CN105086920B - The preparation method of resistance to irradiation organic silicon packaging glue - Google Patents
The preparation method of resistance to irradiation organic silicon packaging glue Download PDFInfo
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Abstract
The present invention provides the preparation method of resistance to irradiation organic silicon packaging glue, and its step is as follows：(1) titanate coupling agent is scattered in the n-butanol aqueous solution that mass fraction is 80%, modification liquid is obtained after being stirred at room temperature, nano-cerium oxide is added into vacuum rotary steam after modification liquid magnetic agitation, condensing reflux, dry to constant weight, grinding obtains modified nano cerium oxide after taking-up；(2) by weight, the modified nano cerium oxide that polyphenyl methyl siloxane, PEEK, EMA and step (1) are obtained is added in banbury and is blended, pellet is obtained after moving to melting extrusion in single screw extrusion machine, cooling granulation；(3) by weight, the pellet that crosslinking agent, tackifier and step (2) are obtained adds high mixer high speed and mixed, add and continue mixed at high speed after inhibitor, add middling speed after catalyst and mix, the organic silicon packaging glue of resistance to irradiation is obtained after discharging.The organic silicon packaging glue that the present invention is prepared has good radiation-resistant property.
Description
Technical field
The present invention relates to packaging plastic, the preparation method of more particularly to resistance to irradiation organic silicon packaging glue.
Background technology
LED encapsulation in the past uses epoxy resin as encapsulating material more, however as the progress of LED technology, asphalt mixtures modified by epoxy resin
Fat is due to easy yellow at high temperature, and the shortcomings of UV resistance is poor can not meet the requirement of high power LED package, and organosilicon
Resin has the advantages that excellent thermostability, pliability, water resistance, weatherability, anti-flammability and low-surface-energy, becomes
The ideal material that current LED encapsulation is used.With the continuous progress of LED technology, the application scenario of organic silicon packaging glue is increasingly
Extensively, wherein the application in larger environment is radiated is also more and more, radiation in this case can cause organosilicon to encapsulate
The aging of glue, the chemical bond that emittance especially γ irradiation can be destroyed in silicone molecules chain, causes the degraded of strand, leads
Mechanical properties decrease is caused than more serious.
Publication No. CN104232009A, publication date are 2014.12.24, apply for the limited public affairs of artificial Chinese Academy of Sciences Guangzhou chemistry
The Chinese patent of compass in ancient China hero material production base discloses " a kind of vinyl MQ resin modified organic silicon packaging plastic and preparation method
And application ", this method is by 0.5~20 mass parts vinyl MQ resin, 100 mass parts containing hydrogen silicone oils and 100~500 mass first
Benzene is mixed, under the protection of nitrogen, adds 0.0002~0.005 mass parts Cattell catalyst, is rotated after being heated to reflux, is obtained MQ
The polysiloxane polymer of resin graft modification；By the polysiloxane polymer of 100 mass parts MQ resin graft modifications, 20~80
The vinyl silicone oil of mass parts first and 2~8 the second vinyl silicone oils of mass parts are well mixed, add 0.0002~0.005 mass
Part Cattell catalyst, pours into mould after stirring, extracts bubble, places, and then solidifies 2~5h at 80~150 DEG C, cold
But it is stripped, obtains vinyl MQ resin modified organic silicon packaging plastic.The organic silicon packaging glue is free of organic solvent, to environment friend
Good, and solidfied material is water white transparency, light transmittance is up to more than 94%, and refractive index also reaches 1.432, but its with it is existing organic
Silicon packaging plastic equally has the problem of radiation-resistant property is not good.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of resistance to irradiation organic silicon packaging glue, prepare
Organic silicon packaging glue has good radiation-resistant property.
In order to solve the above technical problems, the technical scheme is that：
The preparation method of resistance to irradiation organic silicon packaging glue, its step is as follows：
(1) titanate coupling agent is scattered in the n-butanol aqueous solution that mass fraction is 80%, be stirred at room temperature 40 minutes
After obtain modification liquid, nano-cerium oxide is added into modification liquid magnetic agitation 2 hours at 70 DEG C, condensing reflux is depressurized after 1 hour
Revolving 30 minutes, moves in vacuum drying chamber and dries to constant weight, and grinding obtains modified nano cerium oxide after taking-up；
(2) by weight, by 100 parts of polyphenyl methyl siloxanes, 10-12 parts of PEEK, 3-4 parts of EMAs
And the modified nano cerium oxide that 0.8-1.2 parts of steps (1) obtain adds blending 12 minutes in banbury, moves to Single screw extrusion
Pellet is obtained after melting extrusion in machine, cooling granulation；
(3) by weight, pellet 5-10 parts of crosslinking agents, 2-4 parts of tackifiers and 115 parts of steps (2) obtained adds
Enter high mixer high speed to mix 60 minutes, add after 0.1-0.2 parts of inhibitor and continue mixed at high speed 16 minutes, add 0.3-0.5
Middling speed is mixed 40 minutes after part catalyst, and the organic silicon packaging glue of resistance to irradiation is obtained after discharging.
Preferably, in step (1) of the present invention, the weight of titanate coupling agent is the 9% of nano-cerium oxide.
Preferably, in step (2) of the present invention, temperature during blending is 210 DEG C, and rotating speed is 100rpm.
Preferably, in step (2) of the present invention, the temperature of melting extrusion is 190-220 DEG C, the spiral shell of single screw extrusion machine
Bar rotating speed is 40rpm.
Preferably, in step (3) of the present invention, crosslinking agent is ethyl triethoxysilane.
Preferably, in step (3) of the present invention, tackifier is triethoxysilane.
Preferably, in step (3) of the present invention, inhibitor is alkynol.
Preferably, in step (3) of the present invention, rotating speed during mixed at high speed is 2800rpm.
Preferably, in step (3) of the present invention, catalyst is chloroplatinic acid.
Preferably, in step (3) of the present invention, rotating speed when middling speed is mixed is 1200rpm.
Compared with prior art, the invention has the advantages that：
1) nano-cerium oxide is a kind of rare earth oxide, with special electronic structure, and cerium ion has two kinds of valence states ---
Trivalent and tetravalence, trivalent cerium ion can capture positive cave caused by irradiation, and tetravalence cerium ion can capture electronics caused by irradiation, from
And weaken irradiation energy significantly, but the surface-active of nano-cerium oxide is high and in hydrophily, causes it easily to reunite, and organic
Silicon substrate compatability is poor, therefore the present invention is modified by titanate coupling agent to it, titanate coupling agent and nano oxygen
Change cerium and generate chemical bonding, and clad is formd on nano-cerium oxide surface, reduce its surface energy, and titanate esters are even
Connection agent on lipophilic group made the hydrophily on nano-cerium oxide surface into lipophile, improve nano-cerium oxide surface with
Compatibility between organic silicon substrate, so as to effectively improve the radiation-resistant property of packaging plastic.
2) PEEK is that the height that the repeat unit containing a ketonic bond and two ehter bonds in backbone structure is constituted gathers
Thing --- also contain aromatic ring in polyether-ether-ketone, and structure, therefore with good radioresistance, in bulking agent-methacrylic acid
Under the compatibilization of ethyl ester, PEEK can be well dispersed in organic silicon substrate and formed interface is preferably blended, from
And further improve the radiation-resistant property of packaging plastic；In addition, PEEK also has good hydrolytic resistance and anti-flammability, therefore may be used also
Effectively improve the anti-hydrolytic performance and fire resistance of packaging plastic.
Embodiment：
Describe the present invention in detail below in conjunction with specific embodiment, herein illustrative examples and explanation of the invention
For explaining the present invention, but it is not as a limitation of the invention.
Embodiment 1
The preparation method of resistance to irradiation organic silicon packaging glue, its step is as follows：
(1) titanate coupling agent is scattered in the n-butanol aqueous solution that mass fraction is 80%, be stirred at room temperature 40 minutes
After obtain modification liquid, nano-cerium oxide is added into modification liquid magnetic agitation 2 hours at 70 DEG C, condensing reflux is depressurized after 1 hour
Revolving 30 minutes, moves in vacuum drying chamber and dries to constant weight, and grinding obtains modified nano cerium oxide after taking-up, wherein, metatitanic acid
The weight of ester coupling agent is the 9% of nano-cerium oxide；
(2) by weight, by 100 parts of polyphenyl methyl siloxanes, 10.5 parts of PEEK, 3 parts of EMAs with
And it is 210 DEG C that the obtained modified nano cerium oxide of 0.9 part of step (1), which adds temperature in banbury, rotating speed is to be blended under 100rpm
10 minutes, it was melting extrusion at 190-220 DEG C to move to temperature in single screw extrusion machine, and the screw speed of single screw extrusion machine is
Pellet is obtained after 40rpm, cooling granulation；
(3) by weight, by 10 parts of ethyl triethoxysilanes, 2.5 parts of triethoxysilanes and 115 parts of steps
(2) pellet obtained adds high mixer high speed and mixed 60 minutes, and it is high under 2800rpm to add continuation rotating speed after 0.1 part of alkynol
Speed mixing 16 minutes, adds rotating speed after 0.5 part of chloroplatinic acid and is mixed 40 minutes for middling speed under 1200rpm, resistance to irradiation is obtained after discharging
Organic silicon packaging glue.
Embodiment 2
The preparation method of resistance to irradiation organic silicon packaging glue, its step is as follows：
(1) titanate coupling agent is scattered in the n-butanol aqueous solution that mass fraction is 80%, be stirred at room temperature 40 minutes
After obtain modification liquid, nano-cerium oxide is added into modification liquid magnetic agitation 2 hours at 70 DEG C, condensing reflux is depressurized after 1 hour
Revolving 30 minutes, moves in vacuum drying chamber and dries to constant weight, and grinding obtains modified nano cerium oxide after taking-up, wherein, metatitanic acid
The weight of ester coupling agent is the 9% of nano-cerium oxide；
(2) by weight, by 100 parts of polyphenyl methyl siloxanes, 10 parts of PEEK, 3.6 parts of EMAs with
And it is 210 DEG C that the obtained modified nano cerium oxide of 1. parts of steps (1), which adds temperature in banbury, rotating speed is to be blended 10 under 100rpm
Minute, it is melting extrusion at 190-220 DEG C to move to temperature in single screw extrusion machine, and the screw speed of single screw extrusion machine is
Pellet is obtained after 40rpm, cooling granulation；
(3) by weight, by 8 parts of ethyl triethoxysilanes, 3.5 parts of triethoxysilanes and 115 parts of steps (2)
Obtained pellet adds high mixer high speed and mixed 60 minutes, adds after 0.2 part of alkynol and continues rotating speed to mix at a high speed under 2800rpm
Close 16 minutes, add rotating speed after 0.4 part of chloroplatinic acid and mixed 40 minutes for middling speed under 1200rpm, resistance to irradiation is obtained after discharging organic
Silicon packaging plastic.
Embodiment 3
The preparation method of resistance to irradiation organic silicon packaging glue, its step is as follows：
(1) titanate coupling agent is scattered in the n-butanol aqueous solution that mass fraction is 80%, be stirred at room temperature 40 minutes
After obtain modification liquid, nano-cerium oxide is added into modification liquid magnetic agitation 2 hours at 70 DEG C, condensing reflux is depressurized after 1 hour
Revolving 30 minutes, moves in vacuum drying chamber and dries to constant weight, and grinding obtains modified nano cerium oxide after taking-up, wherein, metatitanic acid
The weight of ester coupling agent is the 9% of nano-cerium oxide；
(2) by weight, by 100 parts of polyphenyl methyl siloxanes, 11 parts of PEEK, 3.2 parts of EMAs with
And it is 210 DEG C that the obtained modified nano cerium oxide of 1 part of step (1), which adds temperature in banbury, rotating speed is to be blended 10 under 100rpm
Minute, it is melting extrusion at 190-220 DEG C to move to temperature in single screw extrusion machine, and the screw speed of single screw extrusion machine is
Pellet is obtained after 40rpm, cooling granulation；
(3) by weight, 6 parts of ethyl triethoxysilanes, 3 parts of triethoxysilanes and 115 parts of steps (2) are obtained
The pellet arrived adds high mixer high speed and mixed 60 minutes, and it is mixed at high speed under 2800rpm to add continuation rotating speed after 0.2 part of alkynol
16 minutes, add rotating speed after 0.4 part of chloroplatinic acid and mixed 40 minutes for middling speed under 1200rpm, the organosilicon of resistance to irradiation is obtained after discharging
Packaging plastic.
Embodiment 4
The preparation method of resistance to irradiation organic silicon packaging glue, its step is as follows：
(1) titanate coupling agent is scattered in the n-butanol aqueous solution that mass fraction is 80%, be stirred at room temperature 40 minutes
After obtain modification liquid, nano-cerium oxide is added into modification liquid magnetic agitation 2 hours at 70 DEG C, condensing reflux is depressurized after 1 hour
Revolving 30 minutes, moves in vacuum drying chamber and dries to constant weight, and grinding obtains modified nano cerium oxide after taking-up, wherein, metatitanic acid
The weight of ester coupling agent is the 9% of nano-cerium oxide；
(2) by weight, by 100 parts of polyphenyl methyl siloxanes, 12 parts of PEEK, 3.5 parts of EMAs with
And it is 210 DEG C that the obtained modified nano cerium oxide of 0.8 part of step (1), which adds temperature in banbury, rotating speed is to be blended under 100rpm
10 minutes, it was melting extrusion at 190-220 DEG C to move to temperature in single screw extrusion machine, and the screw speed of single screw extrusion machine is
Pellet is obtained after 40rpm, cooling granulation；
(3) by weight, 9 parts of ethyl triethoxysilanes, 4 parts of triethoxysilanes and 115 parts of steps (2) are obtained
The pellet arrived adds high mixer high speed and mixed 60 minutes, and it is mixed at high speed under 2800rpm to add continuation rotating speed after 0.2 part of alkynol
16 minutes, add rotating speed after 0.3 part of chloroplatinic acid and mixed 40 minutes for middling speed under 1200rpm, the organosilicon of resistance to irradiation is obtained after discharging
Packaging plastic.
Embodiment 5
The preparation method of resistance to irradiation organic silicon packaging glue, its step is as follows：
(1) titanate coupling agent is scattered in the n-butanol aqueous solution that mass fraction is 80%, be stirred at room temperature 40 minutes
After obtain modification liquid, nano-cerium oxide is added into modification liquid magnetic agitation 2 hours at 70 DEG C, condensing reflux is depressurized after 1 hour
Revolving 30 minutes, moves in vacuum drying chamber and dries to constant weight, and grinding obtains modified nano cerium oxide after taking-up, wherein, metatitanic acid
The weight of ester coupling agent is the 9% of nano-cerium oxide；
(2) by weight, by 100 parts of polyphenyl methyl siloxanes, 11.5 parts of PEEK, 4 parts of EMAs with
And it is 210 DEG C that the obtained modified nano cerium oxide of 1 part of step (1), which adds temperature in banbury, rotating speed is to be blended 10 under 100rpm
Minute, it is melting extrusion at 190-220 DEG C to move to temperature in single screw extrusion machine, and the screw speed of single screw extrusion machine is
Pellet is obtained after 40rpm, cooling granulation；
(3) by weight, by 7 parts of ethyl triethoxysilanes, 2.4 parts of triethoxysilanes and 115 parts of steps (2)
Obtained pellet adds high mixer high speed and mixed 60 minutes, adds after 0.1 part of alkynol and continues rotating speed to mix at a high speed under 2800rpm
Close 16 minutes, add rotating speed after 0.3 part of chloroplatinic acid and mixed 40 minutes for middling speed under 1200rpm, resistance to irradiation is obtained after discharging organic
Silicon packaging plastic.
Embodiment 6
The preparation method of resistance to irradiation organic silicon packaging glue, its step is as follows：
(1) titanate coupling agent is scattered in the n-butanol aqueous solution that mass fraction is 80%, be stirred at room temperature 40 minutes
After obtain modification liquid, nano-cerium oxide is added into modification liquid magnetic agitation 2 hours at 70 DEG C, condensing reflux is depressurized after 1 hour
Revolving 30 minutes, moves in vacuum drying chamber and dries to constant weight, and grinding obtains modified nano cerium oxide after taking-up, wherein, metatitanic acid
The weight of ester coupling agent is the 9% of nano-cerium oxide；
(2) by weight, by 100 parts of polyphenyl methyl siloxanes, 10.8 parts of PEEK, 3.4 parts of EMAs
And it is 210 DEG C that the obtained modified nano cerium oxide of 1.1 parts of steps (1), which adds temperature in banbury, rotating speed be under 100rpm altogether
Mixed 10 minutes, it is melting extrusion at 190-220 DEG C to move to temperature in single screw extrusion machine, and the screw speed of single screw extrusion machine is
Pellet is obtained after 40rpm, cooling granulation；
(3) by weight, 5 parts of ethyl triethoxysilanes, 4 parts of triethoxysilanes and 115 parts of steps (2) are obtained
The pellet arrived adds high mixer high speed and mixed 60 minutes, and it is mixed at high speed under 2800rpm to add continuation rotating speed after 0.1 part of alkynol
16 minutes, add rotating speed after 0.5 part of chloroplatinic acid and mixed 40 minutes for middling speed under 1200rpm, the organosilicon of resistance to irradiation is obtained after discharging
Packaging plastic.
After tested, organic silicon packaging glue made from embodiment 1-6 and the radiation-resistant property of comparative example are as shown in the table, its
In：Comparative example is Publication No. CN104232009A patent；
Radiation-resistant property test process is：Co-60 is used to be irradiated for radioactive source to each packaging plastic, close rate is
100Gy/min, accumulated dose is 6 × 105Gy, temperature be 70 DEG C, measured after irradiation each packaging plastic tensile strength rate of descent and
Elongation at break rate of descent.
As seen from the above table, tensile strength rate of descent of the organic silicon packaging glue made from 1-6 of the present invention after irradiation and
Elongation at break rate of descent is significantly lower than comparative example, shows preferable radiation-resistant property.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
Know the personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete without departing from disclosed spirit and institute under technological thought such as
Into all equivalent modifications or change, should by the present invention claim be covered.
Claims (8)
1. the preparation method of resistance to irradiation organic silicon packaging glue, it is characterised in that comprise the following steps：
(1) titanate coupling agent is scattered in the n-butanol aqueous solution that mass fraction is 80%, is stirred at room temperature after 40 minutes and obtains
To modification liquid, by magnetic agitation 2 hours, condensing reflux vacuum rotary steam after 1 hour in nano-cerium oxide addition modification liquid 70 DEG C
30 minutes, move in vacuum drying chamber and dry to constant weight, grinding obtains modified nano cerium oxide after taking-up；
(2) by weight, by 100 parts of polyphenyl methyl siloxanes, 10-12 parts of PEEK, 3-4 parts of EMAs and
The modified nano cerium oxide that 0.8-1.2 parts of steps (1) obtain is added in banbury and is blended 12 minutes, is moved in single screw extrusion machine
Pellet is obtained after melting extrusion, cooling granulation；
(3) by weight, pellet 5-10 parts of crosslinking agents, 2-4 parts of tackifiers and 115 parts of steps (2) obtained adds high
Mixed machine high speed is mixed 60 minutes, is added after 0.1-0.2 parts of inhibitor and is continued mixed at high speed 16 minutes, adds 0.3-0.5 parts and urge
Middling speed is mixed 40 minutes after agent, and the organic silicon packaging glue of resistance to irradiation is obtained after discharging；
In the step (3), rotating speed during mixed at high speed is 2800rpm, and rotating speed when middling speed is mixed is 1200rpm.
2. the preparation method of resistance to irradiation organic silicon packaging glue according to claim 1, it is characterised in that：The step (1)
In, the weight of titanate coupling agent is the 9% of nano-cerium oxide.
3. the preparation method of resistance to irradiation organic silicon packaging glue according to claim 1, it is characterised in that：The step (2)
In, temperature during blending is 210 DEG C, and rotating speed is 100rpm.
4. the preparation method of resistance to irradiation organic silicon packaging glue according to claim 1, it is characterised in that：The step (2)
In, the temperature of melting extrusion is 190-220 DEG C, and the screw speed of single screw extrusion machine is 40rpm.
5. the preparation method of resistance to irradiation organic silicon packaging glue according to claim 1, it is characterised in that：The step (3)
In, crosslinking agent is ethyl triethoxysilane.
6. the preparation method of resistance to irradiation organic silicon packaging glue according to claim 1, it is characterised in that：The step (3)
In, tackifier is triethoxysilane.
7. the preparation method of resistance to irradiation organic silicon packaging glue according to claim 1, it is characterised in that：The step (3)
In, inhibitor is alkynol.
8. the preparation method of resistance to irradiation organic silicon packaging glue according to claim 1, it is characterised in that：The step (3)
In, catalyst is chloroplatinic acid.
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| CN105907342A (en) * | 2016-05-06 | 2016-08-31 | 烟台图文马克化工科技有限公司 | Silicone sealant for aluminum-sheet curtain wall |
| CN106046800B (en) * | 2016-07-18 | 2019-05-14 | 东莞市良展有机硅科技有限公司 | A kind of bi-component high abrasion add-on type liquid silicon rubber and preparation method thereof |
| CN106065184A (en) * | 2016-08-19 | 2016-11-02 | 张志文 | A kind of high folding modified silica-gel material for chip package |
| CN108156675B (en) * | 2017-12-20 | 2021-04-20 | 广东暖丰电热科技有限公司 | Electrothermal film sol and preparation method thereof |
| CN110157072A (en) * | 2019-05-22 | 2019-08-23 | 东莞华尔泰装饰材料有限公司 | A kind of fireproof aluminum-plastic board containing nano-meter flame retardants and its dedicated core material |
| CN115295269B (en) * | 2022-08-14 | 2024-04-19 | 重庆大学 | Irradiation-resistant magnetorheological fluid with high shear yield stress under low magnetic field |
| CN117024925B (en) * | 2023-10-10 | 2024-01-05 | 山东龙兴塑膜科技股份有限公司 | Modified polyester and application thereof in high-temperature-resistant polyester film for carbon tape printing |
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| CN101531789B (en) * | 2009-04-20 | 2011-10-19 | 宝胜科技创新股份有限公司 | Radiation-resistant halogen-free low smoke flame retardant insulating material for cables of nuclear power plants and preparation method |
| CN101735620B (en) * | 2009-12-27 | 2011-08-03 | 周忠坤 | High-temperature resisting methyl vinyl silicone rubber |
| CN101768362B (en) * | 2010-01-12 | 2012-01-04 | 山东大学 | Condensed room temperature vulcanized silicone rubber with radiation-resistant property and preparation method thereof |
| WO2013103537A1 (en) * | 2012-01-04 | 2013-07-11 | Momentive Performance Materials Inc. | Silicone adhesive compositions |
| CN103242801B (en) * | 2013-05-14 | 2015-03-11 | 汕头市骏码凯撒有限公司 | Single-component high-refractivity LED (light-emitting diode) packaging adhesive and preparation method thereof |
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