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分离高碳脂肪酸分子蒸馏工艺技术研究
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摘要
通过采用高压水解法研究高芥酸菜籽油水解制备芥酸的工艺技术条件,分别对反应温度、时间、催化剂浓度和加水量进行单因素试验,优化确定了制备芥酸的工艺条件,芥酸制备工艺参数:反应温度150℃,时间9小时,催化剂浓度0.06g/ml,剂水比2:3。
     通过对芥酸分子蒸馏小试工艺技术参数进行分析,研究了芥酸分子蒸馏装置结构形式、内部构件和装置辅助系统,分别对蒸馏温度、系统真空度、刮膜转速、进料速率及预热温度进行试验研究,试验确定了分离提纯芥酸的工艺技术参数:蒸馏温度210℃,系统真空度9Pa,刮膜转速85rpm,进料速率110g/h,预热温度80℃。
     在小试实验工艺技术参数优化研究基础上,对分子蒸馏提纯芥酸中试蒸馏器及装置进行了设计和试验,推导计算出液膜厚度0.25mm,平均停留时间18s,分子蒸馏器的内径和高度分别为350mm和1200mm,加热蒸发面和内冷面面积分别为0.8m2和2.5m2,用导热油来进行加热,所选用导热油泵的流量为3m3/h。预热器换热面积为1m2;真空系统设计选用JZJ2X系列罗茨泵-旋片泵真空机组,抽气量70L/s。试验结果:芥酸收率可达52%,纯度高达92%。
The process technology conditions of preparation of erucic acid were studied by using high-pressure hydrolysis of erucic acid colza oil, and we did the single factor experiment of reaction temperature, time and amount of catalyst, amount of water to determine optimal conditions for erucic acid preparation. Erucic acid preparation process parameters were that: temperature was 150℃, the time was 9 hours, catalyst concentration was 0.06g/ml, agent water ratio was 2:3.
     Technical parameters of erucic acid molecular distillation in the small scale were analyzed, we studied the structure of erucic acid in the form of molecular distillation, the internal components and devices support system and researched the distillation temperature, system vacuum, wiper speed, feed rate and preheat temperature, and determined acid technology parameters of the separation and purification of erucic:the distillation temperature 210℃, vacuum 9Pa, agitating speed 85rpm, the feed rate 110g/h, preheating temperature 80℃.
     On the basis of optimization study of technical parameters in small scale, distiller and device were designed and tested in the molecular distillation pilot plant test for purification of erucic, the film thickness was designed 0.25mm, mean residence time was 18s, the inner diameter and height of molecular distiller were 350mm and 1200mm, the heated evaporation surface of molecular distiller and inner cold area were 0.8m2 and 2.5m2, conduction oil was used heated, the heat flow pump was 3m3/h, the heat transfer area of preheater was 1m2; JZJ2X series Roots pumps-Rotary Vane vacuum pump unit was designed and selected with the exhaust volume 70L/s. Test result was that:erucic acid yield was 52% and purity was up to 92%.
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