CN105368363B - High power LED package epoxy encapsulation glue as well as preparation method and application thereof - Google Patents
High power LED package epoxy encapsulation glue as well as preparation method and application thereof Download PDFInfo
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- CN105368363B CN105368363B CN201510884805.1A CN201510884805A CN105368363B CN 105368363 B CN105368363 B CN 105368363B CN 201510884805 A CN201510884805 A CN 201510884805A CN 105368363 B CN105368363 B CN 105368363B
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Abstract
The invention discloses a kind of high power LED package epoxy encapsulation glue as well as preparation method and application thereof, the packaging plastic is made up of according to mass percent meter component A 42~47% and B component 53~58%；Component A is made up according to mass percent meter of bisphenol f type epoxy resin 19.85~80%, phenol aldehyde modified organic siliconresin 19.85~80% and Siloxane-Oxyalkylene Copolymers 0.15~0.25%, B component is according to mass percent meter by Korean pine extract solution 14~27%, adipic dihydrazide 72~85%, the benzoyloxy 2 of single benzoic acid resorcinol 0.4~1.0% and 4,2,6,6 tetramethyl piperidines 0.6~1.2% are made.Packaging plastic high temperature resistant of the present invention, ultraviolet light resistant, translucency is good, refractive index is high, and technique is simple, and cost is low, can be widely applied to high power LED package field.
Description
Technical field
The present invention relates to LED technology field, specifically a kind of high power LED package epoxy encapsulation glue and its preparation
Method and purposes.
Background technology
LED illumination is widely used in the fields such as display screen, Landscape Lighting, special lighting as " green illumination ", with
LED light source technology reaches its maturity, and every watt of luminescent lumen increases rapidly, promotes its price reduction of successively decreasing year by year.Look forward to the future, LED is general
Illumination turns into the industrial hot spot of most market potential, thus high-power, high-brightness white-light LED encapsulation problem also becomes increasingly conspicuous.
Common LED encapsulation liquid epoxy material viscosity high (at room temperature more than viscosity 10000cps), glass transition temperature
Spend low (110 DEG C or so), it is difficult to meet the requirement of large power white light LED.Large power white light LED requires that potting resin has preferably
Mobility, higher glass transition temperature, while also require have white light high light transmittance, fire-retardant, uvioresistant, solidification machinery strong
Spend high characteristic.
The encapsulating material of in the market common LED is mainly bisphenol A-type transparent epoxy resin, and power type LED encapsulation material
Market then depends on import, and it has preferably heat-resisting and UV resistant performance, higher compared with the encapsulating material of the country
Refractive index and the lower coefficient of expansion etc., such as international three big silica gel enterprise DOW CORNINGs, step figure, the product of SHIN-ETSU HANTOTAI with high refractive index
Based on organosilicon encapsulating material, high-end encapsulation in the market at home has absolute predominance.Certain recent year also emerges in large numbers
Shuande ACR, Changsha blue star, Jiangyin day magnitude manufacturing enterprise, but it is maintained essentially at the production of low-power encapsulating compound, yield
It is smaller, thus develop high-grade encapsulating products and the popularization for promoting domestic power-type LED is significant.
Conventional epoxies can not fully meet LED encapsulation requirement, and organic siliconresin price is very high, and by external ridge
It is disconnected, thus prepare high temperature resistant and adhesive property is strong, dielectric properties are strong and ultraviolet light resistant, translucency are good be applied to it is high-power
LED encapsulating material is very urgent.
The content of the invention
It is an object of the invention to provide a kind of low cost, low viscosity, bonding force be strong, resistant to elevated temperatures high power LED package
With epoxy encapsulation glue as well as preparation method and application thereof.
To achieve the above object, the present invention provides following technical scheme：
High power LED package epoxy encapsulation glue, it is two-component system, according to mass percent meter, by component A 42
~47% and B component 53~58% form；Described component A is according to mass percent meter, by bisphenol f type epoxy resin 19.85
~80%, phenol aldehyde modified organic siliconresin 19.85~80% and Siloxane-Oxyalkylene Copolymers 0.15~0.25% are made, described
B component is according to mass percent meter, by Korean pine extract solution 14~27%, adipic dihydrazide 72~85%, single benzoic acid isophthalic
Two phenolic esters 0.4~1.0% and 4 benzoyloxy 2,2,6,6 tetramethyl piperidine 0.6~1.2% are made；Described Korean pine carries
The preparation method of liquid is taken, is comprised the following steps：
1) Korean pine root or stem are cleaned, smashed, crossed 40~80 mesh sieves, obtain coarse powder；
2) ethanol solution for being 75~88% toward the volumetric concentrations of 5~6 times of amounts of addition meal quality in coarse powder, immersion 12
~18 hours, be then heated to boiling reflux 3~5 hours, filter, use percolation with 1~1.5ml per minute speed slowly
Diacolation, percolate is collected as liquid of just filtering, is separately deposited；
3) ethanol solution that the volumetric concentration for continuing to add 4~5 times of amounts of meal quality in toward coarse powder is 75~88%, adds
Heat was to boiling reflux 2~3 hours, filtering, used percolation to collect percolate with 1.5~2ml per minute speed slowly diacolation
For continuous liquid of filtering, under 0.07~0.08MPa of vacuum, relative density is 1.18~1.20 when continuous liquid of filtering is concentrated under reduced pressure into 55 DEG C
Lotion；
4) lotion of step 3) is turned to be dissolved in the first liquid of filtering of step 2), obtains Korean pine extract solution.
As the further scheme of the present invention：According to mass percent meter, by component A 44~45% and B component 55~
56% composition；Described component A is according to mass percent meter, by bisphenol f type epoxy resin 45~55%, phenol aldehyde modified organosilicon
Resin 40~50% and Siloxane-Oxyalkylene Copolymers 0.15~0.22% are made, described B component according to mass percent meter, by
Korean pine extract solution 17~23%, adipic dihydrazide 76~82%, single benzoic acid resorcinol 0.4~0.8% and 4- benzene first
Acyloxy -2,2,6,6- tetramethyl piperidines 0.6~0.9% are made.
As the further scheme of the present invention：According to mass percent meter, by 55.6% group of component A 44.4% and B component
Into；Described component A is according to mass percent meter, by bisphenol f type epoxy resin 52.8%, phenol aldehyde modified organic siliconresin
47.02% and Siloxane-Oxyalkylene Copolymers 0.18% be made, described B component is according to mass percent meter, by Korean pine extract solution
18.5%th, adipic dihydrazide 80%, single benzoic acid resorcinol 0.7% and 4- benzoyloxy -2,2,6,6- tetramethyls
Piperidines 0.8% is made.
As the further scheme of the present invention：The solid-liquid ratio of described Korean pine extract solution is 1：3~5.
The described high power LED package preparation method of epoxy encapsulation glue, comprises the following steps：
(1) preparation of component A：Bisphenol f type epoxy resin, phenol aldehyde modified organic siliconresin and polyether-modified are weighed in proportion
Polysiloxanes, stirred 1~2.5 hour at 90~115 DEG C, be well mixed, pack and produce component A；
(2) preparation of B component：Weigh in proportion Korean pine extract solution, adipic dihydrazide, single benzoic acid resorcinol and
4- benzoyloxys -2,2,6,6- tetramethyl piperidines, stirred 2~3 hours at 88~95 DEG C, be well mixed, pack and produce B groups
Point；
(3) by above-mentioned steps (1)~component A made from (2) and B component according to the proportioning of above-mentioned mass percent, mixing
Uniformly solidified, condition of cure is：Solidify 1~1.2 hour in 90~135 DEG C, solidify 3~5 hours then at 110~142 DEG C,
Produce high power LED package epoxy encapsulation glue.
Purposes of the described epoxy encapsulation glue in terms of high power LED package material is prepared.
Compared with prior art, the beneficial effects of the invention are as follows：The present invention is with bisphenol f type epoxy resin and phenol aldehyde modified has
Machine silicones is host, using Siloxane-Oxyalkylene Copolymers as defoamer, using adipic dihydrazide as curing agent, between single benzoic acid
Benzenediol ester is ultra-violet absorber, and with 4- benzoyloxys -2,2,6,6- tetramethyl piperidines are light stabilizer, is had by mixing
There is a Korean pine extract solution of high temperature resistant, corrosion resistance, cured reaction obtains that a kind of high temperature resistant, ultraviolet light resistant, translucency be good, folding
The high epoxy encapsulation glue of rate is penetrated, the preparation technology of the packaging plastic is simple, and cost is low, and glass transition temperature after material solidification
Degree and heat decomposition temperature are high, and adhesive property is strong, can be widely applied to high power LED package field of material technology.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
Embodiment 1
High power LED package epoxy encapsulation glue, it is two-component system, according to quality hundred in the embodiment of the present invention
Divide than meter, be made up of component A 47% and B component 53%；Described component A is according to mass percent meter, by bisphenol F type epoxy tree
Fat 19.85%, phenol aldehyde modified organic siliconresin 80% and Siloxane-Oxyalkylene Copolymers 0.15% are made, described B component according to
Mass percent meter, by Korean pine extract solution 14%, adipic dihydrazide 85%, single benzoic acid resorcinol 0.4% and 4- benzene
Formyloxy -2,2,6,6- tetramethyl piperidines 0.6% are made；The preparation method of described Korean pine extract solution, comprises the following steps：
1) Korean pine root or stem are cleaned, smashed, crossed 40 mesh sieves, obtain coarse powder；
2) ethanol solution for being 88% toward the volumetric concentrations of 5 times of amounts of addition meal quality in coarse powder, soaks 12 hours, connects
And be heated to boiling reflux 3 hours, filter, using percolation, slowly diacolation, collection percolate are with 1.5ml per minute speed
First liquid of filtering, is separately deposited；
3) ethanol solution that the volumetric concentration for continuing to add 4 times of amounts of meal quality in toward coarse powder is 88%, is heated to boiling
Backflow 2 hours is risen, filtering, uses percolation percolate to be collected as continuous liquid of filtering, true with 2ml per minute speed slowly diacolation
Under reciprocal of duty cycle 0.07MPa, the lotion that relative density is 1.20 when liquid of filtering is concentrated under reduced pressure into 55 DEG C will be continued；
4) lotion of step 3) is turned to be dissolved in the first liquid of filtering of step 2), obtains solid-liquid ratio 1：3 Korean pine extract solution.
The described high power LED package preparation method of epoxy encapsulation glue, comprises the following steps：
(1) preparation of component A：Bisphenol f type epoxy resin, phenol aldehyde modified organic siliconresin and polyether-modified are weighed in proportion
Polysiloxanes, stirred 2.5 hours at 90 DEG C, be well mixed, pack and produce component A；
(2) preparation of B component：Weigh in proportion Korean pine extract solution, adipic dihydrazide, single benzoic acid resorcinol and
4- benzoyloxys -2,2,6,6- tetramethyl piperidines, stirred 2 hours at 95 DEG C, be well mixed, pack and produce B component；
(3) by above-mentioned steps (1)~component A made from (2) and B component according to the proportioning of above-mentioned mass percent, mixing
Uniformly solidified, condition of cure is：Solidify 1.2 hours in 90 DEG C, solidify 5 hours then at 110 DEG C, produce high-capacity LED envelope
Dress uses epoxy encapsulation glue.
Embodiment 2
High power LED package epoxy encapsulation glue, it is two-component system, according to quality hundred in the embodiment of the present invention
Divide than meter, be made up of component A 42% and B component 58%；Described component A is according to mass percent meter, by bisphenol F type epoxy tree
Fat 80%, phenol aldehyde modified organic siliconresin 19.85% and Siloxane-Oxyalkylene Copolymers 0.15% are made, described B component according to
Mass percent meter, by Korean pine extract solution 27%, adipic dihydrazide 72%, single benzoic acid resorcinol 0.4% and 4- benzene
Formyloxy -2,2,6,6- tetramethyl piperidines 0.6% are made；The preparation method of described Korean pine extract solution, comprises the following steps：
1) Korean pine root or stem are cleaned, smashed, crossed 40 mesh sieves, obtain coarse powder；
2) ethanol solution for being 88% toward the volumetric concentrations of 5 times of amounts of addition meal quality in coarse powder, soaks 12 hours, connects
And be heated to boiling reflux 3 hours, filter, using percolation, slowly diacolation, collection percolate are with 1.5ml per minute speed
First liquid of filtering, is separately deposited；
3) ethanol solution that the volumetric concentration for continuing to add 4 times of amounts of meal quality in toward coarse powder is 88%, is heated to boiling
Backflow 2 hours is risen, filtering, uses percolation percolate to be collected as continuous liquid of filtering, true with 2ml per minute speed slowly diacolation
Under reciprocal of duty cycle 0.07MPa, the lotion that relative density is 1.20 when liquid of filtering is concentrated under reduced pressure into 55 DEG C will be continued；
4) lotion of step 3) is turned to be dissolved in the first liquid of filtering of step 2), obtains solid-liquid ratio 1：3 Korean pine extract solution.
The described high power LED package preparation method of epoxy encapsulation glue, comprises the following steps：
(1) preparation of component A：Bisphenol f type epoxy resin, phenol aldehyde modified organic siliconresin and polyether-modified are weighed in proportion
Polysiloxanes, stirred 2.5 hours at 90 DEG C, be well mixed, pack and produce component A；
(2) preparation of B component：Weigh in proportion Korean pine extract solution, adipic dihydrazide, single benzoic acid resorcinol and
4- benzoyloxys -2,2,6,6- tetramethyl piperidines, stirred 2 hours at 95 DEG C, be well mixed, pack and produce B component；
(3) by above-mentioned steps (1)~component A made from (2) and B component according to the proportioning of above-mentioned mass percent, mixing
Uniformly solidified, condition of cure is：Solidify 1.2 hours in 90 DEG C, solidify 5 hours then at 110 DEG C, produce high-capacity LED envelope
Dress uses epoxy encapsulation glue.
Embodiment 3
High power LED package epoxy encapsulation glue, it is two-component system, according to quality hundred in the embodiment of the present invention
Divide than meter, be made up of component A 43.8% and B component 56.2%；Described component A is according to mass percent meter, by Bisphenol F type ring
Oxygen tree fat 45%, phenol aldehyde modified organic siliconresin 54.75% and Siloxane-Oxyalkylene Copolymers 0.25% are made, described B component
According to mass percent meter, by Korean pine extract solution 20%, adipic dihydrazide 78%, single and of benzoic acid resorcinol 1.0%
4 benzoyloxy 2,2,6,6 tetramethyl piperidine 1.0% is made；The preparation method of described Korean pine extract solution, including it is following
Step：
1) Korean pine root or stem are cleaned, smashed, crossed 80 mesh sieves, obtain coarse powder；
2) ethanol solution for being 75% toward the volumetric concentrations of 6 times of amounts of addition meal quality in coarse powder, soaks 18 hours, connects
And be heated to boiling reflux 5 hours, filter, using percolation, it is first to collect percolate with 1ml per minute speed slowly diacolation
Filter liquid, separately deposit；
3) ethanol solution that the volumetric concentration for continuing to add 5 times of amounts of meal quality in toward coarse powder is 75%, is heated to boiling
Backflow 3 hours is risen, filtering, using percolation, slowly diacolation, collection percolate are continuous liquid of filtering with 1.5ml per minute speed,
Under vacuum 0.08MPa, the lotion that relative density is 1.18 when liquid of filtering is concentrated under reduced pressure into 55 DEG C will be continued；
4) lotion of step 3) is turned to be dissolved in the first liquid of filtering of step 2), obtains solid-liquid ratio 1：5 Korean pine extract solution.
The described high power LED package preparation method of epoxy encapsulation glue, comprises the following steps：
(1) preparation of component A：Bisphenol f type epoxy resin, phenol aldehyde modified organic siliconresin and polyether-modified are weighed in proportion
Polysiloxanes, stirred 1 hour at 115 DEG C, be well mixed, pack and produce component A；
(2) preparation of B component：Weigh in proportion Korean pine extract solution, adipic dihydrazide, single benzoic acid resorcinol and
4- benzoyloxys -2,2,6,6- tetramethyl piperidines, stirred 3 hours at 88 DEG C, be well mixed, pack and produce B component；
(3) by above-mentioned steps (1)~component A made from (2) and B component according to the proportioning of above-mentioned mass percent, mixing
Uniformly solidified, condition of cure is：Solidify 1 hour in 135 DEG C, solidify 3 hours then at 142 DEG C, produce high power LED package
With epoxy encapsulation glue.
Embodiment 4
High power LED package epoxy encapsulation glue, it is two-component system, according to quality hundred in the embodiment of the present invention
Divide than meter, be made up of component A 43.8% and B component 56.2%；Described component A is according to mass percent meter, by Bisphenol F type ring
Oxygen tree fat 54.75%, phenol aldehyde modified organic siliconresin 45% and Siloxane-Oxyalkylene Copolymers 0.25% are made, described B component
According to mass percent meter, by Korean pine extract solution 20%, adipic dihydrazide 78%, single and of benzoic acid resorcinol 0.8%
4 benzoyloxy 2,2,6,6 tetramethyl piperidine 1.2% is made；The preparation method of described Korean pine extract solution, including it is following
Step：
1) Korean pine root or stem are cleaned, smashed, crossed 80 mesh sieves, obtain coarse powder；
2) ethanol solution for being 75% toward the volumetric concentrations of 6 times of amounts of addition meal quality in coarse powder, soaks 18 hours, connects
And be heated to boiling reflux 5 hours, filter, using percolation, it is first to collect percolate with 1ml per minute speed slowly diacolation
Filter liquid, separately deposit；
3) ethanol solution that the volumetric concentration for continuing to add 5 times of amounts of meal quality in toward coarse powder is 75%, is heated to boiling
Backflow 3 hours is risen, filtering, using percolation, slowly diacolation, collection percolate are continuous liquid of filtering with 1.5ml per minute speed,
Under vacuum 0.08MPa, the lotion that relative density is 1.18 when liquid of filtering is concentrated under reduced pressure into 55 DEG C will be continued；
4) lotion of step 3) is turned to be dissolved in the first liquid of filtering of step 2), obtains solid-liquid ratio 1：5 Korean pine extract solution.
The described high power LED package preparation method of epoxy encapsulation glue, comprises the following steps：
(1) preparation of component A：Bisphenol f type epoxy resin, phenol aldehyde modified organic siliconresin and polyether-modified are weighed in proportion
Polysiloxanes, stirred 1 hour at 115 DEG C, be well mixed, pack and produce component A；
(2) preparation of B component：Weigh in proportion Korean pine extract solution, adipic dihydrazide, single benzoic acid resorcinol and
4- benzoyloxys -2,2,6,6- tetramethyl piperidines, stirred 3 hours at 88 DEG C, be well mixed, pack and produce B component；
(3) by above-mentioned steps (1)~component A made from (2) and B component according to the proportioning of above-mentioned mass percent, mixing
Uniformly solidified, condition of cure is：Solidify 1 hour in 135 DEG C, solidify 3 hours then at 142 DEG C, produce high power LED package
With epoxy encapsulation glue.
Embodiment 5
In the embodiment of the present invention, high power LED package epoxy encapsulation glue, according to mass percent meter, by component A
44.4% and B component 55.6% form；Described component A according to mass percent meter, by bisphenol f type epoxy resin 52.8%,
Phenol aldehyde modified organic siliconresin 47.02% and Siloxane-Oxyalkylene Copolymers 0.18% are made, and described B component is according to quality percentage
Than meter, by Korean pine extract solution 18.5%, adipic dihydrazide 80%, single benzoic acid resorcinol 0.7% and 4- benzoxies
Base -2,2,6,6- tetramethyl piperidines 0.8% are made；The preparation method of described Korean pine extract solution, comprises the following steps：
1) Korean pine root or stem are cleaned, smashed, crossed 40~80 mesh sieves, obtain coarse powder；
2) ethanol solution for being 88% toward the volumetric concentrations of 6 times of amounts of addition meal quality in coarse powder, soaks 18 hours, connects
And be heated to boiling reflux 5 hours, filter, using percolation, it is first to collect percolate with 1ml per minute speed slowly diacolation
Filter liquid, separately deposit；
3) ethanol solution that the volumetric concentration for continuing to add 5 times of amounts of meal quality in toward coarse powder is 88%, is heated to boiling
Backflow 3 hours is risen, filtering, using percolation, slowly diacolation, collection percolate are continuous liquid of filtering with 1.5ml per minute speed,
Under vacuum 0.07MPa, the lotion that relative density is 1.20 when liquid of filtering is concentrated under reduced pressure into 55 DEG C will be continued；
4) lotion of step 3) is turned to be dissolved in the first liquid of filtering of step 2), obtains solid-liquid ratio 1：4 Korean pine extract solution.
The described high power LED package preparation method of epoxy encapsulation glue, comprises the following steps：
(1) preparation of component A：Bisphenol f type epoxy resin, phenol aldehyde modified organic siliconresin and polyether-modified are weighed in proportion
Polysiloxanes, stirred 2.5 hours at 110 DEG C, be well mixed, pack and produce component A；
(2) preparation of B component：Weigh in proportion Korean pine extract solution, adipic dihydrazide, single benzoic acid resorcinol and
4- benzoyloxys -2,2,6,6- tetramethyl piperidines, stirred 3 hours at 92 DEG C, be well mixed, pack and produce B component；
(3) by above-mentioned steps (1)~component A made from (2) and B component according to the proportioning of above-mentioned mass percent, mixing
Uniformly solidified, condition of cure is：Solidify 1.2 hours in 105 DEG C, solidify 5 hours then at 130 DEG C, produce high-capacity LED envelope
Dress uses epoxy encapsulation glue.
Comparative example 1
Component is on the basis of embodiment 5 used by this comparative example, and bisphenol A type epoxy resin is substituted into bisphenol-f type
Prepared by epoxy resin, its preparation method are identical with embodiment 5.
Comparative example 2
Component is on the basis of embodiment 5 used by this comparative example, deletes this component of Korean pine extract solution and obtains
, its preparation method is identical with embodiment 5.
Comparative example 3
Component is on the basis of embodiment 5 used by this comparative example, and bisphenol A type epoxy resin is substituted into bisphenol-f type
Epoxy resin, while also obtained from this component of deletion Korean pine extract solution, its preparation method is identical with embodiment 5.
The comparison of packaging plastic performance
The measure of following performance, the result measured are carried out to packaging plastic made from above-described embodiment 1~5 and comparative example 1~3
As shown in table 1.
1st, viscosity is to test to obtain using NDJ-5 type rotation viscometers；
2nd, gelation time is to test to obtain on gelation time tester using 1g liquid resin compositions；
3rd, bending strength is determined according to GB/T9341-2000；
4th, water absorption rate is that wafer sample is boiled to the water absorption rate after 8h in 100 DEG C of boiling water, the front and rear quality point of record immersion
Not Wei M1 and M2, be calculated according to formula (M2-M1)/M1 × 100%；
5th, shore hardness is determined according to GB/T2411-2008；
6th, refractive index is determined according to GB/T6488-2008；
7th, translucency is determined according to GB/T2410-2008；
8th, glass transition temperature be by the packaging plastic after curing molding 120~130 DEG C carry out 4~16 hours after
Solidification, then use DSC to be measured under air atmosphere between 30~200 DEG C with 20 DEG C/min speed secondary temperature elevation；
9th, solidification thermal decomposition temperature is that the packaging plastic after curing molding is carried out into 4~16 hours at 120~130 DEG C
Solidify afterwards, then use DSC to be measured under air atmosphere between 30~600 DEG C with 20 DEG C/min speed secondary temperature elevation.
The performance of the embodiment 1~5 of table 1 and the gained packaging plastic of comparative example 1~3
As can be known from the above table：The present invention is changed using bisphenol f type epoxy resin and phenol aldehyde modified organic siliconresin as host with polyethers
Property polysiloxanes is defoamer, using adipic dihydrazide as curing agent, using single benzoic acid resorcinol as ultra-violet absorber,
With 4- benzoyloxys -2,2,6,6- tetramethyl piperidines are light stabilizer, by mixing the Korean pine with high temperature resistant, corrosion resistance
Extract solution, cured reaction obtain the epoxy encapsulation glue that a kind of high temperature resistant, ultraviolet light resistant, translucency are good, refractive index is high,
The preparation technology of the packaging plastic is simple, and cost is low, and glass transition temperature and heat decomposition temperature are high after material solidification, caking property
Can be strong, it can be widely applied to high power LED package field of material technology.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that those skilled in the art should for clarity
Using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
It is appreciated that other embodiment.
Claims (6)
1. high power LED package epoxy encapsulation glue, it is two-component system, it is characterised in that according to mass percent meter,
It is made up of component A 42~47% and B component 53~58%；Described component A is according to mass percent meter, by bisphenol F type epoxy
Resin 19.85~80%, phenol aldehyde modified organic siliconresin 19.85~80% and Siloxane-Oxyalkylene Copolymers 0.15~0.25% are made
Into described B component is according to mass percent meter, by Korean pine extract solution 14~27%, adipic dihydrazide 72~85%, single benzene
Formic acid resorcinol 0.4~1.0% and 4 benzoyloxy 2,2,6,6 tetramethyl piperidine 0.6~1.2% are made；It is described
Korean pine extract solution preparation method, comprise the following steps：
1) Korean pine root or stem are cleaned, smashed, crossed 40~80 mesh sieves, obtain coarse powder；
2) ethanol solution for being 75~88% toward the volumetric concentrations of 5~6 times of amounts of addition meal quality in coarse powder, immersion 12~18
Hour, it is then heated to boiling reflux 3~5 hours, filters, use percolation slowly to be oozed with 1~1.5ml per minute speed
Filter, collect percolate as liquid of just filtering, separately deposit；
3) volumetric concentration for continuing to add 4~5 times of amounts of meal quality in the coarse powder after post-processing toward step (2) is 75~88%
Ethanol solution, be heated to boiling reflux 2~3 hours, filter, use percolation slowly to be oozed with 1.5~2ml per minute speed
Filter, collect percolate to continue liquid of filtering, under 0.07~0.08MPa of vacuum, the liquid that continuous will filter is concentrated under reduced pressure into relatively close at 55 DEG C
Spend the lotion for 1.18~1.20；
4) lotion of step 3) is turned to be dissolved in the first liquid of filtering of step 2), obtains Korean pine extract solution.
2. high power LED package according to claim 1 epoxy encapsulation glue, it is characterised in that according to quality hundred
Divide than meter, be made up of component A 44~45% and B component 55~56%；Described component A is according to mass percent meter, by Bisphenol F
Type epoxy resin 45~55%, phenol aldehyde modified organic siliconresin 40~50% and Siloxane-Oxyalkylene Copolymers 0.15~0.22% are made
Into described B component is according to mass percent meter, by Korean pine extract solution 17~23%, adipic dihydrazide 76~82%, single benzene
Formic acid resorcinol 0.4~0.8% and 4- benzoyloxys -2,2,6,6- tetramethyl piperidines 0.6~0.9% are made, above-mentioned
The percentage composition sum of material each component is 100%.
3. high power LED package according to claim 1 epoxy encapsulation glue, it is characterised in that according to quality hundred
Divide than meter, be made up of component A 44.4% and B component 55.6%；Described component A is according to mass percent meter, by Bisphenol F type ring
Oxygen tree fat 52.8%, phenol aldehyde modified organic siliconresin 47.02% and Siloxane-Oxyalkylene Copolymers 0.18% are made, described B groups
Divide according to mass percent meter, by Korean pine extract solution 18.5%, adipic dihydrazide 80%, single benzoic acid resorcinol
0.7% and 4 benzoyloxy 2,2,6,6 tetramethyl piperidine 0.8% be made.
4. high power LED package according to claim 1 epoxy encapsulation glue, it is characterised in that described Korean pine
The solid-liquid ratio of extract solution is 1：3~5.
5. according to the preparation method of any described high power LED package epoxy encapsulation glue of Claims 1 to 4, it is special
Sign is, comprises the following steps：
(1) preparation of component A：Bisphenol f type epoxy resin, phenol aldehyde modified organic siliconresin and polyether-modified poly- silicon are weighed in proportion
Oxygen alkane, stirred 1~2.5 hour at 90~115 DEG C, be well mixed, pack and produce component A；
(2) preparation of B component：Weigh in proportion Korean pine extract solution, adipic dihydrazide, single benzoic acid resorcinol and
4- benzoyloxys -2,2,6,6- tetramethyl piperidines, stir 2~3 hours, be well mixed, packaging is at 88~95 DEG C
Obtain B component；
(3) above-mentioned steps (1)~component A made from (2) and B component are well mixed according to the proportioning of above-mentioned mass percent
Solidified, condition of cure is：Solidify 1~1.2 hour in 90~135 DEG C, solidify 3~5 hours then at 110~142 DEG C, produce
High power LED package epoxy encapsulation glue.
6. according to any described epoxy encapsulation glue of Claims 1 to 4 in terms of high power LED package material is prepared
Purposes.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510884805.1A CN105368363B (en) | 2015-12-01 | 2015-12-01 | High power LED package epoxy encapsulation glue as well as preparation method and application thereof |
| CN201710872087.5A CN107603546A (en) | 2015-12-01 | 2015-12-01 | High power LED package epoxy encapsulation glue as well as preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510884805.1A CN105368363B (en) | 2015-12-01 | 2015-12-01 | High power LED package epoxy encapsulation glue as well as preparation method and application thereof |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201710872087.5A Division CN107603546A (en) | 2015-12-01 | 2015-12-01 | High power LED package epoxy encapsulation glue as well as preparation method and application thereof |
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| CN105368363A CN105368363A (en) | 2016-03-02 |
| CN105368363B true CN105368363B (en) | 2017-12-26 |
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| CN201710872087.5A Withdrawn CN107603546A (en) | 2015-12-01 | 2015-12-01 | High power LED package epoxy encapsulation glue as well as preparation method and application thereof |
| CN201510884805.1A Expired - Fee Related CN105368363B (en) | 2015-12-01 | 2015-12-01 | High power LED package epoxy encapsulation glue as well as preparation method and application thereof |
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| CN201710872087.5A Withdrawn CN107603546A (en) | 2015-12-01 | 2015-12-01 | High power LED package epoxy encapsulation glue as well as preparation method and application thereof |
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| CN108410406A (en) * | 2018-03-12 | 2018-08-17 | 常州五荣化工有限公司 | A kind of preparation method of modified epoxy casting glue |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102618195A (en) * | 2012-01-21 | 2012-08-01 | 金安国纪科技股份有限公司 | Light shading adhesive, laminated plate, preparation method of light shading adhesive, and application of light shading adhesive |
| CN102634313A (en) * | 2012-04-23 | 2012-08-15 | 广州市白云化工实业有限公司 | Epoxy conductive resin applicable to binding of LED (light-emitting diode) chips, and preparation method thereof |
| JP5402955B2 (en) * | 2011-02-01 | 2014-01-29 | 三菱化学株式会社 | Hydrogenated epoxy resin, method for producing the same, and epoxy resin composition |
-
2015
- 2015-12-01 CN CN201710872087.5A patent/CN107603546A/en not_active Withdrawn
- 2015-12-01 CN CN201510884805.1A patent/CN105368363B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5402955B2 (en) * | 2011-02-01 | 2014-01-29 | 三菱化学株式会社 | Hydrogenated epoxy resin, method for producing the same, and epoxy resin composition |
| CN102618195A (en) * | 2012-01-21 | 2012-08-01 | 金安国纪科技股份有限公司 | Light shading adhesive, laminated plate, preparation method of light shading adhesive, and application of light shading adhesive |
| CN102634313A (en) * | 2012-04-23 | 2012-08-15 | 广州市白云化工实业有限公司 | Epoxy conductive resin applicable to binding of LED (light-emitting diode) chips, and preparation method thereof |
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|---|---|
| CN107603546A (en) | 2018-01-19 |
| CN105368363A (en) | 2016-03-02 |
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