CN102643714A - Method for extracting microalgal oil by supercritical CO2 isothermal transformation technology - Google Patents
Method for extracting microalgal oil by supercritical CO2 isothermal transformation technology Download PDFInfo
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- CN102643714A CN102643714A CN2012100611129A CN201210061112A CN102643714A CN 102643714 A CN102643714 A CN 102643714A CN 2012100611129 A CN2012100611129 A CN 2012100611129A CN 201210061112 A CN201210061112 A CN 201210061112A CN 102643714 A CN102643714 A CN 102643714A
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Abstract
The invention relates to a method for extracting microalgal oil by supercritical CO2 isothermal transformation technology. The method comprises the steps of: removing impurities in dried microalgae, and then crushing and grinding; putting the ground microalgae dry powder into an extraction kettle, filling supercritical CO2 into the extraction kettle, and extracting under the conditions that the pressure is 12-25MPa, the temperature is 34-42 DEG C and the time is 150-180min; carrying out isothermal decompression separation on the supercritical CO2 containing solute successively by two stages of separators; and collecting fatty acid oil extract separated out from the bottoms of the two stages of separators to obtain the product. According to the method, organic solvent is not needed in the whole process, so that no residual solvent exits in the extract, and oxidation and thermal cracking are not caused in the extraction process; the oil is high in yield and purity; the product is excellent in quality; the whole set of technology is simple in operation and does not have corresponding post-processing requirement. Meanwhile, the method prevents the microalgal oil from poisoning the human body and polluting the environment in the extracting process.
Description
Technical field
The present invention relates to little algae fatty acid grease extraction, particularly a kind of supercritical CO of using
2The method of isothermal pressure-changing technology extraction microalgae grease.
Background technology
Along with global economy development and population growth, grease is more and more closer with human relation, no matter is as the raw material of biofuel or is processed into protective foods, and grease all has crucial effects.At present, greasy main source remains plant and animal tallow, and still this traditional oil source can not satisfy the various demands in the lives such as people are edible, industry fully.It is high that yet many little algaes contain oil quantity, and according to conservative estimation, the little algae of annual per hectare can produce 30000～50000L grease, and the rich oil plant, like palm and manioca etc., the grease yield of annual per hectare is merely 1300～2400L.
Little algae is to have characteristics such as photosynthetic efficiency height, adaptive capacity to environment is strong, growth is fast, the cycle is short, through illumination, CO are provided
2, simple basic condition such as nutritive medium, water body, just can reach the effect of rapid amplifying breeding, particularly through regulating and control the grease that cultured microalgae can reach high level.Under ideal growth conditions or advantageous environment, the little algae of produce oil only produces a spot of triglyceride level (greasy staple).When the little algae of produce oil is in when stimulating under the unfavourable condition that causes by chemistry or physical environment, synthetic glycerine three esters in a large number, the remarkable change of simultaneous grease and fatty acid component.The grease composition of most of little algaes is mainly triglyceride level and C
14～C
22Longer chain fatty acid, wherein lipid acid is with C
16With C
18Be that lipid acid is main.Little phycobiont is small, and cell walls is abundant mostly, and the oil extraction operating process is wasted time and energy, and needs to consume a large amount of organic extractants.Thereby the technological method of research extraction microalgae grease has important practical usage, more and more receives the extensive concern of Chinese scholars.At present, both at home and abroad the process for extracting of microalgae grease is different, and extraction effect is very different, like extraction process microalgae grease with an organic solvent, has the dissolvent residual problem.
Supercritical CO
2Fluid extraction technology is the stripping technique of new generation of at present domestic and international separate study exploitation; Products obtained therefrom does not have organic contamination, can keep the thermo-sensitivity composition preferably; Product purity is high, yield is high, particularly suitable extracts the effective constituent in the natural animal-plant, is one of important production technique in current " green health " engineering.Supercritical CO
2Be to use the widest supercutical fluid, pure CO
2Emergent pressure be 7.39MPa, critical temperature is 31.06 ℃, is in the CO of emergent pressure and the above state of critical temperature
2Be called as supercritical CO
2Supercritical CO
2Molecular force very little, be similar to gas; And density is very big, approaches liquid, is the state that a kind of gas-liquid is regardless of.Supercritical CO
2Have good mass transfer characteristic, the solute dissolution rate is much faster than liquid, and is more much bigger than gas to the dissolving and the carrying capacity of solid matter.Near stagnation point, the subtle change of pressure and temperature can cause that also some material is at CO
2The very big variation of middle dissolving power.
Supercritical CO
2The isothermal pressure-changing abstraction technique utilizes its special transitive attribute just, and reach material is carried out isolating purpose.Usually after material was dissolved in supercutical fluid (SCF), the maintenance system was temperature-resistant, reduced system pressure, and the solubleness of solute is obviously reduced, thereby with solute and separated from solvent.Compare with traditional SX, supercritical fluid extraction (SFE) has the purity height, and yield is big, good quality of product, and subsequent technique is handled characteristic of simple.Compare with conventional distillation method stripping technique, SFE has that a whole set of technology is succinct, simple to operate, no solvent residue and advantages such as corresponding aftertreatment requirement, energy-saving and environmental protection.
Summary of the invention
The technical problem that the present invention will solve is to the defective of existing microalgae grease extractive technique, and a kind of productive rate, good quality of product that improves fatty acid grease is provided, and grease purity is high uses supercritical CO
2The method of isothermal pressure-changing technology extraction microalgae grease.
The present invention solves the problems of the technologies described above with following technical scheme: its process step is following:
(1) raw materials pretreatment: after the little algae removal of impurities of exsiccant, pulverize, grind, cross 150～250 mesh sieves, screen underflow is little algae dry powder;
(2) load: the little algae dry powder after will pulverizing is packed in the extraction kettle;
(3) extraction: with supercritical CO
2Inject extraction kettle, make the pressure in the extraction kettle remain on 12～25MPa; Extraction temperature remains on 34～42 ℃ in the still, and the extraction time is 150～180min;
(4) separate: after extraction finishes, carry the supercritical CO of solute
2Successively be depressured to 8～15MPa through the primary separator isothermal, the second-stage separator isothermal is depressured to 6～7MPa, collects the fatty acid grease extract of separating out at the bottom of the I and II separator still.
The described little algae dry powder particle degree preferred value of step (1) is 200 orders.
It is 80～85% that the described extraction kettle of step (2) is loaded coefficient.
The described extraction preferred value of step (3) is: pressure 20MPa, 36 ℃ of temperature, time 180min.
The described isolating preferred value of step (4) is: the primary separator isothermal is depressured to 10MPa, and the second-stage separator isothermal is depressured to 6MPa.
Method whole process of the present invention need not used organic solvent, so extract noresidue solvent, and extraction process oxidation can not take place; Also thermo-cracking can not take place, the grease yield is high, purity is high, good quality of product; A whole set of technology is succinct, simple to operate, does not have corresponding aftertreatment requirement.Simultaneously prevented also that extraction process is to the murder by poisoning of human body with to the pollution of environment.
Description of drawings
Fig. 1 uses supercritical CO for the present invention
2The process flow sheet of the method for isothermal pressure-changing technology extraction microalgae grease.
Among Fig. 1: 1-CO
2Storage tank, 2-high pressure compressor, 3-water cooler, 4-pressure, temperature survey, 5-reducing valve, 6-extraction kettle, 7-waste residue scoop, 8-well heater, 9-primary separator, 10-second-stage separator, 11-strainer, 12-surge tank, 13-recycle compressor.
Embodiment
The present invention uses supercritical CO
2Should consider that factors such as raw material pulverizing granularity, extraction temperature, extracting pressure, extraction kettle amount of fill and extraction time are to the influence of oil extraction yield in the method for fluid isothermal pressure-changing technology extraction microalgae grease.Through the experimental study analysis revealed:
The size and the oily yield of 1. little algae crushed particles degree have direct relation.Because granularity is more little, mass transfer area is big more, and more microalgae plant cell wall is broken, and helps extraction;
2. condition one such as keep-uping pressure regularly, recovery of extraction reduces along with the rising gradually of temperature, and the recovery is maximum in the time of 36 ℃;
3. change and other conditions when remaining unchanged as pressure 12～25MPa, the recovery big rangeability can occur with the variation of pressure: pressure continues to raise, and the recovery has increase, but amplification can be more and more littler;
4. the extraction kettle filling is to measure 80～85% to be advisable; The extraction time is controlled at 150～180min and is advisable.
Its concrete process step is following:
1. raw materials pretreatment: the size and the oily yield of little algae crushed particles degree have direct relation.Granularity is more little, and mass transfer area is big more, and more microalgae plant cell wall is broken, and helps extraction.After the little algae removal of impurities of exsiccant, in kibbler, to pulverize, and, cross 150～250 mesh sieves (particle diameter 106～58 μ m) through grinding, screen underflow is little algae dry powder;
2. load: the little algae dry powder after will pulverizing is packed in the extraction kettle, and in order to make full use of high-pressure space, the filling coefficient of extraction kettle gets 80～85%;
3. extraction: with supercritical CO
2Inject extraction kettle, make the pressure in the extraction kettle remain on 12～25MPa; Extraction temperature remains on 34～42 ℃ in the still, and the extraction time is 150～180min;
4. separate: after extraction finishes, carry the supercritical CO of solute
2Successively through the primary separator isothermal be depressured to 8～15MPa, the second-stage separator isothermal is depressured to 6～7MPa, collect the fatty acid grease extract of separating out at the bottom of the I and II separator still and promptly get product.
Embodiment 1:
1. raw materials pretreatment
Little algae dried feed is pulverized and is ground through the removal of impurity, crosses 150 mesh sieves (particle diameter 106 μ m), takes off screen underflow, treats supercritical extraction.
2. little algae is loaded
The thin dry powder of little algae after pulverizing is packed in the extraction kettle 6, load coefficient and get 80%, load the sealing cover of building extraction kettle after accomplishing.
3. extraction
With CO
2The CO of storage tank 1
2Reach after the supercritical state through high pressure compressor 2 compressions, water cooler 3 coolings, inject extraction kettle 6 and extract.Pressure in the extraction kettle keeps 18MPa, and extraction temperature remains on 38 ℃, and the extraction time is controlled at 150min.
4. grease separates
After extracting operation was accomplished, the extraction leftover in the extraction kettle 6 was discharged through bottom collector 7, the supercritical CO in the still
2After carrying 5 step-downs of extract process reducing valve, well heater 8 heat temperature raisings, successively get into primary separator 9, second-stage separator 10.In the primary separator 9, temperature keeps 38 ℃, and pressure drops to 8MPa, the CO that steams
2Discharge from the top, the oil extraction thing is separated out at the bottom of still gradually, but still contains a large amount of CO
2Therefore, need to carry out the secondary isothermal step-down through second-stage separator 10 again and separate, pressure remains on 6MPa, and residue is final extract at the bottom of second-stage separator 10 stills.
Whole supercritical CO
2Extracting system is a round-robin system continuously, from the CO of primary separator 9, second-stage separator 10 top pressure releases discharges
2,, return CO by recycle compressor 13 through strainer 11 and surge tank 12
2In the storage tank 1, supply systemic circulation to use.
Embodiment 2:
1. raw materials pretreatment
Little algae dried feed is pulverized and is ground through the removal of impurity, crosses 200 mesh sieves (particle diameter 75 μ m), takes off screen underflow, treats supercritical extraction.
2. little algae is loaded
The thin dry powder of little algae after pulverizing is packed in the extraction kettle 6, load coefficient and get 85%, load the sealing cover of building extraction kettle after accomplishing.
3. extraction
With CO
2The CO of storage tank 1
2Through high pressure compressor 2 compressions, water cooler 3 coolings reach after the supercritical state, inject extraction kettle 6 and extract.Pressure in the extraction kettle keeps 20MPa, and extraction temperature remains on 42 ℃, and the extraction time is controlled at 160min.
4. grease separates
After extracting operation was accomplished, the extraction leftover in the extraction kettle 6 was discharged through bottom collector 7, the supercritical CO in the still
2After carrying 5 step-downs of extract process reducing valve, well heater 8 heat temperature raisings, successively get into primary separator 9, second-stage separator 10.In the primary separator 9, temperature keeps 42 ℃, and pressure drops to 12MPa, the CO that steams
2Discharge from the top, the oil extraction thing is separated out at the bottom of still gradually, but still contains a large amount of CO
2Therefore, need to carry out the secondary isothermal step-down through second-stage separator 10 again and separate, pressure remains on 6MPa, and residue is final extract at the bottom of separator 10 stills.
The recycle system is with embodiment 1.
Embodiment 3:
1. raw materials pretreatment
Little algae dried feed is pulverized and is ground through the removal of impurity, crosses 250 mesh sieves (particle diameter 58 μ m), takes off screen underflow, treats supercritical extraction.
2. little algae is loaded
The thin dry powder of little algae after pulverizing is packed in the extraction kettle 6, load coefficient and get 83%, load the sealing cover of building extraction kettle after accomplishing.
3. extraction
With CO
2The CO of storage tank 1
2Through high pressure compressor 2 compressions, water cooler 3 coolings reach after the supercritical state, inject extraction kettle 6 and extract.Pressure in the extraction kettle keeps 25MPa, and extraction temperature remains on 34 ℃, and the extraction time is controlled at 180min.
4. grease separates
After extracting operation was accomplished, the extraction leftover in the extraction kettle 6 was discharged through bottom collector 7, the supercritical CO in the still
2After carrying 5 step-downs of extract process reducing valve, well heater 8 heat temperature raisings, successively get into primary separator 9, second-stage separator 10.In the primary separator 9, temperature keeps 34 ℃, and pressure drops to 15MPa, the CO that steams
2Discharge from the top, the oil extraction thing is separated out at the bottom of still gradually, but still contains a large amount of CO
2Therefore, need to carry out the secondary isothermal step-down through second-stage separator 10 again and separate, pressure remains on 7MPa, and residue is final extract at the bottom of separator 10 stills.
The recycle system is with embodiment 1.
Claims (5)
1. use supercritical CO for one kind
2The method of isothermal pressure-changing technology extraction microalgae grease is characterized in that process step is following:
(1) raw materials pretreatment: after the little algae removal of impurities of exsiccant, pulverize, grind, cross 150～250 mesh sieves, screen underflow is little algae dry powder;
(2) load: the little algae dry powder after will pulverizing is packed in the extraction kettle;
(3) extraction: with supercritical CO
2Inject extraction kettle, make the pressure in the extraction kettle remain on 12～25MPa; Extraction temperature remains on 34～42 ℃ in the still, and the extraction time is 150～180min;
(4) separate: after extraction finishes, carry the supercritical CO of solute
2Successively be depressured to 8～15MPa through the primary separator isothermal, the second-stage separator isothermal is depressured to 6～7MPa, collects the fatty acid grease extract of separating out at the bottom of the I and II separator still.
2. the supercritical CO of using as claimed in claim 1
2The method of isothermal pressure-changing technology extraction microalgae grease is characterized in that the described little algae dry powder particle degree preferred value of step (1) is 200 orders.
3. the supercritical CO of using as claimed in claim 1
2The method of isothermal pressure-changing technology extraction microalgae grease is characterized in that it is 80～85% that the described extraction kettle of step (2) is loaded coefficient.
4. the supercritical CO of using as claimed in claim 1
2The method of isothermal pressure-changing technology extraction microalgae grease is characterized in that the described extraction preferred value of step (3) is: pressure 20MPa, 36 ℃ of temperature, time 180min.
5. the supercritical CO of using as claimed in claim 1
2The method of isothermal pressure-changing technology extraction microalgae grease, it is characterized in that the described isolating preferred value of step (4) is: the primary separator isothermal is depressured to 10MPa, and the second-stage separator isothermal is depressured to 6MPa.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104883901A (en) * | 2012-10-17 | 2015-09-02 | 索拉兹米罗凯特营养品有限责任公司 | Microalgal flour granules and process for preparation thereof |
| CN106635405A (en) * | 2016-12-13 | 2017-05-10 | 内蒙古金达威药业有限公司 | Method for realizing supercritical extraction of DHA (docosahexaenoic acid) oil from microalgae powder |
| KR20190029436A (en) * | 2017-09-12 | 2019-03-20 | 주식회사 엘지화학 | Method and apparatus for separating solvent |
| WO2019054671A1 (en) * | 2017-09-12 | 2019-03-21 | 주식회사 엘지화학 | Separation method and separation apparatus for solvent |
| US10264809B2 (en) | 2013-01-28 | 2019-04-23 | Corbion Biotech, Inc. | Microalgal flour |
| US10299500B2 (en) | 2013-11-29 | 2019-05-28 | Corbion Biotech, Inc. | Granules of protein-rich microalgal biomass flour and method for preparing same |
| US11559074B2 (en) | 2013-07-19 | 2023-01-24 | Corbion Biotech, Inc. | Lipid-rich microalgal flour and method for preparing same |
-
2012
- 2012-03-09 CN CN2012100611129A patent/CN102643714A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104883901A (en) * | 2012-10-17 | 2015-09-02 | 索拉兹米罗凯特营养品有限责任公司 | Microalgal flour granules and process for preparation thereof |
| US10264809B2 (en) | 2013-01-28 | 2019-04-23 | Corbion Biotech, Inc. | Microalgal flour |
| US11559074B2 (en) | 2013-07-19 | 2023-01-24 | Corbion Biotech, Inc. | Lipid-rich microalgal flour and method for preparing same |
| US10299500B2 (en) | 2013-11-29 | 2019-05-28 | Corbion Biotech, Inc. | Granules of protein-rich microalgal biomass flour and method for preparing same |
| CN106635405A (en) * | 2016-12-13 | 2017-05-10 | 内蒙古金达威药业有限公司 | Method for realizing supercritical extraction of DHA (docosahexaenoic acid) oil from microalgae powder |
| KR20190029436A (en) * | 2017-09-12 | 2019-03-20 | 주식회사 엘지화학 | Method and apparatus for separating solvent |
| WO2019054671A1 (en) * | 2017-09-12 | 2019-03-21 | 주식회사 엘지화학 | Separation method and separation apparatus for solvent |
| KR102201310B1 (en) | 2017-09-12 | 2021-01-11 | 주식회사 엘지화학 | Method and apparatus for separating solvent |
| US11083979B2 (en) | 2017-09-12 | 2021-08-10 | Lg Chem, Ltd. | Solvent separation method and solvent separation apparatus |
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Application publication date: 20120822 |