A novel low free TDI polyurethane curing agent containing fluorocarbon chain and preparation method thereof

A polyurethane and carbon chain technology, applied in the preparation of amino hydroxyl compounds, chemical instruments and methods, polyurea/polyurethane coatings, etc., can solve the poor performance of TDI-TMP addition curing agent, limited coating construction conditions, two-component Chain extender modification and other issues, to achieve the effect of reducing reaction curing time, improving acid and alkali chemical corrosion resistance, and shortening reaction time

Active Publication Date: 2021-09-21
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Fluorine has many applications in coatings, but there is no modification of the two-component chain extender, and the preparation process is complicated. The construction conditions for the modified coating are relatively limited, and the chain extender is modified with fluorine. It can solve the problems of limited construction conditions of fluorine modification and poor performance of TDI-TMP addition curing agent. For the modification of chain extender curing agent, it can be modified by adding fluorocarbon segment in the coating to improve the performance of the coating film. has important meaning

Method used

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  • A novel low free TDI polyurethane curing agent containing fluorocarbon chain and preparation method thereof
  • A novel low free TDI polyurethane curing agent containing fluorocarbon chain and preparation method thereof
  • A novel low free TDI polyurethane curing agent containing fluorocarbon chain and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] In the reaction kettle, according to the weight ratio of the formula, put 100g of methanol, 104g of perfluoropropylene oxide and 158g of aminomethanol into the kettle, start stirring (175rpm) and reflux and heat up to 45°C to start the reaction, and react for 6h Then stop the reaction and transfer to a rotary evaporator for distillation under reduced pressure at 60°C / -0.1MPa. After the methanol and aminomethanol are completely evaporated, transfer the initial product to the reaction kettle and add 125g perfluoropropylene oxide and 50g Methanol, start stirring (175rpm) and heat up to 65°C to continue the reaction. After 4 hours of reaction, continue to transfer to a rotary evaporator and distill at 60°C / -0.1MPa under reduced pressure, recrystallize and purify with chloroform, and finally obtain 196g of N, N-bis(2-hydroxy-perfluoropropyl)methanol adduct. Put it into the reaction kettle, add 121g of ethyl acetate and 0.8g of tris(2,4-di-tert-butylphenyl)phosphite, start st...

Embodiment 2

[0052]In the reaction kettle, according to the weight ratio of the formula, put 105g methanol, 99g perfluoropropylene oxide and 147g aminomethanol into the kettle respectively, start stirring (165rpm) and reflux and heat up to 40°C to start the reaction, and react for 5h Then stop the reaction and transfer to a rotary evaporator for distillation under reduced pressure at 60°C / -0.1MPa. After the methanol and aminomethanol are completely evaporated, transfer the initial product to the reaction kettle and add 115g perfluoropropylene oxide and 45g Methanol, start stirring (165rpm) and heat up to 65°C to continue the reaction. After 5 hours of reaction, continue to transfer to a rotary evaporator and distill under reduced pressure at 60°C / -0.1MPa, recrystallize and purify with chloroform, and finally obtain 186g of N, N-bis(2-hydroxy-perfluoropropyl)methanol adduct. Put it into the reaction kettle, add 112g of ethyl acetate and 0.6g of N,N-bis-(3-(3,5-di-tert-butyl-4-hydroxyphenyl)...

Embodiment 3

[0056] In the reaction kettle, according to the weight ratio of the formula, put 140g methanol, 114g perfluoropropylene oxide and 179g ethanolamine into the kettle respectively, start stirring (185rpm) and reflux and heat up to 50°C to start the reaction. After 7 hours of reaction Stop the reaction and transfer to a rotary evaporator for distillation under reduced pressure at 60°C / -0.1MPa. After methanol and aminomethanol are completely evaporated, transfer the initial product to a reaction kettle and add 136g of perfluoropropylene oxide and 68g of methanol , start stirring (185rpm) and heat up to 70°C to continue the reaction. After 6 hours of reaction, continue to transfer to a rotary evaporator and distill under reduced pressure at 60°C / -0.1MPa, recrystallize and purify with chloroform, and finally obtain 228g of N,N - Bis(2-hydroxy-perfluoropropyl)ethanol adduct. Put it into the reaction kettle and add 144g of butyl acetate and 1g of tetrakis[β-(3,5-di-tert-butyl-4-hydroxy...

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Abstract

The invention discloses a novel polyurethane addition curing agent containing fluorine carbon chain and a preparation method thereof. The method comprises: reacting perfluoropropylene oxide propane and alcohol amine in two steps under the condition of methanol as a solvent, rotary evaporation and recrystallization to obtain N,N-bis(2-hydroxy-peroxide) containing three hydroxyl groups Fluoropropyl) alcohol amine, N, N-bis (2-hydroxy-perfluoropropyl) alcohol amine, as a chain extender reacting with isocyanate, carries out addition reaction with isocyanate under the mixed catalytic conditions of solvent and catalyst to obtain solid A fluorine-containing carbon chain polyurethane addition curing agent with a content of 75%. The curing agent has strong tolerance and good quick-drying performance. It can be widely used in surface coatings such as wood paints, waterproof coatings and anti-corrosion coatings when combined with polyhydroxy resin components, giving the paint film better hardness and chemical properties of acid and alkali resistance. .

Description

technical field [0001] The invention belongs to the field of synthesis and preparation of coating adduct curing agents, and in particular relates to a novel low-free TDI polyurethane curing agent containing fluorine carbon chains and a preparation method thereof. Background technique [0002] Polyurethane coatings are also called carbamate coatings, which refer to coatings containing a considerable amount of urethane bonds in the paint film. It is a new material that was gradually developed in the middle of the 20th century. In the synthesis of polyurethane coatings, urethane paint films are generally obtained by cross-linking and curing of isocyanate groups (-NCO) and hydroxyl resin groups (-OH). It can not only provide aesthetic properties, such as color and luster, but also protect materials from environmental damage. It has a wide range of construction and can be mixed with a variety of hydroxyl resins. It is widely used in industry, agriculture, scientific research and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C269/02C07C271/28C07C271/58C08G18/78C09D5/08C09D175/04
CPCC07C213/04C07C269/02C08G18/7843C09D5/08C09D175/04C07C271/28C07C271/58C07C215/12C07C215/76
Inventor 黄洪陈雨司徒粤
Owner SOUTH CHINA UNIV OF TECH
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