Synthetic method of waterborne polyurethane adhesive

A technology of water-based polyurethane and synthesis method, which is applied in the direction of polyurea/polyurethane adhesive, adhesive, adhesive type, etc., can solve the problems of poor heat resistance and water resistance of WPU, achieve high initial bonding strength, increase solid content, Good stability and dispersion

Active Publication Date: 2016-03-16
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above various researches, each has its own focus, but the synthesized WPU is mainly linear structure, which makes the heat resistance and water resistance of WPU poor.
However, the introduction of castor oil or modified castor oil into the WPU adhesive structure for shoe materials has not been reported yet.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Preparation of MCO (MCO1)

[0051] 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, in N 2 Under the protection of purging, the temperature was raised to 190°C with stirring and kept 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.

[0052] 1 Preparation of WPU1 (WPU1)

[0053] (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 the...

Embodiment 2

[0059] Preparation of MCO (MCO2)

[0060] 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.

[0061] 1 Preparation of WPU2

[0062] (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

[0069] Preparation of MCO (MCO3)

[0070] 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.

[0071] 1 Preparation of WPU3

[0072] (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

A synthetic method of waterborne polyurethane adhesive is as below: reacting dehydrated polyol, an ionic group-containing diol chain extender and diisocyanate in a reactor, then adding a solvent 1 and a catalyst, continuing the reaction, then adding castor oil or modified castor oil and a solvent 2, reacting, adding a neutralizing agent for neutralization to obtain the intermediate, adding a sulfonic acid group-containing diamine chain extender to the intermediate, stirring, then adding deionized water, uniformly dispersing, then adding an aqueous solution of small molecule diamine chain extender, reacting, removing the solvent under vacuum to obtain a milky white waterborne polyurethane dispersion liquid, and preparing glue by using the milky white aqueous polyurethane dispersion liquid, a thickener, a curing agent and a substrate wetting agent to obtain the waterborne polyurethane adhesive. The waterborne polyurethane adhesive provided by the present invention has the advantages of high solid content, good dispersion stability, high initial bonding strength and good resistance to damp-heat aging.

Description

technical field [0001] The invention belongs to a method for synthesizing a water-based polyurethane adhesive. Background technique [0002] Waterborne polyurethane (WPU) entered the market in the late 1960s. In recent years, with the increasingly stringent environmental regulations and the enhancement of people's awareness of environmental protection, the voice of environmental protection is getting higher and higher, and the research and development of water-based polyurethane has attracted more and more attention. So far, thousands of patent documents and research reports have been published. There are many water-based polyurethane products in wood, construction, fabric, synthetic leather, latex coating, PVC and other materials bonding, glass fiber bundles, flexible packaging, printing materials. It has been widely used in bonding and so on. [0003] Water-based polyurethane uses water instead of organic solvents as the dispersion medium. It is an environmentally friend...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09J175/04C09J175/06C09J175/08C08G18/08C08G18/12C08G18/32C08G18/36C08G18/66
CPCC08G18/0823C08G18/12C08G18/3268C08G18/36C08G18/6662C08G18/6696C08G2170/80C09J175/04C09J175/06C09J175/08C08G18/3228C08G18/3246
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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