【摘要】 以12-羟基硬脂酸和二乙醇胺为原料,采用减压蒸馏脱水进行酰胺化反应和胺解反应二步合成法制备皮革加脂剂中间体12-羟基硬脂酸二乙醇酰胺。采用FT-IR表征原料及12-羟基硬脂酸二乙醇酰胺结构。通过单因素试验探究合成工艺条件,确定优化的合成工艺条件为:12-羟基硬脂酸与二乙醇胺物质的量比为1∶1.03;第一步酰胺化反应温度135℃,反应时间4h;第二步胺解反应中,反应温度70℃,催化剂乙醇钠用量为12-羟基硬脂酸质量的1.5%,反应时间2h。在该优化条件下合成的12-羟基硬脂酸二乙醇酰胺产率可达90.95%。更多还原

【Abstract】 The intermediate of leather fatliquor named 12- hydroxystearic acid diethanolamide was prepared by two- step synthetic method including acylation reaction( using vacuum distillation dehydration) and aminolysis reaction with 12- hydroxystearic acid and diethanolamide used as raw materials. The structures of raw materials and 12- hydroxystearic acid diethanolamide were characterized by Fourier Transform Infrared Spectroscopy( FTIR). The optimal synthesis conditions were determined by single factor experiments. In the first step of acylation reaction,the mole ratio of 12- hydroxystearic acid and diethanolamine is 1: 1.03,the reaction temperature is 135℃ and the reaction time is 4h. In the second step of aminolysis reaction,the reaction temperature is 70℃ and the reaction time is 2h,and the process is carried out with the catalyst sodium ethoxide( 20% w / w sodium ethoxide- ethanol solution) of 1. 5% mass fraction of 12- hydroxystearic acid. The result indicates that under the optimal conditions,the yield of 12- hydroxystearic acid diethanolamide can reach 90. 95%.更多还原