CN105368363A - Epoxy encapsulation adhesive for high power LED encapsulation and preparation method for epoxy encapsulation adhesive and use of epoxy encapsulation adhesive - Google Patents
Epoxy encapsulation adhesive for high power LED encapsulation and preparation method for epoxy encapsulation adhesive and use of epoxy encapsulation adhesive Download PDFInfo
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Abstract
The present invention discloses an epoxy encapsulation adhesive for high power LED encapsulation and a preparation method for an epoxy encapsulation adhesive and use of the epoxy encapsulation adhesive. The encapsulation adhesive consists of 42-47% of a component A and 53-58% of a component B by mass percentage. The component A is prepared from 19.85-80% of bisphenol F epoxy resin, 19.85-80% of phenolic aldehyde modified organosilicone resin and 0.15-0.25% of polyether modified polysiloxane by mass percentage, and the component B is prepared from 14-27% of a Korean pine extraction liquid, 72-85% of adipic dihydrazide, 0.4-1.0% of resorcinol monobenzoate and 0.6-1.2% of 4-benzoyloxyl-2,2,6,6-tetramethylpiperidine by mass percentage. The encapsulation adhesive disclosed by the present invention is resistant to high temperature, resistant to ultraviolet radiation, good in light transmittance, high in refractive index, simple in process and low in cost, so that the encapsulation adhesive can be widely applied to the high power LED encapsulation field.
Description
Technical field
The present invention relates to LED technology field, specifically a kind of high power LED package epoxy encapsulation glue and preparation method thereof and purposes.
Background technology
LED illumination is widely used in the fields such as display screen, Landscape Lighting, special lighting as " green illumination ", and along with LED light source technology reaches its maturity, every watt of luminescent lumen increases rapidly, impels its price reduction of successively decreasing year by year.Look forward to the future, LED general illumination becomes the industrial hot spot of most market potential, and thus encapsulation problem that is high-power, high-brightness white-light LED also becomes increasingly conspicuous.
Common LED liquid epoxy material viscosity high (more than viscosity at room temperature 10000cps), second-order transition temperature low (about 110 DEG C), be difficult to the requirement meeting large power white light LED.Large power white light LED requires that potting resin has good mobility, higher second-order transition temperature, also requires the characteristics such as white light high light transmittance, fire-retardant, uvioresistant, solidification physical strength are high simultaneously.
The packaged material of common LED mainly bisphenol A-type transparent epoxy resin on market, power type LED encapsulation material market then depends on import, it is compared with domestic packaged material, there is better heat-resisting and UV resistant performance, higher specific refractory power and the lower coefficient of expansion etc., if the product of international three large silica gel enterprise DOW CORNINGs, figure advanced in years, SHIN-ETSU HANTOTAI is based on high refractive index organosilicon encapsulating material, high-end encapsulation market at home has absolute predominance.Certain recent year has also emerged in large numbers Shuande ACR, Changsha blue star, sky, Jiangyin magnitude manufacturing enterprise, but substantially maintain the production of low power encapsulating compound, output is also less, thus develops high-grade encapsulating products to promoting that the popularization of domestic power-type LED is significant.
Conventional epoxies can not meet the encapsulation requirement of LED completely, and silicone resin price is very high, and abroad monopolized, therefore prepare high temperature resistant and adhesive property is strong, dielectric properties are strong and the packaged material being applied to great power LED that ultraviolet light resistant, light transmission are good is very urgent.
Summary of the invention
The object of the present invention is to provide a kind of low cost, low viscosity, bounding force strong, resistant to elevated temperatures high power LED package epoxy encapsulation glue and preparation method thereof and purposes.
For achieving the above object, the invention provides following technical scheme:
High power LED package epoxy encapsulation glue is two Component System, according to mass percent, is made up of component A 42 ~ 47% and B component 53 ~ 58%; Described component A is according to mass percent, be made up of bisphenol f type epoxy resin 19.85 ~ 80%, phenol aldehyde modified silicone resin 19.85 ~ 80% and Siloxane-Oxyalkylene Copolymers 0.15 ~ 0.25%, described B component is according to mass percent, by Korean pine extracting solution 14 ~ 27%, adipic dihydrazide 72 ~ 85%, single phenylformic acid resorcinol 0.4 ~ 1.0% and 4-benzoyloxy-2,2,6,6-tetramethyl piperidine 0.6 ~ 1.2% is made; The preparation method of described Korean pine extracting solution, comprises the following steps:
1) Korean pine root or stem are cleaned, shatter, cross 40 ~ 80 mesh sieves, obtain meal;
2) volumetric concentration adding 5 ~ 6 times amount of meal quality in meal is the ethanolic soln of 75 ~ 88%, soak 12 ~ 18 hours, then boiling reflux is heated to 3 ~ 5 hours, filter, adopt percolation with the speed of per minute 1 ~ 1.5ml slowly diacolation, collect percolate for liquid of just filtering, separately deposit;
3) volumetric concentration continuing to add in meal 4 ~ 5 times amount of meal quality is the ethanolic soln of 75 ~ 88%, be heated to boiling reflux 2 ~ 3 hours, filter, adopt percolation with the speed of per minute 1.5 ~ 2ml slowly diacolation, collect percolate for continuous liquid of filtering, under vacuum tightness 0.07 ~ 0.08MPa, when continuous liquid of filtering being evaporated to 55 DEG C, relative density is the lotion of 1.18 ~ 1.20;
4) by step 3) lotion turn be dissolved in step 2) just filter in liquid, obtain Korean pine extracting solution.
As the further scheme of the present invention: according to mass percent, be made up of component A 44 ~ 45% and B component 55 ~ 56%; Described component A is according to mass percent, be made up of bisphenol f type epoxy resin 45 ~ 55%, phenol aldehyde modified silicone resin 40 ~ 50% and Siloxane-Oxyalkylene Copolymers 0.15 ~ 0.22%, described B component is according to mass percent, by Korean pine extracting solution 17 ~ 23%, adipic dihydrazide 76 ~ 82%, single phenylformic acid resorcinol 0.4 ~ 0.8% and 4-benzoyloxy-2,2,6,6-tetramethyl piperidine 0.6 ~ 0.9% is made.
As the further scheme of the present invention: according to mass percent, be made up of component A 44.4% and B component 55.6%; Described component A is according to mass percent, be made up of bisphenol f type epoxy resin 52.8%, phenol aldehyde modified silicone resin 47.02% and Siloxane-Oxyalkylene Copolymers 0.18%, described B component is according to mass percent, by Korean pine extracting solution 18.5%, adipic dihydrazide 80%, single phenylformic acid resorcinol 0.7% and 4-benzoyloxy-2,2,6,6-tetramethyl piperidine 0.8% is made.
As the further scheme of the present invention: the solid-liquid ratio of described Korean pine extracting solution is 1:3 ~ 5.
The preparation method of described high power LED package epoxy encapsulation glue, comprises the following steps:
(1) preparation of component A: take bisphenol f type epoxy resin, phenol aldehyde modified silicone resin and Siloxane-Oxyalkylene Copolymers in proportion, stirs 1 ~ 2.5 hour, mixes, pack and obtain component A at 90 ~ 115 DEG C;
(2) preparation of B component: take Korean pine extracting solution, adipic dihydrazide, single phenylformic acid resorcinol and 4-benzoyloxy-2,2,6,6-tetramethyl piperidine in proportion, stirs 2 ~ 3 hours, mixes, pack and obtain B component at 88 ~ 95 DEG C;
(3) by component A obtained for above-mentioned steps (1) ~ (2) and the B component proportioning according to above-mentioned mass percent, mix and be cured, condition of cure was: in 90 ~ 135 DEG C of solidifications 1 ~ 1.2 hour, again in 110 ~ 142 DEG C of solidifications 3 ~ 5 hours, obtain high power LED package epoxy encapsulation glue.
The purposes in high power LED package material prepared by described epoxy encapsulation glue.
Compared with prior art, the invention has the beneficial effects as follows: the present invention with bisphenol f type epoxy resin and phenol aldehyde modified silicone resin for host, take Siloxane-Oxyalkylene Copolymers as defoamer, take adipic dihydrazide as solidifying agent, with single phenylformic acid resorcinol for UV light absorber, with 4-benzoyloxy-2, 2, 6, 6-tetramethyl piperidine is photostabilizer, by mix have high temperature resistant, the Korean pine extracting solution of erosion resistance, obtain a kind of high temperature resistant through curing reaction, ultraviolet light resistant, light transmission is good, the epoxy encapsulation glue that specific refractory power is high, the preparation technology of this packaging plastic is simple, cost is low, and after material cured second-order transition temperature and heat decomposition temperature high, adhesive property is strong, high power LED package field of material technology can be widely used in.
Embodiment
Below in conjunction with the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, high power LED package epoxy encapsulation glue is two Component System, according to mass percent, is made up of component A 47% and B component 53%; Described component A is according to mass percent, be made up of bisphenol f type epoxy resin 19.85%, phenol aldehyde modified silicone resin 80% and Siloxane-Oxyalkylene Copolymers 0.15%, described B component is according to mass percent, by Korean pine extracting solution 14%, adipic dihydrazide 85%, single phenylformic acid resorcinol 0.4% and 4-benzoyloxy-2,2,6,6-tetramethyl piperidine 0.6% is made; The preparation method of described Korean pine extracting solution, comprises the following steps:
1) Korean pine root or stem are cleaned, shatter, cross 40 mesh sieves, obtain meal;
2) volumetric concentration adding 5 times amount of meal quality in meal is the ethanolic soln of 88%, soaks 12 hours, is then heated to boiling reflux 3 hours, filter, adopt percolation with the speed of per minute 1.5ml slowly diacolation, collect percolate for liquid of just filtering, separately deposit;
3) volumetric concentration continuing to add in meal 4 times amount of meal quality is the ethanolic soln of 88%, be heated to boiling reflux 2 hours, filter, adopt percolation with the speed of per minute 2ml slowly diacolation, collect percolate for continuous liquid of filtering, under vacuum tightness 0.07MPa, when continuous liquid of filtering being evaporated to 55 DEG C, relative density is the lotion of 1.20;
4) by step 3) lotion turn be dissolved in step 2) just filter in liquid, obtain the Korean pine extracting solution of solid-liquid ratio 1:3.
The preparation method of described high power LED package epoxy encapsulation glue, comprises the following steps:
(1) preparation of component A: take bisphenol f type epoxy resin, phenol aldehyde modified silicone resin and Siloxane-Oxyalkylene Copolymers in proportion, stirs 2.5 hours, mixes, pack and obtain component A at 90 DEG C;
(2) preparation of B component: take Korean pine extracting solution, adipic dihydrazide, single phenylformic acid resorcinol and 4-benzoyloxy-2,2,6,6-tetramethyl piperidine in proportion, stirs 2 hours, mixes, pack and obtain B component at 95 DEG C;
(3) by component A obtained for above-mentioned steps (1) ~ (2) and the B component proportioning according to above-mentioned mass percent, mix and be cured, condition of cure was: in 90 DEG C of solidifications 1.2 hours, again in 110 DEG C of solidifications 5 hours, obtain high power LED package epoxy encapsulation glue.
Embodiment 2
In the embodiment of the present invention, high power LED package epoxy encapsulation glue is two Component System, according to mass percent, is made up of component A 42% and B component 58%; Described component A is according to mass percent, be made up of bisphenol f type epoxy resin 80%, phenol aldehyde modified silicone resin 19.85% and Siloxane-Oxyalkylene Copolymers 0.15%, described B component is according to mass percent, by Korean pine extracting solution 27%, adipic dihydrazide 72%, single phenylformic acid resorcinol 0.4% and 4-benzoyloxy-2,2,6,6-tetramethyl piperidine 0.6% is made; The preparation method of described Korean pine extracting solution, comprises the following steps:
1) Korean pine root or stem are cleaned, shatter, cross 40 mesh sieves, obtain meal;
2) volumetric concentration adding 5 times amount of meal quality in meal is the ethanolic soln of 88%, soaks 12 hours, is then heated to boiling reflux 3 hours, filter, adopt percolation with the speed of per minute 1.5ml slowly diacolation, collect percolate for liquid of just filtering, separately deposit;
3) volumetric concentration continuing to add in meal 4 times amount of meal quality is the ethanolic soln of 88%, be heated to boiling reflux 2 hours, filter, adopt percolation with the speed of per minute 2ml slowly diacolation, collect percolate for continuous liquid of filtering, under vacuum tightness 0.07MPa, when continuous liquid of filtering being evaporated to 55 DEG C, relative density is the lotion of 1.20;
4) by step 3) lotion turn be dissolved in step 2) just filter in liquid, obtain the Korean pine extracting solution of solid-liquid ratio 1:3.
The preparation method of described high power LED package epoxy encapsulation glue, comprises the following steps:
(1) preparation of component A: take bisphenol f type epoxy resin, phenol aldehyde modified silicone resin and Siloxane-Oxyalkylene Copolymers in proportion, stirs 2.5 hours, mixes, pack and obtain component A at 90 DEG C;
(2) preparation of B component: take Korean pine extracting solution, adipic dihydrazide, single phenylformic acid resorcinol and 4-benzoyloxy-2,2,6,6-tetramethyl piperidine in proportion, stirs 2 hours, mixes, pack and obtain B component at 95 DEG C;
(3) by component A obtained for above-mentioned steps (1) ~ (2) and the B component proportioning according to above-mentioned mass percent, mix and be cured, condition of cure was: in 90 DEG C of solidifications 1.2 hours, again in 110 DEG C of solidifications 5 hours, obtain high power LED package epoxy encapsulation glue.
Embodiment 3
In the embodiment of the present invention, high power LED package epoxy encapsulation glue is two Component System, according to mass percent, is made up of component A 43.8% and B component 56.2%; Described component A is according to mass percent, be made up of bisphenol f type epoxy resin 45%, phenol aldehyde modified silicone resin 54.75% and Siloxane-Oxyalkylene Copolymers 0.25%, described B component is according to mass percent, by Korean pine extracting solution 20%, adipic dihydrazide 78%, single phenylformic acid resorcinol 1.0% and 4-benzoyloxy-2,2,6,6-tetramethyl piperidine 1.0% is made; The preparation method of described Korean pine extracting solution, comprises the following steps:
1) Korean pine root or stem are cleaned, shatter, cross 80 mesh sieves, obtain meal;
2) volumetric concentration adding 6 times amount of meal quality in meal is the ethanolic soln of 75%, soaks 18 hours, is then heated to boiling reflux 5 hours, filter, adopt percolation with the speed of per minute 1ml slowly diacolation, collect percolate for liquid of just filtering, separately deposit;
3) volumetric concentration continuing to add in meal 5 times amount of meal quality is the ethanolic soln of 75%, be heated to boiling reflux 3 hours, filter, adopt percolation with the speed of per minute 1.5ml slowly diacolation, collect percolate for continuous liquid of filtering, under vacuum tightness 0.08MPa, when continuous liquid of filtering being evaporated to 55 DEG C, relative density is the lotion of 1.18;
4) by step 3) lotion turn be dissolved in step 2) just filter in liquid, obtain the Korean pine extracting solution of solid-liquid ratio 1:5.
The preparation method of described high power LED package epoxy encapsulation glue, comprises the following steps:
(1) preparation of component A: take bisphenol f type epoxy resin, phenol aldehyde modified silicone resin and Siloxane-Oxyalkylene Copolymers in proportion, stirs 1 hour, mixes, pack and obtain component A at 115 DEG C;
(2) preparation of B component: take Korean pine extracting solution, adipic dihydrazide, single phenylformic acid resorcinol and 4-benzoyloxy-2,2,6,6-tetramethyl piperidine in proportion, stirs 3 hours, mixes, pack and obtain B component at 88 DEG C;
(3) by component A obtained for above-mentioned steps (1) ~ (2) and the B component proportioning according to above-mentioned mass percent, mix and be cured, condition of cure was: in 135 DEG C of solidifications 1 hour, again in 142 DEG C of solidifications 3 hours, obtain high power LED package epoxy encapsulation glue.
Embodiment 4
In the embodiment of the present invention, high power LED package epoxy encapsulation glue is two Component System, according to mass percent, is made up of component A 43.8% and B component 56.2%; Described component A is according to mass percent, be made up of bisphenol f type epoxy resin 54.75%, phenol aldehyde modified silicone resin 45% and Siloxane-Oxyalkylene Copolymers 0.25%, described B component is according to mass percent, by Korean pine extracting solution 20%, adipic dihydrazide 78%, single phenylformic acid resorcinol 0.8% and 4-benzoyloxy-2,2,6,6-tetramethyl piperidine 1.2% is made; The preparation method of described Korean pine extracting solution, comprises the following steps:
1) Korean pine root or stem are cleaned, shatter, cross 80 mesh sieves, obtain meal;
2) volumetric concentration adding 6 times amount of meal quality in meal is the ethanolic soln of 75%, soaks 18 hours, is then heated to boiling reflux 5 hours, filter, adopt percolation with the speed of per minute 1ml slowly diacolation, collect percolate for liquid of just filtering, separately deposit;
3) volumetric concentration continuing to add in meal 5 times amount of meal quality is the ethanolic soln of 75%, be heated to boiling reflux 3 hours, filter, adopt percolation with the speed of per minute 1.5ml slowly diacolation, collect percolate for continuous liquid of filtering, under vacuum tightness 0.08MPa, when continuous liquid of filtering being evaporated to 55 DEG C, relative density is the lotion of 1.18;
4) by step 3) lotion turn be dissolved in step 2) just filter in liquid, obtain the Korean pine extracting solution of solid-liquid ratio 1:5.
The preparation method of described high power LED package epoxy encapsulation glue, comprises the following steps:
(1) preparation of component A: take bisphenol f type epoxy resin, phenol aldehyde modified silicone resin and Siloxane-Oxyalkylene Copolymers in proportion, stirs 1 hour, mixes, pack and obtain component A at 115 DEG C;
(2) preparation of B component: take Korean pine extracting solution, adipic dihydrazide, single phenylformic acid resorcinol and 4-benzoyloxy-2,2,6,6-tetramethyl piperidine in proportion, stirs 3 hours, mixes, pack and obtain B component at 88 DEG C;
(3) by component A obtained for above-mentioned steps (1) ~ (2) and the B component proportioning according to above-mentioned mass percent, mix and be cured, condition of cure was: in 135 DEG C of solidifications 1 hour, again in 142 DEG C of solidifications 3 hours, obtain high power LED package epoxy encapsulation glue.
Embodiment 5
In the embodiment of the present invention, high power LED package epoxy encapsulation glue, according to mass percent, is made up of component A 44.4% and B component 55.6%; Described component A is according to mass percent, be made up of bisphenol f type epoxy resin 52.8%, phenol aldehyde modified silicone resin 47.02% and Siloxane-Oxyalkylene Copolymers 0.18%, described B component is according to mass percent, by Korean pine extracting solution 18.5%, adipic dihydrazide 80%, single phenylformic acid resorcinol 0.7% and 4-benzoyloxy-2,2,6,6-tetramethyl piperidine 0.8% is made; The preparation method of described Korean pine extracting solution, comprises the following steps:
1) Korean pine root or stem are cleaned, shatter, cross 40 ~ 80 mesh sieves, obtain meal;
2) volumetric concentration adding 6 times amount of meal quality in meal is the ethanolic soln of 88%, soaks 18 hours, is then heated to boiling reflux 5 hours, filter, adopt percolation with the speed of per minute 1ml slowly diacolation, collect percolate for liquid of just filtering, separately deposit;
3) volumetric concentration continuing to add in meal 5 times amount of meal quality is the ethanolic soln of 88%, be heated to boiling reflux 3 hours, filter, adopt percolation with the speed of per minute 1.5ml slowly diacolation, collect percolate for continuous liquid of filtering, under vacuum tightness 0.07MPa, when continuous liquid of filtering being evaporated to 55 DEG C, relative density is the lotion of 1.20;
4) by step 3) lotion turn be dissolved in step 2) just filter in liquid, obtain the Korean pine extracting solution of solid-liquid ratio 1:4.
The preparation method of described high power LED package epoxy encapsulation glue, comprises the following steps:
(1) preparation of component A: take bisphenol f type epoxy resin, phenol aldehyde modified silicone resin and Siloxane-Oxyalkylene Copolymers in proportion, stirs 2.5 hours, mixes, pack and obtain component A at 110 DEG C;
(2) preparation of B component: take Korean pine extracting solution, adipic dihydrazide, single phenylformic acid resorcinol and 4-benzoyloxy-2,2,6,6-tetramethyl piperidine in proportion, stirs 3 hours, mixes, pack and obtain B component at 92 DEG C;
(3) by component A obtained for above-mentioned steps (1) ~ (2) and the B component proportioning according to above-mentioned mass percent, mix and be cured, condition of cure was: in 105 DEG C of solidifications 1.2 hours, again in 130 DEG C of solidifications 5 hours, obtain high power LED package epoxy encapsulation glue.
Comparative example 1
The component that this comparative example adopts is on the basis of embodiment 5, bisphenol A type epoxy resin is replaced bisphenol f type epoxy resin and obtained, and its preparation method is identical with embodiment 5.
Comparative example 2
The component that this comparative example adopts is on the basis of embodiment 5, and delete this component of Korean pine extracting solution and obtain, its preparation method is identical with embodiment 5.
Comparative example 3
The component that this comparative example adopts is on the basis of embodiment 5, and bisphenol A type epoxy resin is replaced bisphenol f type epoxy resin, and also delete this component of Korean pine extracting solution simultaneously and obtain, its preparation method is identical with embodiment 5.
The comparison of packaging plastic performance
Above-described embodiment 1 ~ 5 and the obtained packaging plastic of comparative example 1 ~ 3 are carried out to the mensuration of following performance, the result recorded is as shown in table 1.
1, viscosity adopts the test of NDJ-5 type rotational viscosimeter to obtain;
2, gelation time adopts 1g liquid resin composition to test on gelation time tester to obtain;
3, flexural strength measures according to GB/T9341-2000;
4, water-intake rate is the water-intake rate after wafer sample is boiled 8h in 100 DEG C of boiling water, and the quality before and after record soaks is respectively M1 and M2, calculates according to formula (M2-M1)/M1 × 100%;
5, shore hardness measures according to GB/T2411-2008;
6, specific refractory power measures according to GB/T6488-2008;
7, light transmission measures according to GB/T2410-2008;
8, second-order transition temperature be by curing molding after packaging plastic carry out the after fixing of 4 ~ 16 hours at 120 ~ 130 DEG C, then adopt DSC to record with the speed secondary temperature elevation of 20 DEG C/min between 30 ~ 200 DEG C under air atmosphere;
9, solidify thermal decomposition temperature be by curing molding after packaging plastic carry out the after fixing of 4 ~ 16 hours at 120 ~ 130 DEG C, then adopt DSC to record with the speed secondary temperature elevation of 20 DEG C/min between 30 ~ 600 DEG C under air atmosphere.
The performance of table 1 embodiment 1 ~ 5 and comparative example 1 ~ 3 gained packaging plastic
As can be known from the above table: the present invention with bisphenol f type epoxy resin and phenol aldehyde modified silicone resin for host, take Siloxane-Oxyalkylene Copolymers as defoamer, take adipic dihydrazide as solidifying agent, with single phenylformic acid resorcinol for UV light absorber, with 4-benzoyloxy-2, 2, 6, 6-tetramethyl piperidine is photostabilizer, by mix have high temperature resistant, the Korean pine extracting solution of erosion resistance, obtain a kind of high temperature resistant through curing reaction, ultraviolet light resistant, light transmission is good, the epoxy encapsulation glue that specific refractory power is high, the preparation technology of this packaging plastic is simple, cost is low, and after material cured second-order transition temperature and heat decomposition temperature high, adhesive property is strong, high power LED package field of material technology can be widely used in.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.
In addition, be to be understood that, although this specification sheets is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should by specification sheets integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
Claims (6)
1. high power LED package epoxy encapsulation glue, is two Component System, it is characterized in that, according to mass percent, is made up of component A 42 ~ 47% and B component 53 ~ 58%; Described component A is according to mass percent, be made up of bisphenol f type epoxy resin 19.85 ~ 80%, phenol aldehyde modified silicone resin 19.85 ~ 80% and Siloxane-Oxyalkylene Copolymers 0.15 ~ 0.25%, described B component is according to mass percent, by Korean pine extracting solution 14 ~ 27%, adipic dihydrazide 72 ~ 85%, single phenylformic acid resorcinol 0.4 ~ 1.0% and 4-benzoyloxy-2,2,6,6-tetramethyl piperidine 0.6 ~ 1.2% is made; The preparation method of described Korean pine extracting solution, comprises the following steps:
1) Korean pine root or stem are cleaned, shatter, cross 40 ~ 80 mesh sieves, obtain meal;
2) volumetric concentration adding 5 ~ 6 times amount of meal quality in meal is the ethanolic soln of 75 ~ 88%, soak 12 ~ 18 hours, then boiling reflux is heated to 3 ~ 5 hours, filter, adopt percolation with the speed of per minute 1 ~ 1.5ml slowly diacolation, collect percolate for liquid of just filtering, separately deposit;
3) volumetric concentration continuing to add in meal 4 ~ 5 times amount of meal quality is the ethanolic soln of 75 ~ 88%, be heated to boiling reflux 2 ~ 3 hours, filter, adopt percolation with the speed of per minute 1.5 ~ 2ml slowly diacolation, collect percolate for continuous liquid of filtering, under vacuum tightness 0.07 ~ 0.08MPa, when continuous liquid of filtering being evaporated to 55 DEG C, relative density is the lotion of 1.18 ~ 1.20;
4) by step 3) lotion turn be dissolved in step 2) just filter in liquid, obtain Korean pine extracting solution.
2. high power LED package epoxy encapsulation glue according to claim 1, is characterized in that, according to mass percent, is made up of component A 44 ~ 45% and B component 55 ~ 56%; Described component A is according to mass percent, be made up of bisphenol f type epoxy resin 45 ~ 55%, phenol aldehyde modified silicone resin 40 ~ 50% and Siloxane-Oxyalkylene Copolymers 0.15 ~ 0.22%, described B component is according to mass percent, by Korean pine extracting solution 17 ~ 23%, adipic dihydrazide 76 ~ 82%, single phenylformic acid resorcinol 0.4 ~ 0.8% and 4-benzoyloxy-2,2,6,6-tetramethyl piperidine 0.6 ~ 0.9% is made.
3. high power LED package epoxy encapsulation glue according to claim 1, is characterized in that, according to mass percent, is made up of component A 44.4% and B component 55.6%; Described component A is according to mass percent, be made up of bisphenol f type epoxy resin 52.8%, phenol aldehyde modified silicone resin 47.02% and Siloxane-Oxyalkylene Copolymers 0.18%, described B component is according to mass percent, by Korean pine extracting solution 18.5%, adipic dihydrazide 80%, single phenylformic acid resorcinol 0.7% and 4-benzoyloxy-2,2,6,6-tetramethyl piperidine 0.8% is made.
4. high power LED package epoxy encapsulation glue according to claim 1, is characterized in that, the solid-liquid ratio of described Korean pine extracting solution is 1:3 ~ 5.
5., according to the preparation method of the arbitrary described high power LED package epoxy encapsulation glue of Claims 1 to 4, it is characterized in that, comprise the following steps:
(1) preparation of component A: take bisphenol f type epoxy resin, phenol aldehyde modified silicone resin and Siloxane-Oxyalkylene Copolymers in proportion, stirs 1 ~ 2.5 hour, mixes, pack and obtain component A at 90 ~ 115 DEG C;
(2) preparation of B component: take Korean pine extracting solution, adipic dihydrazide, single phenylformic acid resorcinol and 4-benzoyloxy-2,2,6,6-tetramethyl piperidine in proportion, stirs 2 ~ 3 hours, mixes, pack and obtain B component at 88 ~ 95 DEG C;
(3) by component A obtained for above-mentioned steps (1) ~ (2) and the B component proportioning according to above-mentioned mass percent, mix and be cured, condition of cure was: in 90 ~ 135 DEG C of solidifications 1 ~ 1.2 hour, again in 110 ~ 142 DEG C of solidifications 3 ~ 5 hours, obtain high power LED package epoxy encapsulation glue.
6. preparing the purposes in high power LED package material according to the arbitrary described epoxy encapsulation glue of Claims 1 to 4.
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| Application Number | Priority Date | Filing Date | Title |
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| 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 |
| 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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| 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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| 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 true CN105368363A (en) | 2016-03-02 |
| CN105368363B CN105368363B (en) | 2017-12-26 |
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| 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 |
| 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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| 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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| 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 CN201510884805.1A patent/CN105368363B/en not_active Expired - Fee Related
- 2015-12-01 CN CN201710872087.5A patent/CN107603546A/en not_active Withdrawn
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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| CN105368363B (en) | 2017-12-26 |
| CN107603546A (en) | 2018-01-19 |
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