED component, there is important influence to its performance and used life.Package material
Material mainly has epoxy resin and organosilicon material.Wherein, the weatherability and chemical stability of organosilicon material are good, especially high folding
Penetrate that rate additional organosilicon packaging plastic curing rate is fast, and linear shrinkage ratio is small, it is a kind of encapsulation haveing excellent performance that light extraction efficiency is high
Material.But it is largely non-polar group that it, which solidifies rear surface, and adhesive property is poor, is subject to certain restrictions its application.
Currently, the method for improving high refractive index additional organosilicon packaging plastic adhesive property is that tackifier are added.But it viscosifies
The synthesis technology of agent is difficult to control, and tackifier can have an adverse effect to the performance of packaging plastic.Therefore, it prepares a kind of comprehensive
The excellent cementability high refractive index additional organosilicon packaging plastic of energy has great importance.
Summary of the invention
The object of the invention is to provide a kind of cementability of high comprehensive performance to solve the deficiency of the prior art
High refractive index additional organosilicon packaging plastic and preparation method thereof.
The present invention is attained in that using following technical solution
A kind of preparation method of cementability high refractive index additional organosilicon packaging plastic, comprising the following steps: by phenyl second
Alkenyl silicone resin, modified phenyl-vinyl silicon oil, phenyl hydrogen-containing silicon oil, the hydrogeneous silicone resin of phenyl, 1- acetenyl -1- cyclohexanol and
Karst catalyst is uniformly mixed, and is removed bubble in 100~150 DEG C of 1~4h of solidification and is obtained cementability high refractive index add-on type
Organic silicon packaging glue；The mass fraction of raw material is as follows:
The contents of ethylene of the phenyl vinyl polysiloxane is 1~8wt%.
Preferably, the preparation method of the modified phenyl-vinyl silicon oil, comprising the following steps: by tetramethyl tetraphenyl ring
Tetrasiloxane, 3- (the third oxygen of 2,3- epoxy) hydroxypropyl methyl dimethoxysilane, 3- methacryloyloxypropyl methyl dimethoxy
Base silane and divinyl tetramethyl disiloxane 100:(10~30 in mass ratio): (10~30): (1~5) is uniformly mixed, so
The 25wt% tetramethylammonium hydroxide methanol solution of 0.02~0.06wt% of reactant gross mass is added afterwards, is warming up to 100~125
DEG C reaction 3~6h, be finally warming up to 150~180 DEG C, vacuum degree be 0.07~0.098 under, remove low molecule, be modified
Phenyl-vinyl silicon oil；
Preferably, the hydrogen content of the phenyl hydrogen-containing silicon oil is 0.3~0.6wt%.
Preferably, the hydrogen content of the hydrogeneous silicone resin of the phenyl is 0.1~0.5wt%.
Preferably, for the Karst catalyst in terms of metal platinum, content is 1000~6000ppm.
The present invention also provides a kind of using the encapsulation of cementability high refractive index additional organosilicon made from the preparation method
Glue.
The present invention is using the above-mentioned attainable beneficial effect of technical solution:
1, the present invention prepares high refractive index add-on type containing the modification phenyl-vinyl silicon oil of epoxy group and ester group using synthesis
Organic silicon packaging glue significantly improves the adhesive property of packaging plastic.Modified phenyl-vinyl silicon oil contains multiple vinyl, Ke Yiti
For Concentrative crosslinking structure, improve the mechanical property of packaging plastic.
2, preparation method of the invention is simple and easy to do, and environmental protection, raw material sources are extensive, industrialized production easy to accomplish.
Specific embodiment
The technical program is explained in detail below in conjunction with specific embodiment.
Embodiment 1
By tetramethyl tetraphenyl cyclotetrasiloxane, 3- (the third oxygen of 2,3- epoxy) hydroxypropyl methyl dimethoxysilane, 3- methyl
Acryloxypropyl dimethoxysilane and divinyl tetramethyl disiloxane 100:10:30:5 in mass ratio mixing
Uniformly, the 25wt% tetramethylammonium hydroxide methanol solution of reactant gross mass 0.06wt% is then added, is warming up to 100 DEG C instead
6h is answered, is finally warming up to 180 DEG C, in the case where vacuum degree is 0.07, removes low molecule, obtains modified phenyl-vinyl silicon oil 1.
It is the phenyl vinyl polysiloxane of 1wt% by 100 mass parts contents of ethylene, the modified phenyl vinyl of 5 mass parts
The phenyl that phenyl hydrogen-containing silicon oil that silicone oil 1,8.5 mass parts hydrogen contents are 0.3wt%, 40 mass parts hydrogen contents are 0.1wt% contains
The Karst catalyst that hydrogen silicone resin, 0.003 mass parts 1- acetenyl -1- cyclohexanol and 1 mass parts platinum content are 1500ppm is mixed
It closes uniformly, removes bubble in 100 DEG C of solidification 4h and obtain cementability high refractive index additional organosilicon packaging plastic.The performance of sample
As shown in table 1.
Embodiment 2
By tetramethyl tetraphenyl cyclotetrasiloxane, 3- (the third oxygen of 2,3- epoxy) hydroxypropyl methyl dimethoxysilane, 3- methyl
Acryloxypropyl dimethoxysilane and divinyl tetramethyl disiloxane 100:30:10:1 in mass ratio mixing
Uniformly, the 25wt% tetramethylammonium hydroxide methanol solution of reactant gross mass 0.02wt% is then added, is warming up to 125 DEG C instead
3h is answered, is finally warming up to 150 DEG C, in the case where vacuum degree is 0.098, removes low molecule, obtains modified phenyl-vinyl silicon oil 2.
It is the phenyl vinyl polysiloxane of 3wt% by 100 mass parts contents of ethylene, the modified phenyl vinyl of 10 mass parts
The phenyl that phenyl hydrogen-containing silicon oil that silicone oil 2,20 mass parts hydrogen contents are 0.6wt%, 16 mass parts hydrogen contents are 0.4wt% is hydrogeneous
The Karst catalyst that silicone resin, 0.008 mass parts 1- acetenyl -1- cyclohexanol and 0.7 mass parts platinum content are 2000ppm is mixed
It closes uniformly, removes bubble in 150 DEG C of solidification 1h and obtain cementability high refractive index additional organosilicon packaging plastic.The performance of sample
As shown in table 1.
Embodiment 3
By tetramethyl tetraphenyl cyclotetrasiloxane, 3- (the third oxygen of 2,3- epoxy) hydroxypropyl methyl dimethoxysilane, 3- methyl
Acryloxypropyl dimethoxysilane and divinyl tetramethyl disiloxane 100:25:10:2 in mass ratio mixing
Uniformly, the 25wt% tetramethylammonium hydroxide methanol solution of reactant gross mass 0.03wt% is then added, is warming up to 115 DEG C instead
4h is answered, is finally warming up to 160 DEG C, in the case where vacuum degree is 0.08, removes low molecule, obtains modified phenyl-vinyl silicon oil 3.
It is the phenyl vinyl polysiloxane of 8wt% by 100 mass parts contents of ethylene, the modified phenyl vinyl of 15 mass parts
The phenyl that phenyl hydrogen-containing silicon oil that silicone oil 3,30 mass parts hydrogen contents are 0.6wt%, 55 mass parts hydrogen contents are 0.5wt% is hydrogeneous
The Karst catalyst that silicone resin, 0.03 mass parts 1- acetenyl -1- cyclohexanol and 1 mass parts platinum content are 5000ppm mixes
Uniformly, removing bubble obtains cementability high refractive index additional organosilicon packaging plastic in 120 DEG C of solidification 3h.The performance of sample is such as
Shown in table 1.
Embodiment 4
By tetramethyl tetraphenyl cyclotetrasiloxane, 3- (the third oxygen of 2,3- epoxy) hydroxypropyl methyl dimethoxysilane, 3- methyl
Acryloxypropyl dimethoxysilane and divinyl tetramethyl disiloxane 100:20:15:4 in mass ratio mixing
Uniformly, the 25wt% tetramethylammonium hydroxide methanol solution of reactant gross mass 0.05wt% is then added, is warming up to 120 DEG C instead
3.5h is answered, is finally warming up to 170 DEG C, in the case where vacuum degree is 0.085, removes low molecule, obtains modified phenyl-vinyl silicon oil 4.
It is the phenyl vinyl polysiloxane of 4wt% by 100 mass parts contents of ethylene, the modified phenyl vinyl of 20 mass parts
The phenyl that phenyl hydrogen-containing silicon oil that silicone oil 4,25 mass parts hydrogen contents are 0.5wt%, 40 mass parts hydrogen contents are 0.35wt% contains
Hydrogen silicone resin, 0.01 mass parts 1- acetenyl -1- cyclohexanol and 0.6 mass parts platinum content are the Karst catalyst of 3000ppm
It is uniformly mixed, removes bubble in 130 DEG C of solidification 2.5h and obtain cementability high refractive index additional organosilicon packaging plastic.Sample
Performance is as shown in table 1.
Embodiment 5
By tetramethyl tetraphenyl cyclotetrasiloxane, 3- (the third oxygen of 2,3- epoxy) hydroxypropyl methyl dimethoxysilane, 3- methyl
Acryloxypropyl dimethoxysilane and divinyl tetramethyl disiloxane 100:15:20:2 in mass ratio mixing
Uniformly, the 25wt% tetramethylammonium hydroxide methanol solution of reactant gross mass 0.04wt% is then added, is warming up to 115 DEG C instead
4.5h is answered, is finally warming up to 165 DEG C, in the case where vacuum degree is 0.09, removes low molecule, obtains modified phenyl-vinyl silicon oil 5.
It is the phenyl vinyl polysiloxane of 3wt% by 100 mass parts contents of ethylene, the modified phenyl vinyl of 25 mass parts
The phenyl that phenyl hydrogen-containing silicon oil that silicone oil 5,20 mass parts hydrogen contents are 0.4wt%, 52 mass parts hydrogen contents are 0.25wt% contains
Hydrogen silicone resin, 0.02 mass parts 1- acetenyl -1- cyclohexanol and 0.5 mass parts platinum content are the Karst catalyst of 4000ppm
It is uniformly mixed, removes bubble in 140 DEG C of solidification 2h and obtain cementability high refractive index additional organosilicon packaging plastic.The property of sample
It can be as shown in table 1.
Comparative example 1
By 100 mass parts contents of ethylene be 1wt% phenyl vinyl polysiloxane, 5 mass parts contents of ethylene be
The phenyl-vinyl silicon oil of 3.4wt%, phenyl hydrogen-containing silicon oil, the 40 mass parts hydrogen contents that 8.5 mass parts hydrogen contents are 0.3wt%
It is for the hydrogeneous silicone resin of phenyl, 0.003 mass parts 1- acetenyl -1- cyclohexanol and 1.5 mass parts platinum contents of 0.1wt%
The Karst catalyst of 1000ppm is uniformly mixed, and is removed bubble in 100 DEG C of solidification 4h and is obtained cementability high refractive index add-on type
Organic silicon packaging glue.The performance of sample is as shown in table 1.
Sample performance test methods are as follows in table 1:
1, it is cut according to the stretching bonding with substrate of GB/T13936-1992 measurement high refractive index additional organosilicon packaging plastic
Shearing stress.
2, according to the refractive index of GB/T614-2006 measurement high refractive index additional organosilicon packaging plastic.
3, according to the tensile strength of GB/T528-2009 measurement high refractive index additional organosilicon packaging plastic.
4, according to the shore D hardness of GB/T531.1-2008 measurement high refractive index additional organosilicon packaging plastic.
Adhesive property, refractive index and the mechanical property of 1 high refractive index additional organosilicon packaging plastic of table
As it can be seen from table 1 the adhesive property of common high refractive index additional organosilicon packaging plastic is poor, to aluminium (Al) and
The adhesive shear strength of polyphthalamide (PPA) substrate is respectively 0.87MPa and 0.46MPa (see comparative example 1).And with originally
The organic silicon packaging glue of the modification phenyl-vinyl silicon oil preparation of invention synthesis, adhesive property, which has, to be significantly improved, and bonding is cut
260% (see embodiment 1-5) can be improved in shearing stress.This is primarily due to modified phenyl-vinyl silicon oil and contains epoxy group and ester
Based polar group, they can form stronger interaction with substrate, and organic silicon packaging glue is made to have good adhesive strength.
As can also be seen from Table 1, the organic silicon packaging glue of the modification phenyl-vinyl silicon oil preparation synthesized with the present invention,
Mechanical property is improved there has also been apparent, and tensile strength has been increased to 3.2MPa or more from 3.02MPa, and shore D hardness is mentioned from 44
Height is to 48 or more.This is because containing multiple vinyl in modified phenyl-vinyl silicon oil, Concentrative crosslinking structure can be provided,
Disperse the external force being subject to effectively.
What has been described above is only a preferred embodiment of the present invention, it is noted that for those of ordinary skill in the art
For, without departing from the concept of the premise of the invention, various modifications and improvements can be made, these belong to the present invention
Protection scope.
Claims (6)
1. a kind of preparation method of cementability high refractive index additional organosilicon packaging plastic, which comprises the following steps:
By phenyl vinyl polysiloxane, modified phenyl-vinyl silicon oil, phenyl hydrogen-containing silicon oil, the hydrogeneous silicone resin of phenyl, 1- acetenyl -1-
Cyclohexanol and Karst catalyst are uniformly mixed, and remove bubble, in 100~150 DEG C of 1~4h of solidification, obtain the refraction of cementability height
Rate additional organosilicon packaging plastic；The mass fraction of raw material is as follows:
The contents of ethylene of the phenyl vinyl polysiloxane is 1~8wt%.
2. the preparation method of cementability high refractive index additional organosilicon packaging plastic as described in claim 1, which is characterized in that institute
The preparation method of modified phenyl-vinyl silicon oil is stated, the following steps are included:
By tetramethyl tetraphenyl cyclotetrasiloxane, 3- (the third oxygen of 2,3- epoxy) hydroxypropyl methyl dimethoxysilane, 3- metering system
Methyl dimethoxysilane and divinyl tetramethyl disiloxane 100:(10~30 in mass ratio): (10~
30): (1~5) is uniformly mixed, and the 25wt% tetramethylammonium hydroxide first of 0.02~0.06wt% of reactant gross mass is then added
Alcoholic solution is warming up to 100~125 DEG C of 3~6h of reaction, is finally warming up to 150~180 DEG C, is 0.07~0.098 in vacuum degree
Under, low molecule is removed, modified phenyl-vinyl silicon oil is obtained.
3. the preparation method of cementability high refractive index additional organosilicon packaging plastic as described in claim 1, which is characterized in that institute
The hydrogen content for stating phenyl hydrogen-containing silicon oil is 0.3~0.6wt%.
4. the preparation method of cementability high refractive index additional organosilicon packaging plastic as described in claim 1, which is characterized in that institute
The hydrogen content for stating the hydrogeneous silicone resin of phenyl is 0.1~0.5wt%.
5. the preparation method of cementability high refractive index additional organosilicon packaging plastic as described in claim 1, which is characterized in that institute
Karst catalyst is stated in terms of metal platinum, content is 1000~6000ppm.
6. a kind of cementability high refractive index additional organosilicon packaging plastic, which is characterized in that the cementability high refractive index addition
Type organic silicon packaging glue is as made from preparation method described in claim 1.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112322252A (en) * | 2020-10-27 | 2021-02-05 | 复旦大学 | High-refractive-index thermosetting organic silicon adhesive for full attachment of liquid crystal display and application thereof |
| CN113480737A (en) * | 2021-07-29 | 2021-10-08 | 广州市白云化工实业有限公司 | Acrylate modified alpha, omega-divinyl siloxane and addition type organic silicon adhesive |
| CN115433541A (en) * | 2022-09-30 | 2022-12-06 | 郑州中原思蓝德高科股份有限公司 | Conductive adhesive and preparation method thereof |
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Application publication date: 20181221 |