CN103849458B - The extracting method of microalgae grease - Google Patents
The extracting method of microalgae grease Download PDFInfo
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- CN103849458B CN103849458B CN201410108480.3A CN201410108480A CN103849458B CN 103849458 B CN103849458 B CN 103849458B CN 201410108480 A CN201410108480 A CN 201410108480A CN 103849458 B CN103849458 B CN 103849458B
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- 238000000034 method Methods 0.000 title claims abstract description 50
- 239000004519 grease Substances 0.000 title claims abstract description 28
- 235000014593 oils and fats Nutrition 0.000 claims abstract description 39
- 239000003960 organic solvent Substances 0.000 claims abstract description 33
- 239000007787 solid Substances 0.000 claims description 26
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 22
- 208000035126 Facies Diseases 0.000 claims description 15
- 238000009835 boiling Methods 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 241000214658 Tetraodon fluviatilis Species 0.000 claims 1
- 239000002253 acid Substances 0.000 abstract description 11
- 150000007524 organic acids Chemical class 0.000 abstract description 9
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 8
- 239000007788 liquid Substances 0.000 abstract description 8
- 239000011707 mineral Substances 0.000 abstract description 8
- 238000000605 extraction Methods 0.000 abstract description 7
- 239000000284 extract Substances 0.000 abstract description 4
- 230000003834 intracellular effect Effects 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 21
- 238000002156 mixing Methods 0.000 description 14
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 8
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 6
- 240000009108 Chlorella vulgaris Species 0.000 description 6
- 235000019253 formic acid Nutrition 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 5
- 210000004027 cell Anatomy 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000001117 sulphuric acid Substances 0.000 description 5
- 235000011149 sulphuric acid Nutrition 0.000 description 5
- 241001536324 Botryococcus Species 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 241000957276 Thalassiosira weissflogii Species 0.000 description 4
- 239000003208 petroleum Substances 0.000 description 4
- 235000007089 Chlorella vulgaris Nutrition 0.000 description 3
- 241001491687 Thalassiosira pseudonana Species 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 3
- 239000000295 fuel oil Substances 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 241000043665 Clenchiella minutissima Species 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- -1 aliphatic organic acid Chemical class 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 239000003225 biodiesel Substances 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- AZHSSKPUVBVXLK-UHFFFAOYSA-N ethane-1,1-diol Chemical compound CC(O)O AZHSSKPUVBVXLK-UHFFFAOYSA-N 0.000 description 1
- 239000003925 fat Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- DUWWHGPELOTTOE-UHFFFAOYSA-N n-(5-chloro-2,4-dimethoxyphenyl)-3-oxobutanamide Chemical compound COC1=CC(OC)=C(NC(=O)CC(C)=O)C=C1Cl DUWWHGPELOTTOE-UHFFFAOYSA-N 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Fats And Perfumes (AREA)
- Extraction Or Liquid Replacement (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The present invention provides the extracting method of a kind of microalgae grease, in microalgae, the mineral acid of the organic acid of mass percent concentration 30% 100% and mass percent concentration 0% 3% is added by the solid-to-liquid ratio that kg:L is 1:3 20, after processing 0.25 5.0h, add organic solvent and carry out the extraction of oils and fats.This method uses organic acid smudge cells first, extracts intracellular oils and fats with organic solvent the most again；Described organic acid and organic solvent also can be simultaneously introduced.Use this technique, can get the yield oils and fats more than more than 90%, and organic acid is easily recycled and recycles, reduce discharge of wastewater, low for equipment requirements, compared with tradition microalgae grease extraction process, this technological operation is simple, and environmental pollution is little, has good industrial applications prospect.
Description
Technical field
The present invention relates to Renewable resource field and biological chemical field, specifically, relate to one
Plant the extracting method of microalgae grease.
Background technology
In recent years, day by day serious due to energy shortage and environmental disruption, development bioenergy is
Become the focus of global concern.Wherein, the bio-fuel-oil with renewable oils and fats as raw material is (biological
Diesel oil or Aviation Fuel etc.) development receive much concern.Want to develop with renewable oils and fats as raw material
Bio-fuel-oil, the sustainable supply of oils and fats is crucial.In recent years, microalgae grease fires as biology
Oil raw material is by domestic and international expert and scholar's extensive concern.It is short that microalgae has life cycle, growth
Speed is fast, is adapted to various planting conditions, and can gather the whole year.It addition,
It is few that microalgae cultivates area occupied, can not utilize general agricultural arable land, saving water resource, be one
Plant the most promising renewable oils fat raw material.But, most microalgae greases all in intracellular,
How effectively crushing microalgae cells to be extracted by the oils and fats of intracellular further be promotion microalgae
The key that oils and fats is applied in field of biological energy source.
The extraction of microalgae grease at present is mainly Mechanical Method smudge cells, uses organic solvent the most again
Extracting, and first extract with organic solvent again with chemical method smudge cells.Wherein, Mechanical Crushing
Method includes high-pressure homogenization, sonioation method, ball-milling method, microwave method etc., these smudge cellses
Method to there is energy consumption big, equipment investment is big, it is difficult to apply further in industrialized production；
And chemical method mainly uses mineral acid logos, typically with strong inorganic acid such as sulphuric acid, hydrochloric acid etc.,
Mineral acid smudge cells exists mineral acid consumption, and (general consumption is for based on microalgae dry biomass greatly
More than 10%), mineral acid is not only difficult to reclaim, and, the mineral acid of high concentration is to equipment
Seriously corroded, environment also can be produced and have a strong impact on by the discharge containing acid waste liquid.Visible, in the urgent need to
Develop novel microalgae grease extraction process and promote that microalgae grease is in biodiesel and biological boat
Application in air-fuel oil preparation field.
Summary of the invention
It is an object of the invention to provide the grease extraction of a kind of oil-producing microalgae.
In order to realize the object of the invention, the extracting method of a kind of microalgae grease of the present invention, by kg:
L is that the solid-to-liquid ratio of 1:3-20 adds the organic of mass percent concentration 30%-100% in microalgae
Acid and the mineral acid of mass percent concentration 0%-3%, after processing 0.25-5.0h, add organic
Solvent carries out the extraction of oils and fats.
In aforementioned extracting method, described organic solvent can be simultaneously introduced in microalgae with organic acid.
In aforementioned extracting method, add organic in microalgae by the solid-to-liquid ratio that kg:L is 1:2-10
Solvent.
In aforementioned extracting method, described organic acid is aliphatic organic acid.Include but not limited to first
Acid, acetic acid and/or propanoic acid etc..
In aforementioned extracting method, described mineral acid include but not limited to sulphuric acid, hydrochloric acid, phosphoric acid and
/ or nitric acid etc..
In aforementioned extracting method, described organic solvent include but not limited to chloroform, petroleum ether and/
Or normal hexane etc., and they and methanol or the mixed liquor of ethanol.
The microalgae related in the present invention include but not limited to Chlorella vulgaris,
Botryococcus sp.、C.vulgaris、C.minutissima、T.fluviatilis、T.
Pseudonana etc..
The present invention provides the new technology that a kind of microalgae grease extracts first, i.e. broken thin with organic acid
Born of the same parents, extract the oils and fats of intracellular with organic solvent the most again；Described organic acid and organic molten
Agent also can be simultaneously introduced.Use this technique, the available yield oils and fats more than more than 90%, and
Organic acid is easily recycled and recycles, and reduces discharge of wastewater, low for equipment requirements, with tradition
Microalgae grease extraction process is compared, and this technological operation is simple, and environmental pollution is little, has very well
Industrial applications prospect.
Detailed description of the invention
Following example are used for illustrating the present invention, but are not limited to the scope of the present invention.If not
Specialize, the routine that technological means used in embodiment is well known to those skilled in the art
Means, raw materials used are commercial goods.
The extracting method of embodiment 1 microalgae grease
With the formic acid solution that mass percent concentration is 60% and microalgae Chlorella vulgaris by
Liquid-solid ratio 10:1(L:kg) after mixing, stir process 1.5 hours under atmospheric boiling point, then use
Organic solvents, chloroform/methanol (volume ratio 1:1) carries out oils and fats extracting, organic solvent and microalgae
Liquid-solid ratio (L:kg) is 3:1, and in centrifugal rear organic facies, available yield is the oils and fats of 92%.
The extracting method of embodiment 2 microalgae grease
With the formic acid solution that mass percent concentration is 70% with microalgae Botryococcus sp. by liquid
Gu ratio is for 6:1(L:kg) mixing, it is simultaneously introduced organic solvents, chloroform/methanol (volume ratio 1:1),
The liquid-solid ratio of organic solvent and microalgae is 3:1 for (L:kg), stir process under atmospheric boiling point
2 hours, in centrifugal rear organic facies, available yield was the oils and fats of 94%.
The extracting method of embodiment 3 microalgae grease
With the acetic acid solution that mass percent concentration is 80% and microalgae Chlorella vulgaris by
Liquid-solid ratio 8:1(L:kg) after mixing, stir process 3 hours under atmospheric boiling point, then with having
Machine solvent chloroform/ethanol (volume ratio 1:1) carries out the liquid of oils and fats extracting, organic solvent and microalgae
Gu be 10:1 than (L:kg), in centrifugal rear organic facies, available yield is the oils and fats of 95%.
The extracting method of embodiment 4 microalgae grease
Mass percent concentration (base is added in the propionic acid solution that mass percent concentration is 70%
In microalgae dry weight) be 0.3% sulphuric acid, gained mixed liquor is pressed with microalgae Botryococcus sp.
Liquid-solid ratio 10:1(L:kg) after mixing, stir process 3.0 hours under atmospheric boiling point, then use
Organic solvent-normal hexane (volume ratio 1:1) carries out the liquid of oils and fats extracting, organic solvent and microalgae
Gu be 4:1 than (L:kg), in centrifugal rear organic facies, available yield is the oils and fats of 90%.
The extracting method of embodiment 5 microalgae grease
Mass percent concentration (base is added in the acetic acid solution that mass percent concentration is 70%
In microalgae dry weight) be 0.2% sulphuric acid, gained mixed liquor and microalgae C.vulgaris are by liquid-solid ratio
For 4:1(L:kg) mixing, it is simultaneously introduced the liquid-solid ratio (L:kg) of normal hexane, organic solvent and microalgae
For 6:1, stir process 3.0 hours under atmospheric boiling point, centrifugal rear organic facies can be received
Rate is the oils and fats of 90%.
The extracting method of embodiment 6 microalgae grease
In the formic acid solution of mass fraction 30%, add mass percent concentration (do based on microalgae
Weight) be 0.5% hydrochloric acid, gained mixed liquor and microalgae C.vulgaris, be 10:1 by liquid-solid ratio
(L:kg) after mixing, stir process 3.0 hours under atmospheric boiling point, then use organic solvents, chloroform
/ ethanol (volume ratio 1:1) carries out the liquid-solid ratio (L:kg) of oils and fats extracting, organic solvent and microalgae
For 8:1, in centrifugal rear organic facies, available yield is the oils and fats of 95%.
The extracting method of embodiment 7 microalgae grease
By formic acid solution that mass percent concentration is 70% with microalgae C.minutissima by liquid
Gu than 10:1(L:kg) after mixing, stir process 0.25 hour under atmospheric boiling point, then with having
Machine solvent petroleum ether/methanol (volume ratio 1:1) carries out oils and fats extracting, organic solvent and microalgae
Liquid-solid ratio (L:kg) is 3:1, and in centrifugal rear organic facies, available yield is the oils and fats of 92%.
The extracting method of embodiment 8 microalgae grease
By acetic acid solution that mass percent concentration is 70% with microalgae T.fluviatilis by liquid-solid ratio
For 10:1(L:kg) after mixing, stir process 2 hours under atmospheric boiling point, then with organic molten
Agent petroleum ether/methanol (volume ratio 2:1) carries out oils and fats extracting, and organic solvent is liquid-solid with microalgae
Being 10:1 than (L:kg), in centrifugal rear organic facies, available yield is the oils and fats of 95%.
The extracting method of embodiment 9 microalgae grease
Acetic acid solution that mass percent concentration is 30% add mass percent concentration (based on
Microalgae dry weight) be 2% hydrochloric acid, gained mixed liquor and microalgae T.fluviatilis are 10 by liquid-solid ratio:
1(L:kg) after mixing, stir process 2 hours under atmospheric boiling point, then use organic solvents, chloroform
/ ethanol alcohol (volume ratio 3:1) carries out the liquid-solid ratio (L:kg) of oils and fats extracting, organic solvent and microalgae
For 5:1, in centrifugal rear organic facies, available yield is the oils and fats of 98%.
The extracting method of embodiment 10 microalgae grease
Propionic acid solution that mass percent concentration is 30% add mass percent concentration (based on
Microalgae dry weight) be 3% sulphuric acid, gained mixed liquor with microalgae T.pseudonana by liquid-solid ratio is
5:1(L:kg) after mixing, stir process 3 hours under atmospheric boiling point, then use organic solvent
Chloroform/methanol (volume ratio 1:1) carries out the liquid-solid ratio of oils and fats extracting, organic solvent and microalgae
(L:kg) being 2:1, in centrifugal rear organic facies, available yield is the oils and fats of 94%.
The extracting method of embodiment 11 microalgae grease
By formic acid solution that mass percent concentration is 70% with microalgae T.pseudonana by liquid-solid
Than being 8:1(L:kg) after mixing, stir process 5 hours under atmospheric boiling point, then with organic
Solvent chloroform/methanol (volume ratio 2:1) carries out oils and fats extracting, and organic solvent is liquid-solid with microalgae
Being 3:1 than (L:kg), in centrifugal rear organic facies, available yield is the oils and fats of 96%.
The extracting method of embodiment 12 microalgae grease
Mass percent concentration (base is added in the acetic acid solution that mass percent concentration is 50%
In microalgae dry weight) be 2% phosphoric acid, gained mixed liquor and microalgae Botryococcus sp. are by liquid-solid
Than being 5:1(L:kg) after mixing, stir process 4.0 hours under atmospheric boiling point, then with organic
Solvent petroleum ether carries out oils and fats extracting, and organic solvent is 3:1 with the liquid-solid ratio (L:kg) of microalgae,
After centrifugal, in organic facies, available yield is the oils and fats of 92%.
The extracting method of embodiment 13 microalgae grease
By formic acid solution that mass percent concentration is 60% with microalgae T.pseudonana by liquid-solid
Than being 9:1(L:kg) after mixing, stir process 2.0 hours under atmospheric boiling point, then with organic
Solvent chloroform carries out oils and fats extracting, and organic solvent is 6:1 with the liquid-solid ratio (L:kg) of microalgae,
After centrifugal, in organic facies, available yield is the oils and fats of 92%.
The extracting method of embodiment 14 microalgae grease
By acetic acid solution that mass percent concentration is 80% with microalgae T.fluviatilis by liquid-solid ratio
For 7:1(L:kg) after mixing, stir process 5.0 hours under atmospheric boiling point, then with organic molten
Agent normal hexane carries out oils and fats extracting, and organic solvent is 7:1 with the liquid-solid ratio (L:kg) of microalgae,
After centrifugal, in organic facies, available yield is the oils and fats of 93%.
Although, the most with a general description of the specific embodiments the present invention has been made in detail
Most description, but on the basis of the present invention, it can be made some modifications or improvements, this is to this
It is apparent from for skilled person.Therefore, on the basis without departing from spirit of the present invention
Upper these modifications or improvements, belong to the scope of protection of present invention.
Claims (1)
1. the extracting method of microalgae grease, it is characterised in that be 30% at mass percent concentration
Acetic acid solution in add the hydrochloric acid that mass percent concentration based on microalgae dry weight is 2%, institute
After mixed liquor mixes by the liquid-solid ratio that L:Kg is 10:1 with microalgae T.fluviatilis, in normal pressure boiling
The lower stir process of point 2 hours, then carry out oils and fats extracting with organic solvents, chloroform and ethanol, wherein,
The volume ratio of chloroform and ethanol is 3:1, and organic solvent is 5:1 with the liquid-solid ratio of microalgae by L:Kg,
After centrifugal, in organic facies, available yield is the oils and fats of 98%.
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| CN105623831B (en) * | 2014-10-28 | 2019-09-10 | 中国石油化工股份有限公司 | A kind of extracting method of microalgae grease |
| CN105695081A (en) * | 2016-03-31 | 2016-06-22 | 唐云龙 | Extraction method for microalgal oil |
| CN109111987A (en) * | 2018-08-30 | 2019-01-01 | 中国海洋大学 | A kind of oil extracting methods |
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