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Method for preparing high-solid-content sulfonic-acid waterborne polyurethane adhesive

A technology of water-based polyurethane with high solid content, applied in polyurea/polyurethane adhesives, adhesives, adhesive types, etc., can solve problems such as difficult process, difficult dispersion and chain extension of prepolymer, increased viscosity, etc., to achieve Low cost, saving time and energy, low viscosity effect

Active Publication Date: 2013-08-14
武汉工大科技园发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the prepolymer synthesized only with hexamethylene diisocyanate is more difficult to disperse and extend the chain, and its viscosity will increase rapidly until it produces a gel. Even if a large amount of solvent is added to disperse, it will become a paste after the solvent is removed. state, which affects its craft and is difficult to commercialize

Method used

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  • Method for preparing high-solid-content sulfonic-acid waterborne polyurethane adhesive
  • Method for preparing high-solid-content sulfonic-acid waterborne polyurethane adhesive

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] one A kind of preparation method of the sulfonic acid type waterborne polyurethane of high solid content, it comprises the steps:

[0033] (1) Synthesis of hydroxyl-terminated sulfonate polyester:

[0034] Under the protection of nitrogen, according to the design formula, 31.586g hexanediol (HDO), 10.534g dimethyl isophthalate-5-sodium sulfonate (SIPM), 0.18g antioxidant triphenyl phosphite, 0.120g Catalyst monobutyltin oxide (Faskat 4100) was put into a four-necked flask equipped with a stirrer, thermometer, water separator, and condenser, and was slowly heated to 140°C with an electric heating mantle, kept for 0.5h, and then pressed at 15°C / h Raise the temperature to 200°C at a speed of 10°C / h. After the system is transparent, the temperature drops to 140°C; then add 30.262g of adipic acid (AD), and raise the temperature to 200°C at a speed of 10°C / h. Reduce to 2.5mgKOH / g resin, the quality of distilled water is 7.6g, cool down to 50°C and discharge, and obtain the ...

Embodiment 2

[0050] one A kind of preparation method of the sulfonic acid type waterborne polyurethane of high solid content, it comprises the steps:

[0051] (1) Synthesis of hydroxyl-terminated sulfonate polyester:

[0052] Under the protection of nitrogen, 36.6g of neopentyl glycol (NPG), 6.38g of SIPM, 0.24g of antioxidant triphenyl phosphite, and 0.160g of catalyst monobutyltin oxide (Faskat 4100) were put into the In the four-necked flask with stirrer, thermometer, water separator, and condenser, heat slowly to 140°C with an electric heating mantle, keep it warm for 0.5h, then raise the temperature to 200°C at a rate of 15°C / h, and cool down to 140°C when the system is transparent , add 37.513g glutaric acid, heat up to 200°C at a rate of 10°C / h, take a sample to measure the acid value after the heat preservation is over, the acid value drops to 3.4mgKOH / g (resin), the quality of distilled water is 10.2g, cool down to Discharge at 50°C to obtain hydroxyl-terminated polyester with s...

Embodiment 3

[0066] one A kind of preparation method of the sulfonic acid type waterborne polyurethane of high solid content, it comprises the steps:

[0067] (1) Synthesis of hydroxyl-terminated sulfonate polyester:

[0068] Under the protection of nitrogen, 20.229g of butanediol (BDO), 11.10g of SIPM, 0.144g of antioxidant triphenyl phosphite, and 0.100g of catalyst monobutyltin oxide (Faskat 4100) were put into a stirring In a four-neck flask with a thermometer, a thermometer, a water separator, and a condenser, heat slowly to 140°C with an electric heating mantle, keep it warm for 0.5h, then raise the temperature to 200°C at a rate of 15°C / h, and drop to 140°C after the system is transparent , then add 16.435g of maleic anhydride (MA), heat up to 200°C at a rate of 10°C / h, take a sample to measure the acid value after the heat preservation is over, the acid value is 4.2mgKOH / g (resin), the quality of distilled water is 6.0g, Cool down to 50°C and discharge to obtain hydroxyl-terminat...

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Abstract

The invention relates to a method for preparing high-solid-content waterborne polyurethane. The method comprises the following steps of: (1) reacting sulfonate-containing sodium dimethyl isophthalate-5-sulfonate with excessive polylol for a while, and then, adding polyacid to react so as to synthesize hydroxyl-terminated polyester; and (2) using the synthesized waterborne polyester as a soft segment, using diisocyanate as a hard segment, adding water to disperse, and carrying out chain extension by using polyamine so as to obtain the high-solid-content waterborne polyurethane. According to the method, the dispersion is easy, a large amount of solvent is not required for being used, the cost is saved, the solvent removal is easy, and the solid content reaches over 50% while lower viscosity is kept, so that the constructability of adhesive liquid is improved, and the adhesive liquid is crystallizable and has better initial viscosity and better adhesive strength; and the used polyester is synthesized autonomously, the raw materials are all common, and the process is simple, so that the cost is saved, and the industrialization is facilitated.

Description

technical field [0001] The invention relates to a preparation method of a sulfonic acid type waterborne polyurethane adhesive with high solid content, belonging to the field of chemical industry. Background technique [0002] Water-based polyurethane has gradually replaced solvent-based polyurethane in many fields due to its non-toxic, non-flammable, environmental protection and energy-saving advantages, and is widely used in leather finishing agents, fabrics, coatings, adhesives and other fields. Among them, water-based polyurethane adhesive is one of its most important applications. [0003] According to the different hydrophilic chain extenders, waterborne polyurethane is mainly divided into two types: carboxylic acid type and sulfonic acid type. Usually, carboxylic acid-type water-based polyurethane is chain-extended by adding small molecules of dimethylol propionic acid or dimethylol butyric acid, and then dispersed with water. Generally, the solid content (that is, th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09J175/06C08G18/75C08G18/73C08G18/66C08G18/46C08G18/32C08G63/688C08G63/78
Inventor 闫福安刘艳平
Owner 武汉工大科技园发展有限公司
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