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Epoxidation modified phenyl silicone resin used for LED packaging adhesive, and preparation method thereof

A technology of phenyl silicone resin and LED encapsulation, applied in the direction of adhesives, etc., can solve the problems of product gel and encapsulation materials, such as easy yellowing mechanical properties, to achieve the effects of eliminating hydroxyl groups, shortening reaction time, and overcoming low efficiency

Inactive Publication Date: 2019-06-14
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation process is simple to operate, but a large amount of active hydrogen will be generated during the reaction, which will lead to the ring opening of the epoxy, thus making the product gel
Moreover, due to the large amount of residual hydroxyl groups in the structure of the synthesized epoxidized modified phenyl silicone resin, the synthesized packaging material has the disadvantages of easy yellowing and poor mechanical properties.

Method used

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  • Epoxidation modified phenyl silicone resin used for LED packaging adhesive, and preparation method thereof
  • Epoxidation modified phenyl silicone resin used for LED packaging adhesive, and preparation method thereof

Examples

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Effect test

Embodiment 1

[0039] This embodiment provides an epoxidation-modified phenyl silicone resin for LED packaging glue and a preparation method thereof.

[0040] (1) Preparation of hydroxyl-terminated phenyl silicone resin

[0041]Take 97.2g of deionized water and 1.71g of D301R basic anion exchange resin in a 250ml four-neck flask equipped with a magnetic stirrer and a temperature controller, and control the reaction temperature to 85°C. Next, 54.69 g of methylphenyldimethoxysilane and 19.8 g of phenyltrimethoxysilane were mixed uniformly, and then added dropwise into the flask. After the raw materials are dripped, start timing. After reacting for 2 h, the catalyst was removed by suction filtration under reduced pressure. Then the filtrate was moved to a separatory funnel for water washing, and the layers were left to stand (the water was in the upper layer and the target product was in the lower layer). Take the lower layer product and carry out vacuum distillation at 100°C and -0.096Mpa t...

Embodiment 2

[0045] This embodiment provides an epoxidation-modified phenyl silicone resin for LED packaging glue and a preparation method thereof.

[0046] (1) Preparation of hydroxyl-terminated phenyl silicone resin

[0047] Take 129.6g of deionized water and 2.24g of D301R basic anion exchange resin in a 250ml four-necked flask equipped with a magnetic stirrer and a temperature controller, and control the reaction temperature to 85°C. Next, 54.69 g of methylphenyldimethoxysilane and 39.66 g of phenyltrimethoxysilane were mixed uniformly, and then added dropwise into the flask. After the raw materials are dripped, start timing. After reacting for 2 h, the catalyst was removed by suction filtration under reduced pressure. Then the filtrate was moved to a separatory funnel for water washing, and the layers were left to stand (the water was in the upper layer and the target product was in the lower layer). Take the lower layer product and carry out vacuum distillation at 100°C and -0.096...

Embodiment 3

[0051] This embodiment provides an epoxidation-modified phenyl silicone resin for LED packaging glue and a preparation method thereof.

[0052] (1) Preparation of hydroxyl-terminated phenyl silicone resin

[0053] Take 97.2g of deionized water and 1.71g of D301R basic anion exchange resin in a 250ml four-neck flask equipped with a magnetic stirrer and a temperature controller, and control the reaction temperature to 85°C. Next, 73.31 g of diphenyldimethoxysilane and 19.8 g of phenyltrimethoxysilane were mixed uniformly, and then added dropwise into the flask. After the raw materials are dripped, start timing. After reacting for 2 h, the catalyst was removed by suction filtration under reduced pressure. Then the filtrate was moved to a separatory funnel for water washing, and the layers were left to stand (the water was in the upper layer and the target product was in the lower layer). Take the lower layer product and carry out vacuum distillation at 100°C and -0.096Mpa to r...

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Abstract

The invention belongs to the technical field of LED packaging adhesive, and more specifically relates to an epoxidation modified phenyl silicone resin used for LED packaging adhesive, and a preparation method thereof. According to the preparation method, hydrolytic sol-gel technology and non-hydrolytic sol-gel technology are combined, hydrolytic sol-gel method is adopted to synthesis an intermediate containing hydroxyl, the intermediate and an epoxy-containing siloxane monomer are subjected to non-hydrolytic sol-gel method dealcoholysis reaction so as to eliminate hydroxyl in modified siliconeresin, epoxy ring opening is prevented effectively, and solidification product high temperature resistance and mechanical performance are improved greatly. According to the preparation method, most epoxy groups are introduced onto product terminal groups, epoxy group activity is increased, it is beneficial for later rapid solidification reaction. The obtained epoxidation modified phenyl siliconeresin is high in light transmittance, and excellent in heat stability; the viscosity ranges from 500 to 10000mpa.s, the molecular weight ranges from 1000 to 8000, the molecular weight distribution index PDI ranges from 1.2 to 1.6, the refractive index ranges from 1.50 to 1.55, and the epoxidation modified phenyl silicone resin can be taken as an LED packaging adhesive material.

Description

technical field [0001] The invention belongs to the technical field of LED packaging adhesives, and in particular relates to an epoxidation-modified phenyl silicone resin for LED packaging adhesives and a preparation method thereof. Background technique [0002] Light-emitting diode (LED) is a new type of light-emitting device with high efficiency, energy saving and environmental protection. And a series of characteristics such as long life. In today's society where energy is relatively scarce and pollution is becoming more and more serious, the wide application of LED is of great significance. LED is mainly composed of chips, leads, brackets, packaging materials and so on. Among them, the packaging material has two main functions, one is to protect the chip and fragile leads, and the other is to improve the light extraction efficiency of the LED. Therefore, the packaging material has an important impact on the service life of the LED, and is a key technology for the prac...

Claims

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Application Information

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IPC IPC(8): C08G77/14C09J183/06
Inventor 潘朝群朱双丽
Owner SOUTH CHINA UNIV OF TECH
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