Macromolecular phosphorus nitrogen flame retardant with cage ring phosphate structure and preparation method
A technology of caged cyclic phosphate ester and molecular phosphorus nitrogen is applied in the field of flame retardant, which can solve the problems of poor compatibility with polymers, easy moisture absorption of compound systems, uneven phase distribution, etc., and achieves good and excellent flame retardant effect. Droplet resistance, the effect of improving the oxygen index
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Embodiment 1
[0023] In a 500mL dry three-necked flask equipped with a mechanical stirrer, a constant pressure dropping funnel, and a condensing reflux device, add 14.4g (0.08mol) of pentaerythritol phosphate and 100mL of refined acetonitrile in sequence, and stir for 1 hour at room temperature under nitrogen protection to make it Dissolve; then weigh 15.3g (0.1mol) of phosphorus oxychloride (the molar ratio of phosphorus oxychloride to pentaerythritol phosphate is 1:0.8) and dissolve it in 100mL of refined acetonitrile, and slowly add it dropwise to the above reaction system , the dropping time is 1h; after 0.5h, slowly heat up to 80°C, reflux and stir for 24h, add anhydrous piperazine after the reaction: 8.6g (0.1mol), acetonitrile 150ml, stir and heat to 80°C for reflux reaction for 24h, depressurize After the solvent is distilled off, a macromolecular phosphorus nitrogen flame retardant with a cage ring phosphate ester structure is obtained as a white powder.
Embodiment 2
[0025] In a 500mL dry three-necked flask equipped with a mechanical stirrer, a constant pressure dropping funnel, and a condensing reflux device, sequentially add 21.6g (0.12mol) of pentaerythritol phosphate and 130mL of refined acetonitrile, and stir at room temperature for 1 h under nitrogen protection to make the Dissolve; then weigh 15.3g (0.1mol) of phosphorus oxychloride (the molar ratio of phosphorus oxychloride to pentaerythritol phosphate is 1:1.2) and dissolve it in 100mL of refined acetonitrile, and slowly add it dropwise to the above reaction system , the dropping time is 1h; after 0.5h, slowly heat up to 80°C, reflux and stir for 24h, add anhydrous piperazine after the reaction: 8.6g (0.1mol), acetonitrile 150ml, stir and heat to 80°C for reflux reaction for 24h, reduce After the solvent is distilled off by pressure, a macromolecular phosphorus nitrogen flame retardant with a cage ring phosphate ester structure is obtained as a white powder.
Embodiment 3
[0027] In a dry 500mL three-necked flask equipped with a mechanical stirrer, a constant pressure dropping funnel, and a condensing reflux device, add 18g (0.1mol) of pentaerythritol phosphate and 100mL of refined acetonitrile in sequence, and stir for 1 hour at room temperature under nitrogen protection to dissolve Then take by weighing 15.3g (0.1mol) phosphorus oxychloride (the mol ratio of phosphorus oxychloride and pentaerythritol phosphate is 1:1.2) and dissolve in the acetonitrile that 100mL refines, and it is slowly added dropwise in the above-mentioned reaction system, Adding time is 1h; after 0.5h, slowly raise the temperature to 80°C, reflux and stir for 24h, add anhydrous piperazine: 8.6g (0.1mol) and 150ml of acetonitrile after the reaction, keep the system temperature at 20°C and stir for 24h, depressurize After the solvent is distilled off, a macromolecular phosphorus nitrogen flame retardant with a cage ring phosphate ester structure is obtained as a white powder....
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