Fluorine-containing polyether graft modified aqueous polyurethane and preparation and application thereof

A technology of water-based polyurethane and graft modification, which is applied in the field of water-based polyurethane, which can solve the problems of pollution and undeveloped problems, and achieve the effects of pollution-free waterproof, excellent self-cleaning performance, and good yellowing resistance

Inactive Publication Date: 2008-04-09
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the research work that has been carried out at home and abroad is still mainly focused on the investigation of t

Method used

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  • Fluorine-containing polyether graft modified aqueous polyurethane and preparation and application thereof
  • Fluorine-containing polyether graft modified aqueous polyurethane and preparation and application thereof
  • Fluorine-containing polyether graft modified aqueous polyurethane and preparation and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Add tribromoneopentyl alcohol (20.0g, 61.5mmol), NaOH (10wt%, 75g), phase transfer catalyst tetrabutylammonium bromide TBAB (0.79 g, 2.46mmol) and CH 2 Cl 2 (100 mL), stirred evenly by magnetic force, then raised the temperature to 35°C for 12 hours, stopped the reaction, and cooled to room temperature. The layers were allowed to stand, the organic matter in the lower layer was removed, the aqueous layer was extracted with dichloromethane, the organic layers were combined, and dried over anhydrous magnesium sulfate. The organic solvent was removed under vacuum. Vacuum distillation, collecting 92-94oC / 4mmHg fraction. 3,3-Dibromomethylbutene oxide was obtained as a colorless liquid (10.5 g, 70% yield). 1H NMR (300 MHz, CDCl3) δ: 3.86 (s, 4H), 4.44 (s, 4H).

[0046] Under nitrogen protection, 3,3-dibromomethylbutene oxide (10.0 g, 40.9 mmol) was added into a 100 mL three-neck flask equipped with a reflux condenser, dropping funnel and thermometer. The phase transfer ...

Embodiment 2

[0053] Under nitrogen protection, neopentyl glycol (7.37g, 70.9mmol), BF 3 ·OEt 2 (4.03g, 28.4mmol) and anhydrous dichloromethane (185mL) were added to a dry 500mL three-necked flask. Stir at room temperature for 30 minutes. Fluorine-containing butylene oxide (120 g, 0.426 mol) was slowly added dropwise to the reaction mixture. This reaction was exothermic, and a slight rise in temperature was found at this time. After the addition was complete, the reaction was continued at room temperature for 6 hours. stop the reaction, the residual BF 3 ·OEt 2 It can be washed off with 2.5wt% sodium bicarbonate aqueous solution, and then washed with hot water at 40°C, and finally the solvent is removed under vacuum. The resulting colorless viscous dihydroxyl fluorine-containing polybutylene oxide with hydroxyl groups at the end of the obtained polymer has a yield of 95% and a hydroxyl value of 42.15-39.14 mgKOH / g.

Embodiment 3

[0055] Under nitrogen protection, methanol (2.27g, 70.9mmol), BF 3 ·OEt 2 (4.03g, 28.4mmol) and anhydrous dichloromethane (185mL) were added to a dry 500mL three-necked flask. Stir at room temperature for 30 minutes. Fluorine-containing butylene oxide (120 g, 0.426 mol) was slowly added dropwise to the reaction mixture. This reaction was exothermic, and a slight rise in temperature was found at this time. After the addition was complete, the reaction was continued at room temperature for 6 hours. Terminate the reaction with 50 ml of 5% methanol solution of sodium methoxide. After stirring for 1 hour, wash with 2.5 wt % sodium bicarbonate aqueous solution and hot water at 40° C., and finally remove the solvent under vacuum. The resulting polymer is a colorless and viscous waxy substance with a methoxy group at one end and a hydroxyl group at the other end, that is, monohydroxyl fluorine-containing polybutylene oxide, with a yield of 93% and a hydroxyl value of 25.3 mgKOH / g. ...

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Abstract

The present invention relates to a fluorine-containing polyether grafting modified waterborne polyurethane, the preparation and the application thereof, a structural general formula of polyurethane is as the formula, wherein, R1 is equal to a polyurethane soft-segment polyol structure, R2 is equal to a polyurethane hard-segment isocyanate structure, R3 is equal to a polyurethane hard-segment chain extender structure, R4 is equal to the fluorine-containing polyether; X is equal to NH and O; the preparation is that: the polyol and the isocyanate react to compound the polyurethane prepolymer, then the waterborne polyurethane are obtained through the chain propagation of a chain extender, then the waterborne polyurethane and the fluorine-containing polyether are carried out a grafting reaction in the big molecules, so as to synthesize the fluorine-containing polyether grafting modified waterborne polyurethane; the application is that: the present invention can be applied to aerospace, aviation, automobiles, electronics, textiles, carpets, leathers, paper making, packaging, washing, machinery, construction and other fields. The present invention adopts the water as the solvent and has no formaldehyde, no or low VOC emission, no bioaccumulation and no toxicity, which is a multifunctional, green, environment protective, water-proof and dirt-proof coating layer and fabric finishing agent.

Description

technical field [0001] The invention belongs to the field of water-based polyurethane, in particular to fluorine-containing polyether graft modified water-based polyurethane and its preparation and application. Background technique [0002] There is currently an increasing demand for high-quality, multifunctional coatings and textiles. With the continuous deepening of research on fluorochemicals, multifunctional coatings and fabrics with water repellency, stain resistance and easy stain release have attracted extensive attention. At the same time, due to the deepening of people's awareness of environmental protection, environmentally friendly, biocompatible water-repellent, anti-fouling and easy-to-decontamination multifunctional coatings and textile finishing agents are more popular. [0003] Because the carbon-fluorine bond of fluoropolymers has a relatively large bond energy and is relatively stable, the fluorine atoms are not only firmly bonded to the carbon atoms, but ...

Claims

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Application Information

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IPC IPC(8): C08G18/83C09K3/18
Inventor 侯再坚孟卫东
Owner DONGHUA UNIV
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