Synthetic method of waterborne polyurethane emulsion

A water-based polyurethane and synthesis method technology, applied in the field of synthesis of water-based polyurethane emulsion, can solve the problems of water-based polyurethane film water absorption, poor storage stability, high viscosity of intermediates, etc., achieve stable dispersion and improve wetting Sexuality and low cost effect

Active Publication Date: 2016-03-02
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In summary, although the water absorption of water-based polyurethane film is reduced to a certain extent and the water resistance is improved to a certain extent by using different cross-linking agents, the compatibility between epoxy resin and polyurethane is poor due to the poor compatibility of acrylate and polyurethane. If the amount of silane crosslinking agent added is too high, the crosslinking will be too high, the viscosity of the intermediate will be too high, and it will be difficult to disperse; even if the dispersion can be achieved, the particle size of the aqueous polyurethane dispersion will increase, and even stratification will occur make its storage stability worse

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Preparation of 1MCO (MCO1)

[0045] Put 100g of castor oil and 9.9g of glycerol into a three-necked flask, add 0.011g of tetra-n-butyl titanate as a catalyst, and stir to raise the temperature to 190°C under the protection of N2 purge, and keep it for 4h. Cool down to room temperature after the reaction. The hydroxyl value of the product is 312.9, the molecular weight is 511, and the functionality is 2.85.

[0046] Preparation of 2WPU1 (WPU1)

[0047] (1) Add 50g of dehydrated polycarbonate diol (molecular weight is 2000), 3.35gDMPA, 22.2gIPDI and 3.36gHDI into a reactor equipped with a stirrer, a thermometer and a condenser, heat to 85°C under stirring and Heat preservation reaction for 1 hour, add 20 g of acetone and 0.03 g of catalyst dibutyltin silicate (T-12), continue the reaction for 1 h, then add 7.67 g of MCO1 and another 20 g of acetone, and then react at 80 ° C for 2 hours, use Di-n-butylamine back titration analysis NCO% content reaches the theoretical va...

Embodiment 2

[0050] Preparation of 1MCO (MCO2)

[0051] Add 100g castor oil and 19.8g glycerol into a 250mL three-necked flask and add 0.012g of sodium methylate (NaOCH 3 ) as a catalyst, stirred and reacted at 180°C for 4h. Sampling analysis showed that its hydroxyl value was 438.2, its molecular weight was 371, and its functionality was 2.9.

[0052] Preparation of 2WPU2

[0053] (1) 50g of dehydrated polycarbonate diol (molecular weight is 2000), 3.35gDMPA, 26.2gH 12 Add MDI and 3.36g HDI into a reactor equipped with a stirrer, a thermometer and a condenser, heat to 85°C under stirring and keep it warm for 1 hour, add 20g of acetone and 0.03g of T-12, and continue the reaction for 1h, then Add 5.56gMCO2 and another 20g of acetone, then react at 60°C for 2 hours, use di-n-butylamine back titration method to analyze the NCO% content to reach the theoretical value, then cool down to 60°C, add 2.5g triethylamine to neutralize for 20 minutes, At the same time, the temperature was lowered ...

Embodiment 3

[0056] Preparation of 1MCO (MCO3)

[0057] Add 200g of castor oil and 9.9g of glycerol into a 250mL three-necked flask and add 0.021g of lead oxide (PbO) as a catalyst, and stir and react at 180°C for 4h. Sampling analysis shows that its hydroxyl value is 241.4 and its molecular weight is 650. Functional The degree is 2.8.

[0058] Preparation of 2WPU3

[0059] (1) Add 50g of dehydrated polycarbonate diol (molecular weight is 2000), 3.35gDMPA, 20.0gMDI and 6.73gHDI into a reactor equipped with a stirrer, thermometer and condenser, heat to 85°C under stirring and Heat preservation reaction for 1 hour, add 20gDMF and 0.03gT-12, continue to react for 1h, then add 9.73gMCO3 and another 20g of acetone, and then react at 60°C for 2 hours, analyze the NCO% content by di-n-butylamine back titration method to reach After the theoretical value, the temperature was lowered to 60°C, and 2.5g of triethylamine was added for neutralization for 20 minutes, while the temperature was lowered ...

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Abstract

Provided is a synthetic method of a waterborne polyurethane emulsion. The synthetic method includes the steps that dehydrated polyhydric alcohol, a diol chain extender containing ion radicals and diisocyanate are added into a reactor for a heat preservation reaction, then a solvent-1 and a catalyst are added for continuing the reaction, then castor oil or modified castor oil and a solvent-2 are added, a neutralizing agent is added for neutralization after the reaction, and an intermediate is obtained; an aqueous solution of a diamine chain extender containing sulfonic groups is added into the intermediate and quickly stirred, then deionized water is slowly added with quick stirring, an aqueous solution of a micromolecular diamine chain extender is added after uniform dispersion and evenly stirred, then a heat preservation reaction is performed, vacuum solvent removal is performed, and the milky waterborne polyurethane dispersion liquid is obtained. The waterborne polyurethane emulsion has the advantages of being high in solid content, good in dispersion stability and good in water resistance and heat resistance.

Description

technical field [0001] The invention provides a method for synthesizing an aqueous polyurethane emulsion. Background technique [0002] Waterborne polyurethane has been widely used in coatings, adhesives, inks and other fields due to its low volatile organic compound (VOC) content and excellent performance. Most of the existing waterborne polyurethanes are linear polyurethane aqueous dispersions, and their coating films have defects such as poor water resistance and poor solvent resistance. There are three ways to improve the water resistance and solvent resistance of water-based polyurethane coatings: one is to reduce the hydrophilic group content of water-based polyurethane as much as possible while stably dispersing; The third is to increase the cross-linking density of water-based polyurethane. There are internal cross-linking and external cross-linking methods to increase the cross-linking density. External linking is to add crosslinking agent and other auxiliary age...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/67C08G18/66C08G18/44C08G18/48C08G18/42C08G18/32C08G18/12
CPCC08G18/0823C08G18/0828C08G18/12C08G18/36C08G18/4238C08G18/4277C08G18/44C08G18/485C08G18/6659C08G18/6662C08G18/6692C08G18/6696C08G18/3857C08G18/3228
Inventor 赵雨花王军威亢茂青殷宁李其峰冯月兰
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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