CN101103805A - A kind of industrial production method of extracting fatty compounds from bee pollen - Google Patents
A kind of industrial production method of extracting fatty compounds from bee pollen Download PDFInfo
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- CN101103805A CN101103805A CNA2007100164603A CN200710016460A CN101103805A CN 101103805 A CN101103805 A CN 101103805A CN A2007100164603 A CNA2007100164603 A CN A2007100164603A CN 200710016460 A CN200710016460 A CN 200710016460A CN 101103805 A CN101103805 A CN 101103805A
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000009776 industrial production Methods 0.000 title claims abstract description 7
- 229940038481 bee pollen Drugs 0.000 title claims abstract 16
- 238000000605 extraction Methods 0.000 claims abstract description 40
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 18
- 238000005469 granulation Methods 0.000 claims abstract description 16
- 230000003179 granulation Effects 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000008187 granular material Substances 0.000 claims abstract description 3
- 239000000284 extract Substances 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 description 37
- 239000003925 fat Substances 0.000 description 32
- 238000010438 heat treatment Methods 0.000 description 11
- 239000012530 fluid Substances 0.000 description 7
- 230000001105 regulatory effect Effects 0.000 description 7
- 238000004332 deodorization Methods 0.000 description 6
- 238000000194 supercritical-fluid extraction Methods 0.000 description 6
- 230000001351 cycling effect Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000002386 leaching Methods 0.000 description 4
- 238000012423 maintenance Methods 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 230000001954 sterilising effect Effects 0.000 description 3
- 238000004659 sterilization and disinfection Methods 0.000 description 3
- 241000256844 Apis mellifera Species 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 1
- 206010010774 Constipation Diseases 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000036737 immune function Effects 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000028327 secretion Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
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- Medicinal Preparation (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Fats And Perfumes (AREA)
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
Technical field:
The invention belongs to food and pharmaceutical raw material large-scale processing method, especially a kind of industrialized preparing process that from the melissa powder, extracts fat compound.
Background technology:
The melissa powder is that honeybee is gathered the pollen of returning, and except that the composition that general pollen is arranged, also contains a small amount of nectar and the secretion added when gathering, and makes it be different from pollen pini aspect physicochemical properties such as viscosity, pollen wall structure.The melissa powder has stronger physiologically active, can strengthen immune function of human body, antitumor, anti-constipation, delay senility, and has beautification function; It is a kind of desirable senior natural nutriment of worth research and development.Contain abundant fat compound in such pollen, extract fat compound in the prior art and extensively adopt organic solvent extractionprocesses such as ether, benzinum.Its major defect is the extraction cost height, and residual organic solvent in the extract, directly influences product quality.CN1052417A discloses the technical scheme of " with supercritical carbon dioxide to deodorization and fresh-keeping of pollen ", and it provides a kind of and being lower than under 40 ℃ the condition pollen has been carried out deodorization, and is fresh-keeping, and keeps the biologically active of its enzyme and the production technology of nutritive value.In supercritical fluid extraction equipment, use high-efficiency adsorbent, being lower than 40 ℃ and pressure in temperature is under the condition of 6-22 MPa (MPa), by CO 2 fluid pollen is carried out continuous extraction and absorption, can obtain deodorization, fresh-keeping pollen.But this technical scheme authority is in carrying out deodorization and fresh-keeping to honeybee medium pollen, and the product of acquisition is the fresh-keeping pollen of deodorization, sterilization.
CN1307092A discloses and " has used CO
2Fat compound in the supercritical extract pollen pini ", provide a kind of from wind being the technical scheme of extracting lipoid material the pollen pini of medium.To put into CO through the pollen pini after super-dry, physical wall breaking or fermenting organism method broken wall and the sterilization treatment
2In the supercritical extraction unit, the CO after the pressurization
2Entering extractor after the heater via heating, fully contact with wherein pollen pini, is that 30-50 ℃, pressure are 8-40MPa, CO in temperature
2Flow velocity is under the condition of 0.5-15L/min, extracts 0.5-2 hour, with the CO of fats extract
2Fluid enters respectively in the firsts and seconds separator behind throttle expansion valve and separates.This technology only limits to pollen pini is carried out the extraction of fat compound, and bigger to viscosity behind the broken wall, easier to be agglomerating, cause inadequate melissa powder extraction of extraction and separation to mention, and the effective recovery rate of this technology only is about 80%, and yield is lower relatively, easily causes wastage of material.
CN1733009 discloses " a kind of method of extracting fat compound from the melissa powder ", and a kind of method of extracting fat compound from the melissa powder is provided.With inserting the extractor that is provided with chuck after the pulverizing of melissa powder, be the CO more than 99% again with purity
2After being liquid, condenser condenses enters high-pressure pump, the liquid CO after the pressurization
2Sending into extractor after the heater via heating, fully contact with powdery melissa powder, is that 30～65 ℃, pressure are 20～40MPa, CO in temperature
2Flow velocity is under the condition of 20～50kg/h, and the CO that extracts fat compound is being carried in continuous extraction 1～3 hour
2Fluid enters the separator that is provided with chuck, after the fat compound that extracts is separated, and CO
2Return condensed device.Its pollen that adopts does not pass through granulation, is powdery melissa powder, CO
2Flow velocity is less, and only suitable laboratory and extraction on a small scale can not be satisfied the large-scale industrial production demand.And, the not clear and definite concrete separation parameter of its technical scheme.
Summary of the invention:
Purpose of the present invention is intended to overcome the deficiencies in the prior art, provides a kind of effective recovery rate higher, does not contain residual organic solvent, but rapid large-scale industrial producing method for extracting fatty compound from the melissa powder.
Purpose of the present invention can realize by following technical measures:
A. earlier with broken wall of melissa pollen,, again this melissa powder granulating raw material is inserted in the extractor then to the melissa powder granulation behind the broken wall;
B. with purity the liquid CO more than 99%
2Send into high-pressure pump, the liquid CO after the pressurization
2Sending into extractor, is that 30～65 ℃, pressure are 20～50MPa, CO in temperature
2Flow velocity is to extract 0.5～1 hour under the condition of 280～380kg/h, is that the separator 1 of 5.8～6.4MPa separates at pressure then, the single extraction compound;
C. will pump into extractor with respect to the edible alcohol of melissa powder granulating raw material weight 5～12%, be that 30～65 ℃, pressure are 20～50MPa, CO in temperature
2Flow velocity is to continue extraction 0.5～1 hour under the condition of 280～380kg/h, is that 7～14MPa, temperature are that 40～60 ℃ separator 1 separates through pressure earlier then, the reextraction compound;
D. merge extract compounds twice, get product.
Purpose of the present invention also can realize by following technical measures:
Described broken wall of melissa pollen rate is for being not less than 85%, and described granule size is 10～100 orders; Described melissa powder water content is 2～8%; Not separated mixture is lower than separator 1 respectively and is at least the separator 2 of 25 ℃ and 5MPa through pressure and temperature in the c operation separator 1, the edible alcohol after the separation with the mixture of fat compound as the entrainer of extraction next time.CO after separating
2By clarifier, condenser, get liquid CO
2Reuse.
The present invention is earlier with broken wall of melissa pollen, again to melissa powder granulation behind the broken wall, after insert in the extractor; Liquid CO
2Send into high-pressure pump, extractor is sent in pressurization back heating, carries out single extraction, send separator then, by regulate separator 1 and separator 2 pressure to and CO
2Gas tank pressure is identical, finishes single extraction and separates; Again edible alcohol is pumped into extractor, carries out reextraction, through separating, at last once, reextraction separate in product in the separating still 1 merge product.Edible alcohol during reextraction separates in the separator 2 uses as the entrainer that extracts next time with the mixture of fat compound.
The present invention with edible alcohol as entrainer, add before the entrainer separator 1 pressure and separator 2 pressure all with CO
2The jar tank pressure is identical, regulates separator 1, separator 2 pressure respectively behind the adding entrainer, and control separator 1 temperature is 40～60 ℃ in the whole extraction process, and separator 2 temperature are 25～45 ℃.
The present invention will put into CO through the different granulation processing melissa powder different with water content
2In the supercritical extraction unit.The extractor of this device and separator all are provided with chuck, available hot water heating and maintenance constant temperature.CO from steel cylinder
2After being liquid, condenser condenses enters high-pressure pump, the CO after pressurization
2Enter extractor after the heater via heating, fully contact, extract, carry the CO of fats extract with granulation melissa powder
2Fluid enters respectively in the firsts and seconds separator behind throttle expansion valve.In separator, because pressure reduces CO
2Fluid density reduces, and is dissolved in CO in a large number
2Fat compound in the fluid will be separated.By regulating separator pressure, temperature, a large amount of fat compounds is separated out from separator 1, have only a spot of fat compound from separator 2, to separate out.And CO
2Fluid is got back to condenser behind flowmeter, clarifier, form circulation.
The present invention liquid CO
2Supercritical extract melissa powder, the fat compound that obtains contain a large amount of different types of unrighted acids, have the immunity of enhancing and other health care.Lipoid material has quality better in the melissa powder that extraction obtains simultaneously, and cost is low, and effectively recovery rate height (can reach more than 97%) is saved raw material, and the product quality height does not contain advantages such as residual organic solvent.Because CO
2Flow velocity is big, and an inventory big (10-50kg) can satisfy the large-scale industrial production demand.
If the disclosed technical scheme of the present invention and CN1052417A is compared, as can be seen, the present invention extracts fat compound from handle different (about 2%-8%) melissa powder of (10～100 order), water content through granulation behind the different broken walls, another is that to extract one from the melissa powder be the fresh-keeping pollen of deodorization, sterilization, the goal of the invention difference of two technical schemes, raw material and effective object difference, the product of acquisition, productive rate etc. are all different.
If the disclosed technical scheme of the present invention and CN1307092A is compared, fat compound, CO in the leaching process are extracted in the present invention's industrialization from handle the different melissa powder of physicochemical properties such as (10～100 order), water content difference (about 2%-8%) and viscosity through granulation behind the different broken walls as can be seen
2Flow is obviously different, leaching process there are differences, set concrete separation parameter simultaneously, the product that obtains is the melissa powder of degreasing and the fat compound that extracts, effective recovery rate of the present invention is up to more than 97%, the goal of the invention difference of two technical schemes, raw material and effective object difference, technical method difference, the product composition of acquisition and effect of extracting etc. are also different.
If the disclosed technical scheme of the present invention and CN1733009 is compared, the present invention is from handling industrialization extraction fat compound (10～100 order) melissa powder, CO in the leaching process through granulation behind the different broken walls as can be seen
2Flow is obviously different, has added entrainer in the leaching process, has set concrete separation parameter simultaneously, makes in the final separator 1 that the ratio of gained fat compound quality is 10-100 in the gained fat compound quality and separator 2: 1.Two production scale differences that technical scheme is fit to, raw material is handled different, the process route difference.
The specific embodiment:
Embodiment 1:
Earlier be 8% with the 10kg water content, sporoderm-broken rate is that 98% melissa powder carries out granulation, is that 10 purpose melissa powder raw materials are inserted CO again with granularity
2In the supercritical extraction unit, extractor and separator are provided with the chuck with hot water heating and maintenance constant temperature, are 99.9% CO by the next purity of circulation
2After condenser condenses is liquid, enter the high-pressure pump pressurization, by entering extractor after the heater heating, fully contact with 10 purpose melissa powder granulating raw materials.In temperature is that 65 ℃, pressure are 20MPa, CO
2Flow velocity is under the condition of 380kg/h, cycling extraction 0.5 hour, and regulating separator 1 pressure is 5.8MPa, finishes single extraction and separates, and gets the single extraction product; To pump into extractor with respect to the edible alcohol of 10 order melissa powder raw material weight 5% again, be that 65 ℃, pressure are 20MPa, CO in temperature
2Flow velocity is under the condition of 380kg/h, continues cycling extraction 1 hour, regulates separator 1 pressure then to 7MPa, and temperature is 40 ℃, finishes reextraction and separates, and gets the reextraction product; Merge once, reextraction separate in separator 1 product of separating out, product.During reextraction in the separator 1 not separated mixture send separator 2, regulating separator 2 pressure is 5.8MPa, temperature is 25 ℃, the edible alcohol after separating with the mixture of fat compound as the entrainer of extraction next time.In the single extraction separator in gained fat compound quality and the reextraction separator ratio of gained fat compound quality be 100: 1; CO after the separation
2Send CO
2Gas tank is reused after being liquid through clarifier, condenser condenses.
Embodiment 2:
Earlier be 2% with the 30kg water content, sporoderm-broken rate is that 86% melissa powder carries out granulation, is that 100 purpose melissa powder raw materials are inserted CO again with granularity
2In the supercritical extraction unit, extractor and separator are provided with the chuck with hot water heating and maintenance constant temperature, are 99.9% CO by the next purity of circulation
2After condenser condenses is liquid, enter the high-pressure pump pressurization, by entering extractor after the heater heating, fully contact with 100 purpose melissa powder granulating raw materials.In temperature is that 50 ℃, pressure are 50MPa, CO
2Flow velocity is under the condition of 280kg/h, continuous extraction 1 hour, and regulating separator 1 pressure is 6.4MPa, finishes single extraction and separates, and gets the single extraction product; To pump into extractor with respect to the edible alcohol of 100 order melissa powder raw material weight 12% again, be that 50 ℃, pressure are 50MPa, CO in temperature
2Flow velocity is under the condition of 280kg/h, continues cycling extraction 0.5 hour, regulates separator 1 pressure then to 14MPa, and temperature is 60 ℃, finishes reextraction and separates, and gets the reextraction product; Merge once, reextraction separate in separator 1 product of separating out, product.During reextraction in the separator 1 not separated mixture send separator 2, regulating separator 2 pressure is 6.4MPa, temperature is 30 ℃, the edible alcohol after separating with the mixture of fat compound as the entrainer of extraction next time.In the single extraction separator in gained fat compound quality and the reextraction separator ratio of gained fat compound quality be 50: 1; CO after the separation
2Send CO
2Gas tank is reused after being liquid through clarifier, condenser condenses.
Embodiment 3:
Earlier be 5% with the 50kg water content, sporoderm-broken rate is that 90% melissa powder carries out granulation, is that 50 purpose melissa powder raw materials are inserted CO again with granularity
2In the supercritical extraction unit, extractor and separator are provided with the chuck with hot water heating and maintenance constant temperature, are 99.9% CO by the next purity of circulation
2After condenser condenses is liquid, enter the high-pressure pump pressurization, by entering extractor after the heater heating, fully contact with 50 purpose melissa powder granulating raw materials.In temperature is that 45 ℃, pressure are 35MPa, CO
2Flow velocity is under the condition of 320kg/h, cycling extraction 45 minutes, and regulating separator 1 pressure is 6.0MPa, finishes single extraction and separates, and gets the single extraction product; To pump into extractor with respect to the edible alcohol of 50 order melissa powder raw material weight 8% again, be that 45 ℃, pressure are 35MPa, CO in temperature
2Flow velocity is under the condition of 320kg/h, continues cycling extraction 40 minutes, regulates separator 1 pressure then to 10MPa, and temperature is 50 ℃, finishes reextraction and separates, and gets the reextraction product; Merge once, reextraction separate in separator 1 product of separating out, product.During reextraction in the separator 1 not separated mixture send separator 2, regulating separator 2 pressure is 6.0MPa, temperature is 25 ℃, the edible alcohol after separating with the mixture of fat compound as the entrainer of extraction next time.In the single extraction separator in gained fat compound quality and the reextraction separator ratio of gained fat compound quality be 60: 1; CO after the separation
2Send CO
2Gas tank is reused after being liquid through clarifier, condenser condenses.
Claims (4)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100164603A CN101103805B (en) | 2007-08-09 | 2007-08-09 | Industrial producing method for extracting fatty compound from melissa pollen |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100164603A CN101103805B (en) | 2007-08-09 | 2007-08-09 | Industrial producing method for extracting fatty compound from melissa pollen |
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| Publication Number | Publication Date |
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| CN101103805A true CN101103805A (en) | 2008-01-16 |
| CN101103805B CN101103805B (en) | 2011-04-06 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2007100164603A Expired - Fee Related CN101103805B (en) | 2007-08-09 | 2007-08-09 | Industrial producing method for extracting fatty compound from melissa pollen |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103540397A (en) * | 2012-07-13 | 2014-01-29 | 北京市蜂业公司 | Extraction method of fat substances rich in pollen |
| CN103610717A (en) * | 2013-12-11 | 2014-03-05 | 哈药集团中药二厂 | Preparation and purification method for bee pollen and acanthopanax senticosus compound extract through supercritical CO2 extraction and organic solvent extraction |
| CN108310797A (en) * | 2018-04-09 | 2018-07-24 | 南通市华安超临界萃取有限公司 | A kind of supercritical fluid recrystallization device |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100443579C (en) * | 2006-06-07 | 2008-12-17 | 中国农业科学院蜜蜂研究所 | Method for extracting bee pollen oil by supercritical fluid |
-
2007
- 2007-08-09 CN CN2007100164603A patent/CN101103805B/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103540397A (en) * | 2012-07-13 | 2014-01-29 | 北京市蜂业公司 | Extraction method of fat substances rich in pollen |
| CN103540397B (en) * | 2012-07-13 | 2015-01-21 | 北京市蜂业公司 | Extraction method of fat substances rich in pollen |
| CN103610717A (en) * | 2013-12-11 | 2014-03-05 | 哈药集团中药二厂 | Preparation and purification method for bee pollen and acanthopanax senticosus compound extract through supercritical CO2 extraction and organic solvent extraction |
| CN103610717B (en) * | 2013-12-11 | 2016-03-09 | 哈药集团中药二厂 | A kind of preparation and purification process adopting SCF-CO 2, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract |
| CN108310797A (en) * | 2018-04-09 | 2018-07-24 | 南通市华安超临界萃取有限公司 | A kind of supercritical fluid recrystallization device |
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| CN101103805B (en) | 2011-04-06 |
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