Organosiloxane-polypropylene oxide block copolymer and preparation method thereof, prepared two-component LED pouring sealant and preparation method thereof

An organosiloxane, polyoxypropylene technology, applied in the directions of polyurea/polyurethane adhesives, adhesives, adhesive types, etc., can solve the problems of complicated preparation methods, many preparation steps, and high material costs, and achieve easy industrial Effects of conversion, increased refractive index, and reduced material cost

Inactive Publication Date: 2020-01-14
SHANDONG INOV NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN105694047B introduces a modified organosilicon polymer containing a ring structure in the main chain and its preparation method. This method uses organic solvents such as toluene and also involves noble metal catalysts. The preparation method is relatively cumbersome and the material cost is relatively high.
Chinese patent CN106633079A introduces an organic-inorganic hybrid material with many preparation steps and relatively difficult industrial transformation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] The preparation method of described organosiloxane-polyoxypropylene block copolymer is as follows:

[0043] (1) Add 297g of octamethylcyclotetrasiloxane and 5.3g of potassium hydroxide to the pressure-resistant reactor, replace the air in the reactor with nitrogen, raise the temperature to 90±5°C, evacuate to -0.09MPa, and react 1h, then raise the temperature to 100°C, continuously add 1830g of propylene oxide into the reaction kettle, fully react for 2h after feeding, and remove the unreacted residual alkylene oxide in a vacuum;

[0044] (2) After cooling down to 75°C, add 75g of pure water, 12.72g of phosphoric acid (mass concentration 70%), 4g of magnesium silicate and aluminum silicate adsorbent for refining, heat up to 105°C, vacuumize and dehydrate for 6 hours, and circulate and filter, that is An organosiloxane-polyoxypropylene block copolymer (number average molecular weight 1975) was obtained. The hydroxyl value is 56.8mgKOH / g, and the viscosity is 781mPa·s. ...

Embodiment 2

[0059] The preparation method of described organosiloxane-polyoxypropylene block copolymer is as follows:

[0060] (1) Add 793g of octaphenylcyclotetrasiloxane and 10g of sodium hydroxide to the pressure-resistant reactor, replace the air in the reactor with nitrogen, raise the temperature to 85°C, evacuate to -0.09MPa, react for 1h, and then Raise the temperature to 100°C, continuously add 2450g of propylene oxide into the reactor, fully react for 2 hours after the addition, and remove the unreacted residual alkylene oxide in a vacuum;

[0061] (2) After cooling down to 75°C, add 120g of pure water, 24g of phosphoric acid (mass concentration 70%), 6g of magnesium silicate and aluminum silicate adsorbent for refining, heat up to 105°C, vacuumize and dehydrate for 6 hours, and circulate and filter to obtain Organosiloxane-polyoxypropylene block copolymer (number average molecular weight 2914). The hydroxyl value is 38.5mgKOH / g, and the viscosity is 1326mPa·s.

[0062] For the...

Embodiment 3

[0074] The preparation method of described organosiloxane-polyoxypropylene block copolymer is as follows:

[0075] (1) Add 920g of 2,4,6-trimethyl-2,4,6-triphenylcyclotrisiloxane and 6g of strong acid cation exchange resin to the pressure-resistant reactor, and replace the reactor with nitrogen Air, heat up to 95°C, vacuumize to -0.09MPa, react for 1h, then heat up to 100°C, continuously add 1450g of propylene oxide into the reaction kettle, fully react for 2h after feeding, remove unreacted residual alkylene oxide in a vacuum ;

[0076] (2) After cooling down to 75°C, add 80g of pure water, 14.4g of phosphoric acid (mass concentration 70%), 4g of magnesium silicate and aluminum silicate adsorbent to refine, heat up to 105°C, vacuumize and dehydrate for 6h, and circulate and filter, that is An organosiloxane-polyoxypropylene block copolymer (number average molecular weight 1024) was obtained. The hydroxyl value is 109.6mgKOH / g, and the viscosity is 451mPa·s.

[0077] For th...

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Abstract

The invention belongs to the technical field of polymer synthesis, and specifically relates to an organosiloxane-polypropylene oxide block copolymer and a preparation method thereof, a prepared two-component LED pouring sealant and a preparation method thereof. Suitable cyclosiloxane is screened as a starting agent, epoxyalkane is a polymerization unit, a copolymer containing an Si-O-Si chain segment and a C-O-C chain segment is obtained by an anion polymerization technology, an epoxyalkane chain segment is copolymerized in an organosiloxane chain segment, thus a material has high temperatureresistance of silicone resin and weather resistance of polyether polyol, and the material cost is lowered. The two-component LED pouring sealant is prepared from the organosiloxane-polypropylene oxideblock copolymer and a bisphenol A modified polyether polyol prepolymer, and the weather resistance and luminescence performance of an LED can be significantly improved; and the preparation method isscientific, reasonable, simple and easy to operate, and industrial conversion is easy.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, and in particular relates to an organosiloxane-polyoxypropylene block copolymer and a preparation method thereof, a prepared two-component LED potting glue and a preparation method thereof. Background technique [0002] With the advancement of science and technology and people's increasing requirements for environmental protection, LED light sources are increasingly favored by people due to their remarkable characteristics of environmental protection, energy saving, and long service life, and they are gradually becoming popular in thousands of households. As an important part of LED light source, the development of potting glue also restricts the development of LED to a certain extent. High-power LED potting adhesives usually use phenyl-containing silicone resin as the main raw material, and the price is relatively high. Chinese patent CN105694047B introduces a modified organosilicon p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/46C09J175/08C09J183/12
CPCC08G77/46C08L2201/08C08L2203/206C09J175/08C08L83/12
Inventor 李剑锋孙兆任张士虎周玉波张德江
Owner SHANDONG INOV NEW MATERIALS CO LTD
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