含硫环状膦酸酯衍生物的合成及其热性能

Synthesis and Thermal Performance of Cyclic Phosphonate Derivatives Containing Sulfur

以三氯化磷、苯和硫粉为原料,用离子液体法绿色合成了硫代苯基膦酰二氯(3);3与季戊四醇或新戊二醇反应合成了两种新型含硫磷系阻燃剂——2,4,8,10-四氧杂-3,9-二磷杂螺环[5.5]十一烷-3,9-二硫-3,9-二苯(1)或5,5-二甲基-2-苯基-2-硫代-1,3-二氧-2-磷杂环己烷(2)。用1H NMR,IR,DSC和TG对其结构和性能进行了表征。结果表明,1具有良好的成炭性和热稳定性。

Diehlorophenylphosphine sulfide （3） was greenly prepared from phosphorus trichloride, benzene and sulfur powder by ionic liquid method. Two novel flame retardants containing phosphorus, 2,4,8,10-tetraoxa-3,9-dithio-3,9-diphenyl-3,9-diphosphaspiro [ 5,5 ] -undecane （ 1 ） or 5,5-dimeth- yl-2-phenyl-2-thio-1,3,2-dioxaphosphorinane（2）, were synthesized by the reaction of 3 with pentaerythritol or neopentyl glycol. The chemical structures and properties of 1 and 2 were determined by 1H NMR, IR, DSC and TG. The results showed that 1 exhibited good char-forming characteristics and thermal stability.