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Novel DOPO-type epoxy resin curing agent and preparation method of same

A new type of compound technology, applied in the field of epoxy resin curing agent, can solve the problems of easy fire and restriction, and achieve the effect of not easy to seep out, small performance and excellent flame retardancy

Active Publication Date: 2017-12-22
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the limiting oxygen index (LOI) of epoxy resin is only 19.8%, which is easy to cause fire and is restricted in many special fields.

Method used

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  • Novel DOPO-type epoxy resin curing agent and preparation method of same
  • Novel DOPO-type epoxy resin curing agent and preparation method of same
  • Novel DOPO-type epoxy resin curing agent and preparation method of same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) in N 2 Under the atmosphere, put a thermometer, condensing reflux, magnetic stirring and N 2 Add DOPO (0.01mol), p-nitrobenzaldehyde (0.01mol) and ethanol (10 mL) into a 250 mL three-neck flask that was passed through, start heating and stirring to dissolve completely, then raise the temperature to 60°C, and 2 Reaction under protective atmosphere for 8h.

[0027] (2) After the reaction is finished, cool to room temperature, filter with suction to obtain a crude product, rinse with deionized water, repeat 3 times, and finally dry in a vacuum oven at 80° C. for 24 hours to obtain an intermediate product.

[0028] (3) Mix the intermediate product (0.01mol) obtained in step (2), iron powder (0.035mol) and hydrochloric acid solution (containing 0.065mol of hydrogen chloride), and stir at room temperature to react quickly, and then add it to the dilute NaOH solution And, extracted and purified with ethyl acetate to obtain the final product.

[0029] figure 1 For the n...

Embodiment 2

[0033] in N 2 Under the atmosphere, put a thermometer, condensing reflux, magnetic stirring and N 2 Add DOPO (0.01mol), p-nitrobenzaldehyde (0.015mol) and ethanol (10mL) in the 250mL three-neck flask that passes through, start to heat and stir to make it dissolve completely, then be warming up to 60 ℃, under N 2 Under the atmosphere of reaction 8h, subsequent steps are the same as steps (2) and (3) in embodiment 1.

Embodiment 3

[0035] in N 2 Under the atmosphere, put a thermometer, condensing reflux, magnetic stirring and N 2 Add DOPO (0.01mol), p-nitrobenzaldehyde (0.015mol) and ethanol 10mL into the 250mL three-necked flask that has been passed through, start heating and stirring to make it dissolve completely, then raise the temperature to 75°C, and 2 Under the atmosphere of reaction 8h, subsequent steps are the same as steps (2) and (3) in embodiment 1.

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Abstract

The invention relates to a novel compound, 10-((4-aminophenyl)(hydroxyl)methyl)-9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, as well as a preparation method of same. The compound is prepared by performing a reaction to raw materials, including DOPO and p-nitrobenzaldehyde, in ethanol or a DMF solvent to obtain an intermediate product, and then reducing the intermediate product with iron powder, and finally neutralizing and purifying the product to obtain the compound. The compound can be used as a curing agent and a flame retardant for epoxy resin. The preparation method employs easy-to-obtained raw materials and has simple processes, so that the compound is convenient to promote and apply.

Description

technical field [0001] The present invention relates to the technical field of epoxy resin curing agent, in particular to a novel epoxy resin curing agent 10-((4-aminophenyl)(hydroxyl)methyl)-9,10-dihydro-9-oxa- 10-phosphaphenanthrene-10-oxide and its preparation method. Background technique [0002] Epoxy resin has excellent mechanical properties, chemical corrosion resistance, electrical insulation, processing performance, and adhesive performance. At the same time, due to the low volatility of epoxy resin during curing, no small molecules are formed, so that its shrinkage is low. It is used in coatings, Adhesives, printed circuit boards, electronic packaging materials, composite materials, aerospace and automotive and other fields are widely used. However, the limiting oxygen index (LOI) of epoxy resin is only 19.8%, which is easy to cause fire and is restricted in many special fields. [0003] Flame retardants can be divided into halogen-containing flame retardants and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/64C08L63/00C07F9/6574
CPCC07F9/657172C08G59/64C08L63/00C08L2201/02C08L2201/22C08L2203/206
Inventor 彭永利张满倪思瑶万春杰熊丽君
Owner WUHAN INSTITUTE OF TECHNOLOGY
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