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Fast epoxy resin curing agent and preparation method thereof

A fast curing, epoxy resin technology, used in the field of curing agents, can solve the problems of affecting the scope of use and performance, poor media resistance, etc., and achieve the effects of low irritation, low odor and low toxicity

Inactive Publication Date: 2009-12-02
ZHANGJIAGANG KABANG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The inventor’s previous patent PCT / CN2004 / 000034 used polyphosphoric acid to react with hydroxyl-containing compounds to prepare acid phosphate ester, which can be quickly cured with epoxy resin at room temperature, but still has the defect of poor medium resistance, which affects the scope of use and performance

Method used

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  • Fast epoxy resin curing agent and preparation method thereof
  • Fast epoxy resin curing agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 740 grams of molecular weight to 400, hydroxyl content is 5mmol / g, linear polyoxypropylene diol (polyether 204) with two functionalities in 2 reactors equipped with stirring, thermometer and dropping device, add dropwise while stirring 177.5 grams of polyphosphoric acid, and protect it with argon gas, control the reaction temperature at about 80 ° C, after the dropwise addition, adjust the temperature at 60 ° C and keep it warm for 2 hours with argon gas, then add 3 grams of water, and continue the heat preservation reaction for 2 hours . Cool down at 30°C, add 50 grams of Zn(CH 3 COO) 2 , and stirred for 2 hours to obtain a light yellow viscous transparent liquid.

[0035] After mixing with epoxy resin 828 at a mass ratio of 40:100, 50 g of the mixture was cured at 25° C. for 15 minutes. The cured product is immersed in water at 25°C, and after 30 days, the weight increases by 1%, and the surface is smooth, which is defined as excellent water resistance.

Embodiment 2

[0039] Add 177.5 grams of polyphosphoric acid to a 1-liter reactor equipped with a stirring, thermometer and dropping device, add 76 grams of propylene glycol dropwise while stirring, and protect it with argon, and control the reaction temperature below 80 ° C. , heat up to 80°C and keep warm for 3 hours to react with argon gas. Then add 5 grams of water, continue to keep warm for 2 hours, cool to 60°C, add 7 grams of calcium naphthenate, continue to stir for 2 hours, cool down to obtain light Brown transparent liquid.

[0040] After mixing with epoxy resin 828 at a mass ratio of 24:100, 50 g of the mixture was cured at 25° C. for 2 minutes. The cured product is immersed in 5% NaOH aqueous solution at 25°C, and after 7 days, the weight increases by 1.5%, and the surface is smooth, which is defined as excellent alkali water resistance.

[0041] Comparative example:

[0042]The same as the above preparation process, except that calcium naphthenate is not added after esterifica...

Embodiment 3

[0044] In order to verify the curing performance of the curing agent and epoxy resin, the curing agent obtained in Example 1 was mixed with epoxy resin 828 at a mass ratio of 40:100, used for bonding stainless steel / stainless steel, and placed at 25°C for 24 hours After that, the average tensile and shear strengths were 25MPa.

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Abstract

The invention discloses a fast epoxy resin curing agent and a preparation method thereof. The preparation method comprises the following steps: (1) hydroxyl compound and phosphoric acid esterifying reagent polyphosphoric acid react under the protection of an inert gas, the hydroxyl transformation rate is controlled to be higher than 95 percent, and then water accounting for 1-5 percent of the weight of the phosphoric acid esterifying reagent is added for hydrolysis, therefore, the content of phosphate mono-ester is caused to be over 60 percent, the content of phosphate di-ester is caused to be no higher than 30 percent, and the content of free phosphoric acid is caused to be no higher than 10 percent; and (2) a metal ion compound is added for reaction and then the product can be obtained. The curing agent obtained according to the preparation method, has the excellent properties of light color, high gloss, difficult oxidization, no yellowing, good weather resistance, and the like after being subjected to curing reaction with epoxy resin. Meanwhile, the curing agent of such type has the advantages of low toxicity, low volatility, low odor and low acrimony, and the color is light and conforms to the requirement of present environmental-friendly development.

Description

Technical field: [0001] The invention relates to a curing agent, in particular to an ion complex phosphate curing agent for epoxy resin. Background technique [0002] Epoxy resin is a very important chemical raw material. Usually, after adding a certain proportion of curing agent and mixing it evenly, it is cured at room temperature or under heating. After curing, it has good mechanical strength, corrosion resistance, and electrical insulation. Widely used in coatings, adhesives, plastics, composite materials and other fields. There are many substances that can cure epoxy resin, and many occasions need to be cured and bonded at room temperature, which requires the use of room temperature curing agents with high activity, low molecular amines such as diethyltriamine, triethyl Tetramine can effectively cure epoxy resin at room temperature, and is a common room temperature curing agent. However, low-molecular amine curing agents have disadvantages such as high odor and toxici...

Claims

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Application Information

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IPC IPC(8): C08G59/40C08K5/523
Inventor 朱麟勇李欣欣朱麟润
Owner ZHANGJIAGANG KABANG NEW MATERIALS
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