两步浸提法提取花椒籽皮油、仁油工艺研究(硕士论文)(可编辑).doc

两步浸提法提取花椒籽皮油、仁油工艺研究(硕士论文) 摘要花椒籽是一种含油量丰富的木本油料和食物蛋白质资源,其理论产量高出花椒果皮 20%,但却因长期未得到合理利用而被废弃填埋或者焚烧近年来,随着我国花椒产量的迅速增长,废弃的花椒籽也与日俱增,如何开发利用花椒籽这一资源, 是目前迫切需要解决的问题本文以陕西韩城大红袍花椒籽为原料,对两步浸提工艺的可行性,皮油、仁油提取工艺的优化以及仁油的脱蜡、脱酸精制进行了较为系统的研究,旨在论证这套新工艺并优化工艺条件为实现生产提供理论依据和数据支撑试验主要结果如下: 1. 陕西韩城大红袍花椒籽含油量 31.70%(w/w),其中皮油 10.00%,仁油 21.70% 2. 选用食用酒精、甲醇、乙酸乙酯、60-90℃石油醚、正己烷、6#溶剂油分别提取 花椒籽皮油、仁油,6#溶剂油提取率较高,且价格低廉,是工业提取油脂常用 溶剂,因此6#溶剂油可作为提取花椒籽皮油、仁油的溶剂 3. 采用两步浸提工艺提取花椒籽皮油,各因素影响的主次顺序为提取次数>溶剂 用量>提取温度>提取时间,以提取时间 160min,提取温度 70℃,溶剂用量25ml/g,提取 3次为昀佳组合。

昀佳条件下花椒籽皮油出油率可达 92.90% 4. 采用两步浸提工艺提取花椒籽仁油,各因素影响的主次顺序为提取次数>溶剂 用量>提取温度>提取时间,提取时间 40min,提取温度 60℃, 溶剂用量 15ml/g,提取 3次为昀佳组合昀佳条件下花椒籽仁油出油率可达 97.51% 5. 两步浸提法提取的花椒籽粗仁油含蜡量 2.02g/100g,酸值 41.10 mgKOH/g 6. 比较了溶剂法、碱炼法对花椒籽仁油的脱蜡效果,碱炼法明显优于溶剂法 7. 影响花椒籽仁油碱炼脱蜡率的因素次序为:温度>时间>氢氧化钾浓度以结 晶温度 8℃,结晶时间 8h,加入的氢氧化钾浓度 0.4mol/L为昀佳组合 8. 采用NaOH对花椒籽仁油碱炼脱酸,影响脱酸率的因素次序为:碱液用量>碱 的浓度>搅拌时间,以搅拌时间10min 、NaOH用量6.55mg/g、碱浓度0.032 mol/L为昀佳组合关键词:花椒籽皮油;花椒籽仁油;两步浸提法;脱蜡;脱酸I Abstract The seeds of Zanthoxylum bungeanum im is a food protein resource and a woody oil plant which is riched in lipid, although its theoretical yield is 20 percent more than the pericarp, it was still discarded and landfilled or burned. Recently, with the rapid growth of Zanthoxylum bungeanum im pericarp production of my country, we have an increasing Zanthoxylum bungeanum im seeds. How to use this discarded resource is a problem to be solved urgentlyThis article studied the possibility of the new method- Two Step extraction technology from seeds of da hong pao Huajiao and optimized the process of crust and kernel oil extraction and system research the kernel oil dewaxing and deacidification technologyThese researches aim at demonstrating and optimizing this new method for industrial production. The main results are as follows: 1. The seed oil content of da hong pao Huajiao is 31.70 percent w/w, includ crust oil 10.00 percent and kernel oil 21.70 percent2. With extracting crust and kernel oil by edible alcohol、methanol、ethyl acetate、60- 90℃ petroleum ether、n-hexane and 6#solvent oil, the extraction rate of 6#solvent oil is h- igher. Besides that, 6#solvent oil is quite cheap and widely used for industrial. So we choo- se 6#solvent oil to extract crust and kernel oil of prickly ash seed3. Using the new method to extract crust oil, the most important factor is the extraction times. Then, the secondly to fourthly important factor is solvent volume、 extraction temper- ature and extraction time. We can get the highest extraction rate of 96 percent when 6# sol- vent oil is 25ml/g under 70℃ and 160 min for 3 times. The most yield of oil is 92.90 perc- ent4. Using the new method to extract kernel oil, the most important factor is the extract- ion times. Then, the secondly to fourthly important factor is solvent volume、extraction te- mperature and extraction time. We can get the highest extraction rate of 97.5 percent when 6# solvent oil is 15ml/g under 60℃ and 40 min for 3 times. The most yield of oil is 97.51 percent 5. The wax content and acid value of kernel oil extracting by new method is 2.02g/100gand 41.10 mgKOH/g in turn6. By comparing the dewaxing rate of solvent method and alkali smelting method, we can see the alkali smelting method is better than the former7. The most important factor which influencing the dewaxing of kernel oil by alkali II smelting method is crystallization temperature. The effect on crystallization time and KOH’s concentration is not primary. We can get the highest dewaxing of 81.92 percent when using 0.4mol/L KOH, under 8℃ and crystallization for 8h8. The most important factor which influencing the deacidification of kernel oil is consumption of alkali solution. The effect on concentration of alkali solution and stirring time is not primary. We can get the highest dewaxing of 95.5 percent when using 0.032mol/L NaOH, and consuming 6.55mg/g alkali solution under stirring for 10min III 目录 第 1 章 绪论1 1.1 花椒的资源分布及其利用现状1 1.1.1 花椒的资源分布1 1.1.2 花椒的生态及经济效益1 1.1.3 花椒的形态特征及化学成分 2 1.2 花椒籽开发利用研究进展. 8 1.2.1 花椒籽的形态特征及化学成分8 1.2.2 花椒籽的工业开发11 1.2.3 花椒籽的综合利用..12 1.2.4 前景与展望..13 1.3 课题研究内容.13 第 2 章 试验研究. 16 2.1 引言.16 2.2 材料与设备.16 2.2.1 试验材料..16 2.2.2 主要设备和仪器..16 2.2.3 主要化学试剂17 2.3 试验内容与方法..17 2.3.1 花椒籽基本成分测定方法.17 2.3.2 花椒籽油的提取..17 2.3.3 花椒籽仁油的精制.20 第 3 章 结果与分析 23 3.1 花椒籽基本成分测定结果.23 3.2 花椒籽油提取试验结果231 3.2.1 花椒籽含油率的测定结果..23 3.2.2 昀佳溶剂筛选试验结果.23 3.2.3 两步浸提工艺可行性验证试验结果.24 3.2.4 两步浸提法提取花椒籽皮油试验结果25 3.2.5 两步浸提法提取花椒籽仁油试验结果29 3.3 花椒籽仁油的精制试验结果32 3.3.1 花椒籽仁油组成含量的测定.32 3.3.2 花椒籽仁油脱蜡工艺试验..32 3.3.3 花椒籽仁油脱酸工艺试验结果38 第 4 章 结论44 参考文献45 致谢48 参加课题及发表文章.49 2第1章 绪论 1.1花椒的资源分布及其利用现状 花椒(Zanthoxylum bungeanum im)属芸香科(Rutaceae)多年生灌木或小乔木,全世界约 250种,广泛分布于亚洲、美洲、非洲及大洋洲的热带和亚热带地区。

[1]花椒主产地在亚洲,主要分布在喜玛拉雅山脉附近 、东南亚半岛及东亚地区,我国约 45种,13变种,品种昀为齐全且广泛作为调味料供人食用 花椒味辛、因其特殊的香气长久以来被作为香辛料广为使用花椒还具。