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Preparation method of toluene diisocyanate trimer curing agent

A technology of trimerization of toluene diisocyanate and isocyanate, applied in organic chemistry, polyurea/polyurethane coatings, coatings, etc., can solve the problems of low NCO content of curing agent, high viscosity, and difficulty in achieving high solid content, and achieve molecular weight Uniform distribution, reduced viscosity, rapid curing and anti-yellowing effects

Active Publication Date: 2013-02-06
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current production situation in our country is to use this method to produce curing agent in order to meet the requirements of environmental protection. The curing agent produced has low NCO content, high viscosity, and the storage time is less than half a year. The content of free isocyanate is always higher than 1.0%, and it is difficult to achieve high solid content, can not solve the fundamental problem

Method used

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  • Preparation method of toluene diisocyanate trimer curing agent
  • Preparation method of toluene diisocyanate trimer curing agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Take 18.8g of bisphenol A and 54.4g of dimethylamine solution, heat and stir at 50°C for 2h, add dropwise 46.5g of formaldehyde solution, raise the temperature to 80°C after dropping, keep the reaction for 2h, then stop heating. The reaction solution was layered, and the yellow organic phase was taken and distilled under reduced pressure at 130°C and -0.095MPa until no white solid was produced. The product was a yellow viscous liquid, which was dissolved in butyl acetate solvent to prepare a catalyst solution. figure 1 It is the infrared spectrogram of alkylaminomethylphenol catalysts, in which the broad peak phenol-OH stretching vibration at 3300~3100cm-1, aromatic hydrocarbon skeleton vibration at 1608cm-1, and phenol C-O stretching vibration at 1361cm-1 and 1256cm-1 prove There is a phenol structure in the product, and 885cm-1 and 841cm-1 are 1,2,4-trisubstituted and 1,2,3,5-tetrasubstituted benzene rings, indicating that one or two Substituents; while 1476cm-1 is th...

Embodiment 2

[0044] Take 18.8g of bisphenol A and 54.4g of dimethylamine solution, heat and stir at 50°C for 2h, add dropwise 46.5g of formaldehyde solution, raise the temperature to 80°C after dropping, keep the reaction for 2h, then stop heating. The reaction solution was layered, and the yellow organic phase was taken and distilled under reduced pressure at 130°C and -0.095MPa until no white solid was produced. The product was a yellow viscous liquid, which was dissolved in butyl acetate solvent to prepare a catalyst solution.

[0045] Pass N 2 Under protection, 100 g of TDI80 and 80 g of butyl acetate were put into the reaction vessel, and stirred at a constant temperature of 50° C. for 10 min. 11 g of a 5% homemade isocyanate trimerization catalyst butyl acetate solution containing alkylaminomethylphenols was added dropwise, and after the dropwise addition was completed, the mixture was stirred and reacted at 50° C. for 6 hours. The free NCO content was detected every 1 hour. When th...

Embodiment 3

[0047] Take 18.8g of bisphenol A and 54.4g of dimethylamine solution, heat and stir at 50°C for 2h, add dropwise 46.5g of formaldehyde solution, raise the temperature to 80°C after dropping, keep the reaction for 2h, then stop heating. The reaction solution was layered, and the yellow organic phase was taken and distilled under reduced pressure at 130°C and -0.095MPa until no white solid was produced. The product was a yellow viscous liquid, which was dissolved in butyl acetate solvent to prepare a catalyst solution.

[0048] Pass N 2 Under protection, 100 g of TDI80 and 80 g of butyl acetate were put into the reaction vessel, and stirred at a constant temperature of 40° C. for 10 min. 11 g of a 5% homemade isocyanate trimerization catalyst butyl acetate solution containing alkylaminomethylphenols was added dropwise, and after the dropwise addition was completed, the mixture was incubated and stirred at 40° C. for 8 hours. The free NCO content was detected every 1 hour. When ...

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Abstract

The invention discloses a preparation method of a polyurethane trimer curing agent. The method comprises the steps of adding toluene diisocyanate and a polar solvent into a reaction vessel under the protection of introduced N2, dripping a catalyst solution containing alkyl amine methyl phenol for trimerization of isocyanate, and performing heat preservation and stirring for reaction for 2-12 hours; detecting the weight percentage of free NCO group, adding isocyanate trimerization inhibitor and performing heat preservation, then stirring for reaction for 0.5-1 hour when the NCO content is 9.5-8.5%; dripping a polar solvent solution of monobasic alcohol, and continuously performing heat preservation, then stirring for reaction for 1-2 hours; stopping the reaction when the weight percentage of NCO reduces to be 8.0-7.0%, and cooling to room temperature, and discharging to obtain a transparent and near water-white product. The preparation method has the beneficial effects that the curing agent is well matched with the resin, is rapidly cured at room temperature, and has the advantages of high compatibility, low viscosity, high mechanical strength and the like.

Description

technical field [0001] The invention relates to a toluene diisocyanate trimer curing agent, in particular to a method for preparing a trimer polyurethane curing agent based on toluene diisocyanate whose free monomer content is lower than 0.7% and whose xylene tolerance is higher than 4 . Background technique [0002] The preparation of isocyanurate group-containing polyurethane curing agents from aliphatic and aromatic diisocyanates has been known for a long time and is described in numerous publications and patents. Toluene diisocyanate (TDI) can be polymerized to form isocyanurate six-membered ring structure (also known as trimer) under catalysis. Since the six-membered ring of isocyanurate has high functionality, high thermal decomposition temperature, and is a rigid ring, it can be quickly cross-linked to form a film when combined with a hydroxyl component, and the film has a high cross-linking density. High hardness, good adhesion, and excellent thermal stability. Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/79C07D251/32C09D175/04
Inventor 张心亚麦志远黄洪陈卓陈焕钦
Owner SOUTH CHINA UNIV OF TECH
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