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Preparation method of tackifier used for organosilicone LED packaging colloidal system

A LED encapsulation and tackifier technology, applied in adhesives, polymer adhesive additives, adhesive additives, etc., can solve problems such as Pt catalyst poisoning, achieve improved adhesion, strong operability, and good mutual solubility Effect

Inactive Publication Date: 2017-02-15
YANTAI DEBANG ADVANCED SILICON MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese invention patent application CN102775611A discloses a method for preparing a tackifier. The method uses organotin to catalyze hydroxyl silicone oil and KH-560 and KH-570 to obtain a tackifier. The tackifier is a colorless or light yellow transparent liquid , when used in two-component addition type silicone resin, the mutual solubility is very good, and there is no discoloration phenomenon, but when this tackifier is used in LED silicone encapsulation adhesive, organotin may poison the Pt catalyst

Method used

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  • Preparation method of tackifier used for organosilicone LED packaging colloidal system
  • Preparation method of tackifier used for organosilicone LED packaging colloidal system
  • Preparation method of tackifier used for organosilicone LED packaging colloidal system

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Experimental program
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Effect test

Embodiment 1

[0020] Add 26.16g 2-acrylic acid 3-(diethoxymethylsilyl) propyl ester (0.12mol), 23.6g gamma-glycidyl etheroxypropyl trimethoxysilane (0.1mol) to 250mL there-necked flask, Stir and mix with a magnet, then raise the temperature to 60°C, add 3.24g deionized water, stir for 30 minutes, then slowly add 0.25g LiOH·H 2 0, after the dropwise addition, react for 5h, then react under vacuum for 1h until the feed liquid does not foam, stop the vacuum, add 1.7g stearic acid, stir and react for 0.5h after adding, stop heating, cool down, and discharge, After the reaction is complete, add 26.15g of n-heptane, wash with water, separate layers, add anhydrous sodium sulfate to dry, filter, put the filtrate in a rotary evaporator, and vacuum remove small molecules at 95°C for 2 hours to obtain a colorless and transparent tackifier.

Embodiment 2

[0022] Add 26.16g 2-acrylic acid 3-(diethoxymethylsilyl) propyl ester (0.12mol), 27.8g gamma-glycidyl etheroxypropyl triethoxysilane (0.1mol) to the 250mL three-necked flask , magnetically stirred and mixed, then heated up to 60°C, added 3.24g deionized water, stirred for 30 minutes, and then slowly added 0.27g LiOH·H to the three-necked flask 2 0, after the dropwise addition, react for 5h, then react for 1h under vacuum conditions, until the feed liquid does not foam, stop the vacuum, add 1.83g stearic acid, stir and react for 0.5h after adding, stop heating, cool down, and discharge, After the reaction is complete, add 26.15g of n-heptane, wash with water, separate layers, add anhydrous sodium sulfate to dry, filter, put the filtrate in a rotary evaporator, and vacuum remove small molecules at 95°C for 2 hours to obtain a colorless and transparent tackifier.

Embodiment 3

[0024] Add 28.16g of 3-trimethoxysilane propyl acrylate (0.12mol) and 22.1g of γ-glycidylpropylmethyldimethoxysilane (0.1mol) to a 250mL three-necked flask, stir and mix with a magnet, and then heat up to 60 ℃, add 3.24g deionized water, stir for 30 minutes, then slowly add 0.25g LiOH·H 2 0, after the dropwise addition, react for 5h, then react under vacuum for 1h until the feed liquid does not foam, stop the vacuum, add 1.7g stearic acid, stir and react for 0.5h after adding, stop heating, cool down, and discharge, After the reaction is complete, add 28.15g of n-heptane, wash with water, separate layers, add anhydrous sodium sulfate to dry, filter, put the filtrate in a rotary evaporator, and vacuum remove small molecules at 95°C for 2 hours to obtain a colorless and transparent tackifier.

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Abstract

The invention relates to a preparation method of a tackifier used for an organosilicone LED packaging colloidal system. The preparation method comprises the following steps: adding siloxane with an acrylate group and siloxane with an epoxy group at the amount-of-substance ratio of 1:(1-1.5) into a reaction flask, stirring and mixing; raising the temperature to 50-70 DEG C, adding deionized water whose amount-of-substance ratio to siloxane with the acrylate group is 1:1.5, stirring for half an hour, adding a basic catalyst into the reaction flask, reacting for 4-6 hours, reacting under the vacuum condition for 0.5-1.5 hours, stopping vacuum operation, adding an acid whose amount is the same with that of the basic catalyst, neutralizing the basic catalyst to neutral, stirring to react for half an hour, stopping heating after finishing neutralizing, cooling, and discharging, wherein the reactions are carried out at the temperature of 50-70 DEG C; adding normal heptane whose mass is the same with that of the siloxane with the acrylate group after the reaction, washing with water, drying, filtering, and using a rotary evaporator to remove a low molecule in vacuum, so as to obtain the colorless transparent tackifier.

Description

technical field [0001] The invention belongs to the technical field of silicone material binders, in particular to a tackifier in an addition-type LED packaging material and a preparation method thereof. [0002] technical background [0003] Addition-type liquid silicone rubber has the characteristics of no by-products in the vulcanization process, extremely low shrinkage and deep vulcanization. It is an important auxiliary material in the LED packaging industry. It is used in electronic components, power circuit modules, large integrated circuit boards, LEDs and other fields. get rapid development. However, since the surface of addition-type liquid silicone rubber is mostly non-polar organic groups after vulcanization, it shows low cohesive energy and lacks reactive groups, so its adhesion to the substrate is poor. , Improving the adhesive properties of addition-type liquid silicone rubber is conducive to further expanding its application in the field of LED packaging. ...

Claims

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Application Information

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IPC IPC(8): C08G77/14C08G77/20C08G77/18C08G77/08C09J11/08C09J183/04C09J183/07C09J183/06
CPCC08G77/14C08G77/08C08G77/18C08G77/20C09J11/08C09J183/04C09J183/06
Inventor 温荣政陈维
Owner YANTAI DEBANG ADVANCED SILICON MATERIALS
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