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Polycarbodiimide-containing polyurethane dispersion and preparation method thereof

A technology of polycarbodiimide and polyurethane dispersions, applied in polyurea/polyurethane coatings, coatings, etc., can solve problems such as poor hydrolysis resistance, and achieve the effects of preventing hydrolysis, excellent crosslinking ability, and excellent reactivity

Inactive Publication Date: 2019-05-14
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problem of poor hydrolysis resistance of polyester polyurethane dispersions, the invention provides a polycarbodiimide-containing polyurethane dispersion and a preparation method thereof

Method used

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  • Polycarbodiimide-containing polyurethane dispersion and preparation method thereof
  • Polycarbodiimide-containing polyurethane dispersion and preparation method thereof
  • Polycarbodiimide-containing polyurethane dispersion and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1 (preparation of polycarbodiimide)

[0033] In a 250ml four-necked flask equipped with a stirrer, a thermometer, an air duct (through nitrogen), and a vacuum adapter (connected to a vacuum pump), first purse with nitrogen and remove the air with a vacuum pump, and add 48.8g (0.2 mol) tetramethylxylylene diisocyanate (TMXDI) and 0.5g catalyst 1-methylphosphole-1-oxide (MPPO), heated to 180 ° C while stirring, and real-time monitoring in the reaction device Changes in isocyanate content, until the NCO content reached 8.2wt%, stop heating. At this moment, the vacuum pump was opened, and the remaining unreacted TMXDI and catalyst (MPPO) were evaporated under reduced pressure. According to the above synthesis method, isocyanate-terminated polycarbodiimide (PCDI) with a degree of polymerization of 4 was prepared.

Embodiment 2

[0034] Embodiment 2 (preparation not containing polycarbodiimide polyurethane dispersion)

[0035] Add 86.68g of polybutylene adipate diol 2000 (PBA2000) into a 500ml three-neck round bottom flask equipped with a condenser, a stirrer and a thermometer, and remove water under vacuum at 120°C and 0.01MPa for 1 hour. When the temperature was lowered to 60°C, 7.58g of hexamethylene diisocyanate (HDI) and 2.5g of isophorone diisocyanate (IPDI), 0.02g of dibutyltin dilaurate (DBTDL) were added as a catalyst, and the temperature was raised to 80°C for 1.5 h. Titrate the remaining amount of -NCO with the di-n-butylamine method until the -NCO content reaches 1.13 wt%. Cool down to 60°C, add 150g of acetone to dissolve. Add 2.2 g of sodium ethylenediaminoethanesulfonate (AAS-Na) and react at room temperature for 20 minutes. Then slowly add 100 g of deionized water at 800 r / min and stir for 20 min to obtain a milky white dispersion. After stirring for 30 min, 1.02 g of isophorone dia...

Embodiment 3

[0036] Embodiment 3 (preparation containing polycarbodiimide polyurethane dispersion)

[0037] Add 86.68g of polybutylene adipate diol 2000 (PBA2000) into a 500ml three-neck round bottom flask equipped with a condenser, a stirrer and a thermometer, and remove water under vacuum at 110°C and 0.01MPa for 2h. When the temperature was lowered to 60°C, 7.58g of hexamethylene diisocyanate (HDI) and 2.28g of isophorone diisocyanate (IPDI), 0.02g of dibutyltin dilaurate (DBTDL) were added as a catalyst, and 1.04g of polymerization degree was added at the same time. 4 TMXDI type polycarbodiimide (PCDI), and then heated up to 90°C, and reacted for 1.5h. Titrate the remaining amount of -NCO with the di-n-butylamine method until the -NCO content reaches 1.12wt%. Cool down to 50°C, add 150g of acetone to dissolve. Add 2.2 g of sodium ethylenediaminoethanesulfonate (AAS-Na) and react at room temperature for 20 minutes. Then slowly add 100 g of deionized water at 800 r / min and stir for 20...

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Abstract

The invention discloses a polycarbodiimide-containing polyurethane dispersion and a preparation method thereof. Polycarbodiimide is introduced at synthetic stage of polyurethane to prepare a hydrolysis-resistant polyester type polyurethane dispersion. The content of carbodiimidein the polyurethane dispersion is larger than or equal to 1mmol / 100g, and a carbodiimide group in emulsion and free carboxyl generated by hydrolysis can rapidly react at the indoor temperature to generate stable ureide, so that a glue film of the polyester type polyurethane emulsion has the advantages of excellent hydrolysis resistance, chemical resistance, mechanical performance and the like.

Description

technical field [0001] The invention belongs to the field of preparation and application of polyurethane, and in particular relates to a polyurethane dispersion containing polycarbodiimide and a preparation method thereof. Background technique [0002] Water-based polyurethane dispersion uses water as the dispersion medium, does not contain organic solvents, and does not emit VOC to pollute the environment. It is a green and environmentally friendly product that can be applied to adhesives, coatings, textile auxiliaries, medicine and hygiene, and construction. materials and printing. However, a single polyester-type water-based polyurethane dispersion often generates carboxyl groups due to the easy hydrolysis of ester groups, and the acidic carboxyl groups accelerate the further hydrolysis of other ester chains, which is an autocatalytic reaction. The hydrolysis of polyurethane shows that the main chain is broken, the molecular weight is reduced, the tensile strength and el...

Claims

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Application Information

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IPC IPC(8): C08G18/79C08G18/12C08G18/42C08G18/66C08G18/32C09D175/06
Inventor 孙东成田仪长
Owner SOUTH CHINA UNIV OF TECH
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