中国皮革

2020, v.49;No.759(03) 7-17

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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

霍文凯;周继博;廖学品;石碧;
HUO Wenkai;ZHOU Jibo;LIAO Xuepin;SHI Bi;National Engineering Laboratory for Clean Technology of Leather Manufacture,Sichuan University;The Key Laboratory of Leather Chemistry and Engineering of Ministry of Education,Sichuan University;

摘要(Abstract):

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6 h,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8 h,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4 h,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7.352 mm,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9.276 mm,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 anhydride(MAH)as starting 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 8 h 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 4 h,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.

关键词(KeyWords): 马来酸酐;十二醇;二乙醇胺;两性型加脂剂;加脂性能
maleic anhydride;dodecanol;diethanolamine;amphoteric fatliquor;fatliquoring properties

Abstract:

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基金项目(Foundation): 国家重点研发计划(2017YFB0308500)

作者(Author): 霍文凯;周继博;廖学品;石碧;
HUO Wenkai;ZHOU Jibo;LIAO Xuepin;SHI Bi;National Engineering Laboratory for Clean Technology of Leather Manufacture,Sichuan University;The Key Laboratory of Leather Chemistry and Engineering of Ministry of Education,Sichuan University;

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