CN103173285B - A method and device for extracting active ingredients in orange peel using a high-pressure solvent - Google Patents
A method and device for extracting active ingredients in orange peel using a high-pressure solvent Download PDFInfo
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Abstract
本发明公开了一种利用高压溶剂提取橘皮中有效成分的方法及装置，该方法包括将新鲜橘皮烘干后，用粉碎机粉碎，然后利用该提取装置以75%乙醇对其进行提取，提取条件为萃取温度85-95℃，萃取压力4-7Mpa，分离温度80-85℃，萃取时间1-2h。本发明对橘皮中的有效成分提取更完全，提取速度更快，溶剂用量小，能耗低。本发明所涉及的提取装置操作简单，设备造价低，有利于规模化生产的推广。
The invention discloses a method and device for extracting active ingredients in orange peel by using a high-pressure solvent. The method includes drying the fresh orange peel, crushing it with a pulverizer, and then using the extraction device to extract it with 75% ethanol. The extraction conditions are extraction temperature 85-95°C, extraction pressure 4-7Mpa, separation temperature 80-85°C, extraction time 1-2h. The invention extracts the active ingredients in orange peel more completely, has faster extraction speed, less solvent consumption and low energy consumption. The extraction device involved in the present invention has simple operation, low equipment cost, and is beneficial to the popularization of large-scale production.
Description
技术领域 technical field
本发明属于植物提取分离技术领域，具体而言，涉及一种利用高压溶剂提取橘皮中有效成分的方法及装置。The invention belongs to the technical field of plant extraction and separation, and in particular relates to a method and a device for extracting active ingredients in orange peel by using a high-pressure solvent.
背景技术 Background technique
柑桔为芸香科植物，是世界上最重要的商品水果。柑桔果皮在医学上称陈皮，柑桔皮中除了含有丰富的芳香油、果胶、色素外，还含有橙皮苷、新橙皮苷、桔皮素、川陈皮素、二氢川陈皮等黄酮类化合物。黄酮类化合物是植物经光合作用产生的一大类植物的次生代谢产物，作为一种功能成分，其主要作用有抗肿瘤、延缓衰老、增强心血管功能、增强免疫力、调解内分泌系统、护肝、抗炎、抗过敏、抑菌、抗病毒等。中国是柑桔生产大国，种植面积大，产量高，目前桔皮除部分用于中药和食品加工外，每年都有相当大的部分还未得到开发利用而被丢弃，既造成资源的浪费，也造成环境的污染。Citrus is a Rutaceae plant and is the most important commercial fruit in the world. Citrus peel is called tangerine peel in medicine. In addition to rich aromatic oil, pectin and pigment, citrus peel also contains hesperidin, neohesperidin, orange peel, nobietin, dihydrotangerine peel, etc. Flavonoids. Flavonoids are secondary metabolites of a large class of plants produced by photosynthesis. As a functional component, their main functions are anti-tumor, anti-aging, enhancing cardiovascular function, enhancing immunity, mediating the endocrine system, protecting the Liver, anti-inflammatory, anti-allergic, antibacterial, antiviral, etc. China is a big country of citrus production, with large planting area and high output. At present, citrus peels are partially used in traditional Chinese medicine and food processing, but a considerable part has not been developed and utilized and is discarded every year, which not only causes waste of resources, but also cause environmental pollution.
现在提取橘皮中有效成分的方法有水蒸汽蒸馏法、有机溶剂萃取法、冷榨法、超临界二氧化碳萃取法等方法。其中水蒸气蒸馏法，冷榨法只能提取橘皮中的芳香油类物质，产品出率极低。超临界二氧化碳萃取法是目前公认比较理想的工艺技术，具有不破坏有效成分，收率高、产品品质稳定的特点，但是存在设备价格昂贵，制作成本高的缺点，无法规模化生产。传统的有机溶剂萃取法，可以将橘皮中的有效成分都提取出来，但是该方法需要消耗大量的溶剂，相应地后期蒸发浓缩环节能耗巨大，同时该法还存在提取效率低、提取时间长等缺点。The methods for extracting active ingredients in orange peels include steam distillation, organic solvent extraction, cold pressing, supercritical carbon dioxide extraction and other methods. Among them, the steam distillation method and the cold pressing method can only extract the aromatic oil substances in the orange peel, and the product yield is extremely low. Supercritical carbon dioxide extraction is currently recognized as an ideal technology. It has the characteristics of not destroying active ingredients, high yield, and stable product quality. However, it has the disadvantages of expensive equipment and high production costs, and cannot be mass-produced. The traditional organic solvent extraction method can extract all the active ingredients in the orange peel, but this method needs to consume a large amount of solvent, and accordingly the energy consumption in the later stage of evaporation and concentration is huge. At the same time, this method also has low extraction efficiency and long extraction time. and other shortcomings.
发明内容 Contents of the invention
鉴于现有技术的不足，本发明的目的在于提供一种利用高压溶剂提取橘皮中有效成分的新工艺，同时提供涉及该工艺的提取装置。In view of the deficiencies in the prior art, the purpose of the present invention is to provide a new process for extracting active ingredients in orange peel using a high-pressure solvent, and provide an extraction device related to the process.
为了实现本发明的目的，发明人通过大量试验研究和探索，最终获得了如下技术方案：In order to achieve the purpose of the present invention, the inventor finally obtained the following technical solutions through a large number of experimental researches and explorations:
一种利用高压溶剂提取橘皮中有效成分的装置，它包括萃取罐、蒸发浓缩和冷凝组合塔、溶剂中转罐和容积泵，萃取罐的上部与蒸发浓缩和冷凝组合塔的下部连接，蒸发浓缩和冷凝组合塔的上部与溶剂中转罐的上部连接，溶剂中转罐的下部通过容积泵与萃取罐的连接，形成循环管路；萃取罐外壁、蒸发浓缩和冷凝组合塔的下部外壁设置有蒸汽循环装置，蒸发浓缩和冷凝组合塔的上部外壁设置有冷却水循环装置，萃取罐设置有调压装置。A device for extracting active ingredients in orange peel with a high-pressure solvent, which includes an extraction tank, a combination tower of evaporative concentration and condensation, a solvent transfer tank and a positive displacement pump, the upper part of the extraction tank is connected with the lower part of the combined tower of evaporative concentration and condensation, and the evaporative concentration The upper part of the combined condensing tower is connected to the upper part of the solvent transfer tank, and the lower part of the solvent transfer tank is connected to the extraction tank through a positive displacement pump to form a circulation pipeline; the outer wall of the extraction tank and the lower outer wall of the evaporative concentration and condensation combined tower are provided with steam circulation device, the upper outer wall of the combined evaporative concentration and condensation tower is provided with a cooling water circulation device, and the extraction tank is provided with a pressure regulating device.
一种利用高压溶剂提取橘皮中有效成分的方法，其步骤如下：A method utilizing high-pressure solvent to extract active ingredients in orange peel, the steps are as follows:
（1）将新鲜橘皮烘干，粉碎机粉碎；(1) Dry the fresh orange peel and pulverize it with a grinder;
（2）在密闭的提取罐中装入粉碎好的物料，然后加入75%的乙醇，加热维持提取罐的温度为85-95℃，同时控制提取罐的压力为4-7Mpa，提取1-2h，分离后得提取液；(2) Put crushed materials in a closed extraction tank, then add 75% ethanol, heat to maintain the temperature of the extraction tank at 85-95°C, and control the pressure of the extraction tank at 4-7Mpa, extract for 1-2h , to obtain the extract after separation;
（3）80-85℃浓缩提取液，得橘皮提取物。(3) Concentrate the extract at 80-85°C to obtain orange peel extract.
上述利用高压溶剂提取橘皮中有效成分的方法，其中步骤（1）中新鲜橘皮在55-60℃下烘干，用粉碎机粉碎后过20目筛网。In the method for extracting active ingredients in orange peels with a high-pressure solvent, the fresh orange peels in step (1) are dried at 55-60° C., pulverized by a pulverizer and passed through a 20-mesh sieve.
上述利用高压溶剂提取橘皮中有效成分的方法，其中步骤（2）中提取罐的温度为90℃，压力为5Mpa。In the above-mentioned method for extracting active ingredients in orange peel by using a high-pressure solvent, the temperature of the extraction tank in step (2) is 90°C and the pressure is 5Mpa.
上述利用高压溶剂提取橘皮中有效成分的方法，其中步骤（3）中浓缩提取液的温度优选为85℃。In the above-mentioned method of extracting active ingredients in orange peel with a high-pressure solvent, the temperature of the concentrated extract in step (3) is preferably 85°C.
一种根据上述装置提取橘皮中有效成分的方法，其特征在于包括如下步骤：A method for extracting active ingredients in tangerine peel according to the above-mentioned device, is characterized in that comprising the steps:
（1）将新鲜橘皮烘干，粉碎机粉碎；(1) Dry the fresh orange peel and pulverize it with a grinder;
（2）将萃取罐装满粉碎好的物料，开启容积泵，利用容积泵由溶剂中转罐中向萃取罐打入75%乙醇，同时通过蒸汽循环装置对萃取罐和蒸发浓缩和冷凝组合塔加温，使萃取罐的萃取温度维持在85-95℃，蒸发浓缩和冷凝组合塔的浓缩温度维持在80-85℃，控制调压装置使萃取罐的萃取压力维持在4-7Mpa，动态萃取1-2h；(2) Fill the extraction tank with crushed materials, turn on the positive displacement pump, and use the positive displacement pump to inject 75% ethanol from the solvent transfer tank into the extraction tank, and at the same time, add 75% ethanol to the extraction tank and the combination tower of evaporation concentration and condensation through the steam circulation device. Temperature, keep the extraction temperature of the extraction tank at 85-95°C, maintain the concentration temperature of the combined evaporative concentration and condensation tower at 80-85°C, control the pressure regulating device to maintain the extraction pressure of the extraction tank at 4-7Mpa, dynamic extraction 1 -2h;
（3）萃取结束后，关闭容积泵，开启调压装置泄压，继续对萃取罐加温回收溶剂，至蒸发浓缩和冷凝塔中无溶剂流出时，关闭蒸汽循环装置，将橘皮渣泄出；(3) After the extraction, turn off the positive displacement pump, turn on the pressure regulating device to release the pressure, continue to heat the extraction tank to recover the solvent, and when there is no solvent flowing out from the evaporation and condensation tower, turn off the steam circulation device and release the orange peel ;
（4）从蒸发浓缩和冷凝组合塔下部得含有橘皮有效成分的提取物。(4) Obtain the extract containing the active ingredients of orange peel from the lower part of the evaporative concentration and condensation combined tower.
上述提取橘皮中有效成分的方法，其中步骤（1）中新鲜橘皮在55-60℃下烘干，用粉碎机粉碎后过20目筛网。The above method for extracting active ingredients in orange peels, wherein in step (1), the fresh orange peels are dried at 55-60°C, pulverized by a pulverizer and passed through a 20-mesh sieve.
上述提取橘皮中有效成分的方法，其中步骤（2）中萃取罐的萃取温度为90℃，萃取压力为5Mpa。In the above method for extracting active ingredients in orange peel, the extraction temperature of the extraction tank in step (2) is 90°C, and the extraction pressure is 5Mpa.
上述提取橘皮中有效成分的方法，其中步骤（2）中提取橘皮的萃取时间优选为90Min。In the above method for extracting active ingredients in orange peel, the extraction time for extracting orange peel in step (2) is preferably 90 Min.
上述提取橘皮中有效成分的方法，其中步骤（2）中蒸发浓缩和冷凝组合塔的浓缩温度优选为85℃。In the above-mentioned method for extracting active ingredients in orange peel, the concentration temperature of the combination tower of evaporative concentration and condensation in step (2) is preferably 85°C.
本发明提取橘皮中有效成分的原理是：以高于溶剂沸点的温度对溶剂进行加温，同时控制溶剂的压力，使溶剂在该温度下仍然保持液体状态。令人意想不到的是，在高压状态下的溶剂与常压下的溶剂相比，既可以对物料中有效成分有更高的溶解能力，其传质与扩散能力也有很大的提高，可以更有效、快速地把有效成分从物料中分离提取出来。The principle of extracting active ingredients in the orange peel of the present invention is: heating the solvent at a temperature higher than the boiling point of the solvent, and simultaneously controlling the pressure of the solvent so that the solvent remains in a liquid state at the temperature. Surprisingly, compared with the solvent under normal pressure, the solvent under high pressure can not only have a higher dissolving ability for the active ingredients in the material, but also have a greatly improved mass transfer and diffusion ability, which can be more effective , Quickly separate and extract the active ingredients from the material.
本发明所涉及的提取装置主要由萃取罐、溶剂中转罐、蒸发浓缩和冷凝组合塔及容积泵四部分组成。整个提取过程均在密闭环境中进行，避免了有机溶剂对人体的伤害，蒸发浓缩设备和冷凝设备合并为一套设备，减少了占地空间和设备的投入，利用溶剂中转罐可以使溶剂循环重复使用，减少了溶剂的消耗及不必要的浪费。The extraction device involved in the present invention is mainly composed of four parts: an extraction tank, a solvent transfer tank, a combination tower of evaporation concentration and condensation, and a positive displacement pump. The whole extraction process is carried out in a closed environment, which avoids the harm of organic solvents to the human body. The evaporation concentration equipment and condensation equipment are combined into one set of equipment, which reduces the investment in space and equipment. The use of solvent transfer tanks can make the solvent cycle repeated. use, reducing solvent consumption and unnecessary waste.
本发明高压溶剂提取橘皮中有效成分的工艺及装置与常规有机溶剂萃取法及装置相比，具有以下优势：Compared with conventional organic solvent extraction method and device, the process and device for extracting active ingredients in orange peel by high-pressure solvent of the present invention have the following advantages:
（1）对橘皮中的有效成分提取更完全，提取速度更快。(1) The active ingredients in the orange peel are extracted more completely and the extraction speed is faster.
（2）萃取溶剂循环利用，溶剂用量小，能耗低。(2) The extraction solvent is recycled, the solvent consumption is small, and the energy consumption is low.
（3）提取装置操作简单，设备造价低。(3) The extraction device is easy to operate and the equipment cost is low.
（4）不仅适用于橘皮中有效成分的提取，同时还可以更换溶剂用于其他天然植物有效成分的提取，非常有利于规模化生产的推广。(4) It is not only suitable for the extraction of active ingredients in orange peel, but also can replace the solvent for the extraction of other natural plant active ingredients, which is very conducive to the promotion of large-scale production.
附图说明 Description of drawings
图为本发明提取橘皮中有效成分的装置示意图；其中：1-萃取罐，2-蒸发浓缩和冷凝组合塔，3-溶剂中转罐，4-容积泵。The figure is a schematic diagram of the device for extracting active ingredients in orange peel of the present invention; wherein: 1-extraction tank, 2-evaporation concentration and condensation combined tower, 3-solvent transfer tank, 4-volume pump.
具体实施方式 Detailed ways
下面结合附图对本发明的工艺及操作方法作进一步阐述：Below in conjunction with accompanying drawing, technology and operation method of the present invention are further elaborated:
将新鲜橘皮在55-60℃下烘干后，用粉碎机粉碎过20目筛网，粉碎好后装入萃取罐①中，把75%乙醇由溶剂中转罐③上方的阀门倒入，加入量占中转罐体积的90%，关闭萃取罐与蒸发浓缩和冷凝组合塔②连接的调压阀，开启容积泵④，将溶剂中转罐中的溶剂由萃取罐下方泵入，同时开启萃取罐与蒸发浓缩和冷凝组合塔下部的蒸汽阀门，开启蒸发浓缩和冷凝组合塔上部的冷却水阀门，调节蒸汽阀门，使萃取罐温度维持在85-95℃，蒸发浓缩塔温度维持在80-85℃,控制调压阀使萃取罐压力维持在4-7Mpa，在此条件下带有橘皮有效成分的溶剂由萃取罐上端流入蒸发浓缩和冷凝组合塔，通过蒸汽加温，溶剂汽化与橘皮提取物分离，汽化后的溶剂升至蒸发浓缩和冷凝组合塔上部，由冷却水冷却变为液态后回流至溶剂中转罐中，通过容积泵继续泵入萃取罐循环使用，萃取结束后，关闭容积泵，完全开启调压阀泄压，继续对萃取罐加温回收溶剂，由视窗观察冷凝塔中无溶剂流出时，关闭蒸汽阀门及冷却水阀门，打开萃取罐将橘皮渣泄出。开启蒸发浓缩和冷凝组合塔下方阀门，用接受桶将橘皮提取物接出。After drying the fresh orange peel at 55-60°C, crush it through a 20-mesh screen with a pulverizer, put it into the extraction tank ① after crushing, pour 75% ethanol from the valve above the
实施例1Example 1
将新鲜橘皮在55℃下烘干，用粉碎机粉碎后过20目筛网。取2500g物料装入萃取罐，开启容积泵，利用容积泵由溶剂中转罐中向萃取罐打入75%的乙醇，同时开启蒸汽阀门对萃取罐和蒸发浓缩塔加温，蒸发浓缩塔温度维持在80-85℃，控制调压阀使萃取罐压力维持在5Mpa，萃取温度控制在85℃、90℃、95℃分别萃取90min。萃取结束后，关闭容积泵，开启调压阀泄压，继续对萃取罐加温回收溶剂，至冷凝塔中无溶剂流出时，关闭蒸汽阀门，将橘皮渣泄出。用接受桶从分离罐下方获得含有橘皮有效成分的提取物。称重分别获得橘皮提取物75g，90g，93g，出率分别为3.00%，3.60%，3.72%。Dry the fresh orange peel at 55°C, crush it with a pulverizer and pass it through a 20-mesh sieve. Take 2500g of material into the extraction tank, turn on the positive displacement pump, use the positive displacement pump to inject 75% ethanol from the solvent transfer tank into the extraction tank, and open the steam valve at the same time to heat the extraction tank and the evaporative concentration tower. The temperature of the evaporative concentration tower is maintained at 80-85°C, control the pressure regulating valve to maintain the pressure of the extraction tank at 5Mpa, and control the extraction temperature at 85°C, 90°C, and 95°C for 90 minutes respectively. After the extraction, close the positive displacement pump, open the pressure regulating valve to release the pressure, continue to heat the extraction tank to recover the solvent, and when no solvent flows out from the condensation tower, close the steam valve to release the orange peel residue. Obtain the extract containing the active ingredient of orange peel from the bottom of the separation tank with a receiving barrel. Weighing obtains orange peel extract 75g, 90g, 93g respectively, and yield is respectively 3.00%, 3.60%, 3.72%.
由上述实例可以看出，橘皮提取率随萃取温度升高而升高，但是当萃取温度升至95℃时，出率提高不大，因此从能耗角度考虑，选择90℃为优选萃取温度。It can be seen from the above examples that the extraction rate of orange peel increases with the increase of the extraction temperature, but when the extraction temperature rises to 95°C, the yield does not increase much, so from the perspective of energy consumption, 90°C is selected as the optimal extraction temperature .
实施例2Example 2
将新鲜橘皮在55℃下烘干，用粉碎机粉碎后过20目筛网。取2500g物料装入萃取罐，开启容积泵，利用容积泵由溶剂中转罐中向萃取罐打入75%的乙醇，同时开启蒸汽阀门对萃取罐和蒸发浓缩塔加温，蒸发浓缩塔温度维持在80-85℃， 萃取温度控制在90℃，控制调压阀使萃取罐压力维持在5Mpa、6Mpa、7Mpa分别萃取90min。萃取结束后，关闭容积泵，开启调压阀泄压，继续对萃取罐加温回收溶剂，至冷凝塔中无溶剂流出时，关闭蒸汽阀门，将橘皮渣泄出。用接受桶从分离罐下方获得含有橘皮有效成分的提取物。称重分别获得橘皮提取物89g，91g，90g，出率分别为3.56%，3.64%，3.60%。Dry the fresh orange peel at 55°C, crush it with a pulverizer and pass it through a 20-mesh sieve. Take 2500g of material into the extraction tank, turn on the positive displacement pump, use the positive displacement pump to inject 75% ethanol from the solvent transfer tank into the extraction tank, and open the steam valve at the same time to heat the extraction tank and the evaporative concentration tower. The temperature of the evaporative concentration tower is maintained at 80-85°C, the extraction temperature is controlled at 90°C, and the pressure regulating valve is controlled to maintain the pressure of the extraction tank at 5Mpa, 6Mpa, and 7Mpa for 90min respectively. After the extraction, close the positive displacement pump, open the pressure regulating valve to release the pressure, continue to heat the extraction tank to recover the solvent, and when no solvent flows out from the condensation tower, close the steam valve to release the orange peel residue. Obtain the extract containing the active ingredient of orange peel from the bottom of the separation tank with a receiving barrel. Weighing obtains orange peel extract 89g, 91g, 90g respectively, and yield is respectively 3.56%, 3.64%, 3.60%.
由上述实例可以看出，橘皮提取率与萃取压力变化关系不大，这是因为只要在一定压力下保持溶剂为液态，其溶解能力与压力无关，因此从设备成本方面考虑，选择5Mpa为优选萃取温度。As can be seen from the above examples, the extraction rate of orange peel has little to do with the change in extraction pressure. This is because as long as the solvent is kept in a liquid state under a certain pressure, its dissolving power has nothing to do with pressure. Therefore, considering the equipment cost, it is preferred to select 5Mpa Extraction temperature.
实施例3Example 3
将新鲜橘皮在55℃下烘干，用粉碎机粉碎后过20目筛网。取2500g物料装入萃取罐，开启容积泵，利用容积泵由溶剂中转罐中向萃取罐打入75%的乙醇，同时开启蒸汽阀门对萃取罐和蒸发浓缩塔加温，蒸发浓缩塔温度维持在80-85℃，, 萃取温度控制在90℃，控制调压阀使萃取罐压力维持在5Mpa萃取90min。萃取结束后，关闭容积泵，开启调压阀泄压，继续对萃取罐加温回收溶剂，至冷凝塔中无溶剂流出时，关闭蒸汽阀门，将橘皮渣泄出。用接受桶从分离罐下方获得含有橘皮有效成分的提取物。称重获得橘皮提取物92g，出率为3.68%。Dry the fresh orange peel at 55°C, crush it with a pulverizer and pass it through a 20-mesh sieve. Take 2500g of material into the extraction tank, turn on the positive displacement pump, use the positive displacement pump to inject 75% ethanol from the solvent transfer tank into the extraction tank, and open the steam valve at the same time to heat the extraction tank and the evaporative concentration tower. The temperature of the evaporative concentration tower is maintained at 80-85°C, the extraction temperature is controlled at 90°C, and the pressure regulating valve is controlled to maintain the pressure of the extraction tank at 5Mpa for 90 minutes of extraction. After the extraction, close the positive displacement pump, open the pressure regulating valve to release the pressure, continue to heat the extraction tank to recover the solvent, and when no solvent flows out from the condensation tower, close the steam valve to release the orange peel residue. Obtain the extract containing the active ingredient of orange peel from the bottom of the separation tank with a receiving barrel. 92g of orange peel extract was obtained by weighing, and the yield was 3.68%.
对比实施例1Comparative Example 1
将新鲜橘皮在55℃下烘干，用粉碎机粉碎后过20目筛网，取50g物料包入滤纸包，以1000ml 75%乙醇为抽提剂，在常压70℃下浸提90min，取出滤纸包，将提取液蒸发浓缩后，获得0.92g橘皮提取物，出率为1.84%。Dry the fresh orange peel at 55°C, crush it with a pulverizer and pass it through a 20-mesh sieve, take 50g of the material and pack it into a filter paper bag, use 1000ml of 75% ethanol as the extractant, and extract it at normal pressure at 70°C for 90min. The filter paper bag was taken out, and after the extract was evaporated and concentrated, 0.92 g of orange peel extract was obtained, and the yield was 1.84%.
由上述对照试验可以看出，本发明所提供的工艺其提取率远远要高于常规的有机溶剂提取工艺。As can be seen from the above comparative experiments, the extraction rate of the process provided by the present invention is far higher than the conventional organic solvent extraction process.
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