摘要
采用刮膜式分子蒸馏装置对C22-三酸二丁一甲酯进行提纯,考察了1级分子蒸馏中,蒸馏温度、蒸馏压力、进料速率和刮膜转速对C22-三酸二丁一甲酯含量和收率的影响。得到1级分子蒸馏提纯C22-三酸二丁一甲酯的适宜分离工艺条件为:蒸馏温度120℃,蒸馏压力40 Pa,进料速率1.2 g/min,刮膜转速240 r/min;在此条件下,C22-三酸二丁一甲酯的含量可达95.6%,收率为85.0%。在蒸馏压力较大情况下,采用多级分子蒸馏可提高产品C22-三酸二丁一甲酯含量,但收率下降,当蒸馏压力增大为80 Pa时,经4级分子蒸馏后,C22-三酸二丁一甲酯含量可达到96.5%,收率由1级分子蒸馏的93.9%下降至78.0%。提纯产物经红外光谱和质谱分析,确定产物为目标产物C22-三酸二丁一甲酯。
C22 - tricarboxylic dibutyl - monomethyl ester was purified and the effects of distillation temperature, distillation pressure, and yield of C22 - tricarboxylic dibutyl - monomethyl tigated. The optimal one - step molecular distillation perature 120 ℃, distillation pressure 40 Pa, feeding feeding by wiped film molecular distiller, rate, scraper speed on the content ester in one - step molecular distillation were invesconditions were obtained as follows： distillation ternrate 1.2 g/min, scraper speed 240 r/min. Under these optimal conditions, the content and yield of C= - tricarboxylic dibutyl - monomethyl ester were 95.6% and 85.0% respectively. The content of C22 - tricarboxylic dibutyl - monomethyl ester increased while the yield decreased when C22 - tricarboxylic dibutyl - monomethyl ester was purified by multi - step molecular distillation with a higher distillation pressure, and the content was up to 96.5% ,while the yielddeclined from 93.9% of one -step molecular distillation to 78.0% when C22 - tricarboxylic dibutyl - monomethyl ester was purified by four - step molecular distillation with distillation pressure 80 Pa. The purified product was determined as C22 - tricarboxylic dibutyl -monomethyl ester by IR and MS.
出处
《中国油脂》
CAS
CSCD
北大核心
2014年第10期74-77,共4页
China Oils and Fats
基金
江苏省前瞻性联合研究项目(BY2012091)
江苏省普通高校研究生科研创新计划(SCZ1113900007)
常州市科技支撑计划项目(CE20115002)
关键词
C22-三酸二丁一甲酯
脂肪酸甲酯
分子蒸馏
提纯
C22 - tricarboxylic dibutyl - monomethyl ester
fatty acid methyl ester
molecular distillation
purification
