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Preparation method of mixed cresol modified meta-xylylene diamine epoxy resin curing agent

A technology of m-xylylenediamine epoxy resin and m-xylylenediamine, which is applied in the chemical field, can solve the problems of low product viscosity, slow curing speed, long pot life, etc., and achieves fast curing speed, smooth surface, high The effect of resistance to salt spray

Inactive Publication Date: 2012-07-04
上海美东生物材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] m-xylylenediamine (hereinafter referred to as MXDA) is a widely used and large amount of epoxy resin amine curing agent. MXDA has low toxicity, low volatility, and can be cured at room temperature. The cured product has good gloss, high hardness, and chemical resistance. Good quality, but MXDA has a high freezing point, crystallization occurs in winter, and it is easy to react with carbon dioxide in the air to form the corresponding carbonate. The salt is insoluble in the epoxy resin base material, which will cause the surface whitening of the cured product. During storage and use It is difficult to construct under low temperature and humidity. In order to overcome the shortcomings of MXDA and expand its application field, a large number of modified MXDA curing agents have appeared. Among the many modification methods, Mannich type modification is the most popular. Attention, the Mannich-type modified MXDA curing agent includes: use nonylphenol or cresol instead of phenol, the product is non-toxic, insoluble in water, has good low-temperature rapid curing performance and plasticity, and can be used in urban drinking water projects and underwater projects and other fields, but its curing speed is slow and the pot life is long; if butyraldehyde is used instead of formaldehyde, the product has low viscosity and good transparency; if p-hydroxybenzaldehyde is used instead of formaldehyde, the curing speed is fast, etc., but it is not suitable for underwater engineering, and, This kind of modified curing agent has surface whitening phenomenon when it is applied in underwater construction

Method used

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  • Preparation method of mixed cresol modified meta-xylylene diamine epoxy resin curing agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] On a 1000mL reaction bottle, equipped with a stirrer, thermometer, feeding port and ventilation tube, 2 Add 95.2g of m-xylylenediamine, 201g of cardanol, and 36.3g of hydroquinone in sequence, and then mix and stir them at 90°C for 30min to 60min until transparent and clear. After adding 7.3g of catalyst NaOH, gradually add Add 30g of paraformaldehyde for 1.5h~2h, then keep the temperature at 90℃ for 3h and then drop to 70℃~80℃ for vacuum dehydration. Keep the polymerization reaction at 140°C for 8 hours; finally cool to 80°C, filter the catalyst NaOH, dilute 20% with toluene and isopropanol (molar ratio 1:1), and discharge.

[0026] Product quality: viscosity 2350mpa.s amine value 174.0mgKOH / g organic volatile matter 16.69% solid content 81.92 gel time 33min (100:135).

Embodiment 2

[0028] On a 1000mL reaction bottle, equipped with a stirrer, thermometer, feeding port and ventilation tube, 2 95.2g of m-xylylenediamine, 201g of cardanol, and 36.3g of hydroquinone were sequentially added into the reaction kettle, and then mixed and stirred at 90°C for 30min to 60min until transparent and clear, and 7.3g of Ba(OH) catalyst was added. 2 Finally, gradually add 30g of paraformaldehyde, 1.5h ~ 2h to complete, then keep at 90°C for 3h, then the temperature drops to 70°C ~ 80°C for vacuum dehydration, vacuum gauge reading 0.08Mpa ~ 0.09Mpa, 1.5h ~ 2h, dehydration After completion, the temperature was raised to 135° C., and the polymerization reaction was maintained for 15 hours; finally cooled to 80° C., diluted 20% with toluene and isopropanol (molar ratio 1:1), and discharged.

[0029] Product quality: viscosity 2400mpa.s; amine value 178.33mgKOH / g; organic volatile content 17.92%; solid content 80.58%; gel time 26min (100:135).

Embodiment 3

[0031] On a 1000mL reaction bottle, equipped with a stirrer, thermometer, feeding port and ventilation tube, 2 95.2g of m-xylylenediamine, 201g of cardanol, and 36.3g of hydroquinone were successively added into the reaction kettle, and then mixed and stirred at 90°C for 30min to 60min until transparent and clear. After adding 7.3g of catalyst triethylamine, Gradually add 30g of paraformaldehyde for 1.5h~2h, then keep the temperature at 90°C for 3h, then reduce the temperature to 70°C~80°C for vacuum dehydration. , the temperature was raised to 135° C., and the polymerization reaction was kept for 20 hours; finally cooled to 80° C., diluted 20% with toluene and isopropanol (molar ratio 1:1), and discharged.

[0032] Product quality: viscosity 2500mpa.s; amine value 177.53mgKOH / g; organic volatile content 15.10%; solid content 82.90%; gel time 34min (100:135).

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Abstract

The invention provides a preparation method of a mixed cresol modified meta-xylylene diamine epoxy resin curing agent. The method comprises the following steps of: adding meta-xylylene diamine into an N2-charged reaction kettle; raising the temperature to 80-95 DEG C; adding hydroquinone; fully mixing; adding cardanol; keeping the temperature at 85-95 DEG C till a solution is clear and transparent; adding a catalyst; gradually adding polyformaldehyde in batches simultaneously; lowering the temperature to 70-80 DEG C; vacuumizing and dehydrating; after dehydrating, raising the temperature to 130-150 DEG C; undergoing a polymerization reaction; cooling to 70-85 DEG C; filtering the catalyst; diluting to 15-25 percent by using an organic solvent; and discharging to obtain the mixed cresol modified meta-xylylene diamine epoxy resin curing agent. A product prepared with the method has the advantages of stable performance, high curing speed, low toxicity, high transparency, unremarkable whitening phenomenon, nontoxicity and freeness of irritation, can be applied to underwater construction, and is a superior sea heavy-duty coating.

Description

Technical field: [0001] The invention relates to the field of chemistry, in particular to a curing agent, in particular to a phenalkamine epoxy resin curing agent, in particular to a preparation method of a mixed phenol modified m-xylylenediamine epoxy resin curing agent. Background technique: [0002] m-xylylenediamine (hereinafter referred to as MXDA) is a widely used and large amount of epoxy resin amine curing agent. MXDA has low toxicity, low volatility, and can be cured at room temperature. The cured product has good gloss, high hardness, and chemical resistance. Good quality, but MXDA has a high freezing point, crystallization occurs in winter, and it is easy to react with carbon dioxide in the air to form the corresponding carbonate. The salt is insoluble in the epoxy resin base material, which will cause the surface whitening of the cured product. During storage and use It is difficult to construct under low temperature and humidity. In order to overcome the shortco...

Claims

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Application Information

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IPC IPC(8): C08G14/073C08G59/62C09D163/00C09D5/08
Inventor 黎明
Owner 上海美东生物材料股份有限公司
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