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Self-inflaming-retarding epoxy resin curing agent containing phosphorus-nitrogen and preparation method thereof

An epoxy resin curing and solvent technology, which is applied in the field of phosphorus and nitrogen-containing self-flame retardant epoxy resin curing agent and its preparation, can solve the problems of complex operation, poor processability, easy decomposition and loss, etc., and achieve high reactivity, relative Good capacitance and easy commercial production

Inactive Publication Date: 2015-06-10
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the use of these flame retardants generally requires a long time of mixing or pre-reaction before adding the curing agent, which makes the operation complicated. In addition, the additive flame retardants also have the disadvantages of easy decomposition and loss, and poor processability.

Method used

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  • Self-inflaming-retarding epoxy resin curing agent containing phosphorus-nitrogen and preparation method thereof
  • Self-inflaming-retarding epoxy resin curing agent containing phosphorus-nitrogen and preparation method thereof
  • Self-inflaming-retarding epoxy resin curing agent containing phosphorus-nitrogen and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1) Synthesis of intermediates

[0031] Add N-phenyl-1,4-phenylenediamine (18.424g, 0.1mol), 4-hydroxybenzaldehyde (12.212g, 0.1mol) and 100ml ethanol in a 250ml three-necked flask equipped with a condenser and a stirrer Solvent, at room temperature, react for 4h, filter the reaction system with filter paper, wash the filtered solid with ethanol solvent 4 times, put it in a vacuum oven to heat up (50°C) and dry to obtain 27.96g of a green solid product, which is an intermediate, The yield is 91.27%.

[0032] 2) Synthesis of curing agent DOPO-RT

[0033] The intermediate (14.418g, 0.05mol) that above-mentioned reaction gains, DOPO (10.8g, 0.05mol) and 100ml dimethylformamide (DMF) solvent join in the 250ml container that is equipped with condenser tube and stirrer to stir, in At room temperature, react for 6 hours, filter the reaction system with filter paper, wash the filtrate several times with ethanol, put it in a vacuum oven (50°C) and dry it to obtain 23.58g of whi...

Embodiment 2

[0035] 1) Synthesis of intermediates

[0036] Add N-phenyl-1,4-phenylenediamine (22.1088g, 0.12mol), 4-hydroxybenzaldehyde (12.212g, 0.1mol) and 100ml ethanol in a 250ml three-necked flask equipped with a condenser and a stirrer Solvent, react at room temperature for 3 hours, filter the reaction system with filter paper, wash the filtered solid with ethanol solvent 4 times, put it in a vacuum oven to heat up (35°C) and dry it to obtain 31.21g of a green solid product, which is an intermediate, The yield reached 90.94%.

[0037] 2) Synthesis of curing agent DOPO-RT

[0038] The intermediate (14.418g, 0.05mol) obtained by the above reaction, DOPO (12.96g, 0.05mol) and 100ml of dimethylformamide (DMF) solvent were added to the 250ml container that was equipped with a condenser tube and a stirrer to stir. At room temperature, react for 5 hours, filter the reaction system with filter paper, wash the filtrate several times with ethanol, put it in a vacuum oven (35°C) and dry it to...

Embodiment 3

[0040]Add N-phenyl-1,4-phenylenediamine (20.2664g, 0.11mol), 4-hydroxybenzaldehyde (12.212g, 0.1mol), DOPO (21.6g, 0.1mol) and 150ml dimethylformamide (DMF) solvent, react at room temperature for 8h, filter the reaction system with filter paper, wash the filtrate 3 times with methanol, put it into a vacuum oven to heat up (40°C ) was dried to obtain 54.0784 g of a white solid product with a yield of 91.29%, which was the flame retardant curing agent DOPO-RT.

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Abstract

The invention discloses a self-inflaming-retarding epoxy resin curing agent containing phosphorus-nitrogen and a preparation method thereof and relates to epoxy resin curing agents. The method comprises the steps that N-phenyl-1, 4-phenylenediamine and 4-hydroxy benzaldehyde are added into a container provided with a condensation pipe and a stirrer for reacting with first solvent, the reaction system is filtered, and solids obtained after the filtering are washed and dried, so that an intermediate body is obtained; the intermediate body, DOPO and second solvent are added into a container provided with a condensation pipe and a stirrer for reacting, the reaction system is filtered, and solids obtained after the filtering are washed and dried, so that the self-inflaming-retarding epoxy resin curing agent containing the phosphorus-nitrogen is obtained; or alternatively, the N-phenyl-1, the 4-phenylenediamine, the 4-hydroxy benzaldehyde and the DOPO are added into a container provided with a condensation pipe and a stirrer sequentially for reacting with solvent, the reaction system is filtered, and articles obtained after the filtering are washed and dried, so that the self-inflaming-retarding epoxy resin curing agent containing the phosphorus-nitrogen is obtained. The curing agent contains two active imino groups, one active hydroxyl group and P and N synergistic flame retardant elements simultaneously and can be used for epoxy resin curing and inflaming retardation.

Description

technical field [0001] The present invention relates to an epoxy resin curing agent, in particular to a curable self-flame-retardant epoxy resin curing agent containing phosphorus and nitrogen containing two active imino groups and an active hydroxyl group, and synergistic flame retardancy of P and N. its preparation method. Background technique [0002] Epoxy resins are widely used in machinery, aerospace, electronics, laminates, adhesives, coatings and other fields. However, due to its poor performance, it must be cured with a curing agent in order to show good physical and chemical properties. In addition, as the industry has increasingly higher requirements for the reliability and safety of epoxy resins, the performance requirements for epoxy resins, especially flame retardancy and heat resistance, have gradually increased. [0003] At present, the curing agents used for curing epoxy resins mainly include polyamines, imidazoles and their derivatives, polyphenols, polyo...

Claims

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Application Information

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IPC IPC(8): C08G59/62C07F9/6571
Inventor 许一婷陈显明戴李宗李奇陈国荣曹莹罗伟昂
Owner XIAMEN UNIV
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