CN103571614A - Preparation method of castor oil and castor oil prepared through same - Google Patents
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- 235000019438 castor oil Nutrition 0.000 title claims abstract description 66
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 41
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 160
- 239000012046 mixed solvent Substances 0.000 claims abstract description 68
- 235000004443 Ricinus communis Nutrition 0.000 claims abstract description 61
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- 239000003921 oil Substances 0.000 claims abstract description 24
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- 238000010298 pulverizing process Methods 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 20
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- ZEMPKEQAKRGZGQ-AAKVHIHISA-N 2,3-bis[[(z)-12-hydroxyoctadec-9-enoyl]oxy]propyl (z)-12-hydroxyoctadec-9-enoate Chemical compound CCCCCCC(O)C\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CC(O)CCCCCC)COC(=O)CCCCCCC\C=C/CC(O)CCCCCC ZEMPKEQAKRGZGQ-AAKVHIHISA-N 0.000 claims 1
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Abstract
本发明提供一种蓖麻油的制备方法,包括蓖麻籽粉碎,以溶剂浸提,得到的混合油脱溶剂;其中所述溶剂为石油醚和乙醚构成的混合溶剂。优选的,所述混合溶剂中石油醚和乙醚的体积比为5:5~9:1;蓖麻籽与所述混合溶剂的质量体积比为1:1~1:7。本发明所述制备方法浸出效率高、能耗少。本发明还提供所述制备方法制备得到的蓖麻油。
The invention provides a preparation method of castor oil, which comprises pulverizing castor beans, leaching with a solvent, and desolventizing the obtained mixed oil; wherein the solvent is a mixed solvent composed of petroleum ether and diethyl ether. Preferably, the volume ratio of petroleum ether and diethyl ether in the mixed solvent is 5:5-9:1; the mass-volume ratio of castor beans to the mixed solvent is 1:1-1:7. The preparation method of the invention has high leaching efficiency and less energy consumption. The invention also provides castor oil prepared by the preparation method.
Description
技术领域technical field
本发明属于油脂工业或化工技术领域,具体是一种利用混合溶剂浸提蓖麻油的制备方法及其制备的蓖麻油。The invention belongs to the technical field of oil industry or chemical industry, in particular to a preparation method for extracting castor oil with a mixed solvent and the prepared castor oil.
背景技术Background technique
蓖麻(Ricinus communis)为大戟科(Euphoribia L)一年生或多年生草本植物,是世界十大油料作物之一,在全世界广为种植,主要产区是印度、中国、巴西等国,产量占全世界产量的90%以上。在我国,蓖麻的产地主要在内蒙古、吉林、山东和山西。蓖麻籽含油率高,约占子重的45-55%,其所含的蓖麻油是唯一含有羟基的天然脂肪酸,具有特殊的理化性质。蓖麻油是重要的化工原料,广泛用于化工、纺织、轻工、医药等部门,主要生产高级润滑油、油漆、涂料、肥皂、油墨、助染剂、增塑剂、聚氨酯、乳化剂等。由于种植蓖麻具有广泛的用途和较高的经济价值,在国民经济中占有重要的地位,特别是当今世界上石油面临耗尽待尽的危机,作为植物源油料的蓖麻由于其具有可持续生产的有点和无可替代的重要价值,正日益受到世界各国的重视,其产业前景非常广阔。Castor (Ricinus communis) is an annual or perennial herbaceous plant of Euphoribia L. It is one of the top ten oil crops in the world and is widely planted in the world. The main producing areas are India, China, Brazil and other countries, and its output accounts for More than 90% of the world's production. In my country, castor is mainly produced in Inner Mongolia, Jilin, Shandong and Shanxi. Castor bean has a high oil content, accounting for about 45-55% of the seed weight. The castor oil contained in it is the only natural fatty acid containing hydroxyl groups, which has special physical and chemical properties. Castor oil is an important chemical raw material, which is widely used in chemical industry, textile, light industry, medicine and other departments. It mainly produces high-grade lubricating oil, paint, coating, soap, ink, dyeing aid, plasticizer, polyurethane, emulsifier, etc. Because planting castor has a wide range of uses and high economic value, it occupies an important position in the national economy. Especially in today's world, oil is facing a crisis of exhaustion. Castor, as a plant source oil, has sustainable The unique and irreplaceable value of production is increasingly being valued by countries all over the world, and its industrial prospects are very broad.
蓖麻油的获得方式主要有机械压榨法和溶剂浸出法两种。机械压榨法包括冷榨法(液压压榨法)和热榨法(螺旋压榨法),但都存在出油率低的问题。溶剂浸出法是将蓖麻籽除杂、去壳、干燥、粉碎、溶剂浸出后,经过精制而得到成品蓖麻油。溶剂浸出法具有成本低、残油少、出油率高的特点。目前,油脂浸出过程常用的溶剂是石油醚和正己烷,但由于蓖麻油的特殊结构,使得石油醚和正己烷浸出蓖麻油的效率不高。申请号为CN101108975A的中国发明专利申请公开了一种采用甲醇浸出蓖麻油的方法。公开号为CN101684429A的中国发明专利申请采用乙醇浸出蓖麻油。上述方法虽然提高了蓖麻油的浸出率,但同时引入许多杂质,增加了蓖麻油精制处理成本。而且都需要加热,能耗高。因此,有必要开发更高效、节能的新的蓖麻油制备方法。There are two main ways to obtain castor oil: mechanical pressing and solvent extraction. Mechanical pressing methods include cold pressing (hydraulic pressing) and hot pressing (screw pressing), but both have the problem of low oil yield. The solvent extraction method is to remove impurities from castor beans, shell them, dry them, pulverize them, extract them with solvents, and then refine them to obtain the finished castor oil. The solvent leaching method has the characteristics of low cost, less residual oil and high oil yield. At present, petroleum ether and n-hexane are commonly used solvents in oil leaching process, but due to the special structure of castor oil, the efficiency of petroleum ether and n-hexane leaching castor oil is not high. The Chinese invention patent application whose application number is CN101108975A discloses a method for leaching castor oil with methanol. The Chinese invention patent application whose publication number is CN101684429A adopts ethanol to leaching castor oil. Though said method has improved the leaching rate of castor oil, introduces many impurities simultaneously, has increased the refining treatment cost of castor oil. And all need heating, energy consumption is high. Therefore, it is necessary to develop a new castor oil preparation method that is more efficient and energy-saving.
发明内容Contents of the invention
针对现有技术的不足,本发明提供一种新的利用溶剂浸出法制备蓖麻油的方法。该方法蓖麻油浸出率高,操作简单,适合工业化生产。Aiming at the deficiencies in the prior art, the invention provides a new method for preparing castor oil by solvent leaching. The method has high extraction rate of castor oil, simple operation and is suitable for industrial production.
为实现上述发明目的,本发明采取如下的技术方案:In order to realize the above-mentioned purpose of the invention, the present invention takes the following technical solutions:
一种蓖麻油的制备方法,包括蓖麻籽粉碎,以溶剂浸提,得到的混合油脱溶剂;所述溶剂为石油醚和乙醚组成的混合溶剂。A preparation method of castor oil comprises the steps of pulverizing castor beans, extracting with a solvent, and desolventizing the obtained mixed oil; the solvent is a mixed solvent composed of petroleum ether and diethyl ether.
优选的,本发明所述的制备方法,具体包括以下步骤:Preferably, the preparation method of the present invention specifically includes the following steps:
(1)蓖麻籽去壳、干燥、粉碎,得到蓖麻籽粉;(1) castor beans are shelled, dried and crushed to obtain castor bean powder;
(2)将步骤1得到的蓖麻籽粉放入容器中,按照所述质量体积比加入所述混合溶剂,搅拌浸提;(2) Put the castor bean powder obtained in step 1 into a container, add the mixed solvent according to the mass volume ratio, and stir and extract;
(3)将步骤2所得到的固-液混合物进行分离,混合油脱溶剂,精制或不精制,即得。(3) Separating the solid-liquid mixture obtained in step 2, desolventizing the mixed oil, refining or not refining, that is.
本发明所述的制备方法中,优选的,所述混合溶剂中石油醚和乙醚的体积比为2:8~8:2。更优选的,所述混合溶剂中石油醚和乙醚的体积比为6:4~8:2。In the preparation method of the present invention, preferably, the volume ratio of petroleum ether and diethyl ether in the mixed solvent is 2:8˜8:2. More preferably, the volume ratio of petroleum ether and diethyl ether in the mixed solvent is 6:4˜8:2.
本发明所述的制备方法中,优选的,蓖麻籽与所述混合溶剂的质量体积比为1:1~1:7。更优选的,蓖麻籽与所述混合溶剂的质量体积比为1:3~1:6。In the preparation method of the present invention, preferably, the mass volume ratio of castor beans and the mixed solvent is 1:1˜1:7. More preferably, the mass volume ratio of castor beans to the mixed solvent is 1:3˜1:6.
本发明所述的制备方法中,优选的,浸提1~3次,每次30~150min。其中浸提1次,优选浸提60~120min;或浸提2~3次,优选每次浸提30~90min。In the preparation method of the present invention, preferably, leaching is performed 1 to 3 times, each time for 30 to 150 minutes. Among them, leaching is done once, preferably for 60-120 minutes; or for 2-3 times, preferably for 30-90 minutes each time.
本发明所述的制备方法中,优选的,浸提时,用电动搅拌器搅拌,电动搅拌器的功率为50W,转速为2-8rpm。In the preparation method of the present invention, preferably, when leaching, stir with an electric stirrer, the power of the electric stirrer is 50W, and the rotation speed is 2-8rpm.
本发明所述利用混合溶剂制备蓖麻油的方法,一般在常温下进行。The method for preparing castor oil using mixed solvents of the present invention is generally carried out at normal temperature.
本发明优选采用真空脱溶法对混合油进行脱溶剂处理,所得溶剂回收循环使用,从而降低成本。In the present invention, the vacuum precipitating method is preferably used to desolventize the mixed oil, and the obtained solvent is recovered and recycled, thereby reducing the cost.
作为一个优选的实施方案,本发明提供一种蓖麻油的制备方法,具体包括以下步骤:As a preferred embodiment, the present invention provides a kind of preparation method of castor oil, specifically comprises the following steps:
(1)蓖麻籽除杂、去壳、干燥、粉碎,得到蓖麻籽粉;(1) Castor beans are removed from impurities, shelled, dried and crushed to obtain castor bean powder;
(2)将步骤1得到的蓖麻籽粉放入容器中,加入混合溶剂,常温下,电动搅拌器搅拌浸提1~3次,每次30~150min;其中,所述混合溶剂由体积比2:8~8:2的石油醚和乙醚构成,蓖麻籽粉和所述混合溶剂的质量体积比为1:1~1:7,电动搅拌器的功率为50W,转速为2-8rpm;(2) Put the castor bean powder obtained in step 1 into a container, add a mixed solvent, and stir and extract 1 to 3 times with an electric stirrer at room temperature, each time for 30 to 150 minutes; wherein, the mixed solvent is determined by volume ratio 2:8~8:2 petroleum ether and diethyl ether, the mass volume ratio of castor bean powder and the mixed solvent is 1:1~1:7, the power of the electric stirrer is 50W, and the speed is 2-8rpm;
(3)将步骤2所得到的固-液混合物进行分离,得到混合油和蓖麻粕;所述混合油真空脱溶剂,即得到蓖麻油;回收的溶剂循环使用,所述蓖麻粕干燥后脱毒作为饲料。(3) Separating the solid-liquid mixture obtained in step 2 to obtain mixed oil and castor meal; the mixed oil is vacuum desolvated to obtain castor oil; the recovered solvent is recycled, and the castor meal is dried Detoxification as feed.
作为一个更优选的实施方案,本发明提供一种蓖麻油的制备方法,具体包括以下步骤:As a more preferred embodiment, the present invention provides a kind of preparation method of castor oil, specifically comprises the following steps:
(1)蓖麻籽除杂、去壳、干燥、粉碎,得到蓖麻籽粉;(1) Castor beans are removed from impurities, shelled, dried and crushed to obtain castor bean powder;
(2)将步骤1得到的蓖麻籽粉放入容器中,加入混合溶剂,常温下,电动搅拌器搅拌浸提1次,浸提60~90min,或电动搅拌器搅拌浸提2~3次,每次30~90min;其中,所述混合溶剂由体积比6:4~8:2的石油醚和乙醚构成,蓖麻籽粉和所述混合溶剂的质量体积比为1:3~1:6,电动搅拌器的功率为50W,转速为2-8rpm;(2) Put the castor bean powder obtained in step 1 into a container, add a mixed solvent, and stir and leach once with an electric agitator at room temperature for 60-90 minutes, or 2-3 times with an electric agitator , each 30~90min; Wherein, described mixed solvent is made of sherwood oil and ether of volume ratio 6:4~8:2, and the mass volume ratio of castor bean powder and described mixed solvent is 1:3~1: 6. The power of the electric mixer is 50W, and the speed is 2-8rpm;
(3)将步骤2所得到的固-液混合物进行分离,得到混合油和蓖麻粕;所述混合油真空脱溶剂,即得到蓖麻油;回收的溶剂循环使用,所述蓖麻粕干燥后脱毒作为饲料。(3) Separating the solid-liquid mixture obtained in step 2 to obtain mixed oil and castor meal; the mixed oil is vacuum desolvated to obtain castor oil; the recovered solvent is recycled, and the castor meal is dried Detoxification as feed.
本发明所述蓖麻油的制备方法的工艺流程,见图1。The technical process of the preparation method of castor oil of the present invention, see Fig. 1.
本发明的另一个目的在于提供所述制备方法制备得到的蓖麻油。Another object of the present invention is to provide castor oil prepared by the preparation method.
本发明的有益效果:Beneficial effects of the present invention:
1、以石油醚和乙醚混合溶剂浸出蓖麻油,浸出率高。相同条件下,本发明所述的混合溶剂蓖麻油浸出率达到80.43%,分别是单一石油醚和单一正己烷的3.3倍和3.8倍,而甲醇、无水乙醇和无水乙醚的蓖麻油浸出率都在75%以下,低于本发明所述混合溶剂。1. The castor oil is leached with a mixed solvent of petroleum ether and ether, and the leaching rate is high. Under the same conditions, the castor oil leaching rate of the mixed solvent of the present invention reaches 80.43%, which is 3.3 times and 3.8 times that of single sherwood oil and single n-hexane respectively, while the castor oil leaching rates of methanol, dehydrated alcohol and anhydrous ether All below 75%, lower than the mixed solvent of the present invention.
2、本发明所述制备方法效率高,采用所述混合溶剂浸提1次,即可浸出80.43%的蓖麻油。2. The preparation method of the present invention has high efficiency, and 80.43% castor oil can be extracted by using the mixed solvent for leaching once.
3、本发明所述制备方法在常温下进行,无需加热,降低了能耗。3. The preparation method of the present invention is carried out at normal temperature without heating, which reduces energy consumption.
4、浸提时采用电动搅拌器搅拌,适合工业化生产。4. Electric stirrer is used for stirring during leaching, which is suitable for industrial production.
因此,本发明所述蓖麻油的制备方法是一种成本低、耗时短、浸出率高和浸出杂质少的蓖麻油浸出新方法。Therefore, the preparation method of castor oil of the present invention is a new castor oil leaching method with low cost, short time consumption, high leaching rate and few leaching impurities.
经过预实验发现,本发明所述混合溶剂的组成、蓖麻籽与混合溶剂的料液比和浸提时间是影响蓖麻油浸提效果的主要因素。因此,通过下面的实验对上述参数进行优选。It is found through preliminary experiments that the composition of the mixed solvent of the present invention, the solid-liquid ratio of castor beans and the mixed solvent and the extraction time are the main factors affecting the extraction effect of castor oil. Therefore, the above parameters are optimized through the following experiments.
1、混合溶剂的组成1. The composition of the mixed solvent
蓖麻籽粉10g放入容器中,加入石油醚(沸点60-90℃)-乙醚组成的混合溶剂,蓖麻籽重量与混合溶剂体积的比例为1:3,常温下,功率50W、转速为5rpm的电动搅拌器搅拌浸提1次,浸提120min;考察混合溶剂中乙醚含量不同时对蓖麻油浸提效果的影响,结果见表1。Put 10g of castor bean powder into a container, add a mixed solvent composed of petroleum ether (boiling point 60-90°C)-diethyl ether, the ratio of castor bean weight to mixed solvent volume is 1:3, at room temperature, the power is 50W, and the speed is The 5rpm electric stirrer stirred and extracted once for 120min; the influence of diethyl ether content in the mixed solvent on the extraction effect of castor oil was investigated, and the results are shown in Table 1.
表1乙醚含量不同对蓖麻油浸提效果的影响The influence of table 1 ether content different on castor oil extraction effect
表1的结果显示,乙醚的加入可以明显提高蓖麻油的浸出率,尤其是乙醚的体积百分含量为20%~80%时。但是乙醚极易挥发,混合溶剂中乙醚的含量过高,会带来安全隐患,不适合工业生产。故混合溶剂的组成优选为石油醚:乙醚=6:4~8:2;更优选的,石油醚:乙醚=7:3The results in Table 1 show that the addition of diethyl ether can significantly increase the leaching rate of castor oil, especially when the volume percentage of diethyl ether is 20% to 80%. However, ether is extremely volatile, and the content of ether in the mixed solvent is too high, which will bring potential safety hazards and is not suitable for industrial production. Therefore, the composition of the mixed solvent is preferably petroleum ether: ether = 6:4 ~ 8:2; more preferably, petroleum ether: ether = 7:3
2、混合溶剂的用量2. The amount of mixed solvent
蓖麻籽粉10g放入容器中,加入体积比为7:3的石油醚(沸程60-90℃)-乙醚组成的混合溶剂,常温下,功率50W、转速为5rpm的电动搅拌器搅拌浸提1次,浸提120min;考察混合溶剂用量对蓖麻油浸提效果的影响,结果见表2。Put 10g of castor bean powder into a container, add a mixed solvent composed of petroleum ether (boiling range 60-90°C)-diethyl ether with a volume ratio of 7:3, and stir with an electric stirrer with a power of 50W and a speed of 5rpm at room temperature. Extract 1 time, leaching 120min; Investigate the influence of the amount of mixed solvent on the extraction effect of castor oil, the results are shown in Table 2.
表2混合溶剂用量对蓖麻油浸提效果的影响The influence of table 2 mixed solvent dosage on castor oil extraction effect
表2的结果显示,增加混合溶剂的用量,可以提高蓖麻油的浸出率;但混合溶剂的体积在蓖麻籽重量的3倍以上时,体系达到平衡,蓖麻油浸出率基本稳定在45%左右。综合成本、效益等因素考虑,混合溶剂用量优选为:蓖麻籽重量与混合溶剂体积比为1:3~1:6。The results in Table 2 show that increasing the amount of mixed solvent can increase the leaching rate of castor oil; but when the volume of mixed solvent is more than 3 times the weight of castor beans, the system reaches equilibrium, and the leaching rate of castor oil is basically stable at about 45%. . Considering factors such as comprehensive cost and benefit, the dosage of the mixed solvent is preferably: the ratio of the weight of castor beans to the volume of the mixed solvent is 1:3-1:6.
3、浸提时间3. Extraction time
蓖麻籽粉10g放入容器中,加入体积比为7:3的石油醚(沸点60-90℃)-乙醚组成的混合溶剂,蓖麻籽重量与混合溶剂体积比为1:3,常温下,功率50W、转速为5rpm的电动搅拌器搅拌浸提1次;考察浸提时间对蓖麻油浸提效果的影响,结果见表3。Put 10g of castor bean powder into a container, add a mixed solvent composed of petroleum ether (boiling point 60-90°C)-diethyl ether with a volume ratio of 7:3, the ratio of the weight of castor beans to the volume of the mixed solvent is 1:3, at room temperature , power 50W, rotating speed is 5rpm electric stirrer stirring extraction 1 time; Investigate the influence of extraction time on castor oil extraction effect, the results are shown in Table 3.
表3浸提时间对蓖麻油浸提效果的影响The influence of table 3 extraction time on castor oil extraction effect
表3结果显示,30~60min范围内,延长浸提时间,可以显著提高蓖麻油的浸出率;但是1次浸提60min以上,浸提时间的延长基本对蓖麻油浸出率没有影响。因此,综合考虑成本、效益等因素,浸提1次,浸提时间优选为60~90min。The results in Table 3 show that within the range of 30 to 60 minutes, prolonging the extraction time can significantly increase the extraction rate of castor oil; however, the extension of the extraction time basically has no effect on the extraction rate of castor oil if the extraction time exceeds 60 minutes. Therefore, considering cost, benefit and other factors comprehensively, the leaching time is preferably 60-90 minutes for one extraction.
4、浸提次数对浸出效果的影响4. The influence of extraction times on the extraction effect
蓖麻籽粉0.5Kg放入容器中,加入体积比为7:3的石油醚(沸点60-90℃)-乙醚组成的混合溶剂,蓖麻籽重量与混合溶剂体积比为1:3,常温下,功率50W、转速为5rpm的电动搅拌器搅拌浸提,每次浸提60min;考察不同浸提次数对蓖麻油浸出率影响,结果见表4和图2。Put 0.5Kg of castor bean powder into a container, add a mixed solvent composed of petroleum ether (boiling point 60-90°C)-diethyl ether with a volume ratio of 7:3, the ratio of the weight of castor beans to the volume of the mixed solvent is 1:3, and store at room temperature The electric stirrer with a power of 50W and a rotating speed of 5rpm was used for stirring and leaching, each time for 60 minutes; the influence of different leaching times on the leaching rate of castor oil was investigated, and the results are shown in Table 4 and Figure 2.
表4浸取次数对浸出效果的影响The impact of table 4 leaching times on leaching effect
表4和图2显示,采用石油醚和乙醚构成的混合溶剂,搅拌浸提1次60min,可浸提出大部分的蓖麻油,浸提两次基本能浸出全部蓖麻油。Table 4 and Figure 2 show that, using a mixed solvent composed of petroleum ether and diethyl ether, stirring and leaching once for 60 minutes, most of the castor oil can be leached out, and almost all the castor oil can be leached out twice.
总之,通过上面的研究,本发明提供一种蓖麻油浸提的优选工艺:In a word, by above research, the present invention provides a kind of optimal process of castor oil leaching:
蓖麻籽粉碎,放入容器中,加入体积比6:4~8:2的石油醚和乙醚组成的混合溶剂,蓖麻籽粉和所述混合溶剂的质量体积比为1:3~1:6,常温下,电动搅拌器搅拌浸提1次,浸提60~90min;The castor beans are pulverized, put into a container, add a mixed solvent composed of petroleum ether and ether with a volume ratio of 6:4 to 8:2, and the mass volume ratio of the castor beans powder to the mixed solvent is 1:3 to 1: 6. At room temperature, stir and extract once with an electric stirrer for 60-90 minutes;
更优选的工艺条件是:More preferred process conditions are:
蓖麻籽粉碎,放入容器中,加入体积比7:3的石油醚和乙醚组成的混合溶剂,蓖麻籽粉和所述混合溶剂的质量体积比为1:3~1:6,常温下,电动搅拌器搅拌浸提1次,浸提60~90min。Pulverize castor beans, put them in a container, add a mixed solvent composed of petroleum ether and diethyl ether with a volume ratio of 7:3, the mass volume ratio of castor bean powder and the mixed solvent is 1:3~1:6, at room temperature , stirring and extracting once with an electric stirrer, and extracting for 60-90 minutes.
为了浸提得更充分,可以浸提2~3次,每次30~90min。In order to extract more fully, it can be extracted 2 to 3 times, 30 to 90 minutes each time.
附图说明Description of drawings
以下,结合附图来详细说明本发明的实施方案,其中:Below, describe embodiment of the present invention in detail in conjunction with accompanying drawing, wherein:
图1显示了本发明所述蓖麻油制备方法的工艺流程图。Fig. 1 has shown the process flow chart of castor oil preparation method of the present invention.
图2显示了浸提次数与蓖麻油浸出率的关系。Figure 2 shows the relationship between the number of extractions and the extraction rate of castor oil.
图3显示了对比例中不同溶剂的蓖麻油浸出率。Fig. 3 has shown the castor oil leaching rate of different solvents in comparative example.
具体实施方式Detailed ways
以下参照具体的实施例来说明本发明。本领域技术人员能够理解,这些实施例仅用于说明本发明,其不以任何方式限制本发明的范围。The present invention will be described below with reference to specific examples. Those skilled in the art can understand that these examples are only used to illustrate the present invention and do not limit the scope of the present invention in any way.
下述实施例中的实验方法,如无特殊说明,均为常规方法。下述实施例中所用的药材原料、试剂材料等,如无特殊说明,均为市售购买产品。下述实施例中所用的石油醚沸程为60~90℃。The experimental methods in the following examples are conventional methods unless otherwise specified. The medicinal raw materials, reagent materials, etc. used in the following examples are all commercially available products unless otherwise specified. The petroleum ether used in the following examples has a boiling range of 60-90°C.
实施例1Example 1
(1)蓖麻籽0.5Kg进行预处理:除去杂质和病虫害、去壳、干燥、粉碎,得到蓖麻籽粉;(1) Pretreatment of 0.5Kg castor beans: removing impurities and pests, shelling, drying, and crushing to obtain castor bean powder;
(2)将步骤1得到的蓖麻籽粉放入容器中,加入体积比为9:1的石油醚-乙醚混合溶剂1.5L(料液比1:3);常温下电动搅拌器搅拌浸提1次,浸提60min;电动搅拌器的功率为50W,转速为2rpm;(2) Put the castor bean powder obtained in step 1 into a container, add 1.5L of petroleum ether-diethyl ether mixed solvent with a volume ratio of 9:1 (solid-liquid ratio 1:3); stir and extract with an electric stirrer at room temperature 1 time, leaching for 60 minutes; the power of the electric stirrer is 50W, and the speed is 2rpm;
(3)将步骤2所得到的固-液混合物过滤分离,得到混合油和蓖麻粕;所述混合油真空脱溶剂,得到蓖麻油0.1557Kg,浸出率58.05%。(3) The solid-liquid mixture obtained in step 2 was separated by filtration to obtain mixed oil and castor meal; the mixed oil was desolvated in vacuum to obtain 0.1557Kg castor oil with an extraction rate of 58.05%.
实施例2Example 2
蓖麻籽0.5Kg,采用与实施例1相似的制备方法;不同之处在于:Castor bean 0.5Kg, adopts the preparation method similar to embodiment 1; Difference is:
混合溶剂中石油醚和乙醚的体积比为7:3,电动搅拌器的转速为4rpm。The volume ratio of petroleum ether and diethyl ether in the mixed solvent was 7:3, and the rotation speed of the electric stirrer was 4 rpm.
制备得到蓖麻油0.2158Kg,浸出率80.43%。The castor oil 0.2158Kg was prepared, and the leaching rate was 80.43%.
实施例3Example 3
蓖麻籽0.5Kg,采用与实施例1相似的制备方法;不同之处在于:Castor bean 0.5Kg, adopts the preparation method similar to embodiment 1; Difference is:
混合溶剂中石油醚和乙醚的体积比为5:5,电动搅拌器的转速为5rpm。The volume ratio of petroleum ether and diethyl ether in the mixed solvent is 5:5, and the rotation speed of the electric stirrer is 5 rpm.
制备得到蓖麻油0.1903kg,浸出率70.95%。0.1903 kg of castor oil was prepared, and the leaching rate was 70.95%.
实施例4Example 4
蓖麻籽0.5Kg,采用与实施例1相似的制备方法;不同之处在于:Castor bean 0.5Kg, adopts the preparation method similar to embodiment 1; Difference is:
加入混合溶剂0.5L(料液比1:1),其中石油醚和乙醚的体积比为7:3,电动搅拌器的转速为5rpm。Add 0.5 L of mixed solvent (solid-liquid ratio 1:1), wherein the volume ratio of petroleum ether and diethyl ether is 7:3, and the rotation speed of the electric stirrer is 5 rpm.
制备得到蓖麻油0.092Kg,浸出率34.23%。Prepare castor oil 0.092Kg, leaching rate 34.23%.
实施例5Example 5
蓖麻籽0.5Kg,采用与实施例1相似的制备方法;不同之处在于:Castor bean 0.5Kg, adopts the preparation method similar to embodiment 1; Difference is:
加入混合溶剂2.5L(料液比1:5),其中混合溶剂中石油醚和乙醚的体积比为7:3,电动搅拌器的转速为8rpm。Add 2.5 L of mixed solvent (solid-liquid ratio 1:5), wherein the volume ratio of petroleum ether and diethyl ether in the mixed solvent is 7:3, and the rotation speed of the electric stirrer is 8 rpm.
制备得到蓖麻油0.2237kg,浸出率83.16%。0.2237 kg of castor oil was prepared, and the leaching rate was 83.16%.
实施例6Example 6
蓖麻籽0.5Kg,采用与实施例1相似的制备方法;不同之处在于:Castor bean 0.5Kg, adopts the preparation method similar to embodiment 1; Difference is:
加入混合溶剂3.5L(料液比1:7),混合溶剂中石油醚和乙醚的体积比为7:3,浸提150min,电动搅拌器的转速为5rpm。Add 3.5L of mixed solvent (solid-liquid ratio 1:7), the volume ratio of petroleum ether and diethyl ether in the mixed solvent is 7:3, leaching for 150min, the speed of electric stirrer is 5rpm.
制备得到蓖麻油0.2316Kg,浸出率86.35%。Prepare castor oil 0.2316Kg, leaching rate 86.35%.
实施例7Example 7
蓖麻籽0.5Kg,采用与实施例1相似的制备方法;不同之处在于:Castor bean 0.5Kg, adopts the preparation method similar to embodiment 1; Difference is:
混合溶剂中石油醚和乙醚的体积比为7:3,浸提1次,浸提30min,电动搅拌器的转速为5rpm。The volume ratio of petroleum ether and diethyl ether in the mixed solvent is 7:3, leaching once, leaching 30min, the speed of the electric stirrer is 5rpm.
制备得到蓖麻油0.1821Kg,浸出率68.27%。Prepare castor oil 0.1821Kg, leaching rate 68.27%.
实施例8Example 8
蓖麻籽0.5Kg,采用与实施例1相似的制备方法;不同之处在于:Castor bean 0.5Kg, adopts the preparation method similar to embodiment 1; Difference is:
混合溶剂中石油醚和乙醚的体积比为7:3,浸提2次,每次浸提60min,电动搅拌器的转速为5rpm。The volume ratio of petroleum ether and diethyl ether in the mixed solvent is 7:3, leaching twice, each leaching 60min, the rotating speed of the electric stirrer is 5rpm.
制备得到蓖麻油0.2464Kg,浸出率91.84%。Prepare castor oil 0.2464Kg, leaching rate 91.84%.
实施例9Example 9
蓖麻籽0.5Kg,采用与实施例1相似的制备方法;不同之处在于:Castor bean 0.5Kg, adopts the preparation method similar to embodiment 1; Difference is:
混合溶剂中石油醚和乙醚的体积比为7:3,浸提3次,每次浸提60min,电动搅拌器的转速为5rpm。The volume ratio of petroleum ether and diethyl ether in the mixed solvent is 7:3, leaching 3 times, each leaching 60min, the rotating speed of the electric stirrer is 5rpm.
制备得到蓖麻油0.2487Kg,浸出率92.73%。The castor oil 0.2487Kg was prepared, and the leaching rate was 92.73%.
实施例10Example 10
蓖麻籽0.5Kg,采用与实施例1相似的制备方法;不同之处在于:Castor bean 0.5Kg, adopts the preparation method similar to embodiment 1; Difference is:
混合溶剂中石油醚和乙醚的体积比为7:3,浸提1次,每次浸提150min,电动搅拌器的转速为5rpm。The volume ratio of petroleum ether and diethyl ether in the mixed solvent is 7:3, leaching once, each leaching 150min, the speed of the electric stirrer is 5rpm.
制备得到蓖麻油0.2163Kg,浸出率80.63%。Prepare castor oil 0.2163Kg, leaching rate 80.63%.
对比例不同溶剂的浸出效果对比Comparison of the leaching effects of different solvents in the comparative example
蓖麻籽0.5Kg,采用与实施例1相似的制备方法;不同之处在于:Castor bean 0.5Kg, adopts the preparation method similar to embodiment 1; Difference is:
溶剂分别采用正己烷、石油醚、甲醇、无水乙醇、无水乙醚和混合溶剂(混合溶剂中石油醚和乙醚的体积比为7:3),浸提1次,浸提120min,电动搅拌器的转速为5rpm。考察不同溶剂对浸出率影响,结果见表5和图3。The solvents are n-hexane, petroleum ether, methanol, absolute ethanol, anhydrous ether and a mixed solvent (the volume ratio of petroleum ether and ether in the mixed solvent is 7:3), leached once for 120min, and the electric stirrer The rotation speed is 5rpm. The influence of different solvents on the leaching rate was investigated, and the results are shown in Table 5 and Figure 3.
表5不同溶剂的浸出效果The leaching effect of different solvents in table 5
表5和图3显示,石油醚-乙醚(7:3)构成的混合溶剂对蓖麻油的浸出率最高,高于其它极性或非极性的单溶剂。Table 5 and Figure 3 show that the mixed solvent composed of petroleum ether-diethyl ether (7:3) has the highest leaching rate of castor oil, which is higher than other polar or non-polar single solvents.
总之,本发明采用所述石油醚和乙醚构成的混合溶剂,蓖麻油的浸出率高。本发明所述蓖麻油的制备方法,操作简便,能耗小,适合工业化。In a word, the present invention adopts the mixed solvent composed of the petroleum ether and ether, and the leaching rate of castor oil is high. The preparation method of the castor oil of the invention has the advantages of simple and convenient operation, low energy consumption and is suitable for industrialization.
以上对本发明具体实施方式的描述并不限制本发明,本领域技术人员可以根据本发明作出各种改变或变形,只要不脱离本发明的精神,均应属于本发明所附权利要求的范围。The above description of the specific embodiments of the present invention does not limit the present invention, and those skilled in the art can make various changes or deformations according to the present invention, as long as they do not depart from the spirit of the present invention, all should belong to the scope of the appended claims of the present invention.
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