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Preparation method of triazinyl fluorine-containing chain extender-modified polyurethane emulsion

A technology of polyurethane emulsion and chain extender, which is applied in the direction of polyurea/polyurethane coatings and coatings, which can solve the problem of insufficient coverage and protection of polyurethane film, the failure of the film's hydrophobic performance to achieve the expected effect, and the inability of fluorine-containing groups Uniform and dense distribution, etc., to achieve the effect of being conducive to hydrophobicity and heat resistance stability, excellent hydrophobicity, and excellent film waterproof performance

Active Publication Date: 2020-03-06
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0016] In the above two method schemes, the fluorine-containing alkyl group is introduced into the waterborne polyurethane in the form of a chain extender or an end-capping agent. This single modification method may cause the fluorine-containing group to be uneven and uneven when the waterborne polyurethane is formed into a film. It is densely distributed on the surface of the film, so that the coverage and protection of the polyurethane film are not sufficient, so the hydrophobic performance of the film fails to achieve the expected effect; and the price of organic fluorine is expensive, if it is used blindly to improve the hydrophobic performance, makes the cost high

Method used

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  • Preparation method of triazinyl fluorine-containing chain extender-modified polyurethane emulsion
  • Preparation method of triazinyl fluorine-containing chain extender-modified polyurethane emulsion
  • Preparation method of triazinyl fluorine-containing chain extender-modified polyurethane emulsion

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preparation example Construction

[0035] A preparation method of a triazine-based fluorine-containing chain extender modified polyurethane emulsion comprises the following steps:

[0036] (1) Synthesis of triazine-based fluorine-containing chain extender:

[0037] Under the condition of ice bath, to the mixture containing acetone and water (m 丙酮 / m 水 =1.3:1) into the flask, add cyanuric chloride, and slowly add the acetone solution of organic fluoroalcohol and NaOH aqueous solution dropwise while stirring, keep the system temperature at 0-5°C, react for 4h; then raise the system temperature to 45°C , then slowly add the acetone solution of ethanolamine and the aqueous solution of NaOH dropwise at the same time, react for 5 hours; continue to heat up, when the system temperature reaches 95°C, add the acetone solution of ethanolamine and aqueous NaOH solution dropwise at the same time, react for another 8 hours, the reaction is completed, and the system is restored to room temperature, filter and wash the filt...

Embodiment 1

[0055] A preparation method of a triazine-based fluorine-containing chain extender modified polyurethane emulsion is as follows:

[0056] (1) Synthesis of triazine-based fluorine-containing chain extender:

[0057] Under the condition of 1 ℃, accurately weigh 1.54g (0.0084mol) cyanuric chloride and add the mixed solution containing 6g of acetone / water (m 丙酮 / m 水 =1.3:1) in a three-necked flask, then 3.04g (0.0084mol) perfluorohexyl alcohol (S104) was dissolved in 6g of acetone, and 3.50g (0.0088mol) of 10% NaOH aqueous solution was slowly added dropwise to the above-mentioned In the system, the dropwise addition is completed in about 2 hours, and the reaction is continued for 2 hours; after the reaction, the temperature is raised to 45°C, and 0.51g (0.0084mol) of ethanolamine in acetone solution and 3.34g (0.0084mol) of ethanolamine are slowly added dropwise into the reaction system The 10% NaOH aqueous solution was added dropwise for about 1.5h, and the reaction was carried...

Embodiment 2

[0063] A preparation method of a triazine-based fluorine-containing chain extender modified polyurethane emulsion is as follows:

[0064] (1) Synthesis of triazine-based fluorine-containing chain extender:

[0065] Under the condition of 2 ℃, accurately weigh 2.31g (0.0125mol) cyanuric chloride and add the mixed solution containing 8g of acetone / water (m 丙酮 / m 水 =1.3:1) in a three-necked flask, then 2.91g (0.0125mol) octafluoropentanol (OFP) was dissolved in 6g of acetone, and 5.25g (0.0132mol) of 10% NaOH aqueous solution was slowly added dropwise to the above-mentioned In the system, the dropwise addition is completed in about 2 hours, and the reaction is continued for 2 hours; after the reaction is completed, the temperature is raised to 45°C, and 0.77g (0.0125mol) of ethanolamine in acetone solution and 5.00g (0.0125mol) of ethanolamine are slowly added dropwise into the reaction system The 10% NaOH aqueous solution was added dropwise for about 1.5h, and the reaction was...

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Abstract

The invention relates to the technical field of polyurethane coating layers, and in particular, relates to a preparation method of a triazinyl fluorine-containing chain extender-modified polyurethaneemulsion. The invention aims to solve the problem of how to modify waterborne polyurethane by utilizing organic fluorine, so as to make the waterborne polyurethane have excellent hydrophobic performance and reduce the preparation cost. The preparation method comprises the steps: 1) synthesis of a triazinyl fluorine-containing chain extender; 2) synthesis of an -NCO-terminated fluorine-containing polyurethane prepolymer; 3) preparation of triazinyl fluorine-containing chain extender-modified polyurethane; and 4) preparation of the triazinyl fluorine-containing chain extender-modified polyurethane emulsion.

Description

technical field [0001] The invention relates to the technical field of polyurethane coatings, in particular to a preparation method of a triazine-based fluorine-containing chain extender modified polyurethane emulsion. Background technique [0002] With the improvement of people's environmental protection concept and quality of life, water-based polyurethane has gradually replaced solvent-based polyurethane due to its advantages such as environmental friendliness, wide application range, and low cost. However, water-based polyurethane uses water as the medium, and the polyurethane molecular chain contains -COOH, -OH and other hydrophilic groups, which makes its water resistance after film formation deteriorate and its use performance is poor. The C-F bond in organic fluorine has large bond energy, high stability, and low surface energy, so fluorine-containing materials show good hydrophobicity and oleophobicity. After introducing fluorine-containing groups or segments into ...

Claims

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Application Information

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IPC IPC(8): C08G18/66C08G18/48C08G18/42C08G18/32C08G18/34C08G18/12C09D175/06C09D175/08
CPCC08G18/12C08G18/348C08G18/3851C08G18/4277C08G18/4854C08G18/6644C08G18/6659C08G18/6677C08G18/6692C09D175/06C09D175/08C08G18/3206
Inventor 许伟王文赵维甲郝丽芬刘红呐王学川
Owner SHAANXI UNIV OF SCI & TECH
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