Preparation method of stimuli-responsive waterborne polyurethane emulsion with high water resistance

A water-based polyurethane and stimuli-responsive technology, applied in polyurea/polyurethane coatings, coatings, etc., can solve the problems of polyurethane water resistance, poor water resistance, etc., to ensure stability, improve compactness and water resistance, and improve The effect of stability

Inactive Publication Date: 2019-07-05
浙江材华科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The Chinese Patent Publication No. CN104672422A discloses a kind of polyurethane resin as the hydrophobic and lipophilic segment, and carboxylic acid alcohol, amino sulfonate, amino acid or hydroxy sulfonate as the hydrophilic terminal compound, and the hydrophilic terminal is connected with the hydrophobic and hydrophilic segment. An emulsifier connected by the reaction of the isocyanate bond of the oil chain segment, but this type of emulsifier still cannot solve the problem of polyurethane water resistance
The water-based polyurethane prepared by the internal emulsification method or the external emulsification method has the problem of poor water resistance, and the problem of poor water resistance has always been a defect of water-based polyurethane, which limits its application in many aspects.
[0005] In order to overcome the problem of poor water resistance of water-based polyurethane, we prepared a stimulus-responsive emulsifier, and then prepared a stimulus-responsive high-water-resistant water-based polyurethane emulsion. By reducing the responsive stimulus, most of the disulfide bonds in the emulsifier can be Break, remove the hydrophilic part of the polymer chain in the system, and enhance the hydrophobic interaction between the hydrophobic part of the emulsifier and the polyurethane to improve the water resistance of the water-based polyurethane

Method used

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  • Preparation method of stimuli-responsive waterborne polyurethane emulsion with high water resistance

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] The preparation of the small molecule initiator that contains disulfide bond: 10g disulfide diol is dissolved in the mixed system of 40mL tetrahydrofuran and 40mL methylene chloride, after dissolving completely, add 9.2mL triethylamine to form solution A; 8.24g2- Bromo-2-methylpropionyl bromide was dissolved in 60mL of dichloromethane to form solution B, and solution B was added dropwise to solution A cooled in an ice bath within 30 minutes through a constant pressure dropping device, and reacted at room temperature for 24 hours; after the reaction, remove the generated salt by suction filtration, remove the solvent by rotary evaporation of the filtrate, rinse the crude product with deionized water, add anhydrous ether for extraction, take the oil phase, repeat washing / extraction 3 times, and use the organic phase obtained without Water MgSO 4 Dry for 4 hours to remove MgSO 4 Afterwards, the filtrate removes ether with rotary evaporation, obtains the small molecular in...

Embodiment 2

[0045] The preparation method of the small molecule initiator and the macromolecule initiator containing a disulfide bond is the same as that of Example 1.

[0046] Stimuli-responsive macromolecular emulsifier preparation: get the above-mentioned 10g macromolecular initiator, 100g hydrophilic monomer N-vinylpyrrolidone and add in the reaction vessel, then add 0.5g catalyst, 0.6g ligand PMDETA, 100mL acetone successively, and react The system was evacuated first, then filled with nitrogen or argon, and reacted at 90°C for 12 hours; after the reaction, the reaction mixture was passed through a neutral alumina column, and the solvent was removed by rotary evaporation, and the crude product was precipitated in ice n-hexane. Unreacted monomers were removed, and the precipitate was dried in a vacuum oven at 45°C for 24 hours to obtain stimuli-responsive emulsifier 2.

[0047] Preparation of stimuli-responsive waterborne polyurethane: the number average molecular weight M n 2000 PPG...

Embodiment 3

[0049] The preparation method of the small molecule initiator and the macromolecule initiator containing a disulfide bond is the same as that of Example 1.

[0050] Preparation of stimuli-responsive macromolecular emulsifier: preparation of stimuli-responsive macromolecular emulsifier: get above-mentioned 10g macromolecular initiator, 150g hydrophilic monomer N-vinylpyrrolidone and add in reaction vessel, then add 0.5g catalyst, 0.6 g ligand PMDETA, 100mL acetone, vacuumize the reaction system first, then fill it with nitrogen or argon, and react at 90°C for 12 hours; after the reaction, pass the reaction mixture through a neutral alumina column, and remove the solvent by rotary evaporation , the crude product was precipitated in ice n-hexane to remove unreacted monomers, and the precipitate was dried in a vacuum oven at 45°C for 24 hours to obtain stimuli-responsive emulsifier 3.

[0051] Preparation of stimuli-responsive waterborne polyurethane: the number average molecular ...

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Abstract

The invention discloses a preparation method of stimuli-responsive waterborne polyurethane emulsion with high water resistance, and relates to the technical field of preparation of polymer polyurethane emulsion. The preparation method includes the following steps that 1, a stimuli-responsive emulsifier is prepared, wherein a small-molecular initiator with disulfide bonds in the middle is synthesized, the synthesized disulfide-bond-containing initiator triggers preparation of a macromolecular initiator from hydrophobic monomers, the macromolecular initiator triggers preparation of the stimuli-responsive emulsifier from hydrophilic monomers; 2, the waterborne polyurethane emulsion with high water resistance is prepared, wherein the prepared stimuli-responsive emulsifier serves as an externalemulsifier for the preparation of the waterborne polyurethane emulsion, and then the stimuli-responsive waterborne polyurethane emulsion with high water resistance is obtained. According to the method, the reduction responsive emulsifier with the middle containing the disulfide bonds, and the stimuli-responsive emulsifier serves as the external emulsifier which can be used for the preparation ofthe stimuli-responsive waterborne polyurethane emulsion with high water resistance.

Description

technical field [0001] The invention belongs to the technical field of polymer polyurethane emulsion preparation, and in particular relates to a preparation method of a stimulus-responsive high water-resistant water-based polyurethane emulsion. Background technique [0002] Water-based polyurethane is a new type of polyurethane system that uses water instead of organic solvents as the dispersion medium. Its molecular structure contains carbamate groups, urea bonds and ionic bonds. It has high cohesive energy and strong adhesion. The ratio of the soft and hard segments adjusts the performance of polyurethane, which makes water-based polyurethane widely used in coatings, adhesives, leather finishing agents, fabric finishing agents, etc. Since water is used as the dispersion medium, water-based polyurethane emulsion has the following advantages over solvent-based polyurethane: (1) the system does not contain toxic -NCO groups, has low odor, is safe and environmentally friendly;...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F226/10C08G63/688C08G18/66C08G18/48C08G18/32C08J3/07C08L75/08C09D175/08
CPCC08F226/10C08F293/005C08F2438/01C08G18/4825C08G18/6674C08G63/6882C08J3/07C08J2375/08C09D175/08
Inventor 李怡霞储著强曹苏毅项羽陈军李军配
Owner 浙江材华科技有限公司
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