Phosphorus and nitrogen containing flame-retardant curing agent for epoxy resin and preparation method for agent
A nitrogen epoxy resin and curing agent technology, which is applied in the field of phosphorus-containing, nitrogen epoxy resin flame retardant curing agent and its preparation, can solve the problems of plastic products cannot be recycled or destroyed, waste the environment, pollution, etc. The effect of protection, convenient post-processing and high purity
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Embodiment 1
[0020] The first step: to the equipment equipped with reflux condenser, thermometer, N 2 Add 50.598g (0.33mol) of phosphorus oxychloride to the 250ml three-necked bottle of the introduction tube and dropping funnel, and 120ml of dichloromethane as a solvent, then add 25.612g (0.35mol) of diethylamine and triethylamine in the dropping funnel 33.393g (0.33mol), feed N 2 Protection, the dropwise addition was completed in 3 hours under ice-bath conditions, the temperature was raised to 20°C, and the reaction was kept for 12 hours. After the reaction, a light yellow liquid slurry is obtained, and the liquid is filtered, rotary evaporated, and vacuum distilled to obtain a colorless transparent liquid, which is an intermediate.
[0021] The second step: equipped with magnetic stirring, dropping funnel, N 2 Add 22.512g (0.2mol) p-phenylenediamine to the 250ml four-necked bottle of the introduction tube and thermometer, add 120ml chloroform as solvent, dissolve 20.418g intermediate i...
Embodiment 2
[0023] The first step: the synthetic method of phosphorus, nitrogen intermediate is the same as embodiment 1.
[0024] The second step: equipped with magnetic stirring, dropping funnel, N 2 Add 22.512g (0.2mol) p-phenylenediamine in the 250ml four-necked bottle of introduction tube and thermometer, add 120ml dichloromethane as solvent, 20.418g (0.1mol) intermediate is dissolved in 20ml dichloromethane, and its Transfer to a constant pressure dropping funnel, raise the temperature to 40°C and start dropwise addition. After 2.0 hours, the dropwise addition is completed, and the reaction is continued for 12 hours. The product can be treated to obtain a light gray solid.
Embodiment 3
[0026] The first step: the synthetic method of phosphorus, nitrogen intermediate is the same as embodiment 1.
[0027] The second step: equipped with magnetic stirring, dropping funnel, N 2 Add 23.798g (0.22mol) of p-phenylenediamine in the 250ml four-neck bottle of the introduction tube and thermometer, add 120ml of dichloromethane as solvent, dissolve 20.418g (0.1mol) of the intermediate in 20ml of dichloromethane, and Transfer to a constant pressure dropping funnel, raise the temperature to 40°C and start dropwise addition. After 2.0 hours, the dropwise addition is completed, and the reaction is continued for 12 hours. The product can be treated to obtain a light gray solid.
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