CN108300565A - A method of it is mixed fatty acid extracted from the wet algal gel of microalgae using subcritical water - Google Patents
A method of it is mixed fatty acid extracted from the wet algal gel of microalgae using subcritical water Download PDFInfo
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- CN108300565A CN108300565A CN201711381550.2A CN201711381550A CN108300565A CN 108300565 A CN108300565 A CN 108300565A CN 201711381550 A CN201711381550 A CN 201711381550A CN 108300565 A CN108300565 A CN 108300565A
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- microalgae
- water
- algal gel
- wet algal
- fatty acid
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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
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/02—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids from fats or fatty oils
- C11C1/04—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids from fats or fatty oils by hydrolysis
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Microbiology (AREA)
- General Chemical & Material Sciences (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Micro-Organisms Or Cultivation Processes Thereof (AREA)
Abstract
The invention discloses a kind of methods mixed fatty acid extracted from the wet algal gel of microalgae using subcritical water, belong to microalgae Biochemical Engineering technical field.The present invention utilizes more violent undercritical conditions, to destroy the cell wall of microalgae, it realizes extraction grease in the wet frustule of slave microalgae rapidly and efficiently and hydrolyzes generation aliphatic acid, wherein, subcritical water is also used as hydrolysis agent as solvent, and environmental friendliness is high, avoids using and recycling for organic solvent, and the present invention directly utilizes the microalgae cell of High water cut, saves the highly energy-consumings link such as microalgae centrifugation, dry.
Description
Technical field
The invention belongs to microalgae Biochemical Engineering technical fields, and in particular to a kind of to be extracted from the wet algal gel of microalgae using subcritical water
The method of fatty acid mixed.
Background technology
Aliphatic acid is important organic chemical industry and fine chemical material, is answered extensively using the downstream derivative object that aliphatic acid is produced as raw material
Add for textile printing and dyeing, food, medicine, daily-use chemical industry, petrochemical industry, rubber and plastic processing, mining, communications and transportation, casting, metal
The various fields such as work, ink, coating and pigment.
Aliphatic acid mainly recycles tall oil through rectifying system from natural oil, paraffin oxidation or from pine papermaking wastewater
.Attention with countries in the world to ecological environment and environmental protection is cut down the protection and taboo of wildwood so that tall oil resource
Yield and quality decline year by year.The aliphatic acid produced at present from higher mammal and higher plant grease through hydrolysis, rectifying accounts for aliphatic acid
4/5 or more of total amount is the main source of world's aliphatic acid.However higher mammal and higher plant oil are similarly subjected to animals and plants life
The limitation of the factors such as long period, Heavy Metal Accumulation, the area that occupies cultivated land, ecological protection, constrains aliphatic acid industrial expansion.
Microalgae type is various and distribution is wide, is most simple ancient rudimentary plant, can directly utilize sunlight, CO2And N, P etc.
Simple nutriment fast-growth simultaneously synthesizes a large amount of greases (mainly triglycerides) in intracellular, does not strive ground with grain, does not strive with people
Water provides new oil resource for aliphatic acid production.It is micro- at present both at home and abroad it is believed that as a kind of new raw material of fatty acid
Algae development potentiality is huge.
The extraction of microalgae aliphatic acid includes two large divisions：Microalgae grease extracts and grease hydrolysis generates aliphatic acid.Wherein hydrolyze
Generate fatty technic acid and technique maturation, therefore the crucial skill in the extraction of microalgae grease always microalgae aliphatic acid industry
Art.There is the characteristics of cell small (between 2-20 μm), cell wall thickness in the high microalgae containing fat found in the world, increase microalgae oil
The difficulty of fat extraction.The extractive technique of existing microalgae grease includes：Organic solvent extraction, ultrasonic wave extraction, is oozed soxhlet type
Pressure extraction, mechanical breaking-wall method extraction, supercritical carbon dioxide extraction etc. thoroughly.These extractive techniques rest on laboratory rank more
Section, complex process, grease extraction efficiency be low, of high cost, high energy consumption, so very big that limit its industrialized application.At present using most
More is the solvent extraction of dry algae powder, and water content is up to 80% or more in microalgae cell, and the only energy consumption of drying process just makes micro-
The added value for the fatty acid product that algae is produced is extremely low.A kind of simple for process therefore, it is necessary to develop, energy consumption is relatively low, practical
Slave microalgae in mixed fatty acid extracted method.
Invention content
In view of the deficiencies of the prior art, utilize subcritical water from the wet algal gel of microalgae the purpose of the present invention is to provide a kind of
Mixed fatty acid extracted method, the present invention use water as spe medium and hydrolysis agent, avoid making for organic solvent
With and recycling, and the present invention directly utilizes the microalgae cell of High water cut, saves the highly energy-consumings link such as microalgae centrifugation, dry.
By a large number of experiments and unremitting effort, inventor is finally obtained the following technical solution：A kind of utilization is subcritical
Water method mixed fatty acid extracted from the wet algal gel of microalgae, the wet algal gel of microalgae is added into reaction kettle, and water conduct is added
Extraction medium is simultaneously passed through nitrogen, and setting reactor pressure is 3-40MPa, and temperature is 250-300 °C, reaction time 10-60min,
So that water is kept subcritical state, obtains hydrolysate after reaction（Croude fatty acids）, cleaned 1-10 times with hot distilled water, product
Afterwards in thermostatic drying chamber drying 2-48h to get to pure hydrolysate（Refined fat acid）；
The final volume ratio of the wet algal gel of microalgae and Extraction medium water is 1:0.5-20.
Preferably, a kind of method mixed fatty acid extracted from the wet algal gel of microalgae using subcritical water as described above,
The wet algal gel water content is 40-90%.
Preferably, a kind of method mixed fatty acid extracted from the wet algal gel of microalgae using subcritical water as described above,
The wet algal gel is obtained by centrifuging or filtering culture medium in advance.
Preferably, a kind of method mixed fatty acid extracted from the wet algal gel of microalgae using subcritical water as described above,
The microalgae is micro- quasi- ball algae, chlorella, scenedesmus, Chaetoceros, Phaeodactylum tricornutum, chrysophyceae, Du Shi algaes, splits pot algae, salt algae, silk
One or more of shape algae.
Compared with prior art, advantages of the present invention is：
1, the present invention realizes slave microalgae rapidly and efficiently using more violent undercritical conditions to destroy the cell wall of microalgae
Grease is extracted in wet frustule and hydrolyzes generation aliphatic acid；Wherein, subcritical water is also used as hydrolysis agent, ring as solvent
Border friendliness is high.
2, the present invention uses water as spe medium and hydrolysis agent, avoids using and recycling for organic solvent, and
The microalgae cell of High water cut can directly be utilized by extracting raw material, be not necessarily to the drying link of frustule, saved a large amount of energy consumption for drying.
3, aliphatic acid recovery rate of the present invention is high, separation is simple, is easy to amplify.
Specific implementation mode
For that can understand the technical characterstic for illustrating the present invention program with reference to specific embodiments be illustrated to the present invention.But
Protection scope of the present invention is not limited to these examples.It is every to include without departing substantially from the change of present inventive concept or equivalent substitute
Within protection scope of the present invention.
Embodiment 1
Weigh the wet algal gel 100g of chlorella（Water content 60%, initial total lipid content 19.7%）, the volume ratio of microalgae mud and water is 1:
1.5, it is placed in reaction kettle and seals, N is passed through into reaction kettle2To 1.5MPa, 280 °C are heated to, is pressurized to 12 MPa, when reaction
Between 0.5 hour, separating still collect product, microalgae conversion rate of fatty acid 94.2%.
For the wet algal gel of chlorella as first passing through in advance obtained by centrifugal treating, centrifugal condition is 3000 rpm, 30 min.
Embodiment 2
Weigh the wet algal gel 100g of chlorella（Water content 60%, initial total lipid content 19.7%, the wet same embodiment of algal gel preparation method
1）, add 140 mL of water, the volume ratio of microalgae mud and water is 1:5, it is placed in reaction kettle and seals, N is passed through into reaction kettle2Extremely
1.5MPa is heated to 300 °C, is pressurized to 20 MPa, 1 hour reaction time, and separating still collects product, microalgae conversion rate of fatty acid
90.3%。
Embodiment 3
Weigh micro- wet algal gel 100g of quasi- ball algae（Water content 50%, initial total lipid content 34.2%）, add 10 mL of water, microalgae mud and water
Volume ratio be 1:1.2, it is placed in reaction kettle and seals, N is passed through into reaction kettle2To 1.5MPa, 280 °C are heated to, is pressurized to
12 MPa, 0.5 hour reaction time, separating still collect product, microalgae conversion rate of fatty acid 97.6%.
Micro- quasi- wet algal gel of ball algae is obtained by filtering culture medium, and filter method is vacuum filtration.
Embodiment 4
Weigh micro- wet algal gel 100g of quasi- ball algae（Water content 50%, initial total lipid content 34.2%, the wet same embodiment of algal gel preparation method
3）, add 450 mL of water, the volume ratio of microalgae mud and water is 1:10, it is placed in reaction kettle and seals, N is passed through into reaction kettle2Extremely
1.5MPa is heated to 300 °C, is pressurized to 30 MPa, 1 hour reaction time, and separating still collects product, microalgae conversion rate of fatty acid
92.3%。
Embodiment 5
Weigh the wet algal gel 100g of scenedesmus（Water content 90%, initial total lipid content 30.7%, wet algal gel preparation method is the same as embodiment 1）,
Microalgae mud is 1 with water volume ratio:9, it is placed in reaction kettle and seals, N is passed through into reaction kettle2To 1.5MPa, 280 °C are heated to,
12 MPa, 0.5 hour reaction time are pressurized to, separating still collects product, microalgae conversion rate of fatty acid 89.7%.
Claims (4)
1. a kind of method mixed fatty acid extracted from the wet algal gel of microalgae using subcritical water, it is characterised in that：By microalgae
Wet algal gel is added into reaction kettle, and water is added and as Extraction medium and is passed through nitrogen, and setting reactor pressure is 3-40MPa, temperature
Degree is 250-300 °C, reaction time 10-60min, so that water is kept subcritical state, croude fatty acids is obtained after reaction, with heat
Distilled water cleans 1-10 time, dries 2-48h in thermostatic drying chamber to get to pure hydrolysis product purification aliphatic acid after product；
The final volume ratio of the wet algal gel of microalgae and Extraction medium water is 1:0.5-20.
2. a kind of method mixed fatty acid extracted from the wet algal gel of microalgae using subcritical water as described in claim 1,
It is characterized in that：The wet algal gel water content is 40-90%.
3. a kind of method mixed fatty acid extracted from the wet algal gel of microalgae using subcritical water as described in claim 1,
It is characterized in that：The wet algal gel is obtained by centrifuging or filtering culture medium in advance.
4. a kind of method mixed fatty acid extracted from the wet algal gel of microalgae using subcritical water as described in claim 1,
It is characterized in that：The microalgae is micro- quasi- ball algae, chlorella, scenedesmus, Chaetoceros, Phaeodactylum tricornutum, chrysophyceae, Du Shi algaes, splits pot
One or more of algae, salt algae, filamentous algae.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711381550.2A CN108300565A (en) | 2017-12-20 | 2017-12-20 | A method of it is mixed fatty acid extracted from the wet algal gel of microalgae using subcritical water |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109666536A (en) * | 2018-11-29 | 2019-04-23 | 河北中科汉禧生物科技有限公司 | The extracting method of omega-fatty acid |
| CN114736113A (en) * | 2022-04-08 | 2022-07-12 | 上海理工大学 | Method for hydrothermal extraction of unsaturated fatty acid in algae |
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| JP3644842B2 (en) * | 1998-03-30 | 2005-05-11 | 独立行政法人科学技術振興機構 | Method for producing organic acid from waste organic matter |
| CN103769205A (en) * | 2013-12-12 | 2014-05-07 | 中国海洋大学 | Preparation method of composite catalyst for hydrothermal liquefaction of oil-contained microalgae |
| CN103981017A (en) * | 2013-06-27 | 2014-08-13 | 中国科学院海洋研究所 | Method used for extracting oil from microalgae wet algae mud |
| CN105247020A (en) * | 2013-03-14 | 2016-01-13 | 藻类系统有限责任公司 | Systems and methods for hydrothermal conversion of biomass |
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2017
- 2017-12-20 CN CN201711381550.2A patent/CN108300565A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3644842B2 (en) * | 1998-03-30 | 2005-05-11 | 独立行政法人科学技術振興機構 | Method for producing organic acid from waste organic matter |
| CN105247020A (en) * | 2013-03-14 | 2016-01-13 | 藻类系统有限责任公司 | Systems and methods for hydrothermal conversion of biomass |
| CN103981017A (en) * | 2013-06-27 | 2014-08-13 | 中国科学院海洋研究所 | Method used for extracting oil from microalgae wet algae mud |
| CN103769205A (en) * | 2013-12-12 | 2014-05-07 | 中国海洋大学 | Preparation method of composite catalyst for hydrothermal liquefaction of oil-contained microalgae |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109666536A (en) * | 2018-11-29 | 2019-04-23 | 河北中科汉禧生物科技有限公司 | The extracting method of omega-fatty acid |
| CN114736113A (en) * | 2022-04-08 | 2022-07-12 | 上海理工大学 | Method for hydrothermal extraction of unsaturated fatty acid in algae |
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Application publication date: 20180720 |