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Preparation method of nonionic waterborne epoxy curing agent

A water-based epoxy and non-ionic technology, used in epoxy resin coatings, coatings, etc., can solve the problems of incomplete separation of amine and solvent, complex process, high energy consumption, easy removal, and preparation methods. Simple, low energy consumption

Active Publication Date: 2012-12-12
CHINA PETROCHEMICAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] CN 101007863 discloses a kind of preparation method of non-ionic water-based epoxy curing agent, but its preparation process is in chain extension reaction, and amine is a large amount of excess, and A large amount of solvent is added during the reaction, and excess amine and solvent need to be removed after the reaction is completed. On the one hand, the boiling point of amine is high, and high temperature and high energy consumption are required to remove excess amine. On the other hand, during the removal process In the process, the amine and the solvent cannot be completely separated; in the further chain extension reaction, a large amount of solvent is added, and after the reaction is completed, the solvent must be removed by distillation under reduced pressure
The whole process is more complicated and consumes more energy

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Put 200g of polyethylene glycol 2000 and 69g of CYD-128 into a 500ml four-necked reaction flask equipped with a reflux condenser, a thermometer, and a stirrer, heat and melt, and distill under reduced pressure at a temperature of 100°C and a vacuum of -0.095MPa for 1 After 1 hour, the temperature was maintained, and a mixed solution of 0.65 g of boron trifluoride ether and 7 g of ethylene glycol ether was added under normal pressure, and the addition was completed dropwise in 70 minutes, and the reaction was maintained for 3 hours to obtain a light-colored solid substance. Take 19g of this substance and 35g of CYD-128 and dissolve it in 2g of ethylene glycol ether at a temperature of 70°C to make a mixed solution, and keep the temperature for later use.

[0028] Put 31g of triethylenetetramine into a 500ml four-necked reaction flask equipped with a reflux condenser, a thermometer, and a stirrer, and add 13g of butyl glycidyl ether dropwise to the reaction flask at room t...

Embodiment 2

[0031] Put 200g of polyethylene glycol 2000 and 69g of CYD-128 into a 500ml four-necked reaction flask equipped with a reflux condenser, a thermometer, and a stirrer, heat and melt, and distill under reduced pressure at a temperature of 100°C and a vacuum of -0.095MPa for 1 After 1 hour, the temperature was maintained, and a mixed solution of 0.65 g of boron trifluoride ether and 7 g of ethylene glycol ether was added under normal pressure, and the addition was completed dropwise in 70 minutes, and the reaction was maintained for 3 hours to obtain a light-colored solid substance. Take 35g of this substance and 40g of E-44 and dissolve it in 3g of propylene glycol methyl ether at a temperature of 60°C to make a mixed solution, and keep the temperature for later use.

[0032] Put 22g of m-phenylenediamine into a 500ml four-necked reaction flask equipped with a reflux condenser, a thermometer and an agitator, and add 16g of phenyl glycidyl ether dropwise to the reaction flask at r...

Embodiment 3

[0035] Put 200g of polyethylene glycol 4000 and 26g of E-44 into a 500ml four-necked reaction flask equipped with a reflux condenser, a thermometer, and a stirrer, heat and melt, and distill under reduced pressure at a temperature of 100°C and a vacuum of -0.095MPa for 1 After 1 hour, the temperature was maintained, and a mixed solution of 0.45 g of boron trifluoride diethyl ether and 8.5 g of ethylene glycol butyl ether was gradually added under normal pressure. The addition was completed dropwise in 50 minutes, and the reaction was maintained for 3 hours to obtain a light-colored solid intermediate substance. Dissolve 40g of this substance and 32g of CYD-1283g in a mixed solution of ethylene glycol butyl ether at a temperature of 65°C, and keep the temperature for use.

[0036]Put 15g of 1,3-propylenediamine into a 500ml four-necked reaction flask equipped with a reflux condenser, a thermometer and a stirrer, and drop 20g of CYDPG660 into the reaction flask at room temperatur...

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Abstract

The invention provides a preparation method of a nonionic waterborne epoxy curing agent, which comprises the following steps: (1) heating and dissolving epoxy resin and polyether polyol, evenly mixing, dropwisely adding catalyst at 50-130 DEG C to carry out polymerization reaction, and after the reaction finishes, dissolving the product in the epoxy resin and solvent to prepare a mixed solution; (2) while stirring, dropwisely adding a monoepoxy compound into basic amine, and reacting at 10-100 DEG C; (3) dropwisely adding the mixed solution in the step (1) into the reaction product in the step (2) at 30-120 DEG C, and enabling the reaction at 10-90 DEG C; and after the reaction finishes, diluting by adding water until the solid content reaches 30-80%, thereby obtaining the nonionic waterborne epoxy curing agent. The method has the advantages of simple technique and mild reaction conditions; the adopted cosolvent has the advantages of low toxicity or no toxicity, and low VOC (volatile organic compound) content; and the substance cured by the product has the advantages of favorable compatibility with epoxy resin and high toughness of the paint film.

Description

technical field [0001] The invention relates to a preparation method of a nonionic water-based epoxy curing agent. Background technique [0002] In recent years, waterborne epoxy coatings have developed rapidly. It is a kind of environment-friendly polymer material, which has many advantages such as low organic solvent content, low odor, chemical resistance, insulation, etc., and has a wide range of uses and application prospects. Curing agent is one of the key factors affecting the performance of two-component epoxy coatings, and is a key component that determines the product process technology and characteristics. Ordinary aliphatic amine room temperature curing agents are more irritating to the human body, and are easy to react with carbon dioxide in the air to form salts or absorb moisture and become white. Therefore, most of the water-based epoxy curing agents that are cured at room temperature in practice use their modified products, including amidated polyamines, pol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G81/00C08G65/48C08G59/14C08G59/50C09D163/00C09D163/02C09D7/12
Inventor 唐光斌任天斌李婧婧任六波
Owner CHINA PETROCHEMICAL CORP
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