CN104892941A - Synthesis process of viscosified phenyl silicone oil for high-power light-emitting diode (LED) packaging - Google Patents
Synthesis process of viscosified phenyl silicone oil for high-power light-emitting diode (LED) packaging Download PDFInfo
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Abstract
The invention discloses a synthesis process of viscosified phenyl silicone oil for high-power light-emitting diode (LED) packaging. The synthesis process comprises the following steps of: synthesizing an epoxy end-capping reagent; dehydrating a methyl cyclosiloxane monomer, a methyl vinyl cyclosiloxane monomer and methyl phenyl cyclosiloxane monomer; adding the epoxy end-capping reagent and a catalyst and performing polymerization reaction; and after the reaction, removing the catalyst and performing vacuum devolatilization; and cooling and discharging. Compared with the traditional silicone oil for LED packaging, the viscosified phenyl silicone oil for high-power LED packaging synthesized by the synthesis process has high refractive index and light transmittance, excellent viscosity and excellent room temperature curing property, and can effectively improve the light output and the high temperature resistance of silica gel for LED packaging.
Description
Technical field
Embodiments of the present invention relate to high power LED package field, and more specifically, embodiments of the present invention relate to a kind of synthesis technique increasing glutinous type high power LED package phenyl silicone oil.
Background technology
Along with national new forms of energy strategy implementation, the research of new energy materials development & application becomes one of emphasis direction of 21 century research.Contact link the closest as in LED industry chain with market, LED encapsulation material is the focus studied in new energy materials industry always.Along with the development of power-type LED device, require more and more higher to the optical property (specific refractory power, transmittance etc.) of LED encapsulation material, require that packaged material has higher hardness simultaneously, excellent high thermal resistance and good bond performance etc.Therefore, original epoxy resin or modified epoxy can not meet the encapsulation needs of power-type LED.The encapsulation of current China LED accounts for global 75%, the whole dependence on import of high power LED package silica gel, and expensive, the development of serious restriction China related industries revolution.High power LED package silica gel development & application, not only has huge economic worth, and can promote effective enforcement of China's related industries sound development and national new forms of energy strategy effectively, has good social value.
Summary of the invention
Instant invention overcomes the deficiencies in the prior art, a kind of synthesis technique increasing glutinous type high power LED package phenyl silicone oil be provided, by-MePhSiO-in regulatory molecule chain and
content and spatial distribution, solve existing high power LED package silica gel demand high refractive index, high transmission rate, resistance to elevated temperatures and a strong cementability difficult problem, obtains increasing glutinous type high power LED package phenyl silicone oil.
For solving above-mentioned technical problem, the invention provides the synthesis technique increasing glutinous type high power LED package phenyl silicone oil, it comprises the following steps:
A, the synthesis of epoxy-capped dose
Glycidyl allyl ether, toluene and platinum catalyst are put into by a certain percentage four neck flasks, 1,1,3,3-tetramethyl disiloxane is placed in dropping funnel; Under temperature 40 DEG C ~ 95 DEG C (being preferably 60 ~ 70 DEG C), nitrogen protection condition, with the speed of per minute 3 ~ 10 by 1,1,3,3-tetramethyl disiloxane is added drop-wise in four neck flasks, after dropwising, be warming up to 95 DEG C ~ 125 DEG C reactions 4 ~ 16 hours (being preferably 95 ~ 100 DEG C of reactions 8 ~ 10 hours), then heat up distillation, the component that 140 ~ 280 DEG C (being preferably 180 ~ 200 DEG C) distills out is epoxy-capped dose 1,1,3,3-tetramethyl--1,3 two [3-(oxiranyhnethoxy) propyl group] sily oxide;
B, raw material dewater
Methyl cyclosiloxane monomer, methylvinylcyclosiloxane monomer and methyl phenyl ring siloxane monomer are added in polymerization reaction kettle, dehydration is vacuumized under temperature 45 ~ 85 DEG C of conditions, vacuum tightness is-0.1 ~-0.098MPa, and limit vacuumizes snare drum enters nitrogen or limit and stir, dewatering time 1 ~ 4 hour;
C, add auxiliary agent, polyreaction
Epoxy-capped dose is added in described polymerization reaction kettle, add the catalyzer Tetramethylammonium hydroxide (alkali glue) of 50 ~ 6000ppm of methyl cyclosiloxane monomer weight or tetrabutylammonium hydroxide phosphorus or potassium hydroxide or cesium hydroxide again, after stirring, be warming up to the polyreaction that 85 ~ 165 DEG C are carried out 2 ~ 10 hours (being preferably 85 ~ 125 degrees Celsius of reactions 6 ~ 8 hours);
D, except catalyzer
The polymerisate obtained by step C is warming up to 145 ~ 175 DEG C, keeps temperature to destroy catalyzer in 1 ~ 2 hour;
E, vacuum volatilization
The product of step D gained is carried out high-temperature vacuum devolatilization under temperature 145 ~ 185 DEG C, vacuum tightness-0.1 ~-0.098MPa condition, is cooled to room temperature, obtains target compound.
The optimum condition of above-mentioned steps A can make epoxy-capped dose 1,1,3,3-tetramethyl--1, the output of 3 two [3-(oxiranyhnethoxy) propyl group] sily oxide is higher, and the optimum condition of step C can accelerate the preparation flow of object product when polyreaction completes substantially.
Product structure formula prepared by the present invention is as follows:
Wherein m, n be greater than zero integer.
The consumption of three kinds of raw material methyl cyclosiloxane monomers (DMC) in the present invention, methylvinylcyclosiloxane monomer (MVC) and methyl phenyl ring siloxane monomer (MPC), can be different according to the difference requirement of the finished product, therefore do not need specifically to limit its usage ratio.The add-on of epoxy-capped dose adjusts as required, general adds methyl phenyl ring siloxane monomer molar number 3 ~ 50 times, but adds other multiple and also can prepare object product of the present invention.
Glycidyl allyl ether described in steps A, platinum catalyst and 1, 1, 3, the mol ratio of 3-tetramethyl disiloxane can adopt 1:(0.001 ~ 0.01): (0.40 ~ 0.50), but be not limited to adopt this ratio, preferred employing 1:0.001:0.45, toluene is as solvent, use and can be convenient to glycidyl allyl ether in right amount, platinum catalyst and 1, 1, 3, 3-tetramethyl disiloxane carries out reacting, the quality of such as toluene can be glycidyl allyl ether, platinum catalyst and 1, 1, 3, one times of the total mass of 3-tetramethyl disiloxane or adjust in right amount.
Described four neck flasks are provided with prolong, nitrogen conduit, internal thermometer.Prolong is used for backflow; Thermometer is for observing temperature.
The vacuum tightness vacuumizing dehydration described in step B is-0.1 ~-0.098MPa, and under above-mentioned vacuum tightness, dehydrating effect is better, and the materials such as the solvent in reaction mass can be avoided to be evacuated removing; And limit vacuumizes snare drum enters nitrogen or limit and stir, improve rate of water loss.
Polyreaction described in step C is carried out under protection of inert gas.Polyreaction is carried out in atmospheric conditions, in order to prevent reaction mass from contacting thus anti-oxidation with air, therefore adopts rare gas element such as nitrogen to protect.
The volatile matter that vacuum volatilization described in step e produces reclaims through condensation and enters step B recycle.
Due to the effect of the lone-pair electron on Sauerstoffatom in epoxy group(ing), make the compound containing epoxy group(ing) have excellent Optical instrument, can strengthen and adhesion between metal and macromolecular material.Therefore, as high power LED package silica gel important component part, with the high phenyl silicone oil of epoxy group(ing) end-blocking, not only there is high refractive index and transmittance, and there is excellent adhesion, realize and seamless gluing between metal and macromolecular material, strengthening packaging plastic work-ing life under long-time hot conditions, is the component that high power LED package silica gel is indispensable.
Compared with prior art, one of beneficial effect of the present invention is: first the present invention has synthesized containing epoxy group(ing) 1,1,3,3-tetramethyl--1,3 two [3-(oxiranyhnethoxy) propyl group] sily oxide (EBA), using it as end-capping reagent, to strengthen phenyl silicone oil Optical instrument, improve the sticking power between end-blocking glue and base material.The increasing of the present invention's synthesis sticks type high power LED package phenyl silicone oil compared with conventional LED package silicone oil, there are higher refractive index and transmittance, excellent cementability, and good self-vulcanizing performance, effectively can improve light output and the resistance to elevated temperatures of LED silica gel.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Embodiment 1
A, the synthesis of epoxy-capped dose: get four neck flasks, prolong, nitrogen conduit are set, internal thermometer; According to mol ratio 1:0.001:0.45, glycidyl allyl ether and platinum catalyst are put into four neck flasks, by 1,1,3,3-tetramethyl disiloxane is placed in dropping funnel, and in four neck flasks, adds glycidyl allyl ether, platinum catalyst and 1,1, the toluene of the total mass one times of 3,3-tetramethyl disiloxane is as solvent; Under temperature 65 DEG C, nitrogen protection condition, with the speed of per minute 5 by 1,1,3,3-tetramethyl disiloxane is added drop-wise in four neck flasks, after dropwising, is warming up to 95 DEG C of reactions 10 hours, then heat up distillation, 195 DEG C of components distilled out are epoxy-capped dose 1,1,3,3-tetramethyl--1,3 two [3-(oxiranyhnethoxy) propyl group] sily oxide; Productive rate 95%.
B, raw material dewater: add in polymerization reaction kettle by methyl cyclosiloxane monomer, methylvinylcyclosiloxane monomer and methyl phenyl ring siloxane monomer according to a certain percentage according to phenyl silicone oil Application Areas, vacuumize under temperature 65 DEG C of conditions, vacuum tightness is-0.1 ~-0.098MPa, and limit vacuumizes snare drum enters nitrogen or limit and stir, dewater 2 hours;
C, add auxiliary agent, polyreaction: be that epoxy-capped dose of steps A gained adds in the raw material dewatered through step B by 1:30 according to epoxy-capped dose and the mol ratio of methyl phenyl ring siloxane monomer in raw material, add the catalyzer Tetramethylammonium hydroxide of the 500ppm of methyl cyclosiloxane total monomer weight described in step B again, be warming up to 110 DEG C after stirring, under normal pressure, nitrogen protection condition, carry out the polyreaction of 7 hours;
D, except catalyzer: the polymerisate obtained by step C is warming up to 160 DEG C, keeps temperature 1.5 hours to destroy catalyzer;
E, vacuum volatilization: the product of step D gained is carried out high-temperature vacuum devolatilization under temperature 165 DEG C, vacuum tightness-0.1 ~-0.098MPa condition, is cooled to room temperature, obtains target compound.Volatile matter reclaims through condensation and enters B, recycle.
Embodiment 2
A, the synthesis of epoxy-capped dose: get four neck flasks, prolong, nitrogen conduit are set, internal thermometer; According to mol ratio 1:0.01:0.5, glycidyl allyl ether and platinum catalyst are put into four neck flasks, by 1,1,3,3-tetramethyl disiloxane is placed in dropping funnel, and in four neck flasks, adds glycidyl allyl ether, platinum catalyst and 1,1, the toluene of the total mass one times of 3,3-tetramethyl disiloxane is as solvent; Under temperature 60 C, nitrogen protection condition, with the speed of per minute 7 by 1,1,3,3-tetramethyl disiloxane is added drop-wise in four neck flasks, after dropwising, is warming up to 100 DEG C of reactions 8 hours, then heat up distillation, 200 DEG C of components distilled out are epoxy-capped dose 1,1,3,3-tetramethyl--1,3 two [3-(oxiranyhnethoxy) propyl group] sily oxide; Productive rate 75%.
B, raw material dewater: add in polymerization reaction kettle by methyl cyclosiloxane monomer, methylvinylcyclosiloxane monomer and methyl phenyl ring siloxane monomer according to a certain percentage according to phenyl silicone oil Application Areas, vacuumize under temperature 70 C condition, vacuum tightness is-0.1 ~-0.098MPa, and limit vacuumizes snare drum enters nitrogen or limit and stir, dewater 1.5 hours;
C, add auxiliary agent, polyreaction: be that epoxy-capped dose of steps A gained adds in the raw material dewatered through step B by 1:35 according to epoxy-capped dose and the mol ratio of methyl phenyl ring siloxane monomer in raw material, add the catalyzer cesium hydroxide of the 3000ppm of methyl cyclosiloxane total monomer weight described in step B again, be warming up to 125 DEG C after stirring, under normal pressure, nitrogen protection condition, carry out the polyreaction of 6 hours;
D, except catalyzer: the polymerisate obtained by step C is warming up to 145 DEG C, keeps temperature 2 hours to destroy catalyzer;
E, vacuum volatilization: the product of step D gained is carried out high-temperature vacuum devolatilization under temperature 155 DEG C, vacuum tightness-0.1 ~-0.098MPa condition, is cooled to room temperature, obtains target compound.Volatile matter reclaims through condensation and enters B, recycle.
Embodiment 3
A, the synthesis of epoxy-capped dose: get four neck flasks, prolong, nitrogen conduit are set, internal thermometer; According to mol ratio 1:0.005:0.40, glycidyl allyl ether and platinum catalyst are put into four neck flasks, by 1,1,3,3-tetramethyl disiloxane is placed in dropping funnel, and in four neck flasks, adds glycidyl allyl ether, platinum catalyst and 1,1, the toluene of the total mass one times of 3,3-tetramethyl disiloxane is as solvent; Under temperature 70 C, nitrogen protection condition, with the speed of per minute 5 by 1,1,3,3-tetramethyl disiloxane is added drop-wise in four neck flasks, after dropwising, is warming up to 97 DEG C of reactions 10 hours, then heat up distillation, 180 DEG C of components distilled out are epoxy-capped dose 1,1,3,3-tetramethyl--1,3 two [3-(oxiranyhnethoxy) propyl group] sily oxide; Productive rate 88%.
B, raw material dewater: add in polymerization reaction kettle by methyl cyclosiloxane monomer, methylvinylcyclosiloxane monomer and methyl phenyl ring siloxane monomer according to a certain percentage according to phenyl silicone oil Application Areas, vacuumize under temperature 50 C condition, vacuum tightness is-0.1 ~-0.098MPa, and limit vacuumizes snare drum enters nitrogen or limit and stir, dewater 3 hours;
C, add auxiliary agent, polyreaction: be that epoxy-capped dose of steps A gained adds in the raw material dewatered through step B by 1:20 according to epoxy-capped dose and the mol ratio of methyl phenyl ring siloxane monomer in raw material, add the catalyzer Tetramethylammonium hydroxide of the 6000ppm of methyl cyclosiloxane total monomer weight described in step B again, be warming up to 85 DEG C after stirring, under normal pressure, nitrogen protection condition, carry out the polyreaction of 8 hours;
D, except catalyzer: the polymerisate obtained by step C is warming up to 175 DEG C, keeps temperature 1 hour to destroy catalyzer;
E, vacuum volatilization: the product of step D gained is carried out high-temperature vacuum devolatilization under temperature 185 DEG C, vacuum tightness-0.1 ~-0.098MPa condition, is cooled to room temperature, obtains target compound.Volatile matter reclaims through condensation and enters B, recycle.
Embodiment 4
A, the synthesis of epoxy-capped dose: get four neck flasks, prolong, nitrogen conduit are set, internal thermometer; According to mol ratio 1:0.01:0.40, glycidyl allyl ether and platinum catalyst are put into four neck flasks, by 1,1,3,3-tetramethyl disiloxane is placed in dropping funnel, and in four neck flasks, adds glycidyl allyl ether, platinum catalyst and 1,1, the toluene of the total mass one times of 3,3-tetramethyl disiloxane is as solvent; Under temperature 40 DEG C, nitrogen protection condition, with the speed of per minute 3 by 1,1,3,3-tetramethyl disiloxane is added drop-wise in four neck flasks, after dropwising, is warming up to 95 DEG C of reactions 12 hours, then heat up distillation, 140 DEG C of components distilled out are epoxy-capped dose 1,1,3,3-tetramethyl--1,3 two [3-(oxiranyhnethoxy) propyl group] sily oxide; Productive rate 67%.
B, raw material dewater: add in polymerization reaction kettle according to mol ratio 70:15:30 by methyl cyclosiloxane monomer, methylvinylcyclosiloxane monomer and methyl phenyl ring siloxane monomer, vacuumize under temperature 45 C condition, vacuum tightness is-0.1 ~-0.098MPa, and limit vacuumizes snare drum enters nitrogen or limit and stir, dewater 4 hours;
C, add auxiliary agent, polyreaction: be that epoxy-capped dose of steps A gained adds in the raw material dewatered through step B by 1:50 according to epoxy-capped dose and the mol ratio of methyl phenyl ring siloxane monomer in raw material, add the catalyzer tetrabutylammonium hydroxide phosphorus of the 50ppm of methyl cyclosiloxane total monomer weight described in step B again, be warming up to 85 DEG C after stirring, under normal pressure, nitrogen protection condition, carry out the polyreaction of 10 hours;
D, except catalyzer: the polymerisate obtained by step C is warming up to 145 DEG C, keeps temperature 2 hours to destroy catalyzer;
E, vacuum volatilization: the product of step D gained is carried out high-temperature vacuum devolatilization under temperature 145 DEG C, vacuum tightness-0.1 ~-0.098MPa condition, is cooled to room temperature, obtains target compound.Volatile matter reclaims through condensation and enters B, recycle.
Embodiment 5
A, the synthesis of epoxy-capped dose: get four neck flasks, prolong, nitrogen conduit are set, internal thermometer; According to mol ratio 1:0.1:1, glycidyl allyl ether and platinum catalyst are put into four neck flasks, by 1,1,3,3-tetramethyl disiloxane is placed in dropping funnel, and in four neck flasks, adds glycidyl allyl ether, platinum catalyst and 1,1, the toluene of the total mass one times of 3,3-tetramethyl disiloxane is as solvent; Under temperature 95 DEG C, nitrogen protection condition, with the speed of per minute 10 by 1,1,3,3-tetramethyl disiloxane is added drop-wise in four neck flasks, after dropwising, is warming up to 125 DEG C of reactions 4 hours, then heat up distillation, 280 DEG C of components distilled out are epoxy-capped dose 1,1,3,3-tetramethyl--1,3 two [3-(oxiranyhnethoxy) propyl group] sily oxide; Productive rate 70%.
B, raw material dewater: add in polymerization reaction kettle according to mol ratio 40:1:65 by methyl cyclosiloxane monomer, methylvinylcyclosiloxane monomer and methyl phenyl ring siloxane monomer, vacuumize under temperature 85 DEG C of conditions, vacuum tightness is-0.1 ~-0.098MPa, and limit vacuumizes snare drum enters nitrogen or limit and stir, dewater 1 hour;
C, add auxiliary agent, polyreaction: be that epoxy-capped dose of steps A gained adds in the raw material dewatered through step B by 1:80 according to epoxy-capped dose and the mol ratio of methyl phenyl ring siloxane monomer in raw material, add the catalyzer potassium hydroxide of the 6000ppm of methyl cyclosiloxane total monomer weight described in step B again, be warming up to 165 DEG C after stirring, under normal pressure, nitrogen protection condition, carry out the polyreaction of 2 hours;
D, except catalyzer: the polymerisate obtained by step C is warming up to 175 DEG C, keeps temperature 1 hour to destroy catalyzer;
E, vacuum volatilization: the product of step D gained is carried out high-temperature vacuum devolatilization under temperature 185 DEG C, vacuum tightness-0.1 ~-0.098MPa condition, is cooled to room temperature, obtains target compound.Volatile matter reclaims through condensation and enters B, recycle.
Although with reference to multiple explanatory embodiment of the present invention, invention has been described here, but, should be appreciated that, those skilled in the art can design a lot of other amendment and embodiment, these amendments and embodiment will drop within spirit disclosed in the present application and spirit.More particularly, in scope disclosed in the present application, multiple modification and improvement can be carried out to the building block of subject combination layout and/or layout.Except the modification of carrying out building block and/or layout is with except improvement, to those skilled in the art, other purposes also will be obvious.
Claims (1)
1. increase the synthesis technique of glutinous type high power LED package phenyl silicone oil, it is characterized in that it comprises the following steps:
A, the synthesis of epoxy-capped dose
Glycidyl allyl ether, toluene and platinum catalyst are put into four neck flasks, 1,1,3,3-tetramethyl disiloxane is placed in dropping funnel; Under temperature 40 ~ 95 DEG C, nitrogen protection condition, with the speed of per minute 3 ~ 10 by 1,1,3,3-tetramethyl disiloxane is added drop-wise in four neck flasks, after dropwising, is warming up to 95 ~ 125 DEG C of reactions 4 ~ 16 hours, then heat up distillation, 140 ~ 280 DEG C of components distilled out are epoxy-capped dose 1,1,3,3-tetramethyl--1,3 two [3-(oxiranyhnethoxy) propyl group] sily oxide;
B, raw material dewater
Methyl cyclosiloxane monomer, methylvinylcyclosiloxane monomer and methyl phenyl ring siloxane monomer are added in polymerization reaction kettle, dehydration is vacuumized under temperature 45 ~ 85 DEG C of conditions, vacuum tightness is-0.1 ~-0.098MPa, and limit vacuumizes snare drum enters nitrogen or limit and stir, dewatering time 1 ~ 4 hour;
C, add auxiliary agent, polyreaction
Epoxy-capped dose is added in described polymerization reaction kettle, add the catalyzer Tetramethylammonium hydroxide of 50 ~ 6000ppm of methyl cyclosiloxane monomer weight or tetrabutylammonium hydroxide phosphorus or potassium hydroxide or cesium hydroxide again, after stirring, be warming up to the polyreaction that 85 ~ 165 DEG C are carried out 2 ~ 10 hours;
D, except catalyzer
The polymerisate obtained by step C is warming up to 145 ~ 175 DEG C, keeps temperature to destroy catalyzer in 1 ~ 2 hour;
E, vacuum volatilization
The product of step D gained is carried out high-temperature vacuum devolatilization under temperature 145 ~ 185 DEG C, vacuum tightness-0.1 ~-0.098MPa condition, is cooled to room temperature, obtains target compound.
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| CN107057068A (en) * | 2017-02-23 | 2017-08-18 | 深圳市新纶科技股份有限公司 | A kind of end epoxy silicon oil and preparation method thereof and its as adhesion promoters purposes |
| CN108148525A (en) * | 2017-12-27 | 2018-06-12 | 杭州之江新材料有限公司 | A kind of organic silicon rigidity-increasing stick and its preparation method and application |
| CN108314787A (en) * | 2018-03-15 | 2018-07-24 | 厦门大学 | A kind of phosphorus-nitrogen containing silicon polymer modified graphene oxide fire retardant and preparation method thereof |
| CN110591098A (en) * | 2019-10-09 | 2019-12-20 | 浙江新安化工集团股份有限公司 | Methyl phenyl vinyl silicone oil and preparation method and application thereof |
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| CN105111445A (en) * | 2015-09-30 | 2015-12-02 | 桂林健评环保节能产品开发有限公司 | Methyl phenyl silicone oil for LED (light emitting diode) potting sealant and preparation method thereof |
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| CN108314787A (en) * | 2018-03-15 | 2018-07-24 | 厦门大学 | A kind of phosphorus-nitrogen containing silicon polymer modified graphene oxide fire retardant and preparation method thereof |
| CN108314787B (en) * | 2018-03-15 | 2020-09-04 | 厦门大学 | Phosphorus-nitrogen-silicon-containing polymer modified graphene oxide flame retardant and preparation method thereof |
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