CN101103805B - Industrial producing method for extracting fatty compound from melissa pollen - Google Patents
Industrial producing method for extracting fatty compound from melissa pollen Download PDFInfo
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- 239000002994 raw material Substances 0.000 claims abstract description 21
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 54
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- 238000000926 separation method Methods 0.000 description 20
- 239000000203 mixture Substances 0.000 description 9
- 239000012530 fluid Substances 0.000 description 7
- 238000000194 supercritical-fluid extraction Methods 0.000 description 7
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 5
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 5
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Abstract
本发明提供一种从蜂花粉中提取脂肪类化合物工业化生产方法。a.先将蜂花粉破壁，然后对破壁后的蜂花粉造粒，再将该蜂花粉造粒原料置入萃取器中；b.将纯度为99％以上的液体CO2送入高压泵，加压后的液态CO2送入萃取器，在温度为30～65℃、压力为20～50MPa、CO2流速为280～380kg/h的条件下萃取0.5～1小时，然后在压力为5.8～6.4MPa的分离器1分离，得一次萃取化合物；c.将相对于蜂花粉造粒原料重量5～12％的食用酒精泵入萃取器，在温度为30～65℃、压力为20～50MPa、CO2流速为280～380kg/h的条件下继续萃取0.5～1小时，然后先经压力为7～14MPa、温度为40～60℃的分离器1分离，得二次萃取化合物；d.合并两次萃取化合物，得产品。The invention provides an industrial production method for extracting fatty compounds from bee pollen. a. First break the bee pollen wall, then granulate the broken bee pollen, and then put the bee pollen granulation raw material into the extractor; b. Send the liquid CO 2 with a purity of more than 99% into the high-pressure pump , the pressurized liquid CO 2 is sent to the extractor, extracted at a temperature of 30-65°C, a pressure of 20-50 MPa, and a CO 2 flow rate of 280-380kg/h for 0.5-1 hour, and then extracted at a pressure of 5.8 Separator 1 with ~6.4MPa separates to obtain an extraction compound; c. Pump 5-12% edible alcohol relative to the weight of bee pollen granulation raw material into the extractor at a temperature of 30-65°C and a pressure of 20-50MPa , CO The flow rate is 280-380kg/h and the extraction is continued for 0.5-1 hour, and then separated by separator 1 with a pressure of 7-14MPa and a temperature of 40-60°C to obtain the secondary extraction compound; d. The compound is extracted twice to obtain the product.
Description
技术领域：Technical field:
本发明属于食品和药品原料大规模加工方法，尤其是一种从蜂花粉中提取脂肪类化合物的工业化生产方法。The invention belongs to a large-scale processing method of food and medicine raw materials, in particular to an industrial production method for extracting fatty compounds from bee pollen.
背景技术：Background technique:
蜂花粉为蜜蜂采集回来的花粉，除有一般花粉的成分外，还含有在采集时加进去的少量花蜜和分泌物，使其在粘度、花粉壁结构等理化性质方面有别于松花粉。蜂花粉具有较强的生理活性，可增强人体免疫功能、抗肿瘤、抗便秘、延缓衰老，具有美容作用；是一种值得研究开发的理想的高级天然营养品。该类花粉中含有丰富的脂肪类化合物，现有技术中提取脂肪类化合物广泛采用乙醚、石油醚等有机溶剂萃取法。其主要缺点是提取成本高，且提取物中残留有机溶剂，直接影响产品质量。CN1052417A公开了《用超临界二氧化碳对花粉进行脱臭保鲜》的技术方案，其提供了一种在低于40℃的条件下，对花粉进行脱臭，保鲜，并保留其酶的生物活性和营养价值的生产工艺。在超临界流体萃取设备中，应用高效吸附剂，在温度低于40℃及压力为6-22兆帕(MPa)的条件下，通过二氧化碳流体对花粉进行连续萃取和吸附，即可获得脱臭，保鲜花粉。但该技术方案权限于对蜜蜂传媒花粉进行脱臭及保鲜，获得的产品是脱臭、灭菌的保鲜花粉。Bee pollen is the pollen collected by bees. In addition to the general pollen components, it also contains a small amount of nectar and secretions added during collection, which makes it different from pine pollen in terms of viscosity, pollen wall structure and other physical and chemical properties. Bee pollen has strong physiological activity, can enhance human immune function, anti-tumor, anti-constipation, delay aging, and has cosmetic effect; it is an ideal high-grade natural nutrition worthy of research and development. This type of pollen is rich in fatty compounds. In the prior art, organic solvent extraction methods such as diethyl ether and petroleum ether are widely used to extract fatty compounds. Its main disadvantage is that the extraction cost is high, and the organic solvent remains in the extract, which directly affects the product quality. CN1052417A discloses the technical scheme of "Using Supercritical Carbon Dioxide to Deodorize and Keep Pollen Fresh", which provides a method of deodorizing and keeping pollen at a temperature lower than 40°C, and retaining its enzyme biological activity and nutritional value. Production Process. In supercritical fluid extraction equipment, high-efficiency adsorbents are used to continuously extract and adsorb pollen through carbon dioxide fluid at a temperature lower than 40°C and a pressure of 6-22 MPa (MPa) to obtain deodorization. Preserved pollen. But this technical scheme is limited to carrying out deodorization and fresh-keeping to honeybee media pollen, and the product obtained is deodorized, sterilized preserved pollen.
CN1307092A公开了《用CO2超临界萃取松花粉中脂肪类化合物》，提供一种从以风为传媒的松花粉中提取脂肪类物质的技术方案。将经过干燥、物理破壁或发酵生物法破壁及灭菌处理后的松花粉放入CO2超临界萃取装置中，加压后的CO2经加热器加热后进入萃取器，与其中的松花粉充分接触，在温度为30-50℃、压力为8-40MPa、CO2流速为0.5-15L/min的条件下，萃取0.5-2小时，带着脂肪类萃取物的CO2流体经节流膨胀阀后分别进入一级和二级分离器中分离。该技术仅限于对松花粉进行脂肪类化合物的萃取，而对破壁后粘度更大，更易成团，造成萃取不充分的蜂花粉萃取及分离未有提及，且该技术有效提取率仅为80％左右，相对得率较低，易造成原料浪费。CN1307092A discloses "Using CO Supercritical Extraction of Fatty Compounds in Pine Pollen", which provides a technical scheme for extracting fatty substances from pine pollen with wind as the medium. Put the pine pollen after drying, physical wall breaking or fermentation biological method wall breaking and sterilization into the CO2 supercritical extraction device, and the pressurized CO2 enters the extractor after being heated by a heater, and the pine pollen therein The pollen is in full contact, under the conditions of temperature 30-50°C, pressure 8-40MPa, CO 2 flow rate 0.5-15L/min, extract for 0.5-2 hours, and the CO 2 fluid with fat extract is throttled After the expansion valve, it enters the primary and secondary separators for separation. This technology is limited to the extraction of fatty compounds from pine pollen, but it does not mention the extraction and separation of bee pollen that is more viscous and easier to form agglomerates after breaking the wall, resulting in insufficient extraction, and the effective extraction rate of this technology is only About 80%, the relative yield is low, and it is easy to cause waste of raw materials.
CN1733009公开了《一种从蜂花粉中提取脂肪类化合物的方法》，提供了一种从蜂花粉中提取脂肪类化合物的方法。将蜂花粉粉碎后置入设有夹套的萃取器，再将纯度为99％以上的CO2经冷凝器冷凝为液体后进入高压泵，加压后的液态CO2经加热器加热后送入萃取器，与粉状蜂花粉充分接触，在温度为30～65℃、压力为20～40MPa、CO2流速为20～50kg/h的条件下，连续萃取1～3小时，携带着萃取脂肪类化合物的CO2流体进入设有夹套的分离器，将萃取出的脂肪类化合物分离后，CO2返回冷凝器。其采用的花粉未经过造粒，为粉状蜂花粉，CO2流速较小，只适合实验室和小规模提取，不能满足大规模工业生产需求。而且，其技术方案未明确具体的分离参数。CN1733009 discloses "A Method for Extracting Fatty Compounds from Bee Pollen", which provides a method for extracting fatty compounds from bee pollen. Put the bee pollen into a jacketed extractor after crushing, and then condense the CO2 with a purity of more than 99% into a liquid through the condenser and then enter the high-pressure pump. The pressurized liquid CO2 is heated by a heater and sent into the The extractor is in full contact with the powdered bee pollen, under the conditions of temperature 30-65°C, pressure 20-40MPa, CO2 flow rate 20-50kg/h, continuous extraction for 1-3 hours, carrying the extracted fat The CO 2 fluid of the compounds enters the jacketed separator, and after separating the extracted fatty compounds, the CO 2 returns to the condenser. The pollen it uses has not been granulated, it is powdery bee pollen, and the flow rate of CO2 is small, which is only suitable for laboratory and small-scale extraction, and cannot meet the needs of large-scale industrial production. Moreover, its technical scheme does not specify specific separation parameters.
发明内容：Invention content:
本发明的目的旨在克服现有技术的不足，提供一种有效提取率较高，不含残留有机溶剂，可快速大规模从蜂花粉中提取脂肪类化合物工业化生产方法。The purpose of the present invention is to overcome the deficiencies of the prior art, to provide a high effective extraction rate, no residual organic solvents, and an industrial production method that can rapidly and large-scale extract fatty compounds from bee pollen.
本发明的目的可通过如下技术措施来实现：The purpose of the present invention can be achieved through the following technical measures:
a.先将蜂花粉破壁，然后对破壁后的蜂花粉造粒，再将该蜂花粉造粒原料置入萃取器中；a. First break the bee pollen wall, then granulate the broken bee pollen, and then put the bee pollen granulation raw material into the extractor;
b.将纯度为99％以上的液体CO2送入高压泵，加压后的液态CO2送入萃取器，在温度为30～65℃、压力为20～50MPa、CO2流速为280～380kg/h的条件下萃取0.5～1小时，然后在压力为5.8～6.4MPa的分离器1分离，得一次萃取化合物；b . Send liquid CO2 with a purity of more than 99% into the high-pressure pump, and then send the pressurized liquid CO2 into the extractor. Extract under the condition of 0.5～1 hour under the condition of /h, then separate in the separator 1 that pressure is 5.8～6.4MPa, obtain once-extracted compound;
c.将相对于蜂花粉造粒原料重量5～12％的食用酒精泵入萃取器，在温度为30～65℃、压力为20～50MPa、CO2流速为280～380kg/h的条件下继续萃取0.5～1小时，然后先经压力为7～14MPa、温度为40～60℃的分离器1分离，得二次萃取化合物；c. Pump 5-12% edible alcohol relative to the weight of the bee pollen granulation raw material into the extractor, and continue under the conditions of a temperature of 30-65°C, a pressure of 20-50MPa, and a CO2 flow rate of 280-380kg/h. Extract for 0.5 to 1 hour, and then firstly separate through the separator 1 with a pressure of 7 to 14 MPa and a temperature of 40 to 60°C to obtain the secondary extraction compound;
d.合并两次萃取化合物，得产品。d. Combining the two extraction compounds to obtain the product.
本发明的目的还可通过如下技术措施来实现：The purpose of the present invention can also be achieved through the following technical measures:
所述的蜂花粉破壁率为不低于85％，所述的造粒粒度为10～100目；所述的蜂花粉含水量为2～8％；c工序分离器1中未被分离的混合物经压力和温度分别低于分离器1并至少为25℃及5MPa的分离器2，分离后的食用酒精与脂肪类化合物的混合物一起的用作下一次萃取的夹带剂。经分离后的CO2通过净化器、冷凝器，得液体CO2重复使用。The wall breaking rate of the bee pollen is not less than 85%, the granulation size is 10-100 mesh; the water content of the bee pollen is 2-8%; The mixture passes through the separator 2 whose pressure and temperature are respectively lower than the separator 1 and at least 25°C and 5MPa, and the separated edible alcohol and the mixture of fatty compounds are used as the entrainer for the next extraction. The separated CO 2 passes through the purifier and condenser to obtain liquid CO 2 for reuse.
本发明先将蜂花粉破壁，再对破壁后蜂花粉造粒，后置入萃取器中；液体CO2送入高压泵，加压后加热送入萃取器，进行一次萃取，然后送分离器，通过调节分离器1及分离器2压力至与CO2气罐压力相同，完成一次萃取分离；再将食用酒精泵入萃取器，进行二次萃取，经分离，最后把一次、二次萃取分离中分离釜1中的产物合并得产品。二次萃取分离中分离器2中的食用酒精与脂肪类化合物的混合物一起作为下一次萃取的夹带剂使用。In the present invention, the bee pollen is broken first, then the broken bee pollen is granulated, and then put into the extractor; the liquid CO2 is sent into the high-pressure pump, heated and sent into the extractor after pressurization, for one extraction, and then sent to the extractor for separation By adjusting the pressure of separator 1 and separator 2 to be the same as the pressure of the CO2 gas tank, the primary extraction and separation are completed; then edible alcohol is pumped into the extractor for secondary extraction, and after separation, the primary and secondary extraction are finally separated During the separation, the products in the separation tank 1 were combined to obtain the product. In the secondary extraction and separation, the edible alcohol in the separator 2 is used together with the mixture of fatty compounds as the entrainer for the next extraction.
本发明以食用酒精作为夹带剂，加入夹带剂前分离器1压力与分离器2压力都与CO2罐罐压相同，加入夹带剂后分别调节分离器1、分离器2压力，整个萃取过程中控制分离器1温度为40～60℃，分离器2温度为25～45℃。The present invention uses edible alcohol as the entraining agent. Before adding the entraining agent, the pressure of separator 1 and separator 2 are the same as the pressure of the CO tank. After adding the entraining agent, the pressures of separator 1 and separator 2 are respectively adjusted. During the whole extraction process Control the temperature of separator 1 to 40-60°C, and the temperature of separator 2 to 25-45°C.
本发明将经过不同造粒处理和含水量不同的蜂花粉放入CO2超临界萃取装置中。该装置的萃取器和分离器都设有夹套，可用热水加热和保持恒温。来自钢瓶的CO2经冷凝器冷凝为液体后进入高压泵，经加压后的CO2经加热器加热后进入萃取器，与造粒蜂花粉充分接触、萃取，携带脂肪类萃取物的CO2流体经节流膨胀阀后，分别进入一级和二级分离器中。在分离器中，由于压力降低，CO2流体密度减小，大量溶解于CO2流体中的脂肪类化合物就会被分离出来。通过调节分离器压力、温度，可以使大量的脂肪类化合物从分离器1中析出，只有少量的脂肪类化合物从分离器2中析出。而CO2流体经流量计、净化器后回到冷凝器，形成循环。In the invention, the bee pollen with different granulation treatments and water contents is put into a CO2 supercritical extraction device. Both the extractor and the separator of the device are equipped with jackets, which can be heated with hot water and kept at a constant temperature. The CO 2 from the steel cylinder is condensed into a liquid by the condenser and then enters the high-pressure pump. The pressurized CO 2 is heated by the heater and then enters the extractor, where it is fully contacted with granulated bee pollen and extracted, and the CO 2 that carries the fat extract After passing through the throttling expansion valve, the fluid enters the primary and secondary separators respectively. In the separator, as the pressure decreases, the density of the CO2 fluid decreases, and a large amount of fatty compounds dissolved in the CO2 fluid will be separated. By adjusting the pressure and temperature of the separator, a large amount of fatty compounds can be separated from the separator 1, and only a small amount of fatty compounds can be separated from the separator 2. The CO 2 fluid returns to the condenser after passing through the flow meter and the purifier, forming a cycle.
本发明用液体CO2超临界萃取蜂花粉，得到的脂肪类化合物含有大量不同种类的不饱和脂肪酸，具有增强免疫力以及其它保健功能。同时经萃取得到的蜂花粉中脂肪类物质具有品质好，成本低，有效提取率高(可达97％以上)，节省原材料，产品质量高，不含残留有机溶剂等优点。由于CO2流速大，一次投料量大(10-50kg)，可以满足大规模工业生产需求。The invention uses liquid CO2 to supercritically extract the bee pollen, and the fat compound obtained contains a large amount of different kinds of unsaturated fatty acids, and has the functions of enhancing immunity and other health care functions. At the same time, the fatty substances in the bee pollen obtained through extraction have the advantages of good quality, low cost, high effective extraction rate (up to more than 97%), saving raw materials, high product quality, and no residual organic solvent. Due to the large flow rate of CO 2 and the large amount of feeding (10-50kg) at one time, it can meet the needs of large-scale industrial production.
如果将本发明与CN1052417A公开的技术方案相比较，可以看出，本发明是从经过不同破壁后造粒处理的(10～100目)、含水量不同的(2％—8％左右)蜂花粉中提取脂肪类化合物，另一个是从蜂花粉中萃取出一个是脱臭、灭菌的保鲜花粉，两个技术方案的发明目的不同，原料及作用对象不同，获得的产品、产率等均不同。If the present invention is compared with the disclosed technical scheme of CN1052417A, it can be seen that the present invention is obtained from honeycombs (10-100 mesh) and different water contents (about 2%-8%) that have undergone different wall-breaking and granulation treatments. One is to extract fat compounds from pollen, the other is to extract deodorized and sterilized preserved pollen from bee pollen. The invention objectives of the two technical solutions are different, the raw materials and objects of action are different, and the obtained products and yields are different. .
如果将本发明与CN1307092A公开的技术方案相比较，可以看出本发明是从经过不同破壁后造粒处理的(10～100目)、含水量不同(2％—8％左右)和粘度等理化性质不同的蜂花粉中工业化提取脂肪类化合物，提取过程中CO2流量明显不同，提取过程存在差异，同时设定了具体的分离参数，获得的产品是脱脂的蜂花粉和萃取出的脂肪类化合物，本发明的有效提取率高达97％以上，两个技术方案的发明目的不同，原料及作用对象不同，技术方法不同，获得的产品成分及萃取效果等也不同。If the present invention is compared with the disclosed technical scheme of CN1307092A, it can be seen that the present invention is granulated from different broken walls (10-100 mesh), different water content (about 2%-8%) and viscosity etc. The industrial extraction of fatty compounds from bee pollen with different physical and chemical properties, the CO 2 flow rate is significantly different during the extraction process, and there are differences in the extraction process. At the same time, specific separation parameters are set. The obtained products are defatted bee pollen and extracted fats Compound, the effective extraction rate of the present invention is as high as 97%. The invention objectives of the two technical solutions are different, the raw materials and objects of action are different, the technical methods are different, and the obtained product components and extraction effects are also different.
如果将本发明与CN1733009公开的技术方案相比较，可以看出本发明是从经过不同破壁后造粒处理的(10～100目)蜂花粉中工业化提取脂肪类化合物，提取过程中CO2流量明显不同，提取过程中添加了夹带剂，同时设定了具体的分离参数，使得最终分离器1中所得脂肪类化合物质量与分离器2中所得脂肪类化合物质量之比为10-100：1。两个技术方案适合的生产规模不同，原料处理不同，工艺路线不同。If the present invention is compared with the disclosed technical scheme of CN1733009, it can be seen that the present invention industrially extracts fatty compounds from bee pollen (10-100 mesh ) after different wall-breaking and granulation treatments. Obviously different, the entrainer is added during the extraction process, and the specific separation parameters are set at the same time, so that the ratio of the mass of the fatty compound obtained in the final separator 1 to the mass of the fatty compound obtained in the separator 2 is 10-100:1. The suitable production scales of the two technical solutions are different, the raw materials are handled differently, and the process routes are different.
具体实施方式：Detailed ways:
实施例1：Example 1:
先将10kg含水量为8％、破壁率为98％的蜂花粉进行造粒，再将粒度为10目的蜂花粉原料置入CO2超临界萃取装置中，萃取器和分离器设有用热水加热和保持恒温的夹套，由循环来的纯度为99.9％的CO2经冷凝器冷凝为液体后，进入高压泵加压，通过加热器加热后进入萃取器，与10目的蜂花粉造粒原料充分接触。在温度为65℃、压力为20MPa、CO2流速为380kg/h的条件下，循环萃取0.5小时，调节分离器1压力为5.8MPa，完成一次萃取分离，得一次萃取产物；再将相对于10目蜂花粉原料重量5％的食用酒精泵入萃取器，在温度为65℃、压力为20MPa、CO2流速为380kg/h的条件下，继续循环萃取1小时，然后调节分离器1压力至7MPa，温度为40℃，完成二次萃取分离，得二次萃取产物；合并一次、二次萃取分离中分离器1析出的产物，得产品。二次萃取时分离器1中未被分离的混合物送分离器2，调节分离器2压力为5.8MPa，温度为25℃，经分离后的食用酒精与脂肪类化合物的混合物一起的用作下一次萃取的夹带剂。一次萃取分离器中所得脂肪类化合物质量与二次萃取分离器中所得脂肪类化合物质量之比为100：1；分离后的CO2送CO2气罐，经净化器、冷凝器冷凝为液体后重复使用。First, 10 kg of bee pollen with a water content of 8% and a wall breaking rate of 98% is granulated, and then the raw material of bee pollen with a particle size of 10 mesh is placed in a CO2 supercritical extraction device. The extractor and separator are equipped with hot water The jacket is heated and maintained at a constant temperature, and the recycled CO2 with a purity of 99.9% is condensed into a liquid by the condenser, then enters the high-pressure pump for pressurization, and enters the extractor after being heated by the heater, and is granulated with 10-mesh bee pollen as raw material Full contact. Under the condition that the temperature is 65°C, the pressure is 20MPa, and the CO flow rate is 380kg/h, the circulation extraction is carried out for 0.5 hours, and the pressure of the separator 1 is adjusted to 5.8MPa to complete an extraction and separation to obtain an extraction product; Edible alcohol with 5% weight of the raw material of bee pollen is pumped into the extractor, and under the conditions of temperature 65°C, pressure 20MPa, and CO flow rate 380kg/h, continue to circulate and extract for 1 hour, and then adjust the pressure of separator 1 to 7MPa , the temperature is 40°C, and the secondary extraction and separation are completed to obtain the secondary extraction product; the product precipitated by the separator 1 in the primary and secondary extraction and separation is combined to obtain the product. During the secondary extraction, the unseparated mixture in separator 1 is sent to separator 2, and the pressure of separator 2 is adjusted to 5.8MPa, and the temperature is 25°C. The separated edible alcohol and the mixture of fatty compounds are used together for the next extraction. Extracted entrainer. The ratio of the mass of fatty compounds obtained in the primary extraction separator to the mass of fatty compounds obtained in the secondary extraction separator is 100:1; the separated CO 2 is sent to the CO 2 gas tank, and after being condensed into a liquid by a purifier and a condenser reuse.
实施例2：Example 2:
先将30kg含水量为2％、破壁率为86％的蜂花粉进行造粒，再将粒度为100目的蜂花粉原料置入CO2超临界萃取装置中，萃取器和分离器设有用热水加热和保持恒温的夹套，由循环来的纯度为99.9％的CO2经冷凝器冷凝为液体后，进入高压泵加压，通过加热器加热后进入萃取器，与100目的蜂花粉造粒原料充分接触。在温度为50℃、压力为50MPa、CO2流速为280kg/h的条件下，连续萃取1小时，调节分离器1压力为6.4MPa，完成一次萃取分离，得一次萃取产物；再将相对于100目蜂花粉原料重量12％的食用酒精泵入萃取器，在温度为50℃、压力为50MPa、CO2流速为280kg/h的条件下，继续循环萃取0.5小时，然后调节分离器1压力至14MPa，温度为60℃，完成二次萃取分离，得二次萃取产物；合并一次、二次萃取分离中分离器1析出的产物，得产品。二次萃取时分离器1中未被分离的混合物送分离器2，调节分离器2压力为6.4MPa，温度为30℃，经分离后的食用酒精与脂肪类化合物的混合物一起的用作下一次萃取的夹带剂。一次萃取分离器中所得脂肪类化合物质量与二次萃取分离器中所得脂肪类化合物质量之比为50：1；分离后的CO2送CO2气罐，经净化器、冷凝器冷凝为液体后重复使用。First, 30kg of bee pollen with a water content of 2% and a wall breaking rate of 86% is granulated, and then the raw material of bee pollen with a particle size of 100 mesh is placed in a CO2 supercritical extraction device. The extractor and separator are equipped with hot water The jacket is heated and maintained at a constant temperature, and the recycled CO2 with a purity of 99.9% is condensed into a liquid by the condenser, then enters the high-pressure pump for pressurization, and enters the extractor after being heated by the heater, and is granulated with 100-mesh bee pollen as raw material Full contact. Under the condition that the temperature is 50°C, the pressure is 50MPa, and the CO2 flow rate is 280kg/h, the continuous extraction is performed for 1 hour, and the pressure of the separator 1 is adjusted to 6.4MPa to complete an extraction and separation to obtain an extraction product; Edible alcohol with 12% raw material weight of bee pollen is pumped into the extractor, under the conditions of temperature 50°C, pressure 50MPa, and CO2 flow rate 280kg/h, continue to circulate and extract for 0.5 hours, and then adjust the pressure of separator 1 to 14MPa , the temperature is 60°C, and the secondary extraction and separation are completed to obtain the secondary extraction product; the product precipitated by the separator 1 in the primary and secondary extraction and separation is combined to obtain the product. During the secondary extraction, the unseparated mixture in separator 1 is sent to separator 2, and the pressure of separator 2 is adjusted to 6.4MPa, and the temperature is 30°C. The separated edible alcohol and the mixture of fatty compounds are used together for the next extraction. Extracted entrainer. The ratio of the mass of fatty compounds obtained in the primary extraction separator to the mass of fatty compounds obtained in the secondary extraction separator is 50:1; the separated CO 2 is sent to the CO 2 gas tank, and after being condensed into a liquid by a purifier and a condenser reuse.
实施例3：Example 3:
先将50kg含水量为5％、破壁率为90％的蜂花粉进行造粒，再将粒度为50目的蜂花粉原料置入CO2超临界萃取装置中，萃取器和分离器设有用热水加热和保持恒温的夹套，由循环来的纯度为99.9％的CO2经冷凝器冷凝为液体后，进入高压泵加压，通过加热器加热后进入萃取器，与50目的蜂花粉造粒原料充分接触。在温度为45℃、压力为35MPa、CO2流速为320kg/h的条件下，循环萃取45分钟，调节分离器1压力为6.0MPa，完成一次萃取分离，得一次萃取产物；再将相对于50目蜂花粉原料重量8％的食用酒精泵入萃取器，在温度为45℃、压力为35MPa、CO2流速为320kg/h的条件下，继续循环萃取40分钟，然后调节分离器1压力至10MPa，温度为50℃，完成二次萃取分离，得二次萃取产物；合并一次、二次萃取分离中分离器1析出的产物，得产品。二次萃取时分离器1中未被分离的混合物送分离器2，调节分离器2压力为6.0MPa，温度为25℃，经分离后的食用酒精与脂肪类化合物的混合物一起的用作下一次萃取的夹带剂。一次萃取分离器中所得脂肪类化合物质量与二次萃取分离器中所得脂肪类化合物质量之比为60：1；分离后的CO2送CO2气罐，经净化器、冷凝器冷凝为液体后重复使用。First, 50kg of bee pollen with a water content of 5% and a wall breaking rate of 90% is granulated, and then the raw material of bee pollen with a particle size of 50 mesh is placed in a CO2 supercritical extraction device. The extractor and separator are equipped with hot water The jacket is heated and maintained at a constant temperature, and the recycled CO2 with a purity of 99.9% is condensed into a liquid by the condenser, then enters the high-pressure pump for pressurization, and enters the extractor after being heated by the heater, and is granulated with 50-mesh bee pollen as raw material Full contact. Under the condition that the temperature is 45°C, the pressure is 35MPa, and the CO2 flow rate is 320kg/h, the circulation extraction is carried out for 45 minutes, and the pressure of the separator 1 is adjusted to 6.0MPa to complete an extraction and separation to obtain an extraction product; Edible alcohol with 8% raw material weight of bee pollen is pumped into the extractor, under the conditions of temperature 45°C, pressure 35MPa, CO2 flow rate 320kg/h, continue to circulate and extract for 40 minutes, then adjust separator 1 pressure to 10MPa , the temperature is 50°C, and the secondary extraction and separation are completed to obtain the secondary extraction product; the product precipitated by the separator 1 in the primary and secondary extraction and separation is combined to obtain the product. During the secondary extraction, the unseparated mixture in separator 1 is sent to separator 2, and the pressure of separator 2 is adjusted to 6.0MPa, and the temperature is 25°C. The separated edible alcohol and the mixture of fatty compounds are used together for the next extraction. Extracted entrainer. The ratio of the mass of fatty compounds obtained in the primary extraction separator to the mass of fatty compounds obtained in the secondary extraction separator is 60:1; the separated CO 2 is sent to the CO 2 gas tank, and after being condensed into liquid by the purifier and condenser reuse.
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