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Partially blocked polyurethane curing agent and preparation method thereof

A polyurethane curing agent and a closed-type technology, which are applied in the field of partially closed-type polyurethane curing agents and their preparation, can solve the problems of high monomer isocyanate content, low solid content of the curing agent system, and increased overall cost of the curing agent, and achieve environmental protection. Good, low energy consumption, low toxicity effect

Active Publication Date: 2011-04-06
WANHUA CHEM BEIJING +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Chinese patent CN1357559A discloses a coating curing agent 4,2'- and 4,4'-diphenylmethane diisocyanate prepolymer and its preparation method, but because of its low solid content in the curing agent system and the free The high content of monomeric isocyanate increases the comprehensive cost of curing agent, and it is easy to cause technical defects of fast curing in the early stage of construction and slow late stage

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] a. In a reaction kettle equipped with a condensing reflux device, pass N 2 For protection, add 465g of MDI-100, 175g of ethyl acetate solvent and 0.07g of stabilizer benzoyl chloride, stir evenly, add 40g of trimethylolpropane and 20g of glycerin, slowly raise the temperature to 70~80℃ and react for 2.5~3 hour, the obtained measured NCO content is an isocyanate prepolymer of 13.0%;

[0044] b. Cool down to 45°C, and slowly add 39g of melted ε-caprolactam and 13g of ethyl acetate dropwise into the flask under uniform stirring, keep the temperature of the reaction system at 50-60°C during the dropping process, and wait to be closed After all the reagents were added, the temperature was raised to 80° C. for 1 hour.

[0045] c. Cool to 50° C. and discharge to obtain 752 g of partially blocked polyurethane curing agent with a solid content of 75%. It has been detected that the NCO content of the partially blocked curing agent is 10.1%, the blocked-NCO content is 2.0%, and ...

Embodiment 2

[0048] a. In a reaction kettle equipped with a condensing reflux device, pass N 2 For protection, add 458.12g of MDI-50, 175g of ethylene glycol ethyl ether acetate solvent and 0.07g of stabilizer phosphoric acid, stir evenly, add 66.88g of trimethylolpropane, slowly raise the temperature to 70-80°C and react for 2.5-3 hours, An isocyanate prepolymer with a measured NCO content of 13.0% was obtained;

[0049] b. Cool down to 45°C and slowly drop the mixed solution of 19.96g of methyl ethyl ketone oxime and 6.65g of n-butyl acetate into the flask under uniform stirring. Hour.

[0050] c. Cool to 50° C. and discharge to obtain 726.61 g of partially blocked polyurethane curing agent with a solid content of 75%. It has been detected that the NCO content of the curing agent is 11.2%, the blocked-NCO content is 1.3%, and the viscosity at 25° C. is 1700 mPa.s.

[0051] Get some closed type curing agent that example 1 makes, carry out curing rate measurement by polyurethane adhesiv...

Embodiment 3

[0053] a. In a reaction kettle equipped with a condensing reflux device, pass N 2 For protection, add 458.04g MDI-50, 175g n-propyl acetate and 0.07g stabilizer benzoyl chloride, stir evenly, add 66.96g 1,2,6-hexanetriol, slowly heat up to 70-80°C and react for 2.5-3 hours , the obtained NCO content is 13.0% isocyanate prepolymer;

[0054] b. Cool down to 45°C, and slowly drop the mixed solution of 42.76g of phenol and 14.25g of ethyl acetate into the flask under uniform stirring.

[0055] c. Cool to 50° C. and discharge to obtain 757 g of partially blocked polyurethane curing agent with a solid content of 75%. It has been detected that the NCO content of the curing agent is 9.5%, the blocked-NCO content is 2.5%, and the viscosity at 25° C. is 2200 mPa.s.

[0056] Get some closed type curing agent that example 1 makes, carry out curing rate measurement by polyurethane adhesive pot life test method, still keep clarification, transparent and flowable state after 24 hours, magn...

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Abstract

The invention discloses a partially blocked polyurethane curing agent and a preparation method thereof. The preparation method mainly comprises the following steps that end-NCO isocyanate prepolymer is obtained from the addition reaction of diphenylmethane diisocyanate and low-molecular polyol in ester solvent, and then the end-NCO isocyanate prepolymer reacts with isocyanate sealant to form the curing agent. The partially blocked polyurethane curing agent has the following characteristics that: a) according to the calculation of NCO by weight, the blocked-NCO content is between 1.0 and 5.0 percent; b) the solid content by weight of the curing agent is 75+ / -2 percent, and the percentage content of the NCO by weight is between 12.0 and 13.0 percent (according to the calculation of the effective percentage of the NCO, the percentage content of the NCO including blocked NCO radicals); and c) the viscosity of the curing agent at 25 DEG C is between 1,500 and 2,500 mPa. s. The invention has the advantages of low toxicity, good storage stability, adjustable curing speed and the like.

Description

technical field [0001] The invention relates to a polyurethane adhesive curing agent and a preparation method thereof, in particular to a partially closed polyurethane curing agent and a preparation method thereof. Background technique [0002] Polyurethane curing agent is a synthetic material widely used in coatings, plastics, rubber, leather, fibers, adhesives and other fields. The production method of polyurethane curing agent at home and abroad usually adopts the reaction of toluene diisocyanate (TDI) and trimethylolpropane to generate TDI / TMP adduct. During the production process of this adduct, some free TDI units that do not participate in the reaction will remain. Free TDI is volatile, highly toxic in the gas phase, and the content of free toluene diisocyanate is too high. During the production and construction of the product, this volatile free monomer is very irritating to the human respiratory system, skin and eyes. , TDI vapor will damage human liver and kidney ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/76C08G18/32C08G18/10
Inventor 陈建君郭虹张平叶桂香
Owner WANHUA CHEM BEIJING
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