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Phosphorus-containing polyamine self-emulsifying epoxy resin curing agent, and preparation method and use thereof

A technology of epoxy resin curing and polyamine epoxy resin, which is applied in the field of phosphorus-containing polyamine self-emulsifying epoxy resin curing agent and its preparation field, and can solve the problems of high cost, increased reaction, and reduced resin crosslinking density and rigidity. , to achieve the effect of low cost, simple process, good and lasting flame retardant effect

Inactive Publication Date: 2015-04-29
HUIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the introduction of DOPO reduces the number of epoxy groups, thus reducing the crosslinking density and rigidity of the resin. Furthermore, the use of DOPO to modify commercial epoxy resins increases the reaction due to the steric hindrance effect of the ring structure, resulting in an increase in cost. Relatively high

Method used

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  • Phosphorus-containing polyamine self-emulsifying epoxy resin curing agent, and preparation method and use thereof
  • Phosphorus-containing polyamine self-emulsifying epoxy resin curing agent, and preparation method and use thereof

Examples

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Embodiment 1

[0030] An embodiment of the phosphorus-containing polyamine self-emulsifying epoxy resin curing agent of the present invention, the phosphorus-containing polyamine self-emulsifying epoxy resin curing agent described in this embodiment is prepared by the following method:

[0031] (1) Preparation of phosphorus-containing polyamine epoxy resin curing agent: Add 0.05 mol triethylenetetramine, 0.1 mol Benzaldehyde and 0.1 mol DOPO, add 150 ml of absolute ethanol as a solvent, 0.6 g of triethylamine as a catalyst, stir, heat up to 80°C and reflux for 12 h, cool to room temperature, pour the reaction solution into deionized water, and a large amount of Precipitate, filter with suction, wash with water three times, recrystallize the crude product with ethanol:water mixture, and dry in vacuum at 60°C for 12 hours to obtain a phosphorus-containing polyamine epoxy resin curing agent;

[0032](2) Preparation of non-ionic water-based epoxy self-emulsifier: Add octadecylamine and solvent p...

Embodiment 2

[0035] An embodiment of the phosphorus-containing polyamine self-emulsifying epoxy resin curing agent of the present invention, the phosphorus-containing polyamine self-emulsifying epoxy resin curing agent described in this embodiment is prepared by the following method:

[0036] (1) Preparation of phosphorus-containing polyamine epoxy resin curing agent: Add 0.05 mol ethylenediamine, 0.1 mol benzene Methanone and 0.1 mol DOPO, add 150 ml of absolute ethanol as a solvent, 0.6 g of triethylamine as a catalyst, stir, heat up to 80°C and reflux for 12 h, cool to room temperature, pour the reaction solution into deionized water, and a large amount of Precipitate, filter with suction, wash with water three times, recrystallize the crude product with ethanol:water mixture, and dry in vacuum at 60°C for 12 hours to obtain a phosphorus-containing polyamine epoxy resin curing agent;

[0037] (2) Preparation of non-ionic water-based epoxy self-emulsifier: Add octadecylamine and solvent ...

Embodiment 3

[0040] An embodiment of the phosphorus-containing polyamine self-emulsifying epoxy resin curing agent of the present invention, the phosphorus-containing polyamine self-emulsifying epoxy resin curing agent described in this embodiment is prepared by the following method:

[0041] (1) Preparation of phosphorus-containing polyamine epoxy resin curing agent: Add 0.05 mol tetraethylenepentamine, 0.1 mol p-tolualdehyde and 0.1 mol DOPO, add 150 ml of absolute ethanol as solvent, 0.6 g of triethylamine as catalyst, stir, heat up to 80°C and reflux for 12 h, cool to room temperature, pour the reaction solution into deionized water, and there is A large amount of precipitation was precipitated, suction filtered, washed three times with water, recrystallized the crude product with ethanol:water mixture, and dried in vacuum at 60°C for 12 hours to obtain a phosphorus-containing polyamine epoxy resin curing agent;

[0042] (2) Preparation of non-ionic water-based epoxy self-emulsifier: I...

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Abstract

The invention discloses a method for preparing a phosphorus-containing polyamine self-emulsifying epoxy resin curing agent. The method comprises the following steps: firstly adding polyamine, aromatic aldehyde or aromatic ketone and DOPO to a four-necked flask, taking absolute ethyl alcohol as a solvent, taking triethylamine as a catalyst, stirring, heating up and performing a reflux reaction, cooling to room temperature, pouring a reaction liquid to deionized water, precipitating out, carrying out suction filtration, washing with water, re-crystallizing a crude product, and drying to obtain a phosphorus-containing polyamine epoxy resin curing agent; then preparing a non-ionic waterborne epoxy self-emulsifying agent; and finally, preparing the phosphorus-containing polyamine self-emulsifying epoxy resin curing agent with DOPO as a side group by using the phosphorus-containing polyamine epoxy resin curing agent and the non-ionic waterborne epoxy self-emulsifying agent. The phosphorus-containing polyamine self-emulsifying epoxy resin curing agent with DOPO as the side group, prepared by the method provided by the invention, has flame retardant, heat resistant and self-emulsifying functions to meet the preparation needs of a fire-retardant and heat-resistant waterborne epoxy paint base material.

Description

technical field [0001] The invention relates to a phosphorus-containing polyamine epoxy resin curing agent and its preparation method and application, in particular to a phosphorus-containing polyamine self-emulsifying epoxy resin curing agent whose side group is DOPO, and its preparation method and application. Background technique [0002] Epoxy resins are widely used in coatings, civil engineering, electronics, etc. due to their excellent electrical, mechanical properties and chemical corrosion resistance. However, the limiting oxygen index (LOI) of most epoxy resin materials is lower than 22%. , are easy to burn in the air, which makes them a great safety hazard during use and limits their application range. Therefore, the preparation of epoxy resins with excellent thermal properties and high flame retardancy has become a research focus. [0003] There are two ways to improve the flame retardant performance of epoxy resin: externally added flame retardant and reactive fl...

Claims

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Application Information

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IPC IPC(8): C08G59/50C09D163/00C09D7/12C09D5/18
Inventor 肖定书刘国聪刘鸿梁浩彭忠利周芳礼
Owner HUIZHOU UNIV
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