Preparation method of organic fluorosiloxane modified polyurethane emulsion containing short fluoroalkyl chain

A silicon-modified polyurethane and organic fluorine technology, applied in polyurea/polyurethane coatings, coatings, etc., can solve the problems of water resistance, solvent resistance, and solvent environmental pollution, and achieve enhanced water resistance and good water repellency , good heat resistance effect

Active Publication Date: 2014-06-18
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This invention adopts the method of solution polymerization, introduces polysiloxane segment modified by organic functional group, and uses organosilicon to modify polyurethane, which can improv...

Method used

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  • Preparation method of organic fluorosiloxane modified polyurethane emulsion containing short fluoroalkyl chain
  • Preparation method of organic fluorosiloxane modified polyurethane emulsion containing short fluoroalkyl chain
  • Preparation method of organic fluorosiloxane modified polyurethane emulsion containing short fluoroalkyl chain

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Add 3.76g (10mmol) of perfluorohexyl propylene oxide into a completely sealed 100ml single-mouth bottle, 15.53g (0.15mol) of an excess concentration of 30% methylamine aqueous solution, add 50ml of solvent methanol, and stir the mixture for 10h under magnetic force. Remove excess methylamine and solvent methanol by rotary evaporation, then add 4.51 g (12 mmol) of perfluorohexyl propylene oxide and a small amount of methanol, and react under reflux at 65°C for 10 h. The solvent was removed by rotary evaporation, and then recrystallized with chloroform. After cooling, 6.28 g of the target product fluorine-containing dihydric alcohol was obtained, with a yield of 80.26%.

Embodiment 2

[0050] Add 6.65g (30mmol) of isophorone diisocyanate, 20.1g (10.05mmol) of polytetrahydrofuran ether glycol, and 4.2 g (2.1mmol), react at 90°C for 2.5h. Dissolve 1.8g (13.4mmol) of dimethylolpropionic acid and 1.05g (1.35mmol) of fluorine-containing diol in 2.0ml of N-methyl-2-pyrrolidone, add them into the reaction bottle, and react at 90°C for 4h. When the reaction temperature dropped to 40°C, triethylamine (1.35 g, 13.4 mmol) was added to neutralize the reaction, and the reaction was maintained for 30 min. Then the temperature in the reaction bottle was lowered to 0°C, and 80.0g (4.45mol) of water was added to disperse for 1h under the action of a high-speed disperser at a speed of 8000r / min, and 0.3g (4.9mmol) of ethylenediamine was added to extend the chain. An organofluorosilicon-modified aqueous polyurethane solution with a solid content of about 30% was obtained.

Embodiment 3

[0052] Add 6.65g (30mmol) of isophorone diisocyanate, 19.3g (9.65mmol) of polytetrahydrofuran ether glycol, and 3.5g of hydroxyl silicone oil into a 250ml four-necked bottle equipped with a nitrogen drying tube, a reflux condenser, a mechanical stirring paddle, and a thermometer. g (1.75mmol), react at 90°C for 1.5h. Dissolve 1.7g (12.7mmol) of dimethylolpropionic acid and 1.75g ​​(2.2mmol) of fluorine-containing diols in 5.0ml of N-methyl-2-pyrrolidone, add them to the reaction bottle, and react at 90°C for 6h . When the reaction temperature dropped to 40°C, 1.3 g (12.8 mmol) of triethylamine was added to neutralize the reaction, and the reaction was maintained for 30 min. Then the temperature in the reaction bottle was lowered to 0°C, and 95.5g (5.3mol) of water was added to disperse for 1h under the action of a high-speed disperser at a speed of 8000r / min, and 0.3g (4.9mmol) of ethylenediamine was added to extend the chain. An organofluorosilicon-modified aqueous polyuret...

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Abstract

The invention relates to a preparation method of an organic fluorosiloxane modified polyurethane emulsion containing a short fluoroalkyl chain. The method comprises the following steps: by taking isophorone diisocyanate as a hard segment and a mixture of polytetrahydrofuran ether diol and hydroxyl silicone oil as a soft segment, heating to 70-110 DEG C to react for 1-8 hours; then, adding dimethylolpropionic acid and fluorine-containing diol as a chain extender for primary chain extension for 1-6 hours; cooling to 25-60 DEG C, adding a neutralizer, stirring for 0.5-1.5 hours, and transferring to a high speed disperser; adding neutralizer and a secondary chain extender, and dispersing for 0.5-3 hours at a high speed to obtain the emulsion which is uniform and stable in grain size. The prepared modified polyurethane emulsion coating not only has better temperature resistance, water resistance, solvent resistance and corrosion resistance, but also has good water repellency and oil repellency.

Description

technical field [0001] The invention relates to a preparation method of organofluorosilicon-modified polyurethane emulsion containing short fluorocarbon chains, and belongs to the technical field of modified polyurethane applications. Background technique [0002] Polyurethane has the advantages of high strength, wide hardness range, low temperature resistance, wear resistance, solvent resistance, good compatibility, high film forming strength, etc. It is widely used in coatings, fabric finishing agents, adhesives, biomedical materials and other fields. However, due to the common defects of polyurethane such as poor thermal stability, poor water resistance, and low initial viscosity, its application is limited. Aiming at the deficiencies and defects of polyurethane, many scientists at home and abroad have been engaged in the modification of polyurethane resin, and there have been a large number of literature reports. The common modification methods are: epoxy resin modificat...

Claims

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Application Information

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IPC IPC(8): C08G18/66C08G18/48C08G18/61C08G18/12C08G18/32C08G18/34C08G18/75C08G18/76C09D175/08
CPCC08G18/0823C08G18/12C08G18/4009C08G18/4854C08G18/61C08G18/6688C08G2150/90C09D175/08C08G18/3812C08G18/3228C08G18/3206
Inventor 王明刚刘舒谭业邦
Owner SHANDONG UNIV
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