Preparation method of water dispersible alkyl/polyether amino silicone resin

A polyether amino and silicone resin technology, applied in the field of silicone resins, can solve the problems of restricting the application of silicone resins, and no patent report on water-dispersible alkyl/polyether amino silicone resins, etc., to improve water solubility, application Scope widening effect

Active Publication Date: 2016-08-17
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Silicone resins are mostly insoluble in water and are mainly used in oil-soluble systems, which limits the application of silicone resins in water-based systems
At present, although there are many research reports on the synthesis and application of silicone resins at home and abroad, there are no patent reports on water-dispersible alkyl / polyether amino silicone resins.

Method used

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  • Preparation method of water dispersible alkyl/polyether amino silicone resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] To a three-necked flask equipped with a thermometer, a reflux condenser, and an electric stirrer, 30 g of methyl hydrogen-containing silicone resin (containing 0.06 mol of Si-H bonds) with a viscosity of 2080 mPa·s and a Si-H bond content of 0.2% were sequentially added, 5.7g (0.05mol) allyl glycidyl ether and 1.14g (0.01mol) α-octene, then stir and pass N 2 Heat up to 70°C under protection, then add 20ppm catalyst chloroplatinic acid to the three-necked flask and keep it warm for 6h. After the reaction, cool down to room temperature to obtain a total of about 36.84g of colorless and transparent liquid, namely the intermediate octyl / 2,3-cyclo Oxypropoxypropyl silicone resin (referred to as octyl / epoxy silicone resin), containing about 0.05mol of epoxy group.

[0024] Continue to add 13.8g (0.06mol) polyetheramine D230 to the intermediate, stir and mix well, then heat up to 120°C for 1h reaction. After the reaction, the unreacted low boilers were evaporated under reduce...

Embodiment 2

[0026] Into a three-necked flask equipped with a thermometer, a reflux condenser, and an electric stirrer, 30 g of methyl hydrogen-containing silicone resin (containing 0.03 mol of Si-H bonds) with a viscosity of 5900 mPa s and a Si-H bond content of 0.1%, and 4.62g (0.0405mol) allyl glycidyl ether and 0.76g (0.0045mol) α-dodecene, then stir and pass N 2 Heat up to 100°C under protection, then add 50ppm catalyst chloroplatinic acid to the three-necked flask and keep it warm for 0.5h, then distill off excess allyl glycidyl ether under reduced pressure at a gauge pressure of 500mmHg and a temperature of 100°C, and cool down to room temperature A total of about 33.67 g of a colorless transparent viscous liquid, namely the intermediate dodecyl / epoxy silicone resin, containing about 0.0255 mol of epoxy groups was obtained.

[0027] Continue to add 7.04g (0.0306mol) of polyetheramine D230 to the intermediate, stir and mix well, then heat up to 45°C for 4h. After the reaction, the u...

Embodiment 3

[0029] Into a three-necked flask equipped with a thermometer, a reflux condenser, and an electric stirrer, 30 g of hydrogen-containing MQ silicone resin (containing 0.24 mol of Si-H bonds) with a viscosity of 130 mPa s and a Si-H bond content of 0.8%, 22.98 g (0.2016mol) allyl glycidyl ether, 12.7g (0.0504mol) α-octadecene and 60g isopropanol-toluene mixed solvent (mass ratio of isopropanol:toluene=1:1), and then Stir and pass N 2 Heated to 80°C under protection, then added 20ppm catalyst 1,3-divinyltetramethyldisiloxane platinum complex to the three-necked flask and kept it warm for 3 hours, then cooled down to room temperature to obtain a total of about 125.68g of Colorless transparent viscous liquid, namely the solution of intermediate octadecyl / epoxy silicone resin, containing about 0.2016mol of epoxy group.

[0030] Continue to add 80.64g (0.2016mol) polyetheramine D400 to the solution of the intermediate, stir and mix well, then heat up to 60°C for 2h reaction. After t...

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Abstract

The invention discloses a method for preparing a water-dispersible alkyl / polyether amino-silicon resin. The method comprises the following steps of firstly carrying out a hydrosilation addition reaction on hydrogen-containing silicone resin, small molecular alkenyl epoxy compound and alpha-olefin according to a molar ratio of Si-H bond to alkylene group C=C double bond of 1: (1.0-1.5), synthesizing an alkyl / epoxy silicone resin intermediate and then carrying out an ammonolysis ring-opening reaction on the intermediate and polyether at 45-120 DEG C to obtain the alkyl / polyether amino-silicon resin. The alkyl / polyether amino-silicon resin prepared according to the invention can be dissolved or dispersed in water to form a stable silicon emulsion or microemulsion after the alkyl / polyether amino-silicon resin is diluted with a solvent, and thus the silicon resin is expected to be used for the field of a water-based finishing agent or a coating material.

Description

technical field [0001] The invention belongs to the field of silicone resins, and in particular relates to a preparation method of a water-emulsifiable and dispersed silicone resin with long carbon chain alkyl groups and polyether amino groups in its structure. Background technique [0002] Silicone resin is a siloxane polymer with Si-O-Si as the main chain and side chains connected to other organic groups, and its structure is highly cross-linked network, trapezoidal or semi-closed cage. Silicone resin has the dual characteristics of organic resin and inorganic materials, and has excellent heat resistance stability, electrical insulation, weather resistance and waterproof, anti-salt spray, anti-mold and biocompatibility, and can be widely used in aerospace, military, Electronic and electrical, rubber and plastics, textile and leather, material processing and modification and other fields. [0003] In the silicone resin, if the structure and type of the organic group connec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G81/00C08G77/38
Inventor 安秋凤魏元博赵洁徐新
Owner SHAANXI UNIV OF SCI & TECH
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