戊二醛-季戊四醇改性氮磷阻燃复鞣剂的合成及应用

Synthesis and Application of Retanning Agent with Nitrogen-Phosphorus Retardant Modified by Glutaraldehyde and Pentaerythritol

采用亚磷酸二甲酯与丙烯酰胺在甲醇钠的催化作用下,反应制得中间体3-二甲氧磷酰基丙酰胺,再与戊二醛反应后用季戊四醇对产物进行改性。通过正交优化试验对其最佳合成条件进行研究,讨论了单体配比、反应温度、反应时间对聚合反应的影响,确定了季戊四醇改性的最佳条件为:丙烯酰胺与季戊四醇的摩尔比1:0.2,反应温度80℃,反应时间1h。将合成的阻燃复鞣剂用于皮革加工工艺,阻燃复鞣剂的用量分别为0%、3%、6%、9%,利用氧指数法、垂直燃烧法、水平燃烧法和烟密度法对复鞣的皮革进行阻燃测试,试验发现,与未施加阻燃复鞣剂相比,氧指数可提高25%,有焰燃烧时间显著降低,烟密度可降低83%,燃烧速率均达到合格水平,所得皮革的厚度得到提高,皮革手感、丰满度、柔软度未受负面影响。

3 - dimethoxy - phosphoryl propinamide was synthesized by the reaction of dimethyl phosphite and acrylamide with sodium methoxide as the catalyst. The obtained product was modified by glutaraldehyde and pentaerythritol in sequence. And the effects of molar ratio, reaction temperature and time were studied and the optimal reaction conditions are obtained by orthogonal method and presented as follows： the momomer ratio of acrylamide and pentaerythritol is 1：0.2, reaction temperature is 80℃ , reaction time is 1 hour. When applied in leather tanning, the dosage of the synthetic retanning agent is 0% , 3% , 6% , 9% respectively. The limited oxygen index, vertical combustion, smoke density and level of detection of combustion were used for characterization of the flame - retardant properties of the above leathers. And the results show that the oxygen index increases 25% , the time of flame burning is reduced significantly, and the smoke density reduces 83% , the burning rate is limited to an acceptable level compared with the blank. And the thickness of leather improves,the handle, the fullness and softness of leather are not affected after treated by the retanning agent.