Water-dispersible HDI-TDI mixed tripolymer curing agent and preparation method thereof

A trimer and curing agent technology, applied in polyurea/polyurethane coatings, coatings, etc., can solve the problems of slow reaction between curing agent and water, poor water dispersibility, poor stability, and high market price, and achieve water dispersibility Good, not easy to yellow, high effective functionality

Inactive Publication Date: 2016-09-21
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aromatic and aliphatic polyisocyanate curing agents are widely used as polyurethane curing agents because of their excellent performance, but both have certain limitations
Due to the existence of the induction effect, the -NCO of aromatic isocyanate reacts with water faster, and when it is used as a water-based polyurethane curing agent after hydrophilic modification, its water dispersion and stability are poor. At the same time, due to the existence of benzene ring, the aromatic isocyanate Isocyanate is easy to oxidize to produce yellowing; the activity of -NCO of aliphatic polyisocyanate curing agent is low, and the curing agent after hydrophilic modification reacts slowly with water, which helps to prolong the pot life, but the coating film prepared by aliphatic isocyanate Hardness is not good, the market price is expensive, and the production cost is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027](1) Under the protection of nitrogen, first put 20g TDI-80, 180g HDI diisocyanate monomer, 30g PEG300 into a 500ml dry four-neck round bottom flask equipped with a thermometer and a stirring paddle, start stirring to stir the materials evenly, Then the temperature was raised to 60°C for heat preservation reaction, and the percentage of -NCO in the system was measured every hour.

[0028] (2) After reacting for 4 hours, add 0.85g β-hydroxypropyl quaternary ammonium base and DMP-30 (mass

[0029] The ratio is 4:1) catalyst, 60 ℃ to continue the heat preservation reaction, measure the percentage of -NCO in the system every hour, when the system reaches the target -NCO percentage of 34 w%, add 0.4g of benzoyl chloride, heat preservation reaction for 1h. Unreacted diisocyanate monomers were removed by thin film distillation.

[0030] (3) Add 7g of DMPA to the trimer obtained in step (2), continue to stir for 70°C heat preservation reaction, add 5.31g of N,N-dimethylethanolam...

Embodiment 2

[0033] (1) Under nitrogen protection, first put 30g TDI-80, 210g HDI diisocyanate monomer, and 23g PEG300 into a 500ml dry four-necked round bottom flask equipped with a thermometer and a stirring paddle, and start stirring to stir the materials evenly. Then the temperature was raised to 65°C for heat preservation reaction, and the percentage content of -NCO in the system was measured every hour.

[0034] (2) After reacting for 3 hours, add 0.98g β-hydroxypropyl quaternary ammonium base and Mannich base 2,2-bis(3,5-bis((dimethylamino)methyl-4-hydroxyphenyl ) propane (mass ratio: 5:1) catalyst, continue the heat preservation reaction at 65°C, measure the percentage of -NCO in the system every hour, and add 0.5g of benzoyl chloride when the system reaches the target -NCO percentage of 35 w%. ℃ heat preservation reaction for 1h. Unreacted diisocyanate monomer was removed by thin film distillation.

[0035] (3) Add 11g of DMPA to the trimer obtained in step (2), continue to stir ...

Embodiment 3

[0038] (1) Under the protection of nitrogen, first put 50g TDI-80, 150g HDI diisocyanate monomer, 25g PEG500 into a 500ml dry four-neck round bottom flask equipped with a thermometer and a stirring paddle, start stirring to stir the materials evenly, and then heat up The temperature was kept at 65°C, and the percentage of -NCO in the system was measured every hour.

[0039] (2) After reacting for 3 hours, add 0.90g of β-hydroxypropyl quaternary ammonium base and DMP-30 (mass ratio: 3:1) catalyst, continue the heat preservation reaction at 65°C, measure the percentage of -NCO in the system every hour, When the system reaches the target-NCO percentage content of 35w%, add 0.3g of benzoyl chloride, and keep the reaction at 65°C for 1h. Unreacted diisocyanate monomers were removed by thin film distillation.

[0040] (3) Add 9g of anionic hydrophilic modifier DMPA to the trimer obtained in step (2), continue to stir for 75°C heat preservation reaction, and add 6.65g of N-methylpyr...

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Abstract

The invention discloses a water-dispersible HDI-TDI mixed tripolymer curing agent and a preparation method thereof. The method comprises steps as follows: (1) diisocyanate monomers and a nonionic hydrophilic modifying agent are put into a round-bottom flask under the protection of nitrogen and heated to reach 50-70 DEG C for a thermal reaction; (2) after the mixture reacts for 2-4 h, a trimerization catalyst is added, the mixture is subjected to a thermal reaction continuously, a polymerization inhibitor is added after the percentage composition of -NCO of the system reaches the target, and the mixture is subjected to the thermal reaction for 0.5-1.5 h; (3) an anion hydrophilic modifying agent is added to a tripolymer obtained in the step (2), the mixture is continuously stirred and subjected to the thermal reaction at the temperature of 60-80 DEG C, a neutralizing agent is added after the mixture reacts for 5-7 h, and the mixture is stirred uniformly, subjected to the thermal reaction for 0.5-1.5 h and discharged after being cooled. The preparation method is simple, and the prepared curing agent has the advantages of good water dispersibility, good storage stability and good film water resistance and can be applied to a water-based bi-component polyurethane coating well.

Description

technical field [0001] The invention belongs to the field of curing agents, in particular to a water-dispersible HDI-TDI mixed trimer curing agent and a preparation method thereof. Background technique [0002] In recent years, the development of low-carbon economy, the improvement of environmental protection laws and regulations in various countries, and the enhancement of people's environmental protection awareness have promoted the coating industry to make great strides in the direction of "green". At the same time, with the strict restrictions on the content of volatile organic compounds (VOC) in coating systems by international regulations, solvent-based coatings have gradually faded out of the market, promoting the development of low-pollution, high-performance, environmentally friendly water-based coatings, two-component water-based polyurethane coatings Especially because it combines the advantages of high performance and low VOC content of two-component solvent-base...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/79C08G18/32C08G18/48C09D175/04
CPCC08G18/3206C08G18/4833C08G18/795C09D175/04
Inventor 黄洪梁林姣曹树坤刘小敏
Owner SOUTH CHINA UNIV OF TECH
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