CN108192284A - A kind of transparent epoxy moulding compound of resisting high-temperature yellowing and preparation method thereof - Google Patents
A kind of transparent epoxy moulding compound of resisting high-temperature yellowing and preparation method thereof Download PDFInfo
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- CN108192284A CN108192284A CN201711383489.5A CN201711383489A CN108192284A CN 108192284 A CN108192284 A CN 108192284A CN 201711383489 A CN201711383489 A CN 201711383489A CN 108192284 A CN108192284 A CN 108192284A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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Abstract
The transparent epoxy moulding compound of a kind of resisting high-temperature yellowing, it is characterised in that the raw material matched by following weight is made：Cycloaliphatic epoxy resin 31 60%, phthalic anhydride curing agent 30 50%, alcohols ring opening agent 2 5%, the system of phosphorus containing benzene accelerating agent 0.1 1%, hindered phenol anti-oxidants 0.1 1%, auxiliary anti-oxidant 0.01 0.05%, silane coupling agent 0.1 1%, releasing agent 0.1 1%, superbrnaching end-hydroxy resin 2 10%.The present invention also provides a kind of preparation methods of the transparent epoxy moulding compound of above-mentioned resisting high-temperature yellowing.The transparent epoxy moulding compound light transmittance of the present invention is high, resisting high-temperature yellowing is functional, and with higher glass transition temperature and excellent bending resistance shear behavior, it disclosure satisfy that the performance requirement of LED encapsulation, the encapsulation of small spacing all-colour LED is particularly applicable to, meets the performance requirement of all-colour LED encapsulation.
Description
Technical field
The present invention relates to the encapsulating materials applied to LED, and in particular to a kind of transparent epoxy moulding compound of resisting high-temperature yellowing
And preparation method thereof.
Background technology
Epoxy molding plastic due to high reliability, low cost, simple production process, suitable for large-scale production etc. it is excellent
Point is widely used in microelectronics Packaging industry, in addition to protecting chip not by extraneous dust, moisture, ion, radiation, machine
Tool impact is outer, also acts mechanical support and the function of heat dissipation.
Traditional epoxy molding plastic is mostly using o-cresol formaldehyde epoxy-phenolic resin system, added with filler and colorant,
Resin after curing is mostly opaque, black, and due to the benzene ring structure in o-cresol formaldehyde epoxy resin, in long term high temperature ring
Yellowing easily occurs in border, therefore optics LED encapsulation fields can not be applied to.
Publication No. is that the Chinese invention patent application specification of CN105504674A discloses one kind for LED package supports
Epoxy molding plastic and its preparation method and application, the epoxy molding plastic are promoted by the epoxy resin, curing agent, curing purified
It is formed into agent, inorganic filler, reflective regulation agent and fire retardant, obtained epoxy molding plastic is heat-resisting, anti-with high heat conduction, height
The advantages that UV, low thermal coefficient of expansion.Publication No. is that the Chinese invention patent application specification of CN102408676A discloses one kind
Environment-friendlyepoxy epoxy molding compound applied to Electronic Packaging polymeric material field and preparation method thereof, the epoxy molding plastic is by epoxy
The compositions such as resin, phenolic resin, filler, carbon black and curing accelerator, obtained epoxy molding plastic are environmentally friendly.On however,
State that the moulding compound transmitance after two kinds of moulding compound plastic packagings is low, and high temperature anti-yellowing property is poor, it is difficult to which meet optics LED encapsulation will
It asks.
Invention content
The technical problems to be solved by the invention are to provide the transparent epoxy moulding compound of a kind of resisting high-temperature yellowing and this
The preparation method of the transparent epoxy moulding compound of resisting high-temperature yellowing, this transparent epoxy moulding compound light transmittance is high, resisting high-temperature yellowing
Can be good, and with higher glass transition temperature and excellent bending resistance shear behavior, disclosure satisfy that the performance of LED encapsulation will
It asks.The technical solution of use is as follows：
The transparent epoxy moulding compound of a kind of resisting high-temperature yellowing, it is characterised in that the raw material matched by following weight is made：It is alicyclic
Epoxy resin 31-60%, phthalic anhydride curing agent 30-50%, alcohols ring opening agent 2-5%, the system of phosphorus containing benzene accelerating agent 0.1-1%, Hinered phenols
Antioxidant 0.1-1%, auxiliary anti-oxidant 0.01-0.05%, silane coupling agent 0.1-1%, releasing agent 0.1-1%, superbrnaching end-hydroxy
Resin 2-10%.
It is preferred that above-mentioned cycloaliphatic epoxy resin is poly- [(2- Oxyranyles) -1,2- cyclohexanediols] 2- ethyl -2- (hydroxyls
Methyl) -1,3- propylene glycols (3:1), hexamethylene -1,2- dicarboxylic acids 2-glycidyl ester, 4,5- 7-oxa-bicyclo[4.1.0s -1,2- two
Formic acid 2-glycidyl ester and one kind in 4- vinyl -1- cyclohexene dicyclic oxides or many of mixture.It is above-mentioned
Cycloaliphatic epoxy resin is solid or liquid, epoxide equivalent 160-200.Compared to common phenol in conventional epoxy moulding compound
Formaldehyde epoxy resin, cycloaliphatic epoxy resin have the following advantages：（1）Epoxide equivalent is small, and crosslink density is big, and thermostabilization is contained in structure
The good rigid structure of property, therefore heat resistance is good；（2）Without phenyl ring, therefore UV resistant and good weatherability；（3）It synthesized
Cheng Buhan Cl, Na plasmas, therefore electrical property is good, especially electrical properties in high temperatures and are-tight property is good.
It is preferred that above-mentioned phthalic anhydride curing agent is the mixed of one or both of 4- methyl hexahydrophthalic anhydrides and 4- methyl tetrahydro phthalic anhydrides
Close object.
It is preferred that above-mentioned alcohols ring opening agent is the mixing of one kind or two of which in ethylene glycol, glycerine and pentaerythrite
Object.Alcohols ring opening agent assists in acid anhydrides open loop, and the carboxylic acid group of generation is made to form densification further with epoxy reaction
Cross-linked structure.
It is preferred that the above-mentioned system of phosphorus containing benzene accelerating agent be triphenylmethylphosphonium bromide phosphine and one kind in triphenyl ethyl phosphonium bromide phosphine or
The mixture of the two.The accelerating agent is water white transparency solid particle, and phthalic anhydride curing agent is soluble under the condition of high temperature.
It is preferred that above-mentioned hindered phenol anti-oxidants be four [β-（3,5- di-tert-butyl-hydroxy phenyls）Propionic acid] pentaerythrite
Ester and β-（3,5- di-tert-butyl-hydroxy phenyls）The mixture of one or both of the positive octadecanol ester of propionic acid.Asphalt mixtures modified by epoxy resin
Fat is placed in the high temperature environment for a long time, and Yellowing easily occurs, and epoxy can effectively be mitigated by adding in hindered phenol anti-oxidants
The hot Yellowing of resin.
It is preferred that above-mentioned auxiliary anti-oxidant is in trisnonylphenyl phosphite and three [2.4- di-tert-butyl-phenyls] phosphite esters
One or both mixture.
It is preferred that above-mentioned silane coupling agent is three ethoxy of γ-glycidyl ether oxygen propyl trimethoxy silicane and γ-aminopropyl
The mixture of one or both of base silane.
It is preferred that above-mentioned releasing agent is the mixture of one or both of zinc stearate and magnesium stearate.
Above-mentioned superbrnaching end-hydroxy resin is as toughener, and great amount of hydroxy group is contained in structure outer end, and reactivity is high, can have
Effect improves the bending resistance shear behavior of epoxy resin.It is preferred that the structural formula of above-mentioned superbrnaching end-hydroxy resin is following structural formula（1）-
（3）In one kind：
（1）
（2）
（3）
The present invention also provides a kind of preparation methods of the transparent epoxy moulding compound of above-mentioned resisting high-temperature yellowing, it is characterised in that including under
State step：
（1）By weight, following raw materials are equipped with：Cycloaliphatic epoxy resin 31-60%, phthalic anhydride curing agent 30-50%, alcohols ring opening agent
2-5%, the system of phosphorus containing benzene accelerating agent 0.1-1%, hindered phenol anti-oxidants 0.1-1%, auxiliary anti-oxidant 0.01-0.05% are silane coupled
Agent 0.1-1%, releasing agent 0.1-1%, superbrnaching end-hydroxy resin 2-10%；
（2）Cycloaliphatic epoxy resin and superbrnaching end-hydroxy tree are added in into cleaning, A agitator tanks that are dry and carrying heating unit
Fat, and it is warming up to 100-110 DEG C（The material in A agitator tanks is heated, its temperature is made to rise to 100-110 DEG C）, with 300-500
Rev/min mixing speed stir 5-20 minutes；
（3）Phthalic anhydride curing agent, alcohols ring opening agent, the system of phosphorus containing benzene accelerating agent, hindered phenol are added in into cleaning, dry B agitator tanks
Class antioxidant, auxiliary anti-oxidant, silane coupling agent and releasing agent are stirred 5-20 minutes with 300-500 revs/min of mixing speed
（It stirs at normal temperatures）, obtain the first mixed liquor；
（4）The first mixed liquor in B agitator tanks is introduced by conduit in A agitator tanks, is stirred at a temperature of 100-110 DEG C
It mixes（The material in A agitator tanks is heated, its temperature is made to be maintained at 100-110 DEG C）, mixing speed is 300-500 revs/min,
Mixing time is 5-15 minutes, obtains the second mixed liquor；
（5）Second mixed liquor is added to extruder by feed hopper（Such as double screw extruder）It squeezes out, is subsequently cooled to 20-30
DEG C, obtain the resisting high-temperature yellowing transparent epoxy moulding compound of sheet（The material that the methods of curtain coating, calendering can be used squeezes out extruder
It is cooled down and forms sheet material）, then the resisting high-temperature yellowing transparent epoxy moulding compound of sheet is ground into particulate material, then will
Pellet grind into powder material, to powder materials except after magnetic, you can obtain the transparent epoxy moulding compound of powdered resisting high-temperature yellowing.It can
The transparent epoxy moulding compound of obtained powdered resisting high-temperature yellowing is pressed into pie, to store in a warehouse, transport and to use.
The transparent epoxy moulding compound light transmittance of the present invention is high, and resisting high-temperature yellowing is functional（Through 150 DEG C of high temperature ageing 500h
Afterwards, significant change will not occur for molding product color）, and with higher glass transition temperature and excellent bending resistance shearing resistance
Performance disclosure satisfy that the performance requirement of LED encapsulation, be particularly applicable to the encapsulation of small spacing all-colour LED, meet all-colour LED
The performance requirement of encapsulation.
Specific embodiment
Embodiment 1
In the present embodiment, the preparation method of the transparent epoxy moulding compound of resisting high-temperature yellowing includes the following steps：
（1）By weight, following raw materials are equipped with：Cycloaliphatic epoxy resin 51.18%（Its cyclohexane -1,2- dicarboxylic acids two shrinks
Glyceride 41.18%, 4- vinyl -1- cyclohexene dicyclic oxide 10%）, phthalic anhydride curing agent 36.8%（It is 4- methyl hexahydrobenzenes
Acid anhydride）, alcohols ring opening agent 4%（It is glycerine）, the system of phosphorus containing benzene accelerating agent 0.2%（It is triphenylmethylphosphonium bromide phosphine）, hindered phenol
Class antioxidant 0.5%（Be β-（3,5- di-tert-butyl-hydroxy phenyls）The positive octadecanol ester of propionic acid）, auxiliary anti-oxidant 0.02%
（It is trisnonylphenyl phosphite）, silane coupling agent 0.5%（It is γ-aminopropyl triethoxysilane）, releasing agent
0.8%（It is zinc stearate）, superbrnaching end-hydroxy resin 6%；
（2）Cycloaliphatic epoxy resin and superbrnaching end-hydroxy tree are added in into cleaning, A agitator tanks that are dry and carrying heating unit
Fat, and it is warming up to 100 DEG C（The material in A agitator tanks is heated, its temperature is made to rise to 100 DEG C）, with 500 revs/min stir
Speed is mixed to stir 10 minutes；
（3）Phthalic anhydride curing agent, alcohols ring opening agent, the system of phosphorus containing benzene accelerating agent, hindered phenol are added in into cleaning, dry B agitator tanks
Class antioxidant, auxiliary anti-oxidant, silane coupling agent and releasing agent are stirred 10 minutes with 500 revs/min of mixing speed（Normal
Temperature is lower to be stirred）, obtain the first mixed liquor；
（4）The first mixed liquor in B agitator tanks is introduced by conduit in A agitator tanks, is stirred at a temperature of 100 DEG C
（The material in A agitator tanks is heated, its temperature is made to be maintained at 100 DEG C）, mixing speed is 500 revs/min, and mixing time is
10 minutes, obtain the second mixed liquor；
（5）The second mixed liquor is added to double screw extruder by feed hopper to squeeze out, 20 DEG C is subsequently cooled to, obtains sheet
Resisting high-temperature yellowing transparent epoxy moulding compound（The material that extruder squeezes out cool down the methods of can be used curtain coating, calendering and shape
Slabbing material）, then the resisting high-temperature yellowing transparent epoxy moulding compound of sheet is ground into particulate material, then particulate material is pulverized
End material, to powder materials except after magnetic, you can obtain the transparent epoxy moulding compound of powdered resisting high-temperature yellowing.
The transparent epoxy moulding compound of obtained powdered resisting high-temperature yellowing can be pressed into pie, to store in a warehouse, to transport
With use.
The structural formula of above-mentioned superbrnaching end-hydroxy resin is as follows：
Embodiment 2
In the present embodiment, the preparation method of the transparent epoxy moulding compound of resisting high-temperature yellowing includes the following steps：
（1）By weight, following raw materials are equipped with：Cycloaliphatic epoxy resin 53.35%（It is poly- [(2- Oxyranyles) -1,2-
Cyclohexanediol] 2- ethyls -2- (methylol) -1,3- propylene glycols (3:1)）, phthalic anhydride curing agent 38.2%（It is 4- methyl six
Hydrogen phthalic anhydride）, alcohols ring opening agent 2%（It is pentaerythrite）, the system of phosphorus containing benzene accelerating agent 0.4%（Wherein triphenylmethylphosphonium bromide phosphine
0.2%, triphenyl ethyl phosphonium bromide phosphine 0.2%）, hindered phenol anti-oxidants 0.5%（Be β-（3,5- di-t-butyl -4- hydroxy benzenes
Base）The positive octadecanol ester of propionic acid）, auxiliary anti-oxidant 0.05%（It is three [2.4- di-tert-butyl-phenyls] phosphite esters）, it is silane coupled
Agent 1%（It is γ-glycidyl ether oxygen propyl trimethoxy silicane）, releasing agent 0.5%（It is magnesium stearate）, terminal hydroxy group over-expense
Change resin 4%；
（2）Cycloaliphatic epoxy resin and superbrnaching end-hydroxy tree are added in into cleaning, A agitator tanks that are dry and carrying heating unit
Fat, and it is warming up to 110 DEG C（The material in A agitator tanks is heated, its temperature is made to rise to 110 DEG C）, with 400 revs/min stir
Speed is mixed to stir 10 minutes；
（3）Phthalic anhydride curing agent, alcohols ring opening agent, the system of phosphorus containing benzene accelerating agent, hindered phenol are added in into cleaning, dry B agitator tanks
Class antioxidant, auxiliary anti-oxidant, silane coupling agent and releasing agent are stirred 15 minutes with 500 revs/min of mixing speed（Normal
Temperature is lower to be stirred）, obtain the first mixed liquor；
（4）The first mixed liquor in B agitator tanks is introduced by conduit in A agitator tanks, is stirred at a temperature of 110 DEG C
（The material in A agitator tanks is heated, its temperature is made to be maintained at 110 DEG C）, mixing speed is 500 revs/min, and mixing time is
8 minutes, obtain the second mixed liquor；
（5）The second mixed liquor is added to double screw extruder by feed hopper to squeeze out, 30 DEG C is subsequently cooled to, obtains sheet
Resisting high-temperature yellowing transparent epoxy moulding compound（The material that extruder squeezes out cool down the methods of can be used curtain coating, calendering and shape
Slabbing material）, then the resisting high-temperature yellowing transparent epoxy moulding compound of sheet is ground into particulate material, then particulate material is pulverized
End material, to powder materials except after magnetic, you can obtain the transparent epoxy moulding compound of powdered resisting high-temperature yellowing.
The transparent epoxy moulding compound of obtained powdered resisting high-temperature yellowing can be pressed into pie, to store in a warehouse, to transport
With use.
Above-mentioned superbrnaching end-hydroxy resin structure is as follows：
Embodiment 3
In the present embodiment, the preparation method of the transparent epoxy moulding compound of resisting high-temperature yellowing includes the following steps：
（1）By weight, following raw materials are equipped with：Cycloaliphatic epoxy resin 45.48%（Its cyclohexane -1,2- dicarboxylic acids two shrinks
Glyceride 31.84%, 4,5- 7-oxa-bicyclo[4.1.0s -1,2- dicarboxylic acid diglycidyl ester 13.64%）, phthalic anhydride curing agent 37.4%（
For 4- methyl tetrahydro phthalic anhydrides）, alcohols ring opening agent 5%（Wherein ethylene glycol 3%, glycerine 2%）, the system of phosphorus containing benzene accelerating agent 0.1%（It is
Triphenyl ethyl phosphonium bromide phosphine）, hindered phenol anti-oxidants 0.5%（Be β-（3,5- di-tert-butyl-hydroxy phenyls）Propionic acid is just
Octadecanol ester）, auxiliary anti-oxidant 0.02%（It is three [2.4- di-tert-butyl-phenyls] phosphite esters）, silane coupling agent 1%（It is
γ-glycidyl ether oxygen propyl trimethoxy silicane）, releasing agent 0.5%（It is magnesium stearate）, superbrnaching end-hydroxy resin
10%；
（2）Cycloaliphatic epoxy resin and superbrnaching end-hydroxy tree are added in into cleaning, A agitator tanks that are dry and carrying heating unit
Fat, and it is warming up to 105 DEG C（The material in A agitator tanks is heated, its temperature is made to rise to 105 DEG C）, with 400 revs/min stir
Speed is mixed to stir 15 minutes；
（3）Phthalic anhydride curing agent, alcohols ring opening agent, the system of phosphorus containing benzene accelerating agent, hindered phenol are added in into cleaning, dry B agitator tanks
Class antioxidant, auxiliary anti-oxidant, silane coupling agent and releasing agent are stirred 20 minutes with 300 revs/min of mixing speed（Normal
Temperature is lower to be stirred）, obtain the first mixed liquor；
（4）The first mixed liquor in B agitator tanks is introduced by conduit in A agitator tanks, is stirred at a temperature of 105 DEG C
（The material in A agitator tanks is heated, its temperature is made to be maintained at 105 DEG C）, mixing speed is 400 revs/min, and mixing time is
12 minutes, obtain the second mixed liquor；
（5）The second mixed liquor is added to double screw extruder by feed hopper to squeeze out, 25 DEG C is subsequently cooled to, obtains sheet
Resisting high-temperature yellowing transparent epoxy moulding compound（The material that extruder squeezes out cool down the methods of can be used curtain coating, calendering and shape
Slabbing material）, then the resisting high-temperature yellowing transparent epoxy moulding compound of sheet is ground into particulate material, then particulate material is pulverized
End material, to powder materials except after magnetic, you can obtain the transparent epoxy moulding compound of powdered resisting high-temperature yellowing.
The transparent epoxy moulding compound of obtained powdered resisting high-temperature yellowing can be pressed into pie, to store in a warehouse, to transport
With use.
The structural formula of above-mentioned superbrnaching end-hydroxy resin is as follows：
Embodiment 4
In the present embodiment, the preparation method of the transparent epoxy moulding compound of resisting high-temperature yellowing includes the following steps：
（1）By weight, following raw materials are equipped with：Cycloaliphatic epoxy resin 52.35%（Wherein poly- [(2- Oxyranyles) -1,2-
Cyclohexanediol] 2- ethyls -2- (methylol) -1,3- propylene glycols (3:1) 31.41%, 4- vinyl -1- cyclohexene diepoxies
Compound 20.94%）, phthalic anhydride curing agent 37.4%（Wherein 4- methyl hexahydrophthalic anhydrides 18.7%, 4- methyl tetrahydro phthalic anhydrides 18.7%）, alcohols
Ring opening agent 2%（It is glycerine）, the system of phosphorus containing benzene accelerating agent 0.4%（It is triphenyl ethyl phosphonium bromide phosphine）, Hinered phenols are anti-oxidant
Agent 1%（Be β-（3,5- di-tert-butyl-hydroxy phenyls）The positive octadecanol ester of propionic acid）, auxiliary anti-oxidant 0.05%（It is three
[2.4- di-tert-butyl-phenyls] phosphite ester）, silane coupling agent 0.5%（It is γ-aminopropyl triethoxysilane）, releasing agent
0.3%（It is magnesium stearate）, superbrnaching end-hydroxy resin 6%；
（2）Cycloaliphatic epoxy resin and superbrnaching end-hydroxy tree are added in into cleaning, A agitator tanks that are dry and carrying heating unit
Fat, and it is warming up to 110 DEG C（The material in A agitator tanks is heated, its temperature is made to rise to 110 DEG C）, with 400 revs/min stir
Speed is mixed to stir 15 minutes；
（3）Phthalic anhydride curing agent, alcohols ring opening agent, the system of phosphorus containing benzene accelerating agent, hindered phenol are added in into cleaning, dry B agitator tanks
Class antioxidant, auxiliary anti-oxidant, silane coupling agent and releasing agent are stirred 10 minutes with 300 revs/min of mixing speed（Normal
Temperature is lower to be stirred）, obtain the first mixed liquor；
（4）The first mixed liquor in B agitator tanks is introduced by conduit in A agitator tanks, is stirred at a temperature of 110 DEG C
（The material in A agitator tanks is heated, its temperature is made to be maintained at 110 DEG C）, mixing speed is 400 revs/min, and mixing time is
10 minutes, obtain the second mixed liquor；
（5）The second mixed liquor is added to double screw extruder by feed hopper to squeeze out, 28 DEG C is subsequently cooled to, obtains sheet
Resisting high-temperature yellowing transparent epoxy moulding compound（The material that extruder squeezes out cool down the methods of can be used curtain coating, calendering and shape
Slabbing material）, then the resisting high-temperature yellowing transparent epoxy moulding compound of sheet is ground into particulate material, then particulate material is pulverized
End material, to powder materials except after magnetic, you can obtain the transparent epoxy moulding compound of powdered resisting high-temperature yellowing.
The transparent epoxy moulding compound of obtained powdered resisting high-temperature yellowing can be pressed into pie, to store in a warehouse, to transport
With use.
The structural formula of above-mentioned superbrnaching end-hydroxy resin is as follows：
Comparative example
The preparation method of the epoxy molding plastic of comparative example includes the following steps：
（1）By weight, following raw materials are equipped with：Novolac epoxy resin 52.22%, phenolic resin 35.76%, glycerine 4%, triphen
Ylmethyl bromide phosphine 0.2%, β-（3,5- di-tert-butyl-hydroxy phenyls）The positive octadecanol ester 0.5% of propionic acid, three nonyl phenyl are sub-
Phosphoesterase 30 .02%, γ-aminopropyl triethoxysilane 0.5%, zinc stearate 0.8%, liquid nbr carboxyl terminal 6%；
（2）Novolac epoxy resin and liquid end carboxyl butyronitrile rubber are added in into cleaning, A agitator tanks that are dry and carrying heating unit
Glue, and it is warming up to 100 DEG C（The material in A agitator tanks is heated, its temperature is made to rise to 100 DEG C）, with 500 revs/min stir
Speed is mixed to stir 10 minutes；
（3）Added in into cleaning, dry B agitator tanks phenolic resin, glycerine, triphenylmethylphosphonium bromide phosphine, β-（Bis- uncles of 3,5-
Butyl -4- hydroxy phenyls）The positive octadecanol ester of propionic acid, trisnonylphenyl phosphite, γ-aminopropyl triethoxysilane and
Zinc stearate is stirred 10 minutes with 500 revs/min of mixing speed（It stirs at normal temperatures）, obtain the first mixed liquor；
（4）The first mixed liquor in B agitator tanks is introduced by conduit in A agitator tanks, is stirred at a temperature of 100 DEG C
（The material in A agitator tanks is heated, its temperature is made to be maintained at 100 DEG C）, mixing speed is 500 revs/min, and mixing time is
10 minutes, obtain the second mixed liquor；
（5）The second mixed liquor is added to double screw extruder by feed hopper to squeeze out, 20 DEG C is subsequently cooled to, obtains sheet
Epoxy molding plastic（The methods of curtain coating, calendering can be used cools down the material that extruder squeezes out and forms sheet material）, then will
The epoxy molding plastic of sheet is ground into particulate material, then by particulate material grind into powder material, to powder materials except after magnetic, you can obtain
Powdered epoxy molding plastic.
The epoxy molding plastic of transparent epoxy moulding compound, comparative example to above example 1-4 is tested for the property, test method and
Test result is as follows：
1st, glass transition temperature is tested
It is carried out according to ISO 11359-2-1999 standards, using the Q20 type differential scanning calorimeter gathered datas of TA companies of the U.S..
2nd, light transmittance is tested
Using the U3900H type ultra-violet and visible spectrophotometer gathered datas of Japanese HITACHI companies.
3rd, bending strength and bending modulus test
It is carried out according to 9341 standards of GB/T, using the TY-8000 type servo-control systems of Jiangsu Tian Yuan testing equipments Co., Ltd
Universal testing machine gathered data.
4th, shearing strength is tested
It is carried out according to SEMI G69-0996 standards, using the TY-8000 type SERVO CONTROLs of Jiangsu Tian Yuan testing equipments Co., Ltd
System universal testing machine gathered data.
After tested, the performance of the epoxy molding plastic of the transparent epoxy moulding compound and comparative example of above-described embodiment 1,2,3,4 is such as
Shown in table 1.
Table 1
Test result is shown：The light transmittance of the transparent epoxy moulding compound of 1-4 of the embodiment of the present invention is high, particularly through a long time high temperature
Afterwards, the transparent epoxy moulding compound of 1-4 of the embodiment of the present invention remains to keep high transparency；The transparent epoxy of 1-4 of the embodiment of the present invention
The resisting high-temperature yellowing of moulding compound is had excellent performance, and is still not in Yellowing after through a long time high temperature.And the epoxy mould of comparative example
Plastic light-transmission rate is relatively low, and after similary time high temperature, transmitance is decreased obviously, and more serious Yellowing occurs.
Claims (10)
1. the transparent epoxy moulding compound of a kind of resisting high-temperature yellowing, it is characterised in that the raw material matched by following weight is made：Alicyclic ring
Race epoxy resin 31-60%, phthalic anhydride curing agent 30-50%, alcohols ring opening agent 2-5%, the system of phosphorus containing benzene accelerating agent 0.1-1%, hindered phenol
Class antioxidant 0.1-1%, auxiliary anti-oxidant 0.01-0.05%, silane coupling agent 0.1-1%, releasing agent 0.1-1%, terminal hydroxy group over-expense
Change resin 2-10%.
2. the transparent epoxy moulding compound of resisting high-temperature yellowing according to claim 1, it is characterized in that：The alicyclic epoxy tree
Fat is poly- [(2- Oxyranyles) -1,2- cyclohexanediols] 2- ethyls -2- (methylol) -1,3- propylene glycols (3:1), hexamethylene
Alkane-1,2- dicarboxylic acids 2-glycidyl ester, 4,5- 7-oxa-bicyclo[4.1.0-1,2- dicarboxylic acid diglycidyl esters and 4- vinyl-1-
One kind or many of mixture in cyclohexene dicyclic oxide.
3. the transparent epoxy moulding compound of resisting high-temperature yellowing according to claim 1, it is characterized in that：The phthalic anhydride curing agent is
The mixture of one or both of 4- methyl hexahydrophthalic anhydrides and 4- methyl tetrahydro phthalic anhydrides.
4. the transparent epoxy moulding compound of resisting high-temperature yellowing according to claim 1, it is characterized in that：The alcohols ring opening agent is
The mixture of one kind or two of which in ethylene glycol, glycerine and pentaerythrite.
5. the transparent epoxy moulding compound of resisting high-temperature yellowing according to claim 1, it is characterized in that：The system of phosphorus containing benzene promotes
Agent is the mixture of one or both of triphenylmethylphosphonium bromide phosphine and triphenyl ethyl phosphonium bromide phosphine.
6. the transparent epoxy moulding compound of resisting high-temperature yellowing according to claim 1, it is characterized in that：The Hinered phenols antioxygen
Agent be four [β-（3,5- di-tert-butyl-hydroxy phenyls）Propionic acid] pentaerythritol ester and β-（3,5- di-t-butyl -4- hydroxyls
Phenyl）The mixture of one or both of the positive octadecanol ester of propionic acid.
7. the transparent epoxy moulding compound of resisting high-temperature yellowing according to claim 1, it is characterized in that：The auxiliary anti-oxidant is three
The mixture of one or both of nonylphenylphosphite and three [2.4- di-tert-butyl-phenyls] phosphite esters.
8. the transparent epoxy moulding compound of resisting high-temperature yellowing according to claim 1, it is characterized in that：The silane coupling agent is
The mixing of one or both of γ-glycidyl ether oxygen propyl trimethoxy silicane and γ-aminopropyl triethoxysilane
Object；Above-mentioned releasing agent is the mixture of one or both of zinc stearate and magnesium stearate.
9. the transparent epoxy moulding compound of resisting high-temperature yellowing according to claim 1, it is characterized in that：The superbrnaching end-hydroxy
The structural formula of resin is following structural formula（1）-（3）In one kind：
（1）
（2）
（3）.
10. the preparation method of the transparent epoxy moulding compound of resisting high-temperature yellowing described in claim 1, it is characterised in that including following
Step：
（1）By weight, following raw materials are equipped with：Cycloaliphatic epoxy resin 31-60%, phthalic anhydride curing agent 30-50%, alcohols ring opening agent
2-5%, the system of phosphorus containing benzene accelerating agent 0.1-1%, hindered phenol anti-oxidants 0.1-1%, auxiliary anti-oxidant 0.01-0.05% are silane coupled
Agent 0.1-1%, releasing agent 0.1-1%, superbrnaching end-hydroxy resin 2-10%；
（2）Cycloaliphatic epoxy resin and superbrnaching end-hydroxy tree are added in into cleaning, A agitator tanks that are dry and carrying heating unit
Fat, and 100-110 DEG C is warming up to, it is stirred 5-20 minutes with 300-500 revs/min of mixing speed；
（3）Phthalic anhydride curing agent, alcohols ring opening agent, the system of phosphorus containing benzene accelerating agent, hindered phenol are added in into cleaning, dry B agitator tanks
Class antioxidant, auxiliary anti-oxidant, silane coupling agent and releasing agent, with 300-500 revs/min of 5-20 points of mixing speed stirring
Clock obtains the first mixed liquor；
（4）The first mixed liquor in B agitator tanks is introduced by conduit in A agitator tanks, is stirred at a temperature of 100-110 DEG C
It mixes, mixing speed is 300-500 revs/min, and mixing time is 5-15 minutes, obtains the second mixed liquor；
（5）The second mixed liquor is added to extruder by feed hopper to squeeze out, 20-30 DEG C is subsequently cooled to, obtains the resistance to of sheet
High temperature xanthochromia transparent epoxy moulding compound, then the resisting high-temperature yellowing transparent epoxy moulding compound of sheet is ground into particulate material, then will
Particulate material grind into powder material, to powder materials except after magnetic, you can obtain the transparent epoxy moulding compound of powdered resisting high-temperature yellowing.
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| CN111117165A (en) * | 2020-01-21 | 2020-05-08 | 汕头市骏码凯撒有限公司 | Halogen-free flame-retardant transparent epoxy molding compound and preparation method thereof |
| CN116769278A (en) * | 2023-05-30 | 2023-09-19 | 江苏恒隆通新材料科技有限公司 | Medium-temperature cured flexible epoxy laminated resin |
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| CN116769278A (en) * | 2023-05-30 | 2023-09-19 | 江苏恒隆通新材料科技有限公司 | Medium-temperature cured flexible epoxy laminated resin |
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