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A kind of preparation method of fluorine-containing polyether modified organosilicon polyol

A technology of fluorine-containing polyether and silicone, which is applied in the field of polymer material intermediates, can solve the problems of poor water resistance and weather resistance, etc., and achieve the effect of simple, efficient and easy control of the process, increasing functionality, and facilitating large-scale industrial production

Active Publication Date: 2020-10-09
MIRACLL CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, although silicone polymer materials prepared purely from silicone polyols have excellent performance, they are still not satisfactory in fields that require high performance such as water resistance, weather resistance, solvent resistance, and dirt resistance.

Method used

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  • A kind of preparation method of fluorine-containing polyether modified organosilicon polyol
  • A kind of preparation method of fluorine-containing polyether modified organosilicon polyol
  • A kind of preparation method of fluorine-containing polyether modified organosilicon polyol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The preparation steps of a kind of fluorine-containing polyether modified silicone polyol are as follows:

[0030] Step 1: Accurately weigh 861g and 1382g of the dried and dehydrated allyl polyether (Mn=420g / mol) and terminal hydrogen-containing fluorosilicone oil (Mn=1382g / mol), respectively, and add a thermometer and stirring device to the reaction In the container, stir evenly under the protection of nitrogen;

[0031] Step 2: Turn on the heating, raise the temperature to 80°C, add 2.2g of Speier-type platinum catalyst (0.5% platinum catalyst isopropanol solution), continue to slowly raise the temperature to 100°C, and catalyze the reaction at constant temperature for 5 hours;

[0032] Step 3: Take a sample and conduct infrared analysis quickly to ensure that there is no characteristic peak of Si-H bond in the infrared spectrum, turn on the vacuum device, reduce the pressure to -0.1Mpa, distill under reduced pressure for 2 hours, remove 67.29g of low boiling substanc...

Embodiment 2

[0034] The preparation steps of a kind of fluorine-containing polyether modified silicone polyol are as follows:

[0035] Step 1: Accurately weigh 976.1g and 1694g of the dried and dehydrated allyl polyether (Mn=454g / mol) and terminal hydrogen-containing fluorosilicone oil (Mn=1694g / mol), respectively, and add the In the reactor, stir evenly under nitrogen protection;

[0036] Step 2: Turn on the heating, raise the temperature to 70°C, add 2.67g of Karsredt-type platinum catalyst (platinum water with a mass fraction of 3000ppm), continue to slowly raise the temperature to 90°C, and carry out constant temperature catalytic reaction for 6 hours;

[0037] Step 3: Take a sample and conduct infrared analysis quickly to ensure that there is no characteristic peak of Si-H bond in the infrared spectrum, turn on the vacuum device, reduce the pressure to -0.1Mpa, distill under reduced pressure for 3 hours, remove 93.45g of low boiling substances, and return to normal pressure Then add ...

Embodiment 3

[0039] The preparation steps of a kind of fluorine-containing polyether modified silicone polyol are as follows:

[0040] Step 1: Accurately weigh 596.2g and 1003g of the dried and dehydrated allyl polyether (Mn=542g / mol) and terminal hydrogen-containing fluorosilicone oil (Mn=2006g / mol), respectively, and add them to a tank equipped with a thermometer and a stirring device In the reactor, stir evenly under nitrogen protection;

[0041] Step 2: Turn on the heating, raise the temperature to 75°C, add 3.2g of Speier-type platinum catalyst (0.5% platinum catalyst in isopropanol solution), continue to slowly raise the temperature to 110°C, and catalyze the reaction at constant temperature for 4.5h;

[0042] Step 3: Take a sample and conduct infrared analysis quickly to ensure that there is no characteristic peak of Si-H bond in the infrared spectrum, turn on the vacuum device, reduce the pressure to -0.1Mpa, distill under reduced pressure for 2 hours, remove 52.77g of low boiling ...

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Abstract

The invention belongs to the technical field of polymer material intermediates, and the matrix relates to a preparation method of a fluorine-containing polyether modified silicone polyol. The invention mainly uses a monoallyl polyether and a terminal hydrogen-containing fluorosilicone to perform hydrosilicon addition reaction to prepare fluorine-containing polyether modified silicone polyol. The fluorine-containing polyether modified silicone polyol prepared by this method can combine the excellent properties of silicone materials and organic fluorine materials, such as heat resistance, hydrolysis resistance, and dirt resistance, etc. At the same time, the terminal ether hydroxyl group has good reactivity and can be widely used The method is applied in the field of chemical modification of polyurethane, epoxy resin, etc., and the reaction process of the method of the present invention does not involve solvent, the process is simple, efficient and easy to control, green and environmentally friendly, and conducive to large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of polymer material intermediates, and in particular relates to a preparation method of fluorine-containing polyether modified silicone polyol. Background technique [0002] Polyether modified polysiloxane is a research and development hotspot at home and abroad in recent years. Through the graft modification of hydrophilic polyether, polysiloxane can be endowed with water solubility, so that it not only has the excellent properties of high and low temperature resistance, aging resistance, and low surface tension of traditional polysiloxane, but also has Lubrication, softness, good spreadability and emulsification stability, etc., so it has broad application prospects in cosmetics, textile finishing agents, spinning oils and defoamers. Polyether-modified polysiloxane is a polyether-siloxane copolymer obtained by introducing a polyether segment through the connection of -Si-C-bond and -Si-O-C-bond in the sil...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/38C08G77/46C08G77/08
CPCC08G77/08C08G77/38C08G77/46
Inventor 刘德富柳群杰宋红玮张生王仁鸿
Owner MIRACLL CHEM
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