CN105199079B - A kind of reflective composition epoxy resin of LED support high strength white - Google Patents
A kind of reflective composition epoxy resin of LED support high strength white Download PDFInfo
- Publication number
- CN105199079B CN105199079B CN201510724283.9A CN201510724283A CN105199079B CN 105199079 B CN105199079 B CN 105199079B CN 201510724283 A CN201510724283 A CN 201510724283A CN 105199079 B CN105199079 B CN 105199079B
- Authority
- CN
- China
- Prior art keywords
- epoxy resin
- curing agent
- composition epoxy
- composition
- weight
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
Abstract
A kind of reflective composition epoxy resin of LED support high strength white, main component include: epoxy resin, anhydride or acids curing agent, curing agent promotor and colorant and toughener.Epoxy resin is selected from the siloxanes that not only four epoxy functionalities containing silicon main chain but also containing epoxy group are modified；The curing agent acid anhydrides is the polyfunctional group acid anhydrides with structure shown in formula (1).The invention also discloses the preparation methods of composition epoxy resin.White reflection composition epoxy resin of the invention has high calorific intensity, with high crosslink density and intensity, low warpage, high reflectance, ageing-resistant performance is excellent, and the initial reflectance at 450nm is increased to 80% or more in 90% or more, 150 degree of 1000h aging back reflection rate, high temperature ageing function admirable, the long-term work after being suitable for high-power LED bracket encapsulation.Continuous moldability can increase to 200 moulds by original 100 mould of continuously moulding, substantially improve operating characteristics.
Description
Technical field
The present invention relates to a kind of composition epoxy resin, especially a kind of reflective asphalt mixtures modified by epoxy resin of LED support high strength white
Oil/fat composition.
Background technique
The advantages that LED is with its environmental protection, energy conservation, rises in Lighting Industry rapidly.At the same time, as LED lamp bead is also by small
Power develops to high-power direction, sent out from illumination to industrial application etc., LED encapsulation material matched with its is also faced with new choose
War.Traditional high-temperature nylon, the materials such as PCT are in high temperature resistant, and high temperature long-time xanthochromia etc. is no longer satisfied requirement, and ring
Oxygen plastic packaging material is with its preferable mechanical performance, and the price of good ageing-resistant and uv-resistance energy and rather moderate is in LED support
On using more and more.Material manufacturer both domestic and external is even more to go into overdrive to be researched and developed, wherein with Hitachi and Ya chemistry
Headed by.Meanwhile each family has also all delivered relevant patent document, more is related to triazine derivative epoxy resin and methyl six
Hydrogen phthalic anhydride either hexahydrophthalic anhydride cooperates obtained by white pigment as curing agent.And use above-mentioned system at present, then it is easy to
Intensity is lower after there is encapsulated moulding, and LED support is relatively soft, it is not easy to it operates, so that continuous moldability is bad, and highest at present
The problems such as can only achieve 100 moulds or so, while with the increase of LED luminous power, to composition epoxy resin in high temperature ageing
Higher requirements are also raised in performance, and reflectivity of the existing product after 150 degrees Celsius of 1000h agings at 450nm is
70% is no longer satisfied requirement.
Summary of the invention
The technical problem to be solved by the present invention is in view of the deficiencies of the prior art, provide a kind of new LED support use
The reflective composition epoxy resin of high strength white, the composition have good adhesive property and mechanical performance, while have compared with
Good intensity, ageing properties and molding performance.
The technical problem to be solved by the present invention is to what is be achieved through the following technical solutions.The present invention is a kind of LED branch
The reflective composition epoxy resin of frame high strength white, its main feature is that, the composition includes: epoxy resin, anhydride are either
Acids curing agent, curing agent promotor, colorant and toughener；The epoxy resin is selected from containing there are four epoxy functionalities
Siloxanes, and the weight of the epoxy resin accounts for the 2-25% of composition epoxy resin total weight.
Silicone compounds in composition epoxy resin of the present invention had both had the main chain of organosilicon structures, ageing-resistant performance
It is excellent, and there is epoxy group, there are higher reactivity, and adhesive property and good mechanical performance.
The technical problems to be solved by the invention can also be achieved through the following technical solutions.Above-described LED branch
The reflective composition epoxy resin of frame high strength white, its main feature is that, the acid anhydride type curing agent is to live with multiple reactions
Property point the polyfunctional group acid anhydrides with structure shown in formula (1).The curing agent increases crosslinking active point, improves reaction speed
Degree and intensity after molding, while there is good ageing-resistant performance.
Formula (1)
The weight of the polyfunctional group anhydride curing agent accounts for the 2-25% of composition epoxy resin total weight.
In the reflective composition epoxy resin of LED support high strength white of the present invention: the curing agent promotes
Agent is not particularly limited, and curing agent promotor can be such that any of curing agent for composition epoxy resin promotees
Into agent, such as tertiary amine, imidazoles and their organic carboxylate, organic metal carboxylate, metal-organic chelate compound, virtue
Race's sulphonic acid ester, organic phosphorus compound, phosphorus compound, and other phosphorus curing agent promotors and its salt, these curing agent promote
Can be used alone into agent can also two kinds of either multiple combinations uses., it is preferable to use halogen in these curing agent promotors
Change quaternary ammonium salt, halogenation quaternary alkylphosphonium salt, caprylate etc. for transparent material and the preferable curing agent promotor of bonding force, wherein solid
Agent promotor accounts for the 0.01-3% of composition epoxy resin total amount.
LED support of the present invention is in the reflective composition epoxy resin of high strength white: the colorant is used to
Improve the whiteness of material, is titanium dioxide, zinc oxide, calcium carbonate, calcium silicates, zirconium oxide, zinc sulphide, magnesia etc., and excellent
Choosing uses titanium dioxide.The type of titanium dioxide is preferably the excellent rutile-type of weather resistance, and the partial size of titanium dioxide is preferred
For 0.03-5um, and further preferably 0.05-2um, to increase its specific surface area and promote covering power.Titanium dioxide can
To be carried out being surface-treated the compatibility and dispersibility to improve it with resin in advance with inorganic or organic substance, and it is especially excellent
It is selected as aluminium, silicon or the surface coated processing of organic compound.The content of colorant is added in 2-60%, preferably 3-40%
When measuring very little, colorability is poor, and the reflectivity of product is lower, is not able to satisfy customer requirement, and additional amount is excessive, leads to product
Molding performance is deteriorated, and mobile performance is lower, leads to lack of fill or mucous membrane, dirty mould.
In the reflective composition epoxy resin of LED support high strength white of the present invention: the toughener is to appoint
What known silicone oil, elastomer silicone, core shell rubbers etc. in composition epoxy resin field, can also select poly- second
The polyalcohols reactive toughening agent such as glycol, neopentyl glycol, glycerine carries out toughening to resin system, while controlling sticking up for product
Qu Chengdu.Here toughener is preferably the reactive toughening agent of polyalcohols.The additive amount of toughener is epoxy composite
The 0.1-10% of object total amount, further preferably 0.2-5%,
In the reflective composition epoxy resin of LED support high strength white of the present invention: can also add as needed
Add inorganic filler.Inorganic filler can be the conventional variety in composition epoxy resin field.Silica, knot including melting
Brilliant silica, aluminium oxide, silicon nitride, aluminium nitride, boron nitride, glass fibre etc..The average grain diameter and shape of inorganic filler
It is not particularly limited, the inorganic filler in addition used can make to include silane coupling agent either titanate ester by coupling agent
What coupling agent treatment was crossed, to enhance the inorganic active filler of adhesive strength between inorganic filler and resin.The content of inorganic filler
Account for the 5-90% of composition epoxy resin total amount, further preferably 20-80%.
In the reflective composition epoxy resin of LED support high strength white of the present invention: as needed, can also add
Coupling agent is added to carry out the intensity between reinforced resin and inorganic filler.These coupling agents can make composition epoxy resin field back warp
Commonly used γ-glycidoxypropyltrimewasxysilane, γ-glycidoxypropyl diethoxy silane
With β-(3,4- expoxycyclohexyl) ethyl trimethoxy silane, the alkoxy silane of amino-functional such as N- β (amino second
Base)-γ-TSL 8330, γ-aminopropyltriethoxywerene werene and N- phenyl-γ-aminopropyl three
Methoxy silane；With alkoxy silane such as γ-mercaptopropyi trimethoxy silane of Mercaptofunctional.The content of coupling agent accounts for
The 0.01-3% of composition epoxy resin total amount, further preferably 0.05-1.5%.
The technical problems to be solved by the invention can also be achieved through the following technical solutions.Above-described high intensity
White reflection composition epoxy resin, its main feature is that can also add release agent as needed, release agent is epoxy composite
Known Brazil wax in object field, sour wax, ester type waxes, polyethylene wax, metallic stearate or be that removal is preferable
Silicone oil.The additional amount of release agent is 0.01-5%, is further selected as 0.03-3%.Content is very little, then does not have the effect of demoulding
Fruit, content is excessive, then the bonding force that will lead to composition epoxy resin and silver-colored frame is insufficient, and then in reliability test below
Middle failure.In order to reach better ageing-resistant performance, preferably ester type waxes and silicone oil, while in order to realize better release property
Can, can preferably by release agent and epoxy resin and curing agent under heating conditions, after fusing, be uniformly mixed, it is cooling after powder
It is broken, then according still further to proportion, it is added during preparing composition epoxy resin.
The technical problems to be solved by the invention can also be achieved through the following technical solutions.Above-described high intensity
White reflection composition epoxy resin can be hindered phenol antioxygen, phosphorus its main feature is that can also add antioxidant as needed
Acid esters kind antioxidant or sulphur antioxidant, such as the antioxidant 2 of Hinered phenols, 6- di-tert-butyl p-cresol, Butylated hydroxy benzene first
Ether, 2,6- di-t-butyl-paraethyl phenol, stearyl-β-(3,5- di-t-butyl -4- hydroxy phenyl) propionic ester, 2,
2 '-di-2-ethylhexylphosphine oxides (4- methyl -6- tert-butyl phenol), 4,4 '-butylidenebis (3- methyl -6- tert-butyl phenol), 3,
Bis- [1,1- dimethyl -2- { β-(3- tert-butyl -4- hydroxyl -5- aminomethyl phenyl) propionyloxy } ethyls] 2,4,8 of 9-,
10- tetra- oxa- loop coil [5,5] hendecane, 1,1,3- tri- (2- methyl -4- hydroxyl -5- tert-butyl-phenyl) butane and 1,
3,5- trimethyls -2,4,6- tri- (3,5- di-t-butyl -4- hydroxybenzyl) benzene, and most preferably 2,6- di-t-butyl pair
Cresols.The antioxidant of phosphoric acid ester: triphenyl phosphite, diphenylalkyl phosphites, phenyldialkyl phosphites, three
(nonyl phenyl) phosphite ester, trilauryl phosphite, three (octadecane) base phosphite esters, triphenyl phosphite,
Distearyl acyl group pentaerythritol diphosphites, three (2,4- di-tert-butyl-phenyl) phosphite esters, diiso decyl pentaerythrite
Diphosphites, two (2,4- di-tert-butyl-phenyl) pentaerythritol diphosphites, three stearyl sorbierite triphosphite esters,
With four (2,4- di-tert-butyl-phenyl) -4,4 '-xenyl bisphosphonates, and most preferably triphenyl phosphite.Sulphur class
Antioxidant: 3,3 '-thiodipropionate of dilauryl -, 3,3 '-thiodipropionate of myristyl-and distearyl -3,
3 '-thiodipropionates.
Though these antioxidant can individually perhaps with two or more be applied in combination phosphorus antioxidant individually or
It is particularly preferred for being applied in combination with phenol antioxidant and phosphorus antioxidant.Antioxidant preferably with 0.01-10wt%, and specifically for
0.03-5wt% is blended into composition epoxy resin.The content of antioxidant is very few to may cause insufficient heat resistance, this can
It can cause to decolourize, and excessive introducing may cause inhibition solidification, and may not be able to realize sufficient ability to cure and intensity.
In the reflective composition epoxy resin of high strength white of the present invention: various additions can also be added as needed
Agent, including ion capturing agent, fire retardant etc. can be introduced under the premise of not influencing advantages of the present invention.
In the reflective composition epoxy resin of high strength white of the present invention: the epoxy resin contains in addition to described
There are four outside the siloxanes of epoxy group, following epoxy resin: triazine derivative epoxy resin, bisphenol epoxies tree can also be contained
Rouge, such as bisphenol-A epoxy resin, Bisphenol F epoxy resin, 3,3 ', 5,5 '-tetramethyl -4,4 '-xenol epoxy resin,
Or 4,4 '-xenol epoxy resin, phenol novolac epoxy resins, cresol novolac epoxy, bisphenol-A phenolic aldehyde are clear
Paint epoxy resin, naphthalene glycol epoxy resin, three hydroxyphenyl methane type epoxy resins (trisphenylol methane epoxy
Resin), the phenol dicyclopentadiene novolac epoxy resin that four hydroxy phenyl ethane epoxy resin and its aromatic ring are hydrogenated.
The content of these epoxy resin accounts for 60% or less the siloxanes weight of epoxy group containing there are four.
In the reflective composition epoxy resin of high strength white of the present invention: the curing agent is in addition to shown in formula (1)
Polyfunctional group acid anhydrides outside, can also be adjacent containing hexahydrophthalic anhydride, methylhexahydrophthalic anhydride, trialkyl tetrahydro
Phthalate anhydride and hydrogenating methyl carbic anhydride etc. do not contain the non-aromatic acid anhydrides of carbon-to-carbon double bond, shown in the acid anhydrides formula (1)
The 80% of polyfunctional group anhydride weight is hereinafter, it is preferred that account for 10-50%.
The technical problems to be solved by the invention can also be achieved through the following technical solutions.The invention also discloses one
The preparation method of high strength white reflective composition epoxy resin of the kind as described in above technical scheme, its main feature is that, step
It is as follows:
(1) preparation of epoxy resin intermediate: at room temperature, by epoxy resin, curing agent and the release agent being related to and
The raw material such as antioxidant are added in reaction kettle according to the proportion in either kneader, and heating stirring is completely melt it；It is molten
After the completion of change, the stress absorption agent measured is added, continues to be stirred to react, it is anti-in the range of 60-100 DEG C to control reaction temperature
It answers, until the resin intermediate of generation, in 150 DEG C of test ICI viscosity numbers in 0.8-2.0P, fast cooling stops reaction, freezing
Afterwards, it crushes, it is spare；
(2) it the preparation of composition epoxy resin: by resin intermediate and other required raw material, weighs, adds according to the ratio
Entering into high-speed mixer to carry out mixed at high speed, resulting mixture is squeezed out by extruder, after rolling, cooling down,
It is ground into partial size appropriate, obtains powdered epoxy composition.
Compared with prior art, composition and preparation method thereof of the invention has following technical effect that
1, the luminous composition epoxy resin of high strength white of the invention, by introducing the epoxy resin containing silicon main chain,
The ageing-resistant performance of resin is improved, while using the curing agent shown in formula (1) with multiple reaction active sites, increasing tree
The reaction active sites of rouge, further enhance intensity and ageing-resistant performance, make the red hardness of its 90s after molding 80 or more, 150
After the aging of DEG C 1000h, reflectivity at 450nm is more suitable the encapsulation of LED bracket 80% or more.
2, when present invention preparation, by the way that first epoxy resin, curing agent, release agent and antioxidant etc. are pre-mixed and instead
It answers, antioxidant and release agent is made to reach molecularly dispersed structure in resin system, and then obtain more good stripping result and resistance to
Ageing properties, while passing through the preparatory reaction of epoxy resin and curing agent, the substance of small molecule is discharged away, epoxy is reduced
The problems such as resin combination stomata in use.By curing agent shown in formula (1), resin combination is further increased
Intensity and ageing-resistant performance make its continuous moldability be increased to 200 moulds by 100 original moulds.
Specific embodiment
The specific technical solution of the present invention described further below, so that those skilled in the art is further understood from this
Invention, without constituting the limitation to its right.
Embodiment 1, a kind of reflective composition epoxy resin of LED support high strength white, the composition includes: asphalt mixtures modified by epoxy resin
Rouge, anhydride either acids curing agent, curing agent promotor, colorant and toughener；The epoxy resin, which is selected from, to be contained
The siloxanes of four epoxy functionalities, and the weight of the epoxy resin accounts for the 2-25% of composition epoxy resin total weight.
Embodiment 2, in the reflective composition epoxy resin of LED support high strength white described in embodiment 1: the acid
Anhydride curing agent is the polyfunctional group acid anhydrides with structure shown in formula (1):
Formula (1)
The weight of the polyfunctional group acid anhydrides accounts for the 2-25% of composition epoxy resin total weight.
Embodiment 3, in the reflective composition epoxy resin of LED support high strength white described in embodiment 1 or 2: epoxy
The ratio between anhydride equivalent in epoxide equivalent and acid anhydrides in resin is 0.5-2.5.
Embodiment 4, the reflective epoxy composite of LED support high strength white described in any one of embodiment 1-3
In object: curing agent promotor is selected from quaternary ammonium halides salt, halogenation quaternary alkylphosphonium salt, caprylate, and curing agent promotor accounts for epoxy resin group
Close the 0.01-3% of object total amount.
Embodiment 5, the reflective epoxy composite of LED support high strength white described in any one of embodiment 1-3
In object: the colorant is selected from the rutile titanium dioxide that partial size is 0.03-5 μm；And colorant accounts for epoxy composite
The 2-60% of object total amount.
Embodiment 6, the reflective composition epoxy resin of LED support high strength white described in any one of embodiment 5
In: the partial size of the titanium dioxide is 0.05-2um, and the titanium dioxide uses aluminium or silicon materials or organic compound in advance
Object carries out surface coated processing；And colorant accounts for the 3-40% of composition epoxy resin total amount.
Embodiment 7, the reflective epoxy composite of LED support high strength white described in any one of embodiment 1-6
In object: the toughener is the reactive toughening agent of polyalcohols；The additive amount of toughener is composition epoxy resin total amount
0.1-10%.
Embodiment 8, the reflective epoxy composite of LED support high strength white described in any one of embodiment 1-7
In object: the composition epoxy resin also contains antioxidant, and the antioxidant is selected from phosphorus antioxidant or phosphorus antioxidant and phenol is anti-
The composition of oxygen agent；The antioxidant accounts for the 0.01-10% of composition epoxy resin total amount.
Embodiment 9, the reflective composition epoxy resin of LED support high strength white described in embodiment 1-8 any one
Preparation method, its step are as follows:
(1) preparation of epoxy resin intermediate: at room temperature, by epoxy resin, curing agent and the release agent being related to and
The raw material such as antioxidant are added in reaction kettle according to the proportion in either kneader, and heating stirring is completely melt it.It is molten
After the completion of change, the stress absorption agent measured is added, continues to be stirred to react, it is anti-in the range of 60-100 DEG C to control reaction temperature
It answers, until the resin intermediate of generation, in 150 DEG C of test ICI viscosity numbers in 0.8-2.0P, fast cooling stops reaction, freezing
Afterwards, it crushes, it is spare.
(2) it the preparation of composition epoxy resin: by resin intermediate and other required raw material, weighs, adds according to the ratio
Entering into high-speed mixer to carry out mixed at high speed, resulting mixture is squeezed out by extruder, after rolling, cooling down,
It is ground into partial size appropriate, obtains powdered epoxy composition.
Embodiment 10, a kind of reflective composition epoxy resin of LED support high strength white, the composition includes: epoxy
Resin, anhydride either acids curing agent, curing agent promotor, colorant and toughener；The epoxy resin, which is selected from, to be contained
There are four the siloxanes of epoxy functionality, and the weight of the epoxy resin accounts for the 10% of composition epoxy resin total weight.
The acid anhydride type curing agent is the polyfunctional group acid anhydrides with structure shown in formula (1), the polyfunctional group acid anhydrides
Weight account for the 8% of composition epoxy resin total weight.
The curing agent promotor is selected from quaternary ammonium halides salt, halogenation quaternary alkylphosphonium salt, caprylate, and curing agent promotor accounts for ring
The 1% of epoxy resin composition total amount.
The partial size of the titanium dioxide is 0.05um, and the titanium dioxide carries out surface with aluminium or silicon materials in advance
The processing of cladding；And colorant accounts for the 15% of composition epoxy resin total amount.
The toughener is the reactive toughening agent of polyalcohols；The additive amount of toughener is that composition epoxy resin is total
The 5% of amount.
The composition epoxy resin also contains antioxidant, the antioxidant be selected from phosphorus antioxidant or phosphorus antioxidant with
The composition of phenol antioxidant；The antioxidant accounts for the 5% of composition epoxy resin total amount.
Steps are as follows for its preparation method:
(1) preparation of epoxy resin intermediate: at room temperature, by epoxy resin, curing agent and the release agent being related to and
The raw material such as antioxidant are added in reaction kettle according to the proportion in either kneader, and heating stirring is completely melt it.It is molten
After the completion of change, the stress absorption agent measured is added, continues to be stirred to react, it is anti-in the range of 60-70 DEG C to control reaction temperature
It answers, until the resin intermediate of generation, in 150 DEG C of test ICI viscosity numbers in 0.8-2.0P, fast cooling stops reaction, freezing
Afterwards, it crushes, it is spare.
(2) it the preparation of composition epoxy resin: by resin intermediate and other required raw material, weighs, adds according to the ratio
Entering into high-speed mixer to carry out mixed at high speed, resulting mixture is squeezed out by extruder, after rolling, cooling down,
It is ground into partial size appropriate, obtains powdered epoxy composition.
Embodiment 11, a kind of reflective composition epoxy resin of LED support high strength white, the composition includes: epoxy
Resin, anhydride either acids curing agent, curing agent promotor, colorant and toughener；The epoxy resin, which is selected from, to be contained
There are four the siloxanes of epoxy functionality, and the weight of the epoxy resin accounts for the 25% of composition epoxy resin total weight.
The acid anhydride type curing agent is the polyfunctional group acid anhydrides with structure shown in formula (1), the polyfunctional group acid anhydrides
Weight account for the 25% of composition epoxy resin total weight.
The curing agent promotor is selected from quaternary ammonium halides salt, halogenation quaternary alkylphosphonium salt, caprylate, and curing agent promotor accounts for ring
The 3% of epoxy resin composition total amount.
The partial size of the titanium dioxide is 2um, and the titanium dioxide carries out surface packet with aluminium or silicon materials in advance
The processing covered；And colorant accounts for the 40% of composition epoxy resin total amount.
The toughener is the reactive toughening agent of polyalcohols；The additive amount of toughener is that composition epoxy resin is total
The 2% of amount.
The composition epoxy resin also contains antioxidant, the antioxidant be selected from phosphorus antioxidant or phosphorus antioxidant with
The composition of phenol antioxidant；The antioxidant accounts for the 2% of composition epoxy resin total amount.
Steps are as follows for its preparation method:
(1) preparation of epoxy resin intermediate: at room temperature, by epoxy resin, curing agent and the release agent being related to and
The raw material such as antioxidant are added in reaction kettle according to the proportion in either kneader, and heating stirring is completely melt it.It is molten
After the completion of change, the stress absorption agent measured is added, continues to be stirred to react, it is anti-in the range of 70-80 DEG C to control reaction temperature
It answers, until the resin intermediate of generation, in 150 degree of test ICI viscosity numbers in 0.8-2.0P, fast cooling stops reaction, freezing
Afterwards, it crushes, it is spare.
(2) it the preparation of composition epoxy resin: by resin intermediate and other required raw material, weighs, adds according to the ratio
Entering into high-speed mixer to carry out mixed at high speed, resulting mixture is squeezed out by extruder, after rolling, cooling down,
It is ground into partial size appropriate, obtains powdered epoxy composition.
Embodiment 12, a kind of reflective composition epoxy resin of LED support high strength white, the composition includes: epoxy
Resin, anhydride either acids curing agent, curing agent promotor, colorant and toughener；The epoxy resin, which is selected from, to be contained
There are four the siloxanes of epoxy functionality, and the weight of the epoxy resin accounts for the 20% of composition epoxy resin total weight.
The acid anhydride type curing agent is the polyfunctional group acid anhydrides with structure shown in formula (1), the polyfunctional group acid anhydrides
Weight account for the 15% of composition epoxy resin total weight.
The curing agent promotor is selected from quaternary ammonium halides salt, halogenation quaternary alkylphosphonium salt, caprylate, and curing agent promotor accounts for ring
The 1% of epoxy resin composition total amount.
The partial size of the titanium dioxide is 1um, and the titanium dioxide carries out surface packet with aluminium or silicon materials in advance
The processing covered；And colorant accounts for the 30% of composition epoxy resin total amount.
The toughener is the reactive toughening agent of polyalcohols；The additive amount of toughener is that composition epoxy resin is total
The 6% of amount.
The composition epoxy resin also contains antioxidant, the antioxidant be selected from phosphorus antioxidant or phosphorus antioxidant with
The composition of phenol antioxidant；The antioxidant accounts for the 10% of composition epoxy resin total amount.
Steps are as follows for its preparation method:
(1) preparation of epoxy resin intermediate: at room temperature, by epoxy resin, curing agent and the release agent being related to and
The raw material such as antioxidant are added in reaction kettle according to the proportion in either kneader, and heating stirring is completely melt it.It is molten
After the completion of change, the stress absorption agent measured is added, continues to be stirred to react, it is anti-in the range of 80-90 DEG C to control reaction temperature
It answers, until the resin intermediate of generation, in 150 DEG C of test ICI viscosity numbers in 0.8-2.0P, fast cooling stops reaction, freezing
Afterwards, it crushes, it is spare.
(2) it the preparation of composition epoxy resin: by resin intermediate and other required raw material, weighs, adds according to the ratio
Entering into high-speed mixer to carry out mixed at high speed, resulting mixture is squeezed out by extruder, after rolling, cooling down,
It is ground into partial size appropriate, obtains powdered epoxy composition.
Embodiment 13, present invention experiment and its result:
Epoxy resin:
The modified siloxanes of four epoxy groups, ProductName X-40-2670, by Shin-Etsu Chemical Co.,
Ltd. production and public offering；
Three (2,3- glycidyl) isocyanates, ProductName TEPIC-S, by Nissan Chemical Industries,
Ltd. it produces.
Curing agent:
The acid anhydrides of structure shown in formula (1)；
Hexahydrophthalic anhydride, ProductName HHPA are provided by wave woods chemical industry (Changzhou) Co., Ltd；
Curing agent promotor:
Tetra-n-butylphosphonium O, O-diethylphosphorodithioate, ProductName
HISHICOLIN PX-4ET is provided by NIPPON CHEMICAL INDUSTRIAL；
Quaternary phosphonium bromide, ProductName U-CAT-5003 are produced by San-Apro Limited；
Colorant:
Titanium dioxide, rutile-type, ProductName KRONOS 2310 are produced by Kronos International Inc.；
Titanium dioxide, rutile-type, ProductName KRONOS 2233 are produced by Kronos International Inc.；
Toughener:
Ethylene glycol is analyzed pure.
Inorganic filler:
Fused silica is provided by Jiangsu Lian Rui new material Co., Ltd；
Antioxidant:
Phosphite ester, hindered phenol composite antioxidant, name of product PUB-370 are provided by one Chemical Co., Ltd. of Guangzhou will；
Release agent: distillation monoglyceride, ProductName, D-95 are produced by Zhangjiagang Zhong Ding additive Co., Ltd；
Composition epoxy resin made from this experiment is taken to carry out coherent detection test:
(1) gel time: by the experimental method of SJ/T 11197-2013, electric hot tray is heated to 175 ± 1 DEG C, is taken
0.3-0.5g sample is placed on electric hot plate, and it is about 5cm that sample, which shakeouts area,2, melting starts timing, with needle-shaped stirring rod tip or
Grafter stirring, powder is gradually become gel state (sample is unable to wire drawing as terminal) from fluid, same to grasp the time required to reading
Make, is repeated twice, takes its average value.
(2) mobility: by the experimental method of SJ/T 11197-2013, using EMMI-1-66 helical flow metal die,
Measure the Spiral flow length (cm) under the following conditions: die head temperature using transfer modling equipment: 175 DEG C, injection pressure:
6.86Mpa(70kgf/cm2), which shows that more greatly mobility is better for evaluating mobility, measurement numerical value.
(3) red hardness 90s(HH90s): at 175 DEG C of mold temperature, injection pressure: 6.86Mpa(70kgf/cm2) condition
Under, composition epoxy resin is added in injection molding barrel, length 115mm, width 9.6mm is molded as, is highly the sample of 5mm
Item.Molding cycle is 90s, after the completion, is opened rapidly, using Shore durometer, to measure the hardness of sample, every group of sample is at least
5 points are measured, are averaged.Its red hardness is higher, and after molded, the intensity of product is higher.
(4) transfer modling press, at 175 DEG C of mold temperature, briquetting pressure 5MPa, curing time 120s reflectivity: are utilized
Under conditions of carry out.According to above-mentioned experiment condition, it is disk of the 30mm with a thickness of 2mm which, which is prepared into diameter,
Reflectance test is carried out on the UV-3600 instrument of Shimadzu.
(5) continuous moldability: on the press of Fushi Sanjia, using 3030 mold, in the mold temperature of 180 degree
Degree, is carried out continuously clear mould three times, after moistening mould three times, under the curing time of 120s, carries out continuously at model measurement.Until mold
Surface occur it is dirty, until there is one of the defects of red ink failure in sticking to mould or LED support.
The prescription and result reference following table of several groups of experiments:
Claims (2)
1. a kind of reflective composition epoxy resin of LED support high strength white, which is characterized in that the composition includes: epoxy
Resin, acid anhydride type curing agent, curing agent promotor, colorant, toughener, inorganic filler, antioxidant and release agent；
The acid anhydride type curing agent is the polyfunctional group acid anhydrides with structure shown in formula (1):
Formula (1)
The siloxanes that the epoxy resin uses four epoxy groups modified, parts by weight 9；
The parts by weight of the acid anhydride type curing agent are 9；
The curing agent promotor quaternary phosphonium bromide, parts by weight 0.2；
The colorant is rutile titanium dioxide, parts by weight 20；
The inorganic filler is fusion silica, parts by weight 60；
The antioxidant is the composite antioxidant that phosphite ester and hindered phenol are formed, parts by weight 0.8；
The release agent is distillation monoglyceride, parts by weight 0.5；
The toughener is polyethylene glycol, parts by weight 0.5.
2. a kind of preparation method of the reflective composition epoxy resin of LED support high strength white as described in claim 1,
It is characterized in that, its step are as follows:
(1) preparation of epoxy resin intermediate: at room temperature, by raw material material epoxy resin, curing agent and the release agent being related to
And antioxidant, it is added in reaction kettle according to the proportion in either kneader, heating stirring is completely melt it；
(2) after the completion of melting, the toughener measured is added, continues to be stirred to react, control model of the reaction temperature at 60-100 DEG C
Interior reaction is enclosed, until the resin intermediate of generation, in 150 DEG C of test ICI viscosity numbers in 0.8-2.0P, fast cooling stops anti-
It answers, after freezing, crushes, it is spare；
(3) it the preparation of composition epoxy resin: by resin intermediate and other required raw material, weighs, is added to according to the ratio
Mixed at high speed is carried out in high-speed mixer, resulting mixture is squeezed out by extruder, after rolling, cooling down, is crushed
At partial size appropriate, powdered epoxy composition is obtained.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510724283.9A CN105199079B (en) | 2015-10-30 | 2015-10-30 | A kind of reflective composition epoxy resin of LED support high strength white |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510724283.9A CN105199079B (en) | 2015-10-30 | 2015-10-30 | A kind of reflective composition epoxy resin of LED support high strength white |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105199079A CN105199079A (en) | 2015-12-30 |
| CN105199079B true CN105199079B (en) | 2019-01-29 |
Family
ID=54947060
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510724283.9A Active CN105199079B (en) | 2015-10-30 | 2015-10-30 | A kind of reflective composition epoxy resin of LED support high strength white |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105199079B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108017879A (en) * | 2016-11-04 | 2018-05-11 | 无锡创达新材料股份有限公司 | A kind of preparation of high-power LED encapsulation white epoxy moulding compound |
| CN107400337A (en) * | 2017-07-27 | 2017-11-28 | 重庆市新森宝科技有限公司 | A kind of epoxy/polyester environment-friendly composite material and preparation method thereof |
| CN108192283A (en) * | 2017-11-24 | 2018-06-22 | 木林森股份有限公司 | Production method of organic silicon modified epoxy resin composition for L ED bracket |
| CN109957209B (en) * | 2017-12-25 | 2021-08-17 | 北京科化新材料科技有限公司 | Epoxy resin composition, resin product, preparation method thereof and resin product |
| CN112341755B (en) * | 2019-08-07 | 2023-01-17 | 北京科化新材料科技有限公司 | Yellowing-resistant transparent epoxy resin packaging material and preparation method and application thereof |
| CN114908627B (en) * | 2022-05-19 | 2023-09-01 | 西南科技大学 | Basic magnesium sulfate cement-based self-luminous brick material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101942073A (en) * | 2009-07-07 | 2011-01-12 | 日本化药株式会社 | Optical semiconductor sealing curable resin composition and cured article thereof |
| CN104619498A (en) * | 2012-08-16 | 2015-05-13 | 三菱瓦斯化学株式会社 | Resin sheet, support body with resin layer, laminate plate, and metal-clad laminate plate |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013008680A1 (en) * | 2011-07-13 | 2013-01-17 | 株式会社ダイセル | Curable epoxy resin composition |
| CN102850984A (en) * | 2012-09-19 | 2013-01-02 | 江苏华海诚科新材料有限公司 | Low-stress epoxy resin composition applicable to packaging small-size surface mounted devices |
| CN103641998B (en) * | 2013-12-24 | 2016-05-04 | 江苏华海诚科新材料股份有限公司 | The white epoxy resin composition that LED reflector is used |
-
2015
- 2015-10-30 CN CN201510724283.9A patent/CN105199079B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101942073A (en) * | 2009-07-07 | 2011-01-12 | 日本化药株式会社 | Optical semiconductor sealing curable resin composition and cured article thereof |
| CN104619498A (en) * | 2012-08-16 | 2015-05-13 | 三菱瓦斯化学株式会社 | Resin sheet, support body with resin layer, laminate plate, and metal-clad laminate plate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105199079A (en) | 2015-12-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105199079B (en) | A kind of reflective composition epoxy resin of LED support high strength white | |
| CN100564448C (en) | A kind of method for preparing molded epoxy resin sheet and products thereof | |
| CN102002237B (en) | White heat-curable silicone/epoxy hybrid resin composition | |
| JP5110311B2 (en) | Method for producing thermosetting epoxy resin composition | |
| WO2016179770A1 (en) | Pbt engineering plastic composition used for nmt | |
| CN101864259B (en) | SIS (Styrene-Isoprene-Styrene) hot melt adhesive for car light adhesion and preparation method thereof | |
| CN106349645B (en) | Thermosetting epoxy resin composition for encapsulating optical semiconductor element and optical semiconductor device using the same | |
| CN109777039B (en) | Epoxy resin composition rubber cake for chip LED packaging and preparation method and packaging process thereof | |
| CN110194942A (en) | A kind of low-temperature rapid thermal cured one-component epoxy adhesive and preparation method thereof | |
| CN108017879A (en) | A kind of preparation of high-power LED encapsulation white epoxy moulding compound | |
| CN105219033A (en) | There is the thermoplastic resin composition of excellent reflectivity | |
| CN104788899B (en) | A kind of high heat-resisting yellowing-resistant thermoset epoxy composition | |
| WO2016179769A1 (en) | Hyperbranched resin-toughened pbt engineering plastic composition | |
| TWI671325B (en) | White thermosetting epoxy resin composition, reflector for optical semiconductor element formed by the composition, and optical semiconductor device having the same | |
| CN106188975B (en) | A kind of soft high transparent and fire-retardant heat-resistant polyvinyl chloride material of spy and preparation method thereof | |
| CN110128782A (en) | Compatible anticorrosive composition epoxy resin of a kind of copper wire and preparation method thereof | |
| JP2012172012A (en) | Thermosetting epoxy resin composition and optical semiconductor device | |
| CN113861630B (en) | Polyester resin composition and preparation method and application thereof | |
| CN106459567A (en) | Polyester resin composition for reflective materials and reflection plate containing same | |
| CN112852371B (en) | Small-spacing epoxy plastic packaging material applied to outdoor display screen and preparation method thereof | |
| JP6274092B2 (en) | Thermosetting epoxy resin composition for optical semiconductor element sealing and optical semiconductor device using the same | |
| WO2016074207A1 (en) | White epoxy moulding compound | |
| JP5924840B2 (en) | Thermosetting epoxy resin composition | |
| CN109867923A (en) | A kind of polyester molding compounds and the preparation method and application thereof | |
| CN105542382A (en) | Plastic shell of electricity meter and application of plastic shell |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 222047 Jiangsu Lianyungang Lianyungang economic and Technological Development Zone Lingang Industrial Zone, east of Gu Wei Road and East Avenue North. Patentee after: JIANGSU HUAHAI CHENGKE NEW MATERIAL CO., LTD. Address before: 222047 Jiangsu Lianyungang Lianyungang economic and Technological Development Zone Lingang Industrial Zone, east of Gu Wei Road and East Avenue North. Patentee before: Jiangsu Huahai Chengke New Materials Co.,Ltd. |
|
| CP01 | Change in the name or title of a patent holder |