季戊四醇磷酸酯三聚氰胺盐合成工艺研究

Stucly on synthetic process of melamine salt of pentaerythritol phosphate as flame retardant

以磷酸、季戊四醇、三聚氰胺为原料合成了膨胀型阻燃剂季戊四醇磷酸酯三聚氰胺盐。考察了酸醇物质的量的比、催化剂用量、带水剂用量、酯胺质量比和反应时间等因素对反应过程的影响。确定了最佳反应条件:n(磷酸)∶n(季戊四醇)=5∶1,催化剂NKC-9用量为酸醇总质量的8%,m(甲苯)∶m(季戊四醇)=1.60∶1,酯化温度不低于108℃,酯化时间8 h,该条件下酯收率为74.4%。在m(季戊四醇磷酸酯)∶m(三聚氰胺)=1∶2,反应温度为90℃,反应时间为2 h的条件下,所得产品季戊四醇磷酸酯三聚氰胺盐500℃时的残炭率为51.0%。

The non-halogen intumescent flame retardant,melamine salt of pentaerythritol phosphate（MPP） was synthesized from phosphoric acid（P）,pentaerythritol（PT） and melamine（M） with NKC-9 cation exchange resin as catalyst.The effects of reaction conditions,such as mole ratio of P to PT,NKC-9 catalyst dosage,mass ratio of toluene to PT,mass ratio of pentaerythritol phosphate to M and reaction time were examined.The optimum esterification reaction conditions were as follows：mole ratio,n（P） ∶ n（PT）=5∶1;NKC-9 cation exchange resin as catalyst dosage,8 %（mass of catalyst relative to total mass of P and PT）;mass ratio,m（toluene） ∶ m（PT）=1.60∶1;reaction temperature,≤108 ℃;reaction time,8 h.The yield of pentaerythritol phosphate by the process can achieve 74.4 %.The optimum reaction conditions for pentaerythritol phosphate and M were as follows：mass ratio,m（pentaerythritol phosphate） ∶ m（M）=1∶2;reaction temperature,≤90 ℃;reaction time,2 h.When MPP was heated to 500 ℃,the char residue was 51.0%.