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T-chain unit phenyl-containing MTQ silicon resin and preparation method thereof

A technology of silicone resin and phenyltrimethoxysilane, which is applied in the field of MTQ type silicone resin containing phenyl in the T chain segment and its synthesis, can solve the problems of reducing the optical efficiency of semiconductor lighting devices and large differences in refractive index, and achieve improvement Effects of light efficiency, reducing the difference in refractive index, and increasing the phenyl content

Active Publication Date: 2013-01-30
HANGZHOU NORMAL UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to solve the problem that when MTQ silicone resin is used as a silicone rubber reinforcing filler, the refractive index difference between the packaging material and the LED chip is large due to the small refractive index, and the optical efficiency of the semiconductor lighting device is reduced, the present invention proposes a MTQ containing phenyl in the T chain Type silicone resin and preparation method thereof, the present invention can not only improve the light efficiency of semiconductor lighting devices, but also improve the mechanical properties of packaging materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] In a 250 mL three-necked flask with a stirrer and a thermometer sleeve, add 4.0 g (0.222 mol) deionized water and 5.5 g (0.120 mol) absolute ethanol. After stirring, add 3.3 g (0.0204 mol) A solution composed of methyl disiloxane and 4.1 g (0.022 mol) 1,3-divinyltetramethyl disiloxane, then add 1.10 g of concentrated hydrochloric acid (0.0108 mol) with a concentration of 36 wt%, and raise the temperature When the temperature reaches 30°C, add dropwise a mixture of 20.9 g (0.1005 mol) tetraethoxysilane and 3.1 g (0.0157 mol) phenyltrimethoxysilane, drop it in within 5 minutes, and then maintain the reaction at 50°C for 4 hours. Add 20.0 g (0.2174 mol) of toluene and extract for 0.5 h when the temperature is lowered to 40℃, then cool to room temperature, wash with water to neutrality, add anhydrous calcium chloride to dry until it is clear and transparent, filter to remove the salt, and rotate to evaporate to remove the toluene solvent to obtain transparency MTQ resin soli...

Embodiment 2

[0035] In a 250 mL three-necked flask equipped with a stirrer and a thermometer sleeve, add 12.2 g (0.6778 mol) deionized water and 5.2 g (0.113 mol) absolute ethanol. After stirring, add 2.4 g (0.0148 mol) A solution composed of methyl disiloxane and 3.6 g (0.0194 mol) 1,3-divinyltetramethyl disiloxane, then add 1.80 g of concentrated hydrochloric acid (0.0178 mol) with a concentration of 36 wt%, and raise the temperature When the temperature reaches 50°C, a mixture of 21.4 g (0.1029 mol) tetraethoxysilane and 4.7 g (0.0237 mol) phenyltrimethoxysilane is added dropwise, and the drop is completed within 10 minutes, and then the reaction is maintained at 70°C for 2 hours. Add 18.0 g (0.1957 mol) of toluene and extract for 2h when the temperature is lowered to 50℃, then cool to room temperature, wash with water to neutrality, add anhydrous calcium chloride to dry until it is clear and transparent, filter to remove the salt, and rotary evaporation to remove the toluene solvent to o...

Embodiment 3

[0039] In a 250 mL three-necked flask with a stirrer and a thermometer sleeve, add 12.2 g (0.6778 mol) of deionized water and 5.1 g (0.1109 mol) of absolute ethanol. After stirring, add 2.1 g (0.013 mol) of ethanol. A solution composed of methyl disiloxane and 3.1 g (0.0167 mol) 1,3-divinyl tetramethyl disiloxane, then add 2.50 g of concentrated hydrochloric acid (0.0247 mol) with a concentration of 36 wt%, and raise the temperature When the temperature reaches 60°C, add dropwise a mixture of 20.9 g (0.1005 mol) tetraethoxysilane and 7.4 g (0.0374 mol) phenyltrimethoxysilane, drop it in within 20 minutes, and then maintain the reaction at 70°C for 1 hour. After cooling to 60℃, add 40.0 g (0.4348 mol) of toluene and extract for 2.5 hours, then cool to room temperature, wash with water to neutrality, add anhydrous calcium chloride to dry until it is clear and transparent, filter to remove salt, and rotary evaporation to remove toluene solvent to obtain MTQ Resin solid.

[0040] Th...

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Abstract

The invention relates to the field of organic polymer chemistry and discloses a T-chain unit phenyl-containing MTQ silicon resin and a preparation method thereof. The T-chain unit phenyl-containing MTQ silicon resin solves the problem that a MTQ silicon resin as a silicon rubber reinforcement filler leads to a large difference between refractive indexes of a packaging material and a LED chip because of a small refractive index of the MTQ silicon resin and thus optical efficiency of a semiconductor lighting device is reduced. The preparation method comprises that tetraethoxysilane as a Q chain unit source, phenyltrimethoxysilane as a T chain unit source, hexamethyldisiloxane as an M chain unit source and 1,3-divinyltetramethyldisiloxane as an M chain unit source undergo a co-hydrolytic condensation reaction in the presence of hydrochloric acid as a catalyst to produce the T-chain unit phenyl-containing MTQ silicon resin. The T-chain unit phenyl-containing MTQ silicon resin can improve luminous efficacy of a semiconductor lighting device and improve mechanical properties of a packaging material. The preparation method allows mild reaction conditions, has simple processes and is suitable for large-scale industrial production.

Description

Technical field [0001] The invention relates to the field of organic polymer chemistry, in particular to an MTQ type silicone resin containing phenyl groups in T chain links and a synthesis method thereof. Background technique [0002] MTQ type silicone resin is a kind of silicone resin, which consists of monofunctional silicone-oxygen chain link (R 1 R 2 R 3 SiO 1 / 2 , M chain link), trifunctional siloxane chain link (R 4 SiO 3 / 2 , T chain link) and tetrafunctional siloxane chain link (SiO 4 / 2 , Q chain link) silicone resin with core-shell structure produced by co-hydrolysis-condensation reaction of organosilicon compound, the core layer is composed of Q chain sections, and the shell layer is composed of M chain sections and T chain sections. With the organic group R on the spherical shell 1 , R 2 ,R 3 And R 4 The change, MTQ silicone resin has different properties. When the organic group R 1 , R 2 ,R 3 And R 4 When all are methyl, MTQ silicone resin is also called methyl MTQ si...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/20C08G77/06C09K3/10
Inventor 伍川张宝华董红蒋剑雄程大海陈世龙
Owner HANGZHOU NORMAL UNIVERSITY
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