题名 | 从甘蔗制糖滤泥中提取蔗蜡和高级烷醇的研究 |
作者 | 鞠娜 |
学位类别 | 硕士 |
答辩日期 | 2008-06-10 |
授予单位 | 中国科学院过程工程研究所 |
授予地点 | 过程工程研究所 |
导师 | 刘会洲 |
关键词 | 甘蔗制糖滤泥 蔗蜡 浸取 高级烷醇 高效液相色谱 亚临界密闭浸出过滤反应器 |
其他题名 | Study on Leaching Sugarcane Wax and Policosanol from Refinery Sugar Sludge |
学位专业 | 化学工艺 |
中文摘要 | 广西目前是我国最大的产糖区,每年产糖量占全国的50%以上,2003/2004年,我国的蔗糖产量达到了588 万吨,生产l吨糖会产生1.2 吨滤泥(含水50%),粗略统计我国的滤泥资源是丰富而巨大的。糖厂每年排出大量的滤泥其中含有许多宝贵的资源,只是由于滤泥的杂质过多很难提取和利用。本文就是研究从滤泥中提取蔗蜡,以提高甘蔗的综合利用价值。 采用高效液相色谱法,正相色谱技术,在流动相为正己烷:异丙醇=90:10,流动相速度为1 mL/min的条件下,采用蒸发光散射检测器进行检测,使用空气作为雾化气,雾化温度为41.5℃,对蔗蜡标准品进行检测,色谱图上分离出清晰的三个色谱峰,说明蔗蜡标准品中含有三大类极性不同的物质。将此三类物质通过高效液相色谱接出,分别对其进行红外光谱的测定,根据官能团判断此三类物质分别为酯类、酸类和醇类。然后,选用标准样品硬脂酸乙酯、硬脂酸、十八醇(都是含有十八个碳原子的化合物,避免了不同碳原子数对出峰顺序的干扰),在相同的色谱条件下进入高效液相色谱进行检测,检测到的出峰顺序,与蔗蜡中各组分的出峰顺序是一致的。 采用溶剂浸取法对甘蔗制糖滤泥进行浸取以制取蔗蜡,分别考察了一次浸取剂、二次浸取剂以及最后的分离方法对浸取蔗蜡的影响。最终选择的工艺条件为:一次浸取采用丙酮作为浸取剂,二次浸取选择正己烷或者石油醚作为浸取剂,采用蒸馏回收溶剂法对产物进行分离,蔗蜡的浸出率为2.5%,溶剂回收率为40%。 使用甘蔗制糖滤泥作为原材料,采用二步浸取法直接从甘蔗制糖滤泥中提取天然高级烷醇类化合物。实验得出的较佳工艺条件为以25%~28%氨水溶液作一步浸取剂,在90℃的条件下浸取3 h,然后再用石油醚作为二步浸取剂,在60℃的条件下浸取2 h,最后得到的高级烷醇类化合物的浸出率为90%左右。该工艺与文献已有的报道相比,过程简单,操作条件温和,产品收率较高,可作为天然高级烷醇混合物的重要来源之一。 采用设计的亚临界密闭浸出过滤反应器,在常温下由甘蔗制糖滤泥浸取蔗蜡。采用该反应器提取时间短,30 min就可以完成整个浸取过程;提取温度低,常温25℃下提取,避免了在提取过程中蔗蜡因高温熔化的变性。 |
英文摘要 | Guangxi is the largest area of sugar-production in China, every year’s sugar yield occupies 50% of the country. In the years of 2003/2004, the production of cane sugar reached 5.88 million ton. When 1 ton sugar is produced, it will produce 1.2 ton sludge. Therefore, the refinery sugar sludge is very abundance in our country. There are many useful resources in refinery sugar sludge, but it has too many impurities to use. HPLC was used in this study to analyze sugarcane wax under the following conditions: The mobile phase was hexane and isopropanol with proportion of 90:10, mobile phase flow rate was 1mL/min. ELSD was used as the detector, air was as the atomization gas, atomization temperature was 41.5℃.There were three peaks shown on the chromatography, which indicated that there were three substances with different polarity existed in the sugarcane wax. From FTIR analysis, they were ether, fatty acid and fatty alcohol separately according to their functional group. Then, stearic acid ethyl, stearate and 18 alcohol were selected as standard samples and analyzed by HPLC under the same conditions, the retention time of each sample was the same as that of each substance in the sugarcane wax. The method of solvent leaching was used to leach sugarcane wax from refinery sugar sludge. The effects of the first leaching, the second leaching and the final separation method were examined. The optimized conditions were that acetone was used as the first leaching solvent, hexane or petroleum ether was used as the second leaching solvent, the final product was separated by distillation. Under these conditions, the yield of sugarcane wax was 2.5%, and the solvent recovery was 40%. Policosanol was also produced from refinery sugar sludge directly by bi-step leaching method. To use refinery sugar sludge as the raw material, two leaching method to get the policosanol directly. The optimized conditions were as follows: 25%~28% ammonia was used as the first leaching solvent, leaching the refinery sugar sludge about 3 hours under 90℃, then, petroleum ether was used as the second leaching solvent, leaching the residue obtained from the first step leaching about 2 hours under 60℃, 90% policosanol was obtained. Compared with the reported method, this method was simple in process, mildness in conditions and high in yield. Sugarcane wax was leached from refinery sugar sludge in a designed subcritical-leaching and filtrating-reactor under room temperature. The result showed that the react-time was short(30min), temperature was low(25℃), which avoided the denaturalization of sugarcane wax at high temperature. |
语种 | 中文 |
公开日期 | 2013-09-13 |
页码 | 79 |
内容类型 | 学位论文 |
源URL | [http://ir.ipe.ac.cn/handle/122111/1223] ![]() |
专题 | 过程工程研究所_研究所(批量导入) |
推荐引用方式 GB/T 7714 | 鞠娜. 从甘蔗制糖滤泥中提取蔗蜡和高级烷醇的研究[D]. 过程工程研究所. 中国科学院过程工程研究所. 2008. |
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