Epoxy resin flame retardance curing agent containing phosphorus and nitrogen and preparation method of epoxy resin flame retardance curing agent
A nitrogen epoxy resin and curing agent technology, applied in the field of chemical curing agent and its preparation, can solve problems such as fire hazards, and achieve the effects of convenient post-processing, mild conditions and high purity
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Embodiment 1
[0027] The first step: to the equipment equipped with reflux condenser, thermometer, N 2 Add 300ml of acetonitrile as a solvent into the 500ml three-neck flask of the introduction tube and magnet, and then add 26.9g of PEPA and 23.0g of POCl 3 . Access to N 2 Protected, the temperature was raised to 80°C for 20h. After the reaction, a light yellow liquid slurry is obtained, and the liquid is filtered, rotary evaporated, and dried to obtain a light yellow viscous liquid, which is the intermediate.
[0028] The second step: in the tank equipped with magnetic stirring, dropping funnel, N 2 Add 50ml of acetonitrile as a solvent into the 100ml four-necked bottle of the introduction tube and thermometer, and then add 13.60g of m-xylylenediamine; dissolve 14.85g of the intermediate in 20ml of acetonitrile, and transfer the solution to a constant pressure dropping funnel, ice Start dropwise addition under the bath, after 2.0 hours of dropwise addition, raise the temperature to 50°...
Embodiment 2
[0030] The first step: the synthetic method of phosphorus, nitrogen intermediate is the same as embodiment 1.
[0031] The second step: equipped with magnetic stirring, dropping funnel, N 2 Add 60ml of acetonitrile as a solvent into the 100ml four-necked flask of the introduction tube and thermometer, and then add 20.40g of m-xylylenediamine; dissolve 22.25g of the intermediate in 30ml of acetonitrile, and transfer it to a constant pressure dropping funnel, ice Start dropwise addition under the bath, after 2.0 hours of dropwise addition, raise the temperature to 50°C, keep the temperature for 16 hours, and end the reaction. After treatment, a white solid can be obtained.
Embodiment 3
[0033] The first step: the synthetic method of phosphorus, nitrogen intermediate is the same as embodiment 1.
[0034] The second step: equipped with magnetic stirring, dropping funnel, N 2 Add 100ml of acetonitrile as a solvent to the 250ml four-necked bottle of the introduction tube and thermometer, and then add 40.80g of m-xylylenediamine; dissolve 44.50g of the intermediate in 60ml of acetonitrile, and transfer it to a constant pressure dripping funnel, and put it in an ice bath After 3.0 hours of dropping, the temperature was raised to 50°C, and the temperature was kept for 24 hours to complete the reaction. After treatment, a white solid was obtained.
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