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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 poor media resistance, affecting the scope of use and performance, and achieve low odor, low irritation, and good weather resistance.

Inactive Publication Date: 2011-11-23
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 linear polyoxypropylene glycol (polyether 204) with a molecular weight of 400 and a hydroxyl content of 5 mmol / g to two reactors equipped with stirring, thermometer and dripping devices, and add them dropwise while stirring 177.5 grams of polyphosphoric acid, protected by argon, control the reaction temperature to around 80°C, after the addition, adjust the temperature at 60°C and keep it warm for 2 hours with argon, then add 3 grams of water and continue the reaction for 2 hours. . Cool down at 30℃, add 50g Zn(CH 3 COO) 2 , The reaction was 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 grams of the mixture was cured at 25°C for 15 minutes. The cured product is immersed in water at 25°C, and the weight gain is 1% after 30 days, and the surface is smooth, which is defined as excellent water resistance.

Embodiment 2

[0039] Add 177.5 grams of polyphosphoric acid into a 1-liter reactor equipped with stirring, thermometer and dripping device, add 76 grams of propylene glycol dropwise while stirring, and pass argon protection to control the reaction temperature to be lower than 80°C. After the addition is complete , Warm up to 80°C and keep warm and argon for reaction for 3 hours. Then add 5 grams of water, continue to keep the temperature for 2 hours, cool to 60°C, add 7 grams of calcium naphthenate, continue to stir and react for 2 hours, and cool down to obtain light Brown transparent liquid.

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

[0041] Comparative example:

[0042] The same preparation process as ...

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, and then used for bonding of stainless steel / stainless steel, and placed at 25°C for 24 hours After that, the average tensile shear strength was 25MPa.

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PUM

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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 type phosphate curing agent for epoxy resin. Background technique [0002] Epoxy resin is a very important chemical raw material. It is usually cured under normal temperature or heating conditions after adding a certain proportion of curing agent, and it has good mechanical strength, corrosion resistance and electrical insulation after curing. It is widely used in coatings, adhesives, plastics, composite materials and other fields. There are many materials that can cure the epoxy resin. In many cases, it is necessary to cure and bond at room temperature. This requires the use of a more active room temperature curing agent, low molecular amines such as diethyltriamine and triethyl Tetraamines can effectively cure epoxy resins at room temperature, and are common room temperature curing agents. However, low-molecular-weight amine curing agents have shortcomings such as high odor and tox...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/40C08K5/523
Inventor 朱麟勇李欣欣朱麟润
Owner ZHANGJIAGANG KABANG NEW MATERIALS