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将马铃薯淀粉酸水解,非水条件下与三氯氧磷交联,制得氯化淀粉磷酸酯(SPC),后者分别与二乙醇胺、三聚氰酰胺反应合成2种环保型膨胀阻燃剂二羟乙基淀粉磷酰胺(SPE)与淀粉磷酸酯密胺(SPM)。测定二者含磷量,最高分别可达0.157%(wt,质量分数,下同)、0.169%。以XRD、IR表征了原料和样品结构。将2种阻燃剂分别与聚氨酯原料混合,采用全水发泡工艺制备系列阻燃聚氨酯(IFR-PU),以极限氧指数(LOI)及垂直燃烧实验对阻燃样品进行阻燃性能测试。结果表明,随着SPE、SPM添加量的增加,聚氨酯的LOI值逐渐增大,当SPE的添加量为30%时,LOI值为22.4%,未达阻燃级别。而SPM的添加量为30%时,LOI值可达29%,达到阻燃UL-94-V0级别,SPM的阻燃效果较SPE更好。
The potato starch was acid-hydrolyzed and cross-linked with phosphorus oxychloride under non-aqueous conditions to obtain chlorinated starch phosphate ester (SPC). The latter was respectively reacted with diethanolamine and melamine to synthesize two environmentally friendly intumescent flame retardants Dihydroxyethyl starch phosphoramide (SPE) and starch phosphate melamine (SPM). Determination of phosphorus content of the two, the highest respectively up to 0.157% (wt, mass fraction, the same below), 0.169%. The XRD, IR characterization of the raw materials and sample structure. A series of flame retardant polyurethanes (IFR-PU) were prepared by the whole water foaming process. The flame retardancy of the flame retardant samples was tested by limiting oxygen index (LOI) and vertical burning test. The results showed that with the addition of SPE and SPM, the LOI of polyurethane increased gradually. When the amount of SPE was 30%, the LOI was 22.4%, which did not reach the level of flame retardancy. However, when the addition of SPM was 30%, the LOI value reached 29%, reaching the level of UL-94-V0. The flame retardant effect of SPM was better than that of SPE.