CN109504531A - A kind of CO2The method of grease in supercritical extract microalgae - Google Patents
A kind of CO2The method of grease in supercritical extract microalgae Download PDFInfo
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- CN109504531A CN109504531A CN201710834844.XA CN201710834844A CN109504531A CN 109504531 A CN109504531 A CN 109504531A CN 201710834844 A CN201710834844 A CN 201710834844A CN 109504531 A CN109504531 A CN 109504531A
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- Prior art keywords
- algae powder
- micro
- extraction
- algae
- oil
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Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0292—Treatment of the solvent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D2011/007—Extraction using a solvent in the gas phase
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
- Fats And Perfumes (AREA)
Abstract
The present invention relates to a kind of CO2The method of grease in supercritical extract microalgae comprising be used for CO after dispersing agent is added in micro- algae powder2The step of supercritical extract.After dispersing agent is added in algae powder, the dispersant particle for being dispersed in the rigidity inside algae powder will not be deformed when by high pressure, and the active force between dispersant particle and between dispersing agent and algae powder is supported the shape of entire algae powder-dispersant system, because of mutual extruding hardened phenomenon does not occur for algae powder in extraction process, Co 2 supercritical fluid can smoothly enter in frustule and therefrom dissolve out algae oil, thus can shorten supercritical CO2The time of fluid extraction algae oil.
Description
Technical field
The present invention relates to algae oils to extract field, more specifically it relates to a kind of CO2The side of grease in supercritical extract algae powder
Method.
Background technique
It is always the research neck for utilizing microalgae production high added value fatty acid or biodiesel that algae oil is extracted from frustule
Hot spot in domain.
In general, extracting algae oil from frustule using the method for extraction.Traditional extracting process is that first broken algae is thin
Then born of the same parents are added extract liquor extraction, separate organic phase, obtain grease after evaporating solvent.This method extracts algae oil recovery rate
It is very high, but it is cumbersome, and step is more, to expend a large amount of manpower and material resources.Especially after expansion scale, extraction cost is especially high.
Further, since the use of organic solvent, it is likely that lead to residual organic solvent in the algae oil extracted, if extracted algae oil is
It is used as the additive of food or feed, there will be there may be the hidden danger to humans and animals health.
Supercritical CO2The principle of fluid extraction is the relationship of the solvability and its density using supercritical fluid, i.e., sharp
Influence with pressure and temperature to supercritical fluid solvability and carry out.In the supercritical state, by supercritical fluid with
Substance contact to be separated, extracts it selectively the ingredient of polarity size, boiling point height and molecular size range successively
Out.Certainly, corresponding each obtained extract of pressure limit is unlikely to be single, but can control condition and most preferably compared
Then the blending constituent of example makes supercritical fluid become common gases by the method for decompression, heating, extracted substance is then complete
Or basic precipitation, thereby achieving the purpose of separation and purification, so supercritical CO2Fluid extraction process is by extraction and separation process
It is composed.
Supercritical CO2The advantages of fluid extraction is: 1) basic do not use may be to the harmful organic solvent of human or animal；
2) cost is relatively low, and the separation of extractant is easy to.Therefore, the albumen, grease, polysaccharide which is frequently utilized in microalgae etc.
It extracts.Due to being directly powdery after microalgae separation drying, more solution is crushed.
Use supercritical CO2During ingredient in fluid extraction microalgae, in order to keep CO2Supercriticality, need
Using High Voltage, this will lead to, and algae powder is hardened, to hinder the contact of supercritical fluid with algae powder.In the prior art, it solves
The method of this problem is to extend extraction time in kettle.In general, using routine CO2In the method for supercritical extract algae oil,
CO2The extraction time of fluid is 30-60min, and pressure is maintained at 25-35MPa.High pressure is maintained for a long time, and instrument and equipment is consumed
Damage is serious, influences the service life of instrument and equipment, and consuming energy.
Therefore, it is necessary to a kind of new extracting process to shorten CO2The extraction time of supercritical fluid.
Summary of the invention
In order to solve the above problem, the present invention provides a kind of CO2The method of grease in supercritical extract microalgae comprising
CO is used for after dispersing agent is added in micro- algae powder2The step of supercritical extract.
After dispersing agent is added in algae powder, the dispersant particle of the rigidity inside algae powder is dispersed in by height
It will not be deformed when pressure, and the active force between dispersant particle and between dispersing agent and algae powder makes entire algae powder-
The shape of dispersant system is supported, and because of mutual extruding hardened phenomenon does not occur for algae powder in extraction process,
Co 2 supercritical fluid can smoothly enter in frustule and therefrom dissolve out algae oil, thus can shorten supercritical CO2Fluid
Extract the time of algae oil.
In a preferred embodiment, the dispersing agent is the two of 10-2000 μm of partial size that adsorption has vegetable oil
Silicon oxide particle.Vegetable oil can improve extraction efficiency as entrainer.
In one embodiment, the vegetable oil is one of corn oil, soybean oil, peanut oil or other plant oil
Or multiple combinations.
In one embodiment, the dispersing agent obtains by the following method: adding in Xiang Suoshu silica dioxide granule
It by the vegetable oil of the total restatement 1-5% of the silica dioxide granule, is uniformly mixed, adsorbs the silica particles
The vegetable oil.The vegetable oil that silica dioxide granule large specific surface area is then added is more, and silica dioxide granule specific surface area is small then to be added
The vegetable oil entered is few.
In one embodiment, comprising the following steps:
S1: micro- algae powder is prepared；
S2: the dispersing agent is prepared；
S3: by micro- algae powder with by micro- total restatement 5-20% of algae powder the dispersant it is uniform, obtain
To algae powder-mixture of dispersing agents；
S4: the algae powder-mixture of dispersing agents is put into extraction kettle and carries out CO2Supercritical fluid extraction.
In an embodiment, S1, micro- algae powder from microalgae culture by collecting frustule and dry
It arrives, the water content of micro- algae powder is not higher than 5%.Water content is also one of the reason for causing algae powder hardened, lower aqueous
It is hardened that rate can be such that algae powder is less easy.
In one embodiment, in S4, the CO2The condition of supercritical fluid extraction are as follows: 35-45 DEG C of temperature, extraction
Pressure is 25-35MPa, CO2Flow is 250~300Lh-1, extraction time 15-20min.CO in the prior art2Shooting flow
The time of body extraction algae oil is generally 30-60min, and the present invention is by preventing algae powder is hardened from shortening CO2Supercritical fluid enters
Time in frustule improves work efficiency to reducing extraction time to 15-20min, reduces energy consumption and equipment damage
Consumption.
In a specific embodiment, the microalgae is schizochytrium.
Detailed description of the invention
Fig. 1 is the extraction yield statistical chart of method and conventional method of the invention under different extraction times.
Specific embodiment
Hereinafter principles and features of the present invention are described by taking schizochytrium as an example, example is served only for explaining this
Invention, is not intended to limit the scope of the present invention.
1. preparing algae powder
The schizochytrium culture for being cultivated and being induced oil-producing is collected, after algal gel is lyophilized, moisture content is dried into and is lower than
5%, algae powder can agglomerate when due to drying, so for being crushed one time again with pulverizer, obtaining dry algae before extracting
Powder.It is extracted and is detected by organic solvent, learn that its oil content is 39.7%.
2. preparing desiccant
Appropriate silica coarse crystal is taken, partial size presses silica between 10-2000 μm, in plane of crystal sprinkling
The total restatement 1-5% vegetable oil of particle (including corn oil, soybean oil, peanut oil, sprinkling, crystal large specific surface area then increase plant
Oil content, crystal specific surface area is small, then reduces content of vegetable oil).
3. algae powder is mixed with desiccant
It by the silica crystals of adsorption vegetable oil, is mixed with algae powder, obtains algae powder-mixture of dispersing agents, the two
Mass ratio is 5-20%, determines that adding proportion, large specific surface area then reduce ratio also according to the specific surface area of crystal, compares table
Area is small, then increases ratio.
4.CO2Supercritical fluid extraction
Algae powder-mixture of dispersing agents is put into extraction kettle, CO is carried out2Supercritical fluid extraction, extraction conditions are as follows: temperature
35-45 DEG C, extracting pressure 25-35MPa, CO2Flow is 250-300L h-1, extraction time 15-20min.
It compares in the conventional way, extracts different time, Comparing extraction rate.
The grease obtained weight of extraction yield=extraction/algae powder weight
As a result as shown in Figure 1, using the method for the present embodiment after extraction time is in 15min or more, extraction yield reaches
35% or more, when extraction time is to 20min or more, extraction yield is stablized 38% or so.And conventional method is used to carry out CO2It is super
Supercritical fluid extraction needs extraction time in 30min or more, can be only achieved satisfied extraction results.As it can be seen that this implementation
The CO that the method for example greatly shortens2The extraction time of supercritical fluid.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of CO2The method of grease in supercritical extract microalgae, which is characterized in that be included in micro- algae powder and dispersion is added
CO is used for after agent2The step of supercritical extract.
2. the method according to claim 1, wherein the dispersing agent is the partial size that adsorption has vegetable oil
10-2000 μm of silica dioxide granule.
3. according to the method described in claim 2, it is characterized in that, the vegetable oil be corn oil, soybean oil, peanut oil or its
One of his vegetable oil or multiple combinations.
4. according to the method described in claim 2, it is characterized in that, the dispersing agent obtains by the following method: Xiang Suoshu bis-
The vegetable oil of the total restatement 1-5% of the silica dioxide granule is pressed in addition in silicon oxide particle, is uniformly mixed, is made the dioxy
Vegetable oil described in silicon carbide particle adsorption.
5. the method according to claim 1, wherein the following steps are included:
S1: micro- algae powder is prepared；
S2: the dispersing agent is prepared；
S3: by micro- algae powder with by micro- total restatement 5-20% of algae powder the dispersant it is uniform, obtain algae
Powder-mixture of dispersing agents；
S4: the algae powder-mixture of dispersing agents is put into extraction kettle and carries out CO2Supercritical fluid extraction.
6. according to the method described in claim 5, it is characterized in that, micro- algae powder passes through from microalgae culture in S1
It collects frustule and is dried to obtain, the water content of micro- algae powder is not higher than 5%.
7. according to method described in claim 5, which is characterized in that in S4, the CO2The condition of supercritical fluid extraction are as follows: temperature
35-45 DEG C of degree, extracting pressure 25-35MPa, CO2Flow is 250~300L h-1, extraction time 15-20min.
8. method according to any one of claims 1-7, which is characterized in that the microalgae is schizochytrium.
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| CN201710834844.XA CN109504531A (en) | 2017-09-15 | 2017-09-15 | A kind of CO2The method of grease in supercritical extract microalgae |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110029019A (en) * | 2019-05-06 | 2019-07-19 | 浙江师范大学 | The method that supercritical carbon dioxide carries ethyl alcohol extraction microalgae grease secretly |
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| CN103347998A (en) * | 2011-02-11 | 2013-10-09 | 纳幕尔杜邦公司 | Method for forming and extracting solid pellets comprising oil-containing microbes |
| CN104206562A (en) * | 2014-09-17 | 2014-12-17 | 南京以标能源有限责任公司 | Method for preparing DHA (Docosahexaenoic acid)-enriched vegetable oil by adopting one-step process |
| CN106190543A (en) * | 2016-07-13 | 2016-12-07 | 甘肃长清生物科技有限责任公司 | A kind of method of subcritical fluid extraction Semen Lini oil |
-
2017
- 2017-09-15 CN CN201710834844.XA patent/CN109504531A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103347998A (en) * | 2011-02-11 | 2013-10-09 | 纳幕尔杜邦公司 | Method for forming and extracting solid pellets comprising oil-containing microbes |
| CN104206562A (en) * | 2014-09-17 | 2014-12-17 | 南京以标能源有限责任公司 | Method for preparing DHA (Docosahexaenoic acid)-enriched vegetable oil by adopting one-step process |
| CN106190543A (en) * | 2016-07-13 | 2016-12-07 | 甘肃长清生物科技有限责任公司 | A kind of method of subcritical fluid extraction Semen Lini oil |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110029019A (en) * | 2019-05-06 | 2019-07-19 | 浙江师范大学 | The method that supercritical carbon dioxide carries ethyl alcohol extraction microalgae grease secretly |
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