干法制备磷-氮膨胀型阻燃剂的研究

Study on preparation of a novel phosphor-nitrogen intumescent flame retardant by dry method

以磷酸、五氧化二磷、季戊四醇和三聚氰胺为原料,采用干法(不添加任何溶剂)合成了一种磷-氮膨胀型阻燃剂。IR分析发现合成阻燃剂具有与磷酸酯三聚氰胺盐类似的P=O和P-O-C双环结构。反应温度、时间和原料配比对酯化反应有明显的影响。酯化反应温度宜控制在120-130℃之间,反应时间2.5小时,加入五氧化二磷可以提高酯化反应的转化率,磷酸与五氧化二磷的摩尔比控制在2:1为宜。热重分析表明,该阻燃剂的起始分解温度为190℃左右,700℃时的成炭率约为30%。该阻燃剂受热后膨胀倍数约为30-50倍,SEM分析发现,阻燃剂膨胀炭层外表面连续、平滑、颗粒之间连结紧密,炭层为内部为多孔结构,空隙大小分布均匀,孔径约为150-200μm之间,这样的泡层结构能更好的起到隔热的效果。

A novel phosphorus-nitrogen containing intumescent flame retardant was prepared by dry method（without adding any sol- vent） using H3 PO4, P2O5, pentaerythritol and melamine as raw materials. IR analysis found that the synthetic flame retardant had the P = O and P-O-C double-ring structure, same as phosphate ester melamine salts. The reaction temperature, time and the ratio of raw materials had significant effect on the esterification reaction. The esterification reaction temperature should be controlled between 120℃ and 130℃, and the reaction time should be 2. 5 hours. The conversion rate of esteriflcation could be improved by adding P, Os to the reaction, and preferential mole rate between H3PO4 and P205 should be 2：1. Thermogravimetrie analysis showed that the starting decomposition temperature of the flame retardant was 190℃, and at 700℃, the carbonaceous residue rate was about 30% ~ The expansion ratio of the flame retardant after heated was about 30 to 50 times,SEM analysis found that the exteral surfance of the expansion carbon layer was continuous and smooth, and the interior of the expansion carbon layer was uniformly porous structures, and the aperture size was about 150-200μm,such porous structures could provide have better adiabatic effect.