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Low free MDI monomer bicomponent solvent-free

A two-component polyurethane, solvent-free technology, applied in the field of polyurethane adhesives, can solve the problems of high viscosity, slow curing speed of the adhesive, poor leveling and other problems, and achieve the effect of fast curing speed, superior performance and lower production costs.

Inactive Publication Date: 2013-01-30
GOOD CHEM SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the mass percentage of NCO in this patent is only 0.5~8%. The lower NCO content will lead to the disadvantages of slow curing speed, excessive viscosity and poor leveling of the adhesive during use.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0023] A method for preparing a solvent-free two-component polyurethane adhesive with low free MDI monomers, including the preparation of A component-terminated OH polyol and the preparation of B-component-terminated NCO polyurethane prepolymer, characterized in that: the A component is composed of binary Alcohol and long carbon chain aliphatic dibasic acid and / or aromatic dibasic acid are obtained by esterification reaction, component B is made of MDI monomer, vegetable oil modified polyol and / or polyester polyol according to NCO / OH=3~5.5 : 1 (molar ratio) reaction is obtained, the preparation of B component comprises the following steps:

[0024] 1) Dehydrate the vegetable oil-modified polyol and polyester polyol until the water content (mass percentage) of the polyol system is less than 0.05%, add MDI monomer and molecular weight regulator, and heat up to 70-80 °C to react to the hydroxyl group in the system completely;

[0025] 2) Add the trimerization catalyst to continu...

Embodiment 1

[0042] Preparation of Component A:

[0043] 1) Add 106.1g of diethylene glycol, 177.05g of neopentyl glycol, 153.2g of 1,4-butanediol (containing 4.4 moles of OH in total) into the reaction kettle, and heat it to 80-100°C to make the binary alcohol is completely dissolved;

[0044] 2) Add 43.2g dimerized fatty acid, 263.0g adipic acid, 232.5g terephthalic acid (containing 3.1 moles of COOH in total), pass through the nitrogen protection weakly, heat up to 130~160℃ for esterification reaction, when the water output of the system reaches After 60-80% of the theoretical effluent value of the esterification reaction, the temperature is raised to 200-220 °C to continue the reaction;

[0045] 3) When the acid value drops below 15mgKOH / g, stop flowing nitrogen, evacuate until the vacuum degree is 0.266kPa, carry out esterification under reduced pressure until the acid value is less than 1.0mgKOH / g, cool down and discharge to obtain A component.

[0046]The viscosity of the obtained...

Embodiment 2

[0053] Preparation of Component A:

[0054] 1) Take 69.12g dimerized fatty acid, 319.6g azelaic acid, 124.59g isophthalic acid, (containing 2.8 moles of COOH in total) 99.75g diethylene glycol, 186.95g neopentyl glycol, 151.40g 1,4-butanedi The alcohol (containing 4.5 moles of OH in total) was added to the reaction kettle, and it was weakly protected by nitrogen, and the temperature was raised to 130-160 °C to carry out the esterification reaction. Continue the reaction at ~220°C;

[0055] 2) When the acid value drops below 15mgKOH / g, stop flowing nitrogen, evacuate to a vacuum of 0.266kPa, carry out esterification under reduced pressure until the acid value is less than 1.0mgKOH / g, cool down and discharge to obtain A component.

[0056] The viscosity at 25°C of the obtained A component was 1050 mPa·s, and the hydroxyl value was 164 mgKOH / g.

[0057] Preparation of component B:

[0058] 1) Take 120 g of polycaprolactone diol with a molecular weight of 1000 and 60 g of epoxi...

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Abstract

A method of producing a solvent-free two-component polyurethane adhesive having low content of free diphenylmethane diisocyanate (MDI) monomer is provided. The method includes esterifying dihydric alcohol and diacid to obtain component A, reacting MDI monomer with polyol to obtain component B according to the mole ratio of NCO / OH=3~5.5:1. The production of component B includes dehydrating polyol until the water content (mass percent) is less than 0.05%, adding the MDI monomer and a molecular weight regulator, heating to the temperature of 70~80? until the hydroxyl groups in the reaction system are completely reacted; adding a trimerization-catalyst to proceed a trimerization reaction until the reaction is completed, then the reaction is finished and the component B is obtained. The method has simple process, low production cost. The polyurethane adhesive obtained has low content of free MDI monomer, fast curing speed, high solvent resistance and hydrolysis resistance. There is no solvent contained in the component A and component B of the solvent-free adhesive, which is environmental-friendly and energy-saving, and the adhesive has good storage stability and is favorable for transporting and applying.

Description

technical field [0001] The invention relates to a polyurethane adhesive, in particular to a two-component solvent-free polyurethane adhesive with low free MDI monomers. Background technique [0002] With the improvement of the country's environmental protection requirements, the discharge of solvents should be gradually limited, and the use of solvent-based adhesives should be gradually reduced. [0003] Solvent-free composite technology fully meets the requirements of high efficiency, environmental protection and energy saving. It has the technical advantages of simple process flow, small equipment footprint, low raw material consumption, low energy consumption, low maintenance cost, high production speed, and no solvent residue in composite products. , will not cause damage to the safety of the product. The risk of fire in the production process is greatly reduced and safer. The two-component solvent-free adhesive is applied without solvent, which is not limited by the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09J175/06
CPCC08G18/7664C08G18/42C08G18/092C09J175/06
Inventor 李建明许玉良王小妹李树泉
Owner GOOD CHEM SCI & TECH