分步碱液滴加法合成膨胀型阻燃剂b-MAP  

Synthesis of Intumescent Flame Retardant bMAP by Fractional Alkali Liquor Dropping

作　　者：周箭[1] 杨辉[1] 陈日新 

机构地区：[1]浙江大学纳米科学与技术中心,杭州310027 [2]杭州浙大多元新材料有限公司,杭州310027

出　　处：《化工进展》2005年第6期651-655,共5页Chemical Industry and Engineering Progress

基　　金：国家科技型中小企业技术创新基金(No.03C26213300585)资助项目。

摘　　要：分析了膨胀型阻燃剂2,4,8,10四氧3,9二磷螺环[5,5]十一烷3,9-二氧3,9二三聚氰胺盐(bMAP)的合成工艺,采用分步碱液滴加的新方法合成了bMAP,获得了较高的产率(产率为93%～97.9%)。通过FTIR、DMX500超导NMR、ESI质谱、SEM以及元素分析进一步确认了bMAP的分子结构和形貌特征。研究发现,碱液的添加量与最后产物的产率及纯度相关,通过比较产物IR谱图中的非取代的P=O峰值的大小,可以定性地获知产物纯度的高低,当NaOH的添加量为0.19mol(与合成产物的摩尔比为1.9∶1)时,获得bMAP的产率为97.9%。同时对bMAP/PP复合材料做了相关的力学和阻燃性能测试。The process for synthesis of intumescent flame retardant dimelamine salt of 3,9 bis(hydroxy) 2,4,8,10 tetraox 3,9 diphosphaspiro[5,5]undecane 3,9 dioxide ((b MAP)) was analyzed. High yields (93%~97.9% yield) of b MAP were obtained by fractional alkali liquor dropping.The highest yield (97.9% yield) was achieved when the dropping content of NaOH was 0.19mol (equivalent to a molar ratio of a b MAP product :1.9 NaOH molecule). Molecular structure and micrography patterns of b MAP were further confirmed by FT IR, DMX500 NMR, ESI, SEM and EA(elementary analysis). The result of P=O wavenumbers (melamine salt was not synthesized) in FT IR showed the purity of final products. (Furthermore), mechanical (properties) and flame retardancy of b MAP/PP composites were tested.

关 键 词：膨胀型阻燃 b—MAP 三氯氧磷 季戊四醇 三聚氰胺 分步碱液滴加 

分 类 号：TQ314.2[化学工程—高聚物工业]