Water-soluble blocked polyurethane curing agent and preparation method and application thereof

A polyurethane curing agent, closed-type technology, applied in polyurea/polyurethane adhesives, polyurea/polyurethane coatings, adhesives, etc., can solve the problems of high product molecular weight, decreased effective functional group ratio of curing agent, low solid content, etc.

Active Publication Date: 2019-11-08
FOSHAN JINGXIN HUIMING TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In some of these methods, due to the addition of hydrophilic groups, the effective functional group ratio of the curing agent is reduced, that is, the NCO% is low; in some cases, due to the modification of hydrophilic substances, the molecular weight of the product is larger and the solid content is lower, resulting in The existing water-based closed polyurethane curing agent still has a variety of quality problems to be improved, and it cannot meet the multi-variety requirements of water-based high-temperature baking varnish and water-based high-temperature glue.

Method used

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  • Water-soluble blocked polyurethane curing agent and preparation method and application thereof
  • Water-soluble blocked polyurethane curing agent and preparation method and application thereof
  • Water-soluble blocked polyurethane curing agent and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] Step 1: preparing a partial block of isocyanate;

[0066] In the prepolymerization kettle, add 100g IPDI and 50g acetone, add 35g methyl ethyl ketone oxime dropwise at room temperature, drop it in 1.5 hours, the temperature does not exceed 52 ° C, and obtain a partial closure of IPDI (component A).

[0067] Step 2: preparing partially blocked polyisocyanate prepolymers containing hydrophilic carboxyl groups;

[0068] Adopt process 1, the specific process is: in the reactor, add 250g acetone and 66.7g dimethylol butanoic acid, heat to 50 ℃ and dissolve completely, dropwise add 0.3g dibutyltin dilaurate catalyst (due to IPDI, HDI The reactivity of the trimer is low), and the component A is added dropwise, and the dropwise addition is completed in about 1 hour, during which the temperature is kept at 50±2°C. After the dropwise addition, keep it at 50°C for 1 hour, rise to below 60°C for 10 hours, then add 246.5g of HDI trimer (NCO% is 23.0%), add 0.3g of dibutyltin dilaur...

Embodiment 2

[0072] Step 1: preparing a partial block of isocyanate;

[0073] Add 100g of IPDI and 40g of acetone to prepolymerization kettle 1, raise the temperature to 50°C and add 35g of methyl ethyl ketone oxime dropwise for 1 hour, and the dropping temperature is 50-52°C to obtain component A.

[0074] In prepolymerization kettle two, add 328g HDI trimer (NCO% is 23.0%) and 50g acetone, add 51g methyl ethyl ketoxime dropwise at normal temperature, dropwise finish in 1 hour, dropwise temperature does not exceed 50 ℃, obtains component B.

[0075] Step 2: preparing partially blocked polyisocyanate prepolymers containing hydrophilic carboxyl groups;

[0076] Adopt process 1, the specific process is: in the reactor, add 250g acetone and 67g dimethylol propionic acid, heat to 50 ℃ and completely dissolve, dropwise add 0.3g stannous octoate catalyst, stir evenly, first add component A, The addition was completed in about 1 hour, during which the temperature was kept at 50±2°C, and reacted ...

Embodiment 3

[0080] Step 1: preparing a partial block of isocyanate;

[0081] In the reactor, add the prepolymer of 582gTDI and trimethylolpropane (solid content is 75%, NCO% is 13.0%), 100gMDI, 200g acetone, 80g propylene glycol methyl ether acetate, after mixing evenly, add under normal temperature 91 g of methyl ethyl ketoxime was added over 1.5 hours at a temperature not exceeding 50° C. to obtain a partially blocked isocyanate (component C).

[0082] Step 2: preparing partially blocked polyisocyanate prepolymers containing hydrophilic carboxyl groups;

[0083] Adopt process 2, the specific process is: raise the temperature in the reactor to 50°C, add 67g of dimethylolpropionic acid in 5 times, add it within 1 hour, keep it at 50±2°C for 1 hour after the addition, and then Raise the temperature to 60±2°C and react for 6 hours.

[0084] Step 3: preparing a water-soluble closed polyurethane curing agent;

[0085] Lower the temperature of the material in the reactor to 50°C, slowly add...

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Abstract

The invention discloses a water-soluble blocked polyurethane curing agent and a preparation method and application thereof. The preparation method comprises the following steps: partially blocking isocyanate, then reacting the partially blocked isocyanate with dihydroxymethylcarboxylic acid to form a product A, and then enclosing all the remaining -NCO in the product A to obtain the water-solubleblocked polyurethane curing agent. The blocked polyurethane curing agent of the invention is mainly composed of a trifunctional isocyanate prepolymer, and has the advantages of small molecular weight,high solid content, high NCO%, good water solubility and dissolvability in water at any ratio; and the curing agent is very convenient to use, is mainly used in combination with water-based resin forpreparation of water-based stoving varnish and water-based high-temperature adhesives, and has good application prospects in the coating of heat-sensitive materials.

Description

technical field [0001] The invention relates to a polyurethane curing agent, in particular to a water-soluble closed polyurethane curing agent and its preparation method and application. Background technique [0002] With the continuous improvement of environmental protection regulations and law enforcement methods, high-pollution chemical companies are changing jobs, and the raw materials used are constantly changing from solvent-based to solvent-free and water-based. In recent years, the application range of water-based coatings and water-based adhesives has continued to expand, and the application of room-temperature curing materials has been popularized rapidly, but the application of high-temperature curing materials has not been smooth, mainly due to the water-based coatings and water-based high-temperature adhesives. There are few types of closed polyurethane curing agents, and the unblocking temperature is high and the scope of application is narrow. Tracing it to i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/34C08G18/10C08G18/28C09D175/04C09D175/14C09J175/04
CPCC08G18/10C08G18/286C09D175/04C09D175/14C09J175/04C08G18/348
Inventor 周建明刘晓鸿周国豪何绍群陆佩仪
Owner FOSHAN JINGXIN HUIMING TECH CO LTD
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