一种两性皮革加脂剂的合成及其应用性能研究

Synthesis of an amphoteric fatliquoring agent and its application performances

以马来酸酐(MAH)为起始材料,依次与十二醇、二乙醇胺进行酯化反应,最后通过磺化制得了一种两性型加脂剂MADD-SUL。分别以酯化率和磺化率为指标,通过单因素试验确定了各步的较佳反应条件。第一步酯化反应生成MADE的较佳反应时间为6h,温度为90℃,马来酸酐与十二醇物质的量之比为1:1,催化剂为1%的无水乙酸钠第二步酯化反应生成MADD时以0.5%的亚磷酸为催化剂,反应时间为8h,温度为170℃,MADE与二乙醇胺物质的量之比为2:1。磺化反应的反应时间为4h,温度为80℃,MADD与亚硫酸钠物质的量之比为1:2。通过傅里叶变换红外光谱(FT-IR)和核磁共振氢谱(1H-NMR)对制备的加脂剂的结构进行了表征,然后将MADD-SUL应用于常规蓝湿革加脂工艺,同时与市售加脂剂MF进行对比。结果表明:使用MF加脂后皮革样品的柔软度为7.352mm,二氯甲烷萃取物含量为5.667%,而MADD-SUL加脂后革样的柔软度为9.276mm,二氯甲烷萃取物含量为5.608%,MADD-SUL的综合应用性能优于MF。

An amphoteric fatliquoring agent(MADD-SUL)was prepared using maleic anhycli.ide(MAH)as starthing material.MAH was esterified in sequence with dodecanol and diethanolamine,and then sulfonated with sodium sulfite.The optimum reaction conditions of each step were determined through single-factor experiments with the rate of esterification and sulfonation as indicators.In the synthesis of MADE by the esterification reaction of MAH and dodecanol,1%anhydrous sodium acetate was used as catalyst.The results indicate that the optimum reaction time is 6 hours,the temperature is 90℃ and the molar ratio of MAH to dodecanol is 1:1.Moreover,it is found that the optimum reaction time for the second esterification to synthesis MADD is 8h with temperature at 170℃.The molar ratio of MADE to diethanolamine is 2:1,and the catalyst is 0.5%phosphorous acid.As for the sulfonation reaction,the reaction time is 4h,the reaction temperature is 80℃,and the molar ratio of MADD to sodium sulfite is 1:2.The structure of prepared fatliquoring agent MADD-SUL was characterized by FT-IR and 1H-NMR and its application performances were compared with commercial fatliquoring agent MF.It is found that the softness of leather fatliquored MADD-SUL is 9.276 mm and the content of methylene chloride extract is 5.608%,better than that of MF,which is 7.352 mm and 5.667% respectively suggesting the excellent properties of prepared amphoteric fatliquoring agent.