Method for synthesizing phosphorus-containing polyester for fire retardant electronic packaging material
A technology of electronic packaging materials and synthesis methods, which is applied in the field of electronic packaging materials, can solve problems such as inability to realize continuous production, and achieve the effects of stable production, simple synthesis process, and easy control of conditions
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Embodiment 1
[0035] Add 12.07g of ethylene glycol, 8.76g of 2-methyl 1,3 propanediol, and 233.26g of neopentyl glycol to a 1L four-neck flask equipped with a heating mantle, stirrer, thermometer, distillation column, and condenser tube, heat and stir to melt Finally, add 5.69g of adipic acid, 110g of terephthalic acid, 6.47g of isophthalic acid, 133.45g of CEPPA, 202.28g of DDP and 0.6g of tetrabutyl titanate. Esterified water is distilled out. During the reaction process, the temperature of the distillation column is controlled not to be higher than 100°C, and then a segmented esterification reaction is carried out, heating at 180-220°C for 5 hours, heating at 220-240°C for 4 hours, and heating at 240-270°C React for 3-5 hours, when the acid value of the reaction system is less than 18mgKOH / g, carry out vacuum polycondensation, the vacuum degree is -0.05MPa, and the vacuuming time is 30min; when the acid value is between 2-5mgKOH / g, lower the temperature To 200°C, add 224.47g of trimellit...
Embodiment 2
[0038]Add 10.54g of ethylene glycol, 9.56g of 2-methyl 1,3 propanediol, and 254.46g of neopentyl glycol to a 1L four-neck flask equipped with a heating mantle, stirrer, thermometer, distillation column, and condenser tube, heat and stir to melt Finally, add 6.21g of adipic acid, 120g of terephthalic acid, 7.06g of isophthalic acid, 236.58g of CEPPA, 73.56g of DDP and 0.6g of tetrabutyl titanate. Esterified water is distilled out. During the reaction, the temperature of the distillation column is controlled not to be higher than 100°C, and then a segmented esterification reaction is carried out, heating at 180-220°C for 5 hours, heating at 220-240°C for 4 hours, and heating at 240-270°C React for 3 to 5 hours. When the acid value of the reaction system is less than 18mgKOH / g, vacuum polycondensation is carried out. The vacuum degree is -0.05MPa, and the vacuuming time is 30 minutes; 200°C, add 228.56g of trimellitic anhydride to block, react at 170-190°C for 1.5h, then vacuumiz...
Embodiment 3
[0041] Add 8.23g of ethylene glycol, 9.96g of 2-methyl 1,3 propanediol, and 265.07g of neopentyl glycol into a 1L four-neck flask equipped with a heating mantle, agitator, thermometer, distillation column and condenser, heat and stir to melt Finally, add 6.47g of adipic acid, 125g of terephthalic acid, 7.35g of isophthalic acid, 293.82g of CEPPA and 0.6g of tetrabutyl titanate. The water is distilled out, and the temperature of the distillation column is controlled not to be higher than 100°C during the reaction, and then a segmented esterification reaction is carried out, and the reaction is heated at 180-220°C for 5 hours, 220-240°C for 4 hours, and 240-270°C for 3-3 hours. 5h, when the acid value of the reaction system is less than 18mgKOH / g, conduct vacuum polycondensation, the vacuum degree is -0.05MPa, and the vacuuming time is 30min; when the acid value is between 2 and 5mgKOH / g, cool down to 200°C , adding 221.07g of trimellitic anhydride to end capping, reacting at 17...
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