CN104277222A - Phenyl hydrogen-containing silicone resin for LED encapsulation and preparation method of phenyl hydrogen-containing silicone resin - Google Patents
Phenyl hydrogen-containing silicone resin for LED encapsulation and preparation method of phenyl hydrogen-containing silicone resin Download PDFInfo
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- CN104277222A CN104277222A CN201310288318.XA CN201310288318A CN104277222A CN 104277222 A CN104277222 A CN 104277222A CN 201310288318 A CN201310288318 A CN 201310288318A CN 104277222 A CN104277222 A CN 104277222A
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Abstract
The invention discloses phenyl hydrogen-containing silicone resin for LED encapsulation and a preparation method of the phenyl hydrogen-containing silicone resin. The phenyl hydrogen-containing silicone resin comprises the following raw materials: an acid catalyst, water glass, phenyl alkoxy silane, absolute ethyl alcohol, a hydrogen end-capping agent and an extracting agent. According to the preparation method, environment-friendly and cheap organic matters are adopted as solvents; and water glass, phenyl alkoxy silane and a small molecule hydrogen-containing material are subjected to cohydrolysis and polycondensation at room temperature, so as to prepare a phenyl hydrogen-containing crosslinking agent with excellent performance. According to the method, the process is simple, an organic solvent can be recycled, and the method is environment-friendly and energy-saving. The phenyl hydrogen-containing silicone resin prepared by the method has excellent properties such as high refractive index, high light transmittance, high-temperature and low-temperature resistance, and good weather fastness.
Description
Technical field
The present invention relates to organosilicon macromolecule compound technical, in particular to a kind of LED phenyl Silicon Containing Hydrogen resin and preparation method thereof.
Background technology
LED(Light-Emitting Diode, photodiode) be a kind of semiconductor electronic component that can be luminous, be the one of semiconductor diode, electric energy conversion can be become luminous energy.LED illumination market is considered to LED application most important, most with prospects always.Due to its have that volume is little, current consumption is low, long service life, high brightness, low in calories, environmental protection and the advantage such as sturdy and durable, LED photodiode has boundless market outlook in illumination application.
As the liquid silicone macromolecule crosslink agent of LED encapsulation material, even structure, highly transparent and the large feature of refractive index should be had with its crosslinked packaged material obtained, this just require containing hydrogen silicone oil should with packaged material structural similitude or close.In disclosed technology, the hydrogeneous linking agent of LED phenyl has two kinds at present: a kind of by forming containing silicon hydride chlorid and non-hydrogeneous hydrolyzing chlorosilane polycondensation, products therefrom composition very different under different ratios of raw materials and hydrolysising condition in this method, cause repeatability and the poor controllability of product, and the three wastes are many, seriously polluted; Another adopts phenyl siloxane and ring hydrogen siloxane to be hydrolyzed under catalyst action polycondensation, the hydrogeneous linking agent of phenyl of this kind of method production is chain structure, differ larger with packaged material structure, and hydrogen group skewness, cannot excellent, the packaged material of even structure.
Summary of the invention
In order to solve the problem, the invention provides and a kind of there is LED phenyl Silicon Containing Hydrogen resin of the premium propertiess such as high refractive index, high transmission rate, high-low temperature resistant, good weatherability and preparation method thereof.
To achieve these goals, according to an aspect of the present invention, provide a kind of LED phenyl Silicon Containing Hydrogen resin, comprise following raw material: an acidic catalyst, water glass, phenyl alkoxysilane, dehydrated alcohol, ring hydrogen siloxane, hydrogen end-capping reagent, extraction agent.
Especially, described raw material also comprises: ring hydrogen siloxane.Described ring hydrogen siloxane is one or more in tetramethyl-tetrahydrochysene cyclotetrasiloxane, trimethylammonium three hydrogen cyclotrisiloxane, hexamethyl dihydro cyclotetrasiloxane, tetraphenyl tetrahydrochysene cyclotetrasiloxane, phenylbenzene six hydrogen cyclotetrasiloxane and triphenyl three hydrogen cyclotrisiloxane.Especially, described phenyl alkoxysilane be following in one or more: phenyl triethoxysilane, phenyltrimethoxysila,e, aminomethyl phenyl dimethoxysilane, aminomethyl phenyl diethoxy silane, dimethoxydiphenylsilane, diphenyl diethoxy silane, Phenylmethoxy diethoxy silane, diphenylmethyl methoxylsilane methyldiphenyl methoxylsilane, methyldiphenylethoxysilane, triphenylmethoxy silane, triphenyl Ethoxysilane, 1,3-dimethyl-1,1,3,3-tetraphenyl-sily oxide.
Especially, described hydrogen end-capping reagent is 1,1,3,3-tetramethyl--1,3-dihydro sily oxide.
Especially, described an acidic catalyst is the one or wherein multiple in the fat of sulfuric acid, hydrochloric acid, strong-acid type cation exchange tree.Especially, described extraction agent is one or more in toluene, dimethylbenzene, hexamethyldisiloxane.
Preferably, described water glass consumption is 0.1-1 times of organoalkoxysilane total mass; The phenyl group total mole number of described phenyl alkoxysilane is 0.5-5 with the ratio of the total mole number of Si-H group in ring hydrogen siloxane and hydrogen end-capping reagent; The quality of described hydrogen end-capping reagent is the 10-90wt% of phenyl alkoxysilane and ring hydrogen siloxane total mass; The consumption of described an acidic catalyst is the 0.5-7wt% of water glass, phenyl alkoxysilane and ring hydrogen siloxane total amount; Described dehydrated alcohol quality is the 60-90wt% of phenyl alkoxysilane and ring hydrogen siloxane total mass; The quality of described extraction agent is the 15-30wt% of reaction system total mass.
Especially, described modulus of water glass is 2-4, and solid content is 10%-40wt%.
Especially, when described an acidic catalyst is hydrochloric acid, solid content is 36.5wt%.
According to another aspect of the present invention, provide a kind of preparation method of LED phenyl Silicon Containing Hydrogen resin, comprise the steps:
A. add sodium silicate solution in oxytropism catalyzer and carry out reaction 60 to 400 seconds;
B. add the ethanol solution of phenyl alkoxysilane, react 5 to 20 minutes;
C. add hydrogen end-capping reagent, at ambient temperature, react 20 to 60 minutes;
D. add extraction agent, under 50 to 80 degrees celsius, react 0.5 to 8 hours, stratification, gets organic layer;
E. organic layer is extremely neutral with deionized water wash, and is dried to clear;
F. dried organic layer removing low-boiling-point substance, obtains phenyl Silicon Containing Hydrogen resin.
Wherein, also comprised before described step c: the ethanol solution adding one or more of ring hydrogen siloxane, react 20 to 30 minutes.
Wherein, carry out drying in described step f with siccative to organic layer, siccative is one or both in Calcium Chloride Powder Anhydrous, anhydrous magnesium sulfate.
Wherein, go the operational condition of low-boiling-point substance to be in described step g: vacuum tightness is-0.08 to-0.096MPa, and temperature is 150-240 degree Celsius, the de-low time is 3 hours.
The organism that aforesaid method adopts environmental protection inexpensive, as solvent, adopts the cohydrolysis polycondensation under normal temperature condition of water glass, phenyl alkoxysilane and small molecules hydrogenous material, has prepared a kind of hydrogeneous linking agent of phenyl of premium properties.This kind of method technique is simple, organic solvent recoverable, energy-conserving and environment-protective.The phenyl Silicon Containing Hydrogen resin viscosity adopting aforesaid method obtained is adjustable between 500-100000mPas, specific refractory power is adjustable between 1.45-1.55, hydrogen content is adjustable between 0.2-1.0wt%, has the premium propertiess such as high refractive index, high transmission rate, high-low temperature resistant, good weatherability.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly understand, hereinafter embodiments of the invention are described in detail.It should be noted that, when not conflicting, the embodiment in the application and the feature in embodiment can arbitrary combination mutually.
Example 1:
Present embodiment illustrates a kind of preparation method of LED phenyl Silicon Containing Hydrogen resin, concrete steps are as follows:
Step S101: add 1.2g(g and represent gram in the there-necked flask of 250ml drying) hydrochloric acid (36.5wt%), rapid stirring at 30 DEG C, adds 12g solid content 30%, modulus is the water glass of 2, hydrolysis time 120 seconds;
Step S102: add phenyltrimethoxysila,e 38g, the mixture of dimethoxydiphenylsilane 20g and dehydrated alcohol 76g, reacts 20 minutes;
Step S103: add 1,1,3,3-tetramethyl--1,3-dihydro sily oxide 38g, react 20 minutes;
Step S104: add 40 g toluene again, be warmed up to 75 DEG C of backflows 4 hours, then stopped reaction, stratification, gets organic layer;
Step S105: get organic layer and with deionized water wash to neutral, be dried to Calcium Chloride Powder Anhydrous as clear as crystal;
Step S106: after filtration, is warming up to 160 DEG C organic layer normal pressure, after reclaiming majority of organic solvent, removes low-boiling-point substance, obtain clear benzene hydrogen silicone resin product at 160 DEG C and-0.08MPa.
The productive rate adopting this method gained phenyl Silicon Containing Hydrogen resin is 85%, and specific refractory power is 1.47, and hydrogen content is 0.6%, and viscosity is 700mPas.
Example 2:
Present embodiment illustrates the another kind of preparation method of LED phenyl Silicon Containing Hydrogen resin, concrete steps are as follows:
Step S201: add 2.4g concentrated hydrochloric acid (36.5wt%), rapid stirring at 30 DEG C in the there-necked flask of 250ml drying, add 24g solid content 25%, modulus is the water glass of 2, hydrolysis time 60 seconds;
Step S202: add phenyltrimethoxysila,e 33g, the mixture of dimethoxydiphenylsilane 16g and dehydrated alcohol 30g, reacts 10 minutes;
Step S203: add, the mixture of tetramethyl-tetrahydrochysene cyclotetrasiloxane 16g and dehydrated alcohol 15g, reacts 30 minutes;
Step S204: add 1,1,3,3-tetramethyl--1,3-dihydro sily oxide 20g, react 40 minutes;
Step S205: add 40g toluene, be warmed up to 75 DEG C of backflows 5 hours, then stopped reaction, stratification, gets organic layer;
Step S206: by organic layer deionized water wash to neutral, be dried to as clear as crystal with Calcium Chloride Powder Anhydrous;
Step S207: after filtration, is warming up to 160 DEG C organic layer normal pressure, after reclaiming majority of organic solvent, removes low-boiling-point substance, obtain clear product benzene hydrogen silicone resin at 160 DEG C and-0.08MPa.
The productive rate adopting this method gained phenyl Silicon Containing Hydrogen resin is 80%, and specific refractory power is 1.45, and hydrogen content is 0. 52%, and viscosity is 15000 mPas.
Example 3:
Present embodiment illustrates the another kind of preparation method of LED phenyl Silicon Containing Hydrogen resin, concrete steps are as follows:
Step S301: add the 4.8g vitriol oil in the there-necked flask of 250ml drying, rapid stirring at 25 DEG C, add 9.6g solid content 20%, modulus is the water glass of 2, hydrolysis time 60 seconds;
Step S302: add phenyltrimethoxysila,e 32g, the mixture of aminomethyl phenyl diethoxy silane 37g and 56g dehydrated alcohol, reacts 20 minutes;
Step S303: add 1,1,3,3-tetramethyl--1,3-dihydro sily oxide 24g, react 40 minutes;
Step S304: add 40g hexamethyldisiloxane, be warmed up to 65 DEG C of backflows 6 hours, then stopped reaction, stratification, gets organic layer;
Step S305: organic layer is extremely neutral with deionized water wash, is dried to as clear as crystal with Calcium Chloride Powder Anhydrous;
Step S306: filter and remove calcium chloride, and organic layer normal pressure is warming up to 160 DEG C, after reclaiming majority of organic solvent, removes low-boiling-point substance at 160 DEG C and-0.08MPa, obtains clear phenyl Silicon Containing Hydrogen resin.
Adopt the productive rate 75% of this method gained phenyl Silicon Containing Hydrogen resin, specific refractory power is 1.50, and hydrogen content is 0.43, and viscosity is 3000mPas.
Example 4:
Present embodiment illustrates the another kind of preparation method of LED phenyl Silicon Containing Hydrogen resin, concrete steps are as follows:
Step S401: add the 3g vitriol oil in the there-necked flask of 250ml drying, rapid stirring at 25 DEG C, adds 12g solid content 10%, modulus is the water glass of 3, hydrolysis time 60s;
Step S402: the mixture adding phenyltrimethoxysila,e 80g and dehydrated alcohol 50g, reacts 15 minutes;
Step S403: the mixture adding tetramethyl-tetrahydrochysene cyclotetrasiloxane 6g and dehydrated alcohol 10g, reacts 30 minutes;
Step S404: add 1,1,3,3-tetramethyl--1,3-dihydro sily oxide 16g, react 30 minutes;
Step S405: add 50g hexamethyldisiloxane, be warmed up to 65 DEG C of backflows 8 hours, then stopped reaction, stratification, gets organic layer;
Step S406: organic layer is extremely neutral with deionized water wash, is dried to as clear as crystal with Calcium Chloride Powder Anhydrous;
Step S407: after filtration, is warming up to 160 DEG C organic layer normal pressure, after reclaiming majority of organic solvent, removes low-boiling-point substance, obtain clear product phenyl Silicon Containing Hydrogen resin at 160 DEG C and-0.08MPa.
The productive rate adopting this method gained phenyl Silicon Containing Hydrogen resin is 70%, and specific refractory power is 1.52, and hydrogen content is 0.33%, and viscosity is 90000mPas.
The foregoing is only the preferred embodiments of the present invention.Phenyl Silicon Containing Hydrogen resin of the present invention is not limited to LED field, it can be applied in other field and go.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (14)
1. a LED phenyl Silicon Containing Hydrogen resin, is characterized in that, comprise following raw material: an acidic catalyst, water glass, phenyl alkoxysilane, dehydrated alcohol, hydrogen end-capping reagent, extraction agent.
2. a kind of LED phenyl Silicon Containing Hydrogen resin as claimed in claim 1, it is characterized in that, described raw material also comprises: ring hydrogen siloxane.
3. a kind of LED phenyl Silicon Containing Hydrogen resin as claimed in claim 1, it is characterized in that: described phenyl alkoxysilane be following in one or its arbitrary combination: phenyl triethoxysilane, phenyltrimethoxysila,e, aminomethyl phenyl dimethoxysilane, aminomethyl phenyl diethoxy silane, diphenyl diethoxy silane, Phenylmethoxy diethoxy silane, diphenylmethyl methoxylsilane, methyldiphenyl methoxylsilane, methyldiphenylethoxysilane, triphenylmethoxy silane, triphenyl Ethoxysilane, 1, 3-dimethyl-1, 1, 3, 3-tetraphenyl-sily oxide.
4. a kind of LED phenyl Silicon Containing Hydrogen resin as claimed in claim 2, is characterized in that: described ring hydrogen siloxane is one or more in tetramethyl-tetrahydrochysene cyclotetrasiloxane, trimethylammonium three hydrogen cyclotrisiloxane, hexamethyl dihydro cyclotetrasiloxane, tetraphenyl tetrahydrochysene cyclotetrasiloxane, phenylbenzene six hydrogen cyclotetrasiloxane and triphenyl three hydrogen cyclotrisiloxane.
5. a kind of LED phenyl Silicon Containing Hydrogen resin as claimed in claim 1, is characterized in that: described hydrogen end-capping reagent is 1,1,3,3-tetramethyl--1,3-dihydro sily oxide.
6. a kind of LED phenyl Silicon Containing Hydrogen resin as claimed in claim 1, is characterized in that: described an acidic catalyst is the one or wherein multiple in sulfuric acid, hydrochloric acid, strongly acidic cation-exchange.
7. a kind of LED phenyl Silicon Containing Hydrogen resin as claimed in claim 1, is characterized in that: described extraction agent is one or more in toluene, dimethylbenzene, hexamethyldisiloxane.
8., as a kind of LED phenyl Silicon Containing Hydrogen resin as described in arbitrary in claim 1 to 7, it is characterized in that, also comprise:
Described water glass consumption is 0.1-1 times of organoalkoxysilane total mass;
The phenyl group total mole number of described phenyl alkoxysilane is 0.5-5 with the ratio of the total mole number of Si-H group in ring hydrogen siloxane and hydrogen end-capping reagent;
The quality of described hydrogen end-capping reagent is the 10-90wt% of phenyl alkoxysilane and ring hydrogen siloxane total mass;
The consumption of described an acidic catalyst is the 0.5-7wt% of water glass, phenyl alkoxysilane and ring hydrogen siloxane total amount;
Described dehydrated alcohol quality is the 60-90wt% of phenyl alkoxysilane and ring hydrogen siloxane total mass;
The quality of described extraction agent is the 15-30wt% of reaction system total mass.
9., as a kind of LED phenyl Silicon Containing Hydrogen resin as described in arbitrary in claim 1 to 7, its feature also comprises: described modulus of water glass is 2-4, and solid content is 10%-40wt%.
10., as a kind of LED phenyl Silicon Containing Hydrogen resin as described in arbitrary in claim 1 to 7, it is characterized in that: when described an acidic catalyst is hydrochloric acid, solid content is 36.5wt%.
11. 1 kinds of preparation methods preparing LED phenyl Silicon Containing Hydrogen resin according to claim 1, it is characterized in that, described method comprises the steps:
A. add sodium silicate solution in oxytropism catalyzer and carry out reaction 60 to 400 seconds;
B. add the ethanol solution of phenyl alkoxysilane, react 5 to 20 minutes;
C. add hydrogen end-capping reagent, at ambient temperature, react 20 to 60 minutes;
D. add extraction agent, under 50 to 80 degrees celsius, react 0.5 to 8 hours, stratification, gets organic layer;
E. organic layer is extremely neutral with deionized water wash, and is dried to clear;
F. dried organic layer removing low-boiling-point substance, obtains phenyl Silicon Containing Hydrogen resin.
The 12. LED preparation methods of phenyl Silicon Containing Hydrogen resin as claimed in claim 11, is characterized in that, also comprised before described step c: the ethanol solution adding one or more of ring hydrogen siloxane, react 20 to 30 minutes.
13. LED preparation methods of phenyl Silicon Containing Hydrogen resin as described in claim 11 or 12, is characterized in that, comprising: carry out drying with siccative to organic layer in described step f, and siccative is one or both in Calcium Chloride Powder Anhydrous, anhydrous magnesium sulfate.
14. LED as described in claim 11 or 12 preparation method of phenyl Silicon Containing Hydrogen resin, it is characterized in that, go the operational condition of low-boiling-point substance to be in described step g: vacuum tightness is-0.08 to-0.096MPa, and temperature is 150-240 degree Celsius, the de-low time is 3 hours.
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