Preparation technology of phosphorus nitrogen series expansion type fire retardant
An intumescent flame retardant and preparation technology, which is applied in the direction of fireproof coatings, etc., can solve the problems of poor compatibility of polyolefins, high hygroscopicity, synthesis yield and environmental protection, etc.
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Embodiment 1
[0025] Add 68g of pentaerythritol and 250ml of phosphorus oxychloride to a 500ml three-necked flask, place it in an oil bath at 110°C, stir vigorously for 24 hours, and absorb the hydrogen chloride gas produced by the reaction with an aqueous NaOH solution. After the reaction, it was cooled with an ice water bath, filtered under reduced pressure, washed with dichloromethane, and the filtrate was vacuum dried at room temperature (20°C) for 6 hours to obtain a white solid powder (yield 76%). Dissolve 29.7g of the white solid powder in a three-necked flask containing 250ml of water, place it in a water bath at 90°C, stir and react for 0.5 hours, and then add 100ml of 2mol / L NaOH aqueous solution dropwise for 1 hour. Add dropwise Continue the reaction for 10 minutes after completion. Then add 25.2g of melamine, add 1g of sodium stearate after reacting for 1 hour, continue to stir and reflux for 1 hour. After the reaction, it was cooled with an ice water bath, filtered under reduced pr...
Embodiment 2
[0028] Add 68g of pentaerythritol and 250ml of phosphorus oxychloride to a 500ml three-necked flask, place it in an oil bath at 110°C, stir vigorously for 24 hours, and absorb the hydrogen chloride gas produced by the reaction with an aqueous NaOH solution. After the reaction, it was cooled with an ice water bath, filtered under reduced pressure, washed with dichloromethane, and the filtrate was vacuum dried at room temperature (20°C) for 6 hours to obtain a white solid powder (yield 76%). Dissolve 29.7g of the white solid powder in a three-necked flask containing 250ml of water, place it in a water bath at 90°C, stir and react for 0.5 hours, and then add 2mol / L NaHCO dropwise. 3 The aqueous solution is 100ml, the dripping time is 1 hour, and the reaction is continued for 10 minutes after the dripping is completed. Then add 25.2g of melamine, add 1g of sodium stearate after reacting for 1 hour, continue to stir and reflux for 1 hour. After the reaction, it was cooled with an ice w...
Embodiment 3
[0030] Add 68g of pentaerythritol and 250ml of phosphorus oxychloride to a 500ml three-necked flask, place it in an oil bath at 110°C, stir vigorously for 24 hours, and absorb the hydrogen chloride gas produced by the reaction with an aqueous NaOH solution. After the reaction, it was cooled with an ice water bath, filtered under reduced pressure, washed with dichloromethane, and the filtrate was vacuum dried at room temperature (20°C) for 6 hours to obtain a white solid powder (yield 76%). Dissolve 29.7g of the white solid powder in a three-necked flask containing 250ml of water, place it in a water bath at 90°C, stir and react for 0.5 hours, and then add 100ml of 2mol / L NaOH aqueous solution dropwise for 1 hour. Add dropwise Continue the reaction for 10 minutes after completion. Then, 25.2 g of melamine was added, and after 1 hour of reaction, 1 g of sodium dodecylbenzene sulfonate was added, and the stirring was continued for 1 hour at reflux. After the reaction, it was cooled w...
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Abstract
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