N-羟甲基丙烯酰胺螺环磷酸酯的合成及表征

Synthesis and Characterization of N- methylol acrylamide spiro cyclic phosphate

摘要:

以N-羟甲基丙烯酰胺（NMA）和螺环磷酰二氯（SPDPC）为原料，合成了N-羟甲基丙烯酰胺螺环磷酸酯(SPMA)。通过紫外光谱跟踪了反应进程，确定了反应时间和反应机理。结果发现反应1h，体系达到最佳平衡状态；反应首先发生在NMA的-NH-上，而NMA的-OH通过平衡反应与SPDPC作用，生成了最终产物。所得产品SPMA熔点126-130℃，其结构用傅里叶红外光谱进行了表征；用TG法测定了SPMA的热稳定性，发现SPMA初始分解温度（失重3%时的温度）为313℃，最大失重速率对应的温度为343℃，800℃下仍残留32.6%，具有很好的热稳定性和成炭性能。用SPMA阻燃整理棉布，载药量为5%时，极限氧指数提高2个百分点，续燃和阴燃时间缩短70%以上。

Abstract:

A spiro-cyclic phosphate SPMA was synthesized from N-Methylol acrylamide (NMA) and pentaerythritol spiro phosphoryl dichloride(SPDPC).The reaction time and reaction mechanism were determined by tracking the reaction process using ultraviolet spectrum. It was found that the reaction could achieve the optimum state of chemical equilibrium in 1h. At first, the –NH- of NMA quickly reacted with SPDPC, then the –OH slowly reacted to form the final product by equilibrium reaction. The melt point of the product SPMA is 126～130 ℃. The thermal stability of SPMA was evaluated by Thermogravimetry and it was found that SPMA has better thermal stability and carbonization performance with 313℃of the initial decomposition temperature, 343℃ of the maximum weight loss temperature (Tmax) and 32.6% of residue under 800℃. With SPMA flame retardant finishing of cotton cloth and the addition was 5%, the limiting oxygen index increased by 2%, the combustion and smoldering time reduced by more than 70%.