CN103059301A - Phenyl hydrogenous reticular silicone resin for encapsulating LED (Light Emitting Diode) and preparation method thereof - Google Patents
Phenyl hydrogenous reticular silicone resin for encapsulating LED (Light Emitting Diode) and preparation method thereof Download PDFInfo
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- CN103059301A CN103059301A CN2012105323132A CN201210532313A CN103059301A CN 103059301 A CN103059301 A CN 103059301A CN 2012105323132 A CN2012105323132 A CN 2012105323132A CN 201210532313 A CN201210532313 A CN 201210532313A CN 103059301 A CN103059301 A CN 103059301A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Abstract
The invention relates to the field of organic silicon materials, disclosing high-refractive index phenyl hydrogenous reticular silicone resin for encapsulating an LED (Light Emitting Diode) and a preparation method thereof. The organic silicon resin is the phenyl hydrogenous organic silicone resin with a reticular structure. According to the preparation method, alkoxy silane is used for replacing chlorosilane in the prior art, and a non-toxic harmless extraction agent is used for replacing toluene in the prior art, so that human bodies cannot be damaged, and the environment cannot be polluted. The phenyl hydrogenous organic silicon resin provided by the invention not only has the characteristics of high refractive index, high light transmittance, high clearness and transparency and the like, but also has higher compatibility and dispersibility. Hydrogen can make a platinum addition reaction and peroxide initiate a cross-linking reaction so as to make silicone rubber have excellent performance such as high resilience, tearing resistance, impact resistance, heat resistance, radiation resistance, and long service life.
Description
Technical field
The present invention relates to the organic silica gel Material Field, is a kind of silicone resin for LED encapsulation and preparation method thereof specifically.
Background technology
LED(Lighting Emitting Diode) being led lighting, is a kind of light emitting semiconductor device.The light-emitting devices such as photodiode (LED) are emerging environmental protection light sources, and actively promote the use of countries in the world.And for the luminous element encapsulation of the type material, except requiring to possess from the function of outer protection luminous element, for the brightness that prevents luminous element reduces, also require to possess the transparency of height.
At present, mainly to adopt the Resins, epoxy with good transparency be packaged material to the LED packaged material.Use Resins, epoxy as the LED of packaged material behind life-time service owing under the UV-irradiation of led chip emission, can xanthochromia occur inevitably, cause its transmittance to descend Dimming.Based on more and more higher to the requirement of LED packaged material, Resins, epoxy can not satisfy the encapsulation requirement of LED.Through the years of researches development, have and adopt the organic silica gel material (patent No. is CN101414655) with high refractive index, optical throughput can improve 5-8%.The LED product of the encapsulation that silicone resin material is made, it is good to have high-clarity (transmittance is greater than 95%), radiation hardness, thermotolerance, shine for a long time without xanthochromia, can not crack through high temperature, greatly prolong the work-ing life of LED packaged material and the superior advantages such as cementability, its performance is far superior to Resins, epoxy.Along with development trend now, the energy in short supply, putting before environmental protection and the strategy of sustainable development, increasing Resins, epoxy will be replaced by silicone resin.
The organic silica gel material is divided into two types: a kind of is the methylsiloxane glue material of low-refraction, and another kind is the phenyl organosilicon material with high refractive index.The organic silica gel material that generally uses on the market mainly is the methylsiloxane glue material, and current power-type LED because the specific refractory power of methylsiloxane glue material is low, can not satisfy power type LED encapsulation just in flourish and widespread use fully.Phenyl organic silica gel material has the characteristics such as high refractive index, thermotolerance be good, and the LED packaged material that more is applicable to power-type than methylsiloxane glue material uses.
The hydrogeneous organic silica gel material of phenyl of report all is to use phenyl hydrogen-containing silicon oil both at home and abroad.Because the molecular structure cross-linking effect of phenyl hydrogen-containing silicon oil is poor, cross-linking density is not enough, the rebound resilience that finally causes preparing the gained packaged material is poor, anti tear and anti-impact force are poor, and has the defect problems such as pollution to environment and electronic product, poor heat resistance.
Summary of the invention
In order to address the above problem, the invention provides a kind ofly have that high refractive index, high transmission rate, clear, rebound resilience are good, the hydrogeneous cancellated silicone resin of phenyl of the excellent properties such as anti tear, anti-impact force, thermotolerance are good, radiation hardness, long service life.
The present invention is achieved in that
Silicone resin is used in a kind of LED encapsulation, and described silicone resin is for having the hydrogeneous silicone resin of cancellated phenyl.
Preferably, described silicone resin is represented by following general formula:
Wherein, R, R 〞, R " ' be the straight or branched alkyl of identical or not identical 1～6 carbon atom, or be the straight or branched aryl of identical or not identical 6～20 carbon atoms, or be the aralkyl of identical or not identical 7～20 carbon atoms; R ＇ is the hydrogen base.In the hydrogeneous silicone resin of phenyl provided by the invention, its hydrogen base is at two ends, and its hydrogen base of silicone resin of the prior art is at side chain, when participating in reaction, the hydrogeneous resin reaction speed of phenyl of the present invention can be faster than silicone resin of the prior art, and reaction is also very abundant, and in fact a lot of hydrogen bases of silicone resin of the prior art fail to participate in reaction.
Preferably, R is phenyl, styroyl.R 〞, R " ' identical or not identical methyl, ethyl or phenyl, styroyl.
Another object of the present invention provides a kind of method of the environment friendly and pollution-free hydrogeneous cancellated silicone resin of the above-mentioned phenyl of preparation: described method comprises the steps:
A) under acid catalyst, drip the silane agent contain the hydrogen functional group, polyreaction is carried out in the silane agent that contains phenyl functional group;
B) add extraction agent, the hydrogeneous silicone resin of based target product phenyl, the control temperature of reaction is 50～90 ℃, the reaction times is 1～7 hour;
C) product is left standstill, the layer that anhydrates is washed neutrality with distilled water with the hydrogeneous silicone resin of phenyl, obtains being dissolved in the hydrogeneous silicone resin solution of phenyl of extraction agent;
D) with the hydrogeneous silicone resin solution of the phenyl of neutrality, be the membrane filtration of 0.5 ~ 5 μ m with the aperture after, low-boiling-point substance is removed in underpressure distillation, obtains the hydrogeneous silicone resin of phenyl.
Adopt among the present invention and contain the silane agent of phenyl functional group and polyreaction is carried out in the silane agent of hydrogeneous basic functional group, the effect of end-blocking has also been played in the silane agent of hydrogeneous basic functional group, in the reaction building-up process, reduce the use of end-capping reagent, improved effective productive rate of product.Different according to the requirement of product in building-up process, and adopt the reactants of different amounts: as if need the high silicone resin of hardness, then to adopt the high reactant of hydrogen content or increase the reacting weight of hydrogeneous functional silanes agent; Otherwise, then adopt the low reactant of hydrogen content or reduce the reacting weight of hydrogeneous functional silanes agent.
Preferably, the described structural formula that contains the silane agent of phenyl functional group is: R
1(R
2O)
3Si, wherein, R
1Be the straight or branched aryl of 6～20 carbon atoms or the aralkyl of 7～20 carbon atoms; R
2Straight or branched alkyl, acyloxy for 1-6 carbon atom.The described silane agent that contains phenyl functional group can for but be not limited to as follows:
Phenyl triethoxysilane;
Styroyl (trimethoxy) silane;
Phenyltrimethoxysila,e;
Phenylbenzene diethoxy siloxanes;
The phenyl methyl diethoxy silane;
The styroyl methylsiloxane.
Preferably, the structural formula of the described hydrogen functional group's of containing silane agent is:
Wherein, R
1, R
2, R
3, R
4Straight or branched alkyl or the straight or branched aryl of 6～20 carbon atoms or the aralkyl of 7～20 carbon atoms for 1～6 identical or not identical carbon atom; N is 1～20 round values.
The silane agent of described hydrogeneous basic functional group can for but be not limited to as follows:
Tetramethyl disiloxane;
Decamethyl dihydro five siloxanes.
Preferably, described extraction agent is isomeric alkane or methyl oligosiloxane.Isomeric alkane can for but be not limited to listed Permethyl 99A., isohexadecane; The methyl oligosiloxane can for but be not limited to listed hexamethyldisiloxane, decamethyl tetrasiloxane.
Optionally, a) step is the in the preparation process: under acid catalyst, drip and contain hydrogen functional group's silane agent, the silane agent of two functionality, the silane agent of phenyl functional group.
According to the silane agent of two functionality of selecting, can increase resin the phenyl amount that contains, strengthen spatial configuration of molecules etc., the specific refractory power of finally enhancing product performance, tear resistance etc.Preferably, the structural formula of the silane agent of described two functionality is: R
1(R
2O)
2Si R
3, R wherein
1, R
3Be straight or branched alkyl or the straight or branched aryl of 6～20 carbon atoms or the aralkyl of 7～20 carbon atoms of 1～6 identical or not identical carbon atom, R
2Be straight or branched alkyl, acyloxy or the electronegative group of 2～6 carbon atoms.The silane agent of described two functionality can for but be not limited to as follows:
Dimethoxydiphenylsilane;
Dimethyldiethoxysilane;
Dimethyldimethoxysil,ne;
The phenylbenzene diethoxy silane;
The phenyl methyl diethoxy silane.
The hydrogeneous silicone resin of phenyl provided by the invention not only has the characteristics such as high refractive index, high transmission rate, clear, and this phenyl Silicon Containing Hydrogen resin has good consistency and dispersiveness, thereby hydrogeneously makes that platinum addition reaction and superoxide cause that crosslinking reaction makes that the silicon rubber rebound resilience is good, the excellent properties such as anti tear, anti-impact force, thermotolerance are good, radiation hardness, long service life.
The preparation method of the hydrogeneous silicone resin of phenyl provided by the invention does not adopt chlorosilane of the prior art, nontoxic extraction agent to replace toluene of the prior art, can not damage human body, can be to environment yet.Adopt the phenyl base Silicon Containing Hydrogen resin of present method preparation to have excellent performance, reaction conditions is gentle, the reaction times is short, simple to operate, and raw material is easy to get, cost is low, environmentally safe, be convenient to suitability for industrialized production.
Embodiment
Embodiment 1:
The hydrochloric acid that in the four-hole boiling flask of stirring, reflux condensing tube, thermometer and dropping funnel, adds respectively 170g distilled water, 0.8g1N, mix, drip 246.14g phenyl triethoxysilane, 201.50g tetramethyl disiloxane, add again 87g dehydrated alcohol, 10g hydrochloric acid and 138g hexamethyldisiloxane extraction agent and carry out cohydrolysis-polycondensation, temperature of reaction is 65 ℃, the control reaction times is 5h, standing demix after reaction finishes, water is removed, with distilled water organic phase is washed neutrality.With the aperture be behind the membrane filtration of 0.5 μ m with the organic phase of neutrality, underpressure distillation (110～130 ℃/-0.096Mpa) remove low-boiling-point substance, obtain the hydrogeneous cancellated silicone resin of phenyl of clear.The hydrogeneous web-like silicon resin of this phenyl has that high transmission rate, high refractive index, clear, good heat resistance, radiation hardness, rebound resilience are good, the cementability of anti tear, anti-impact force, end properties is better, shear bonding strength has the characteristics such as significant effect.
Embodiment 2:
The hydrochloric acid that in the four-hole boiling flask of stirring, reflux condensing tube, thermometer and dropping funnel, adds respectively 170g distilled water, 1.0g1N, mix, drip 339.51g styroyl (trimethoxy) silane, 201.50g decamethyl dihydro five siloxanes, 100g dehydrated alcohol, 15g hydrochloric acid and 400g isohexadecane extraction agent and carry out cohydrolysis-polycondensation, temperature of reaction is 90 ℃, the control reaction times is 1h, standing demix after reaction finishes, water is removed, with distilled water organic phase is washed neutrality.With the aperture be behind the membrane filtration of 1.5 μ m with the organic phase of neutrality, underpressure distillation (110～130 ℃/-0.096Mpa) remove low-boiling-point substance, obtain the hydrogeneous cancellated silicone resin of phenyl of clear.
Embodiment 3:
The hydrochloric acid that in the four-hole boiling flask of stirring, reflux condensing tube, thermometer and dropping funnel, adds respectively 200g distilled water, 1.0g1N, mix, dripping 246.14g phenyl triethoxysilane, 201.50g tetramethyl disiloxane, 70g dehydrated alcohol, 10g hydrochloric acid and 270g hexamethyldisiloxane extraction agent is hydrolyzed-polycondensation, temperature of reaction is 50 ℃, the control reaction times is 7h, after reaction finishes, standing demix, water is removed, with distilled water organic phase is washed neutrality.With the aperture be behind the membrane filtration of 0.5 μ m with the organic phase of neutrality, underpressure distillation (110～130 ℃/-0.096Mpa) remove low-boiling-point substance, obtain the hydrogeneous cancellated silicone resin of phenyl of clear.
Embodiment 4:
The hydrochloric acid that in the four-hole boiling flask of stirring, reflux condensing tube, thermometer and dropping funnel, adds respectively 200g distilled water, 1.0g1N, mix, drip 246.14g phenyl triethoxysilane, 195.49g dimethoxydiphenylsilane, 201.50g tetramethyl disiloxane, add again 100g dehydrated alcohol, 12g hydrochloric acid and 400g Permethyl 99A. extraction agent and carry out cohydrolysis-polycondensation, temperature of reaction is 80 ℃, the control reaction times is 2.5h, standing demix after reaction finishes, water is removed, with distilled water organic phase is washed neutrality.With the aperture be behind the membrane filtration of 2.5 μ m with the organic phase of neutrality, underpressure distillation (110～130 ℃/-0.096Mpa) remove low-boiling-point substance, obtain the hydrogeneous cancellated silicone resin of phenyl of clear.
Embodiment 5:
With stirring, reflux condensing tube, add respectively 170g distilled water in the four-hole boiling flask of thermometer and dropping funnel, 1.0g1N hydrochloric acid, mix, drip 339.51g styroyl (trimethoxy) silane, 201.50g tetramethyl disiloxane, 195.49g dimethyldimethoxysil,ne, add again the 100g dehydrated alcohol, 12g hydrochloric acid and 200g decamethyl tetrasiloxane extraction agent carry out cohydrolysis-polycondensation, temperature of reaction is 85 ℃, the control reaction times is 2h, after reaction finishes, standing demix, water is removed, with distilled water organic phase is washed neutrality.With the aperture be behind the membrane filtration of 5 μ m with the organic phase of neutrality, underpressure distillation (110～130 ℃/-0.096Mpa) remove low-boiling-point substance, obtain the hydrogeneous cancellated silicone resin of phenyl of clear.
The hydrogeneous web-like silicon resin property of phenyl that above-described embodiment 1～5 is provided and the impact of LED organosilicon encapsulating material performance done following test, test result sees table 1, table 2 for details:
The performance of the hydrogeneous base net shape of table 1 phenyl silicone resin
The hydrogeneous base net shape of table 2 phenyl silicone resin is on the impact of LED organosilicon encapsulating material performance
Wherein SH-303 is to be the phenyl Silicon Containing Hydrogen resin of selling on the market, and SH-303 produces for profit standing grain company.
Above-mentioned test result can be found out, adopts the standby LED(luminous element of phenyl Silicon Containing Hydrogen resin provided by the invention) encapsulation all obtained effective improvement with silica gel material specific refractory power, tensile strength, bonding strength than prior art products.
More than technical scheme that the embodiment of the invention is provided be described in detail, used specific case herein principle and the embodiment of the embodiment of the invention are set forth, the explanation of above embodiment is only applicable to help to understand the principle of the embodiment of the invention; Simultaneously, for one of ordinary skill in the art, according to the embodiment of the invention, all will change on embodiment and range of application, in sum, this description should not be construed as limitation of the present invention.
Claims (8)
1. silicone resin is used in a LED encapsulation, and it is characterized in that: described silicone resin is for having the hydrogeneous silicone resin of cancellated phenyl.
2. silicone resin is used in LED encapsulation as claimed in claim 1, and it is characterized in that: described silicone resin is represented by following general formula:
Wherein, R, R 〞, R " ' be the straight or branched alkyl of identical or not identical 1～6 carbon atom, or be the straight or branched aryl of identical or not identical 6～20 carbon atoms, or be the aralkyl of identical or not identical 7～20 carbon atoms; R ＇ is the hydrogen base.
3. one kind prepares claim 1 or 2 described LED encapsulation with the method for silicone resins, and it is characterized in that: described method comprises the steps:
A) under acid catalyst, drip the silane agent contain the hydrogen functional group, polyreaction is carried out in the silane agent that contains phenyl functional group;
B) add extraction agent, the hydrogeneous silicone resin of based target product phenyl, the control temperature of reaction is 50～90 ℃, the reaction times is 1～7 hour;
C) product is left standstill, the layer that anhydrates is washed neutrality with distilled water with the hydrogeneous silicone resin of phenyl, obtains being dissolved in the hydrogeneous silicone resin solution of phenyl of extraction agent;
D) with the hydrogeneous silicone resin solution of the phenyl of neutrality, be the membrane filtration of 0.5 ~ 5 μ m with the aperture after, low-boiling-point substance is removed in underpressure distillation, obtains the hydrogeneous silicone resin of phenyl.
4. the LED for preparing as claimed in claim 3 encapsulates the method for using silicone resin, and it is characterized in that: the described structural formula that contains the silane agent of phenyl functional group is: R
1(R
2O)
3Si, wherein, R
1Be the straight or branched aryl of 6～20 carbon atoms or the aralkyl of 7～20 carbon atoms; R
2Straight or branched alkyl, acyloxy for 1-6 carbon atom.
5. the LED for preparing as claimed in claim 3 encapsulates the method for using silicone resin, and it is characterized in that: the structural formula of the described hydrogen functional group's of containing silane agent is:
Wherein, R
1, R
2, R
3, R
4Straight or branched alkyl or the straight or branched aryl of 6～20 carbon atoms or the aralkyl of 7～20 carbon atoms for 1～6 identical or not identical carbon atom; N is 1～20 round values.
6. the LED for preparing as claimed in claim 3 encapsulates the method for using silicone resin, and it is characterized in that: described extraction agent is isomeric alkane or methyl oligosiloxane.
7. encapsulate the method for using silicone resin such as the described LED for preparing of one of claim 4 ~ 6, it is characterized in that: a) step is the in the preparation process: under acid catalyst, drip and contain hydrogen functional group's silane agent, the silane agent of two functionality, the silane agent of phenyl functional group and carry out polyreaction.
8. the LED for preparing as claimed in claim 7 encapsulates the method for using silicone resin, and it is characterized in that: the structural formula of the silane agent of described two functionality is: R
1(R
2O)
2Si R
3, R wherein
1, R
3Be straight or branched alkyl or the straight or branched aryl of 6～20 carbon atoms or the aralkyl of 7～20 carbon atoms of 1～6 identical or not identical carbon atom, R
2Be straight or branched alkyl, acyloxy or the electronegative group of 2～6 carbon atoms.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210532313.2A CN103059301B (en) | 2012-12-11 | 2012-12-11 | Phenyl hydrogenous reticular silicone resin for encapsulating LED (Light Emitting Diode) and preparation method thereof |
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|---|---|---|---|
| CN201210532313.2A CN103059301B (en) | 2012-12-11 | 2012-12-11 | Phenyl hydrogenous reticular silicone resin for encapsulating LED (Light Emitting Diode) and preparation method thereof |
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Cited By (3)
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| CN104610546A (en) * | 2013-11-04 | 2015-05-13 | 上海华明高技术（集团）有限公司 | Preparation method of annular reticular silicon resin |
| CN107286347A (en) * | 2017-07-25 | 2017-10-24 | 仲恺农业工程学院 | A kind of method that the hydrogeneous silicones of phenyl is prepared with Methyl Hydrogen Polysiloxane Fluid |
| CN107286899A (en) * | 2017-05-19 | 2017-10-24 | 合肥市惠科精密模具有限公司 | A kind of Micro LED screens are encapsulated with high-strength anti-aging silica gel |
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| CN107286899A (en) * | 2017-05-19 | 2017-10-24 | 合肥市惠科精密模具有限公司 | A kind of Micro LED screens are encapsulated with high-strength anti-aging silica gel |
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| CN103059301B (en) | 2015-02-25 |
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Effective date of registration: 20170330 Address after: 528400 Guangdong Torch Development Zone, Zhongshan science and Technology West Wu Song Road, No. 1, No. four, building 8, room Patentee after: Zhongshan cohesion silicone Technology Co., Ltd. Address before: 510630 Guangzhou province high tech Industrial Development Zone, Guangzhou Science City spectrum West Road, No. 108, on the first floor of the workshop on the eastern side of the room, room 69 Patentee before: Cao Jianlin |