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Solvent-free waterborne polyisocyanate curing agent and preparation method and application thereof

A polyisocyanate, solvent-free technology, applied in the directions of adhesive additives, polymer adhesive additives, non-polymer adhesive additives, etc., can solve problems such as technical difficulties and difficult manufacturing processes, and achieve good hydrophilicity. , excellent water dispersibility and storage stability, good water resistance and high strength

Active Publication Date: 2018-10-16
FOSHAN JINGXIN HUIMING TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] CN105949436A discloses a water-dispersible HDI-TDI mixed trimer curing agent. The trimer is first prepared, and after removing unreacted monomers, directly add dimethylolpropionic acid (DMPA) in solid state The solvent-free HDI-TDI trimer is reacted to produce a solvent-free curing agent. The manufacturing process is relatively difficult, because DMPA cannot be dissolved in the trimer, and the solid material will adhere to the wall of the reactor after being stirred.
In a word, the technical difficulty of preparing the solvent-free polyisocyanate curing agent process method disclosed in the existing literature is still relatively large, and the realization of industrial production still needs further research, and the increasingly competitive demand of the market forces those skilled in the art to study Solvent-based polyisocyanate curing agent for more technical development

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0030] The preparation method of this solvent-free water-based polyisocyanate curing agent is to dissolve the dicarboxylate sulfonate in an organic solvent, react with a polyisocyanate prepolymer to generate a polyisocyanate prepolymer containing a sulfonic acid group, and then distill out Organic solvents to obtain a solvent-free water-based polyisocyanate curing agent.

[0031] Preferably, in the preparation method, the molar ratio of dicarboxysulfonate to polyisocyanate prepolymer is (0.03-0.2):1; the amount of organic solvent added is 3-10 times the mass of dicarboxysulfonate.

[0032] Preferably, in the preparation method, the organic solvent is N-methylpyrrolidone (NMP).

[0033] Preferably, in the preparation method, the dicarboxysulfonate is an alkali metal dicarboxysulfonate; further preferably, in the preparation method, the dicarboxysulfonate is sodium dicarboxysulfonate; still more preferably, in the preparation method , Dicarboxysulfonate is sodium phthalic acid-...

Embodiment 1

[0062] The preparation method of the solvent-free aqueous polyisocyanate curing agent of embodiment 1 is as follows:

[0063] a) Add 24g of isophthalic acid-5-sodium sulfonate and 230g of N-methylpyrrolidone into the reaction vessel, heat up to 60°C and stir to dissolve for 1 hour, then add 200g of HDI trimer (solvent-free, NCO%=23%) , mix and stir well.

[0064] b) Add 0.8g of antioxidant 1010, close the reactor, feed nitrogen, react at 50-80°C for 8 hours, and when the NCO percentage of the reactant decreases by nearly 9%, stop the reaction, and then add 200g of HDI for trimerization body, stir to mix evenly.

[0065] c) Fill the kettle with nitrogen heated to 80°C from the bottom of the reactor to bubble the liquid in the kettle, the evaporated NMP and the charged nitrogen enter the condenser under vacuum, and the fractionated NMP enters the storage tank for recovery Standby; after 3 hours, no liquid drops flow out from the outlet of the condenser, and when the residual N...

Embodiment 2

[0068] The preparation method of the solvent-free aqueous polyisocyanate curing agent of embodiment 2 is as follows:

[0069] a) Add 32g of isophthalic acid-5-sodium sulfonate and 250g of N-methylpyrrolidone into the reaction vessel, heat up to 60°C and stir to dissolve for 1 hour, then add 200g of HDI biuret (solvent-free, NCO%=22%) , mix and stir well.

[0070] b) Add 0.8g of antioxidant 1010, close the reactor, feed nitrogen, react at 50-80°C for 9 hours, and stop the reaction when the NCO percentage of the reactant decreases by nearly 8%, and then add 200g of HDI to dilute Urea, stir to mix well.

[0071] c) Fill the kettle with nitrogen heated to 80°C from the bottom of the reactor to bubble the liquid in the kettle, the evaporated NMP and the charged nitrogen enter the condenser under vacuum, and the fractionated NMP enters the storage tank for recovery Standby; after 3 hours, no liquid drops flow out from the outlet of the condenser, and when the residual NMP content ...

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Abstract

The invention discloses a solvent-free waterborne polyisocyanate curing agent and a preparation method and application thereof. The solvent-free waterborne polyisocyanate curing agent is polyisocyanate prepolymer containing sulfonic acid groups. The preparation method includes: dissolving dicarboxyl sulfonate into an organic solvent, allowing the solution to have reaction with polyisocyanate prepolymer, and distilling to remove the organic solvent to obtain the solvent-free waterborne polyisocyanate curing agent. The solvent-free waterborne polyisocyanate curing agent is truly free of VOC discharge, excellent in water dispersity and storage stability, high in NCO content, low in viscosity, capable of being coordinated with various resin containing hydroxyl, carboxyl or amino to prepare double-component polyurethane coating and double-component polyurethane adhesive, and capable of allowing a product to be good in water resistance and high in strength.

Description

technical field [0001] The invention relates to a solvent-free water-based polyisocyanate curing agent and its preparation method and application. Background technique [0002] With the enhancement of people's awareness of environmental protection and the strengthening of the implementation of national environmental protection laws and regulations, the water-based research of two-component polyurethane coatings and polyurethane adhesives is in full swing. Most of the isocyanate-based water-based curing agents also contain certain solvents, and there is still the problem of volatile organic solvent toxicity. [0003] CN105949436A discloses a water-dispersible HDI-TDI mixed trimer curing agent. The trimer is first prepared, and after removing unreacted monomers, directly add dimethylolpropionic acid (DMPA) in solid state The solvent-free HDI-TDI trimer is reacted to produce a solvent-free curing agent. The manufacturing process is relatively difficult, because DMPA cannot be ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/38C08G18/73C08G18/75C08G18/79C09D7/48C09D7/65C09D167/08C09J11/06C09J11/08C09J133/00C09J175/04
CPCC08G18/0828C08G18/3855C08G18/73C08G18/755C08G18/792C09D7/48C09D7/65C09D167/08C09J11/06C09J11/08C09J133/00C09J175/04
Inventor 刘晓鸿周建明何绍群
Owner FOSHAN JINGXIN HUIMING TECH CO LTD
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