CN107129860A - A kind of extracting method of microalgae grease - Google Patents
A kind of extracting method of microalgae grease Download PDFInfo
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- CN107129860A CN107129860A CN201710328139.2A CN201710328139A CN107129860A CN 107129860 A CN107129860 A CN 107129860A CN 201710328139 A CN201710328139 A CN 201710328139A CN 107129860 A CN107129860 A CN 107129860A
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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
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L1/00—Liquid carbonaceous fuels
- C10L1/02—Liquid carbonaceous fuels essentially based on components consisting of carbon, hydrogen, and oxygen only
-
- 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
- C11B1/108—Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
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- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
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- General Chemical & Material Sciences (AREA)
- Fats And Perfumes (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The present invention relates to a kind of extracting method of microalgae grease, the extracting method comprises the following steps：(1) pre-process：Take eutectic solvent to be well mixed with micro- algae powder, mixed liquor is stirred at room temperature, then mixed liquor is centrifuged, after gained solid phase is freeze-dried, obtain micro- algae powder by pretreatment；(2) grease is extracted：Micro- algae powder and organic solvent by pretreatment is added in extractor, heating is extracted；(3) post-process：The extract solution of gained is cooled to room temperature after grease is extracted, and adds deionized water, is stood after stirring, finally takes upper organic phase to boil off organic solvent in rotary evaporator, obtain microalgae grease.The extracting method of microalgae grease of the present invention has the advantages that cost is low, recovery rate is high, environmental protection.
Description
Technical field
The present invention relates to technical field of biodiesel preparation, more particularly to a kind of extracting method of microalgae grease.
Background technology
The advantages such as microalgae has that photosynthetic efficiency is high, growth rate is fast, strong environmental adaptability and lipid-producing height, be
Most potential biodiesel raw material.Prior art typically extracts the grease in microalgae using organic solvent extractionprocess.However,
The microalgae cell of most of species has a cellulosic cell membrane, cell wall thickness and quality is hard, and microalgae grease is wrapped in into it
In, if directly extracting microalgae grease using conventional organic solvents, the cell membrane of microalgae cell is difficult to rupture in extraction process,
Cause the microalgae grease amount discharged from cell few, cause extraction efficiency relatively low.Therefore, to further improve organic solvent extraction
The extraction efficiency to microalgae grease is followed the example of, generally requires before extraction to pre-process microalgae cell, microalgae cell wall is existed
Rupture is easier during extraction.
The method for having occurred pre-processing microalgae cell with acid or alkali in the prior art.The main knot of microalgae cell wall
Composition point is cellulose and hemicellulose.Sulfuric acid, hydrochloric acid etc. can cause cellulose and hemicellulose to hydrolyze, so as to reduce fibre
The degree of polymerization and crystallinity of dimension element and hemicellulose, make microalgae cell wall generation degraded be therefore easier in extraction process broken
Split.Sodium hydroxide, potassium hydroxide etc. can weaken the hydrogen bond between cellulose and hemicellulose, and microalgae cell wall can equally occurred
Degraded.But, acid or alkali can corrode production equipment, and the acid base concentration of the produced waste water of microalgae cell pretreatment declines,
It is difficult to recycle, directly discharge again can pollute the environment such as water body, farmland, it is necessary to could discharge by processing.
Ionic liquid, refers to the room temperature fused salt being made up of zwitterion, and it has non-volatile, chemical property stable, wide electric
The advantages of chemical potential window and property Modulatory character.Ionic liquid is including cellulose, hemicellulose, wooden to biomaterial
Element etc. all shows good dissolubility, and trial is pre-processed with ionic liquid to microalgae cell at present.Common application
More is imidazoles, pyridine ionic liquid, primary raw material such as alkyl substituted imidazole, alkyl the substitution pyrrole of such ionic liquid
Pyridine etc. derives from oil, is volatile organic matter mostly, and expensive.The preparation method of ionic liquid has direct synthesis
Method, indirect synthesis technique, microwave process for synthesizing, ultrasonic synthesis and electrochemical synthesis etc., these preparation method processes are complicated, lead to
Often need to use the material for being also easy to produce pollution environment in volatile solvent, building-up process, and the height that consumes energy.There are some researches show, from
Sub- liquid has toxicity and biological degradability is poor.Disadvantage mentioned above seriously limits ionic liquid in microalgae cell pretreatment
Extensive use.
The content of the invention
Based on this, it is an object of the present invention to provide a kind of extracting method of microalgae grease, the extracting method is from low common
Molten solvent is pre-processed to microalgae cell, and combines the technology of organic solvent extraction microalgae grease, with cost is low and extraction
The high advantage of rate.
The technical solution adopted by the present invention is as follows：
A kind of extracting method of microalgae grease, comprises the following steps：
(1) pre-process：Take eutectic solvent to be well mixed with micro- algae powder, mixed liquor is stirred at room temperature, then to mixing
Liquid is centrifuged, and after gained solid phase is freeze-dried, obtains micro- algae powder by pretreatment；The eutectic solvent by
Hydrogen bond receptor and hydrogen bond donor Hybrid Heating are made, and the hydrogen bond receptor is one kind in Choline Chloride, glycine betaine and quaternary ammonium salt
Or multiple combinations, the hydrogen bond donor is one or more combinations in polyalcohol, carboxylic acid compound and amides compound；
(2) grease is extracted：Micro- algae powder and organic solvent by pretreatment is added in extractor, heating is carried
Take；
(3) post-process：The extract solution of gained is cooled to room temperature after grease is extracted, and adds deionized water, quiet after stirring
Put, finally take upper organic phase to boil off organic solvent in rotary evaporator, obtain microalgae grease.
Eutectic solvent (Deep eutectic solvent, DES) is to be made by hydrogen bond receptor and hydrogen bond donor by hydrogen bond
Formed, because the hydrogen bond and Van der Waals force that are formed between component hinder the recrystallization of system, and then reduced with mutual association
The fusing point of system, therefore fusing point of the fusing point less than each component of eutectic solvent, it is under normal temperature condition generally with shape of liquid
Formula is present, so pretreatment can be carried out at room temperature, convenient operation.
In preprocessing process, on the hydrogen bond receptor and cellulose molecular chain, hemicellulose molecule chain in eutectic solvent
Hydroxyl form hydrogen bond action so that the hydrogen bond action of the intermolecular and respective intramolecular of cellulose and hemicellulose weakens,
So as to reduce the degree of polymerization and crystallinity of cellulose and hemicellulose, microalgae cell wall is set to occur degraded therefore in step (2)
Grease is easier to rupture during extracting, it is easier to discharges microalgae grease, and then effectively improves recovery rate.
The present invention is pre-processed from eutectic solvent to microalgae cell, and compared to acid, base reagent, eutectic solvent exists
After the centrifugally operated of pretreatment can direct reuse, reduce production cost and post processing cost, it is low compared to ionic liquid
Congruent melting solvent is made by raw material Hybrid Heating, and preparation method is simple, it is low to consume energy, and need not use volatility in preparation process molten
Agent, and no coupling product generation, therefore more environmental protection.The extracting method for the microalgae grease that the present invention is provided solves acid, alkali
With the problem of the high expensive of ionic liquid pretreatment microalgae and pollution environment, with higher economic benefit and environmental benefit.
Further, in step (1), the hydrogen bond receptor in the eutectic solvent is Choline Chloride, and hydrogen bond donor is sweet
Oil, ethanedioic acid, citric acid, lactic acid or urea, the mol ratio of the hydrogen bond receptor and hydrogen bond donor is 1:1~3.
The molecular formula of Choline Chloride is HOCH2CH2N(CH3)3Cl, is conventional eutectic solvent hydrogen bond receptor, and it is originated
It is easy to get, is also a kind of plant photosynthesis promoter frequently as poultry and livestock feed additive, it is nontoxic, it is environmentally friendly.Pre-
In processing, the Cl in Choline Chloride-With hydroxyl hydrogen formation O-H ... Cl in cellulose or hemicellulose-Connection, realizes that reduction is fine
The degree of polymerization and crystallinity of dimension element and hemicellulose, the purpose for making microalgae cell wall degrade.Glycerine, lactic acid, urea are all
Human body and the metabolite of animal, it is nontoxic.Ethanedioic acid, citric acid be widely present with plant, it is nontoxic, to environment
It is friendly.
The fusing point of eutectic solvent strengthens and reduced with the ability of hydrogen bond donor and hydrogen bond receptor formation hydrogen bond, between component
Proportioning it is also closely related.The fusing point of eutectic solvent is lower, and its operating temperature range at room temperature is bigger, makes pretreatment can
Carried out with lower in the range of wider room temperature.In addition, eutectic solvent is due to the hydrogen bond action between component, mobility is reduced,
Proportioning of its viscosity also between component is relevant, if the viscosity of eutectic solvent is excessive, is unfavorable in pretreatment centrifuging behaviour
The progress of work and separating effect.The present invention is by selecting suitable hydrogen bond donor and hydrogen bond receptor, and by hydrogen bond receptor and hydrogen bond
The proportioning of donor is adjusted to optimum range, eutectic solvent is obtained relatively low fusing point and viscosity.
Further, in step (1), micro- algae powder is chlorella, Chlorococcum or grid algae.Micro- algae powder is city
Sell product or cultivate gained.
Further, in step (1), the moisture content of micro- algae powder by mass percentage is 1%~3%, total fat
Content is 10%~25%.Using dry micro- algae powder as raw material, the harmful effect that moisture is caused to preprocessing process can be reduced.
Further, in step (1), the amount ratio of the eutectic solvent and micro- algae powder is (5~10) mL eutectic
Solvent:The micro- algae powders of 1g, it is ensured that there are enough eutectic solvents to be acted on microalgae cell wall, while reducing unnecessary eutectic
Solvent load, reduces the treating capacity centrifuged, reduces energy consumption.
Further, in step (1), the time that mixed liquor is stirred at room temperature is 12h~72h, it is to avoid processing time is too short,
Eutectic solvent is not enough to the degradation effect of microalgae cell wall, also avoids processing time long, and microalgae cell wall is in pretreatment
Just rupture in advance, discharge microalgae grease and mixed with eutectic solvent, both are difficult to separate, be unfavorable for the extraction of microalgae grease.
Further, in step (1), the temperature of freeze-drying is -80 DEG C~-40 DEG C, and the time is 24h~48h, is both ensured
Oil quality in micro- algae powder is not destroyed, and moisture can be thoroughly removed again, it is to avoid moisture causes bad to oil extraction processes
Influence.
Further, in step (2), in step (2), the organic solvent is n-hexane, ethyl acetate, ethanol and methanol
In one or more combinations.
Further, in step (2), the amount ratio of the organic solvent and micro- algae powder is organic molten for (10~40) mL
Agent:The micro- algae powders of 1g, it is ensured that have enough organic solvents fully to extract microalgae grease, are used while reducing unnecessary organic solvent
Amount, reduces the treating capacity of post processing, reduces energy consumption.
Further, in step (2), it is 50 DEG C~90 DEG C to heat the temperature extracted, and the time is 0.25h~2.5h,
Suitable extraction conditions are favorably improved recovery rate of the organic solvent to microalgae grease.
Embodiment
Embodiment 1
Prepare eutectic solvent：By 1:Choline Chloride and urea are well mixed by 1 mol ratio, are heated under 90 DEG C of constant temperature
2h is stirred, colourless transparent liquid is obtained, is cooled to after room temperature and obtains eutectic solvent.
The extraction of microalgae grease is carried out according to the following steps：
(1) pre-process：By 5mL eutectic solvents:The amount ratio of 1g chlorella algae powders, take the eutectic solvent for preparing with
Chlorella algae powder is well mixed, the magnetic agitation mixed liquor 24h at 23 DEG C~28 DEG C of room temperature, then with 10000rpm rotating speed pair
Mixed liquor centrifugal treating 10min, removes a layer solid phase.Lower floor's solid phase is washed with deionized again 3 times, every time washing after with
Then the solid phase washed is placed in -80 DEG C of freeze-drying to cleaning mixture centrifugal treating 10min by 6000rpm rotating speed
48h is freeze-dried in machine, the chlorella algae powder by pretreatment is obtained.
(2) grease is extracted：By 10mL n-hexanes:The amount ratio of 1g chlorella algae powders, by n-hexane and by pretreatment
Chlorella algae powder is added in extractor, and 2h is extracted at 50 DEG C.
(3) post-process：The extract solution of gained is cooled to room temperature after grease is extracted, and adds deionized water, stirs 10min
After stand, finally take upper organic phase to boil off n-hexane in rotary evaporator, obtain chlorella grease.
In the present embodiment, the moisture content of raw material pellet algae powder used by mass percentage is 1.05%, and total fat contains
Measure as 10.33%, total carbohydrates content is 33.03%.
The chlorella algae powder grease extraction efficiency of the present embodiment is 75.52%.
Embodiment 2
Prepare eutectic solvent：By 1:Choline Chloride and glycerine are well mixed by 2 mol ratio, are heated under 80 DEG C of constant temperature
2h is stirred, colourless transparent liquid is obtained, is cooled to after room temperature and obtains eutectic solvent.
The extraction of microalgae grease is carried out according to the following steps：
(1) pre-process：By 25mL eutectic solvents:The amount ratio of 1g Chlorococcum algae powder, takes the eutectic solvent prepared
It is well mixed with Chlorococcum algae powder, the magnetic agitation mixed liquor 24h at 23 DEG C~28 DEG C of room temperature, then with 10000rpm rotating speed
To mixed liquor centrifugal treating 10min, a layer solid phase is removed.Lower floor's solid phase is washed with deionized again 3 times, every time washing after with
Then the solid phase washed is placed in -80 DEG C of freeze-drying to cleaning mixture centrifugal treating 10min by 6000rpm rotating speed
48h is freeze-dried in machine, the Chlorococcum algae powder by pretreatment is obtained.
(2) grease is extracted：By 10mL ethyl acetate:The amount ratio of 1g Chlorococcum algae powder, by ethyl acetate and by pre- place
The Chlorococcum algae powder of reason is added in extractor, and 2h is extracted at 50 DEG C.
(3) post-process：The extract solution of gained is cooled to room temperature after grease is extracted, and then adds deionized water, stirs
Stood after 10min, finally take upper organic phase to boil off ethyl acetate in rotary evaporator, obtain Chlorococcum grease.
In the present embodiment, the moisture content of raw material Chlorococcum algae powder used by mass percentage is 2.25%, and total fat contains
Measure as 20.58%, total carbohydrates content is 34.18%.
The Chlorococcum algae powder grease extraction efficiency of the present embodiment is 80.90%.
Embodiment 3
Prepare eutectic solvent：By 1:Choline Chloride and ethanedioic acid are well mixed by 3 mol ratio, are added under 70 DEG C of constant temperature
Thermal agitation 2h, obtains colourless transparent liquid, is cooled to after room temperature and obtains eutectic solvent.
The extraction of microalgae grease is carried out according to the following steps：
(1) pre-process：By 40mL eutectic solvents:The amount ratio of 1g grid algae powders, take the eutectic solvent for preparing with
Grid algae powder is well mixed, the magnetic agitation mixed liquor 72h at 23 DEG C~28 DEG C of room temperature, then with 10000rpm rotating speed to mixed
Liquid centrifugal treating 10min is closed, a layer solid phase is removed.Lower floor's solid phase is washed with deionized again 3 times, every time with 6000rpm after washing
Rotating speed the solid phase washed be placed in -80 DEG C of freeze drier to cleaning mixture centrifugal treating 10min, then freezed
48h is dried, the grid algae powder by pretreatment is obtained.
(2) grease is extracted：By 10mL ethyl acetate-ethanol mixed solvents:The amount ratio of 1g grid algae powders, by acetic acid second
Ester-alcohol mixed solvent and the grid algae powder of process pretreatment are added in extractor, and 2h is extracted at 50 DEG C.The acetic acid second
In ester-alcohol mixed solvent, the volume ratio of ethyl acetate and ethanol is 1:1.
(3) post-process：The extract solution of gained is cooled to room temperature after grease is extracted, and then adds deionized water, stirs
Stood after 10min, finally take upper organic phase to boil off ethyl acetate-ethanol mixed solvent in rotary evaporator, obtain grid algae
Grease.
In the present embodiment, the moisture content of raw material grid algae powder used by mass percentage is 3.00%, total lipid content
For 24.67%, total carbohydrates content is 36.78%.
The grid algae powder grease extraction efficiency of the present embodiment is 66.92%.
Comparative example 1
This comparative example extracts microalgae grease and eliminates step (1) pretreatment, other steps, raw material, reagent and technological parameter
It is identical with embodiment 1.
The chlorella algae powder grease extraction efficiency of this comparative example is 52.3%.
Comparative example 2
This comparative example extracts microalgae grease and eliminates step (1) pretreatment, other steps, raw material, reagent and technological parameter
It is identical with embodiment 2.
The Chlorococcum algae powder grease extraction efficiency of this comparative example is 54.83%.
Comparative example 3
This comparative example extracts microalgae grease and eliminates step (1) pretreatment, other steps, raw material, reagent and technological parameter
It is identical with embodiment 3.
The grid algae powder grease extraction efficiency of this comparative example is 55.46%.
The present invention is pre-processed from eutectic solvent to microalgae cell, when making grease extraction efficiency from without pretreatment
52.03%~55.46% improve to 66.92%~80.90%.
Relative to prior art, the present invention improves the feature of environmental protection and sustainability of microalgae grease extraction process, and it is economical
Benefit and environmental benefit are considerable.
Embodiment described above only expresses the several embodiments of the present invention, and it describes more specific and detailed, but simultaneously
Can not therefore it be construed as limiting the scope of the patent.It should be pointed out that coming for one of ordinary skill in the art
Say, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Scope.
Claims (10)
1. a kind of extracting method of microalgae grease, it is characterised in that comprise the following steps：
(1) pre-process：Take eutectic solvent to be well mixed with micro- algae powder, mixed liquor is stirred at room temperature, then mixed liquor is entered
Row is centrifuged, and after gained solid phase is freeze-dried, obtains micro- algae powder by pretreatment；The eutectic solvent is by hydrogen bond
Acceptor and hydrogen bond donor Hybrid Heating are made, and the hydrogen bond receptor is one kind or many in Choline Chloride, glycine betaine and quaternary ammonium salt
Combination is planted, the hydrogen bond donor is one or more combinations in polyalcohol, carboxylic acid compound and amides compound；
(2) grease is extracted：Micro- algae powder and organic solvent by pretreatment is added in extractor, heating is extracted；
(3) post-process：The extract solution of gained is cooled to room temperature after grease is extracted, and adds deionized water, is stood after stirring, most
After take upper organic phase to boil off organic solvent in rotary evaporator, obtain microalgae grease.
2. the extracting method of microalgae grease according to claim 1, it is characterised in that：In step (1), the eutectic is molten
Hydrogen bond receptor in agent is Choline Chloride, and hydrogen bond donor is glycerine, ethanedioic acid, citric acid, lactic acid or urea, the hydrogen bond receptor
Mol ratio with hydrogen bond donor is 1:1~3.
3. the extracting method of microalgae grease according to claim 1, it is characterised in that：In step (1), micro- algae powder
For chlorella, Chlorococcum or grid algae.
4. the extracting method of microalgae grease according to claim 3, it is characterised in that：In step (1), micro- algae powder
Moisture content by mass percentage is 1%~3%, and total lipid content is 10%~25%.
5. the extracting method of the microalgae grease according to claim any one of 1-4, it is characterised in that：It is described in step (1)
The amount ratio of eutectic solvent and micro- algae powder is (5~10) mL eutectic solvents:The micro- algae powders of 1g.
6. the extracting method of microalgae grease according to claim 5, it is characterised in that：In step (1), stir at room temperature mixed
The time for closing liquid is 12h~72h.
7. the extracting method of microalgae grease according to claim 5, it is characterised in that：In step (1), the temperature of freeze-drying
Spend for -80 DEG C~-40 DEG C, the time is 24h~48h.
8. the extracting method of microalgae grease according to claim 1, it is characterised in that：In step (2), the organic solvent
For the one or more combination in n-hexane, ethyl acetate, ethanol and methanol.
9. the extracting method of microalgae grease according to claim 8, it is characterised in that：In step (2), the organic solvent
Amount ratio with micro- algae powder is (10~40) mL organic solvents:The micro- algae powders of 1g.
10. the extracting method of microalgae grease according to claim 8, it is characterised in that：In step (2), heating is carried
The temperature taken is 50 DEG C~90 DEG C, and the time is 0.25h~2.5h.
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| CN108893185A (en) * | 2018-07-26 | 2018-11-27 | 河西学院 | The method that magnetic hydrophobic eutectic solvent auxiliary homogenate extraction prepares microalgae grease |
| CN109503323A (en) * | 2018-10-29 | 2019-03-22 | 广东工业大学 | A kind of preprocess method extracting natural d-borneol from Borneolum leaf piece |
| CN109971547A (en) * | 2019-04-28 | 2019-07-05 | 中国农业科学院烟草研究所 | A method of utilizing deep congruent melting solvent extraction wormwood essential oil |
| CN109985418A (en) * | 2019-04-22 | 2019-07-09 | 南京师范大学常州创新发展研究院 | A kind of extracting method and application of active material extracting solution |
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| CN108893185A (en) * | 2018-07-26 | 2018-11-27 | 河西学院 | The method that magnetic hydrophobic eutectic solvent auxiliary homogenate extraction prepares microalgae grease |
| CN108893185B (en) * | 2018-07-26 | 2021-08-20 | 河西学院 | Method for preparing microalgae grease by magnetic hydrophobic eutectic solvent assisted flash extraction |
| US11845909B2 (en) | 2018-09-10 | 2023-12-19 | Eni S.P.A. | Method for the extraction of bio-oil from algal biomass |
| CN112771139B (en) * | 2018-09-10 | 2023-04-11 | 艾尼股份公司 | Method for extracting bio-oil from algal biomass |
| WO2020053118A1 (en) * | 2018-09-10 | 2020-03-19 | Eni S.P.A. | Method for the extraction of bio-oil from algal biomass |
| CN112771139A (en) * | 2018-09-10 | 2021-05-07 | 艾尼股份公司 | Method for extracting bio-oil from algal biomass |
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