CN103849458A - Extraction method of microalgae oil - Google Patents
Extraction method of microalgae oil Download PDFInfo
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- CN103849458A CN103849458A CN201410108480.3A CN201410108480A CN103849458A CN 103849458 A CN103849458 A CN 103849458A CN 201410108480 A CN201410108480 A CN 201410108480A CN 103849458 A CN103849458 A CN 103849458A
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- acid
- algae
- organic solvent
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- grease
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- 238000000605 extraction Methods 0.000 title claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 59
- 239000003960 organic solvent Substances 0.000 claims abstract description 40
- 150000007524 organic acids Chemical class 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 239000004519 grease Substances 0.000 claims description 47
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 20
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 10
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 9
- 239000011707 mineral Substances 0.000 claims description 9
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 8
- 240000009108 Chlorella vulgaris Species 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 235000019253 formic acid Nutrition 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 6
- 241001536324 Botryococcus Species 0.000 claims description 5
- 241001491687 Thalassiosira pseudonana Species 0.000 claims description 5
- 241000957276 Thalassiosira weissflogii Species 0.000 claims description 5
- 235000007089 Chlorella vulgaris Nutrition 0.000 claims description 4
- 241000043665 Clenchiella minutissima Species 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 3
- 241000195493 Cryptophyta Species 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- -1 aliphatics organic acid Chemical class 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 235000019260 propionic acid Nutrition 0.000 claims description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 150000007522 mineralic acids Chemical class 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- 239000007787 solid Substances 0.000 description 28
- 238000009835 boiling Methods 0.000 description 14
- 239000000203 mixture Substances 0.000 description 14
- 239000012074 organic phase Substances 0.000 description 14
- 238000003756 stirring Methods 0.000 description 14
- 239000000243 solution Substances 0.000 description 12
- 210000004027 cell Anatomy 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- 239000000295 fuel oil Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002551 biofuel Substances 0.000 description 2
- 239000000446 fuel Substances 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
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process 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
- 239000000284 extract 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
- 230000005226 mechanical processes and functions Effects 0.000 description 1
- 238000002360 preparation method Methods 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 invention provides an extraction method of microalgae oil. The oil is extracted by the following steps: adding 30-100% by mass of organic acid and 0-3% by mass of inorganic acid into microalgae in a solid-to-liquid ratio of kg: L of 1: (3-20); treating for 0.25-5.0 hours; and adding an organic solvent to extract oil. According to the method, the organic acid is adopted for the first time to crush cells, and then, the oil in cells is extracted by the organic solvent. The organic acid and the organic solvent can be further added at the same time. By adopting the process, oil with the yield greater than 90% can be obtained, and the organic acid is easy to recover and recycle, so that wastewater discharge is reduced, and the demand on equipment is low. Compared with conventional extraction processes of microalgae oil, the extraction method provided by the invention is simple to operate and less in environmental pollution, and has a good industrialized application prospect.
Description
Technical field
The present invention relates to renewable resources field and biological chemical field, specifically, relate to a kind of extracting method of microalgae grease.
Background technology
In recent years, day by day serious due to energy shortage and environmental disruption, development bioenergy has become the focus of global concern.Wherein, the bio-fuel-oil taking renewable grease as raw material (biofuel or Aviation Fuel etc.) development receives much concern.Want the bio-fuel-oil of development taking renewable grease as raw material, the sustainable supply of grease is crucial.In recent years, microalgae grease is subject to domestic and international expert and scholar's extensive concern as bio-fuel-oil raw material.It is short that micro-algae has life cycle, and growth velocity is fast, can adapt to various planting conditions, and can gather the whole year.In addition, it is few that micro-algae is cultivated area occupied, can not utilize general agricultural arable land, and saving water resource, is the very promising renewable oils fat raw material of one.But most microalgae greases are all in born of the same parents, how effective crushing microalgae cells also further extracts the grease in born of the same parents is to promote the key of microalgae grease in the application of bioenergy field.
The extraction of microalgae grease is at present mainly mechanical process smudge cells, and then uses organic solvent extracting, and first uses organic solvent extracting with chemical method smudge cells again.Wherein, mechanical crushing method comprises high-pressure homogenization method, sonioation method, ball milled, microwave method etc., and the method for these smudge cellses exists energy consumption large, and facility investment is large, is difficult to further application in suitability for industrialized production; And chemical method mainly adopts mineral acid logos, the general strong inorganic acid of using is as sulfuric acid, hydrochloric acid etc., there is mineral acid consumption large (general consumption is based on the more than 10% of micro-algae dry biomass) in mineral acid smudge cells, mineral acid is not only difficult to reclaim, and, the mineral acid of high density is serious to equipment corrosion, containing acid waste liquid discharge, environment also can be produced and be had a strong impact on.Visible, promote the application of microalgae grease in biofuel and biological Aviation Fuel preparation field in the urgent need to the microalgae grease extraction process of development of new.
Summary of the invention
The object of this invention is to provide a kind of grease extracting method 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, the solid-to-liquid ratio that is 1:3-20 by kg:L adds the organic acid of mass percent concentration 30%-100% and the mineral acid of mass percent concentration 0%-3% in micro-algae, process after 0.25-5.0h, add organic solvent to carry out the extraction of grease.
In aforementioned extracting method, described organic solvent can add in a subtle way in algae with organic acid simultaneously.
In aforementioned extracting method, the solid-to-liquid ratio that is 1:2-10 by kg:L adds organic solvent in micro-algae.
In aforementioned extracting method, described organic acid is aliphatics organic acid.Include but not limited to formic acid, acetic acid and/or propionic acid etc.
In aforementioned extracting method, described mineral acid includes but not limited to sulfuric acid, hydrochloric acid, phosphoric acid and/or nitric acid etc.
In aforementioned extracting method, described organic solvent includes but not limited to chloroform, sherwood oil and/or normal hexane etc., and the mixed solution of they and methyl alcohol or ethanol.
The micro-algae relating in the present invention includes but not limited to Chlorella vulgaris, Botryococcus sp., C.vulgaris, C.minutissima, T.fluviatilis, T.pseudonana etc.
The novel process that the present invention provides a kind of microalgae grease to extract first, uses organic acid smudge cells, and then the grease in born of the same parents is extracted with organic solvent; Described organic acid and organic solvent also can add simultaneously.Adopt this technique, can obtain yield and be greater than more than 90% grease, and organic acid is easy to reclaim and recycle, reduce discharge of wastewater, low for equipment requirements, compared with traditional microalgae grease extraction process, this technological operation is simple, and environmental pollution is little, has good industrial applications prospect.
Embodiment
Following examples are used for illustrating the present invention, but are not used for limiting the scope of the invention.If do not specialize, the conventional means that in embodiment, technique means used is well known to those skilled in the art, the raw materials used commercial goods that is.
The extracting method of embodiment 1 microalgae grease
The formic acid solution that is 60% with mass percent concentration with micro-algae Chlorella vulgaris by liquid-solid ratio 10:1(L:kg) mix after, stir process 1.5 hours under atmospheric boiling point, use again organic solvents, chloroform/methyl alcohol (volume ratio 1:1) to carry out grease extracting, the liquid-solid ratio (L:kg) of organic solvent and micro-algae is 3:1, can obtain yield and be 92% grease in centrifugal rear organic phase.The extracting method of embodiment 2 microalgae greases
The formic acid solution that is 70% with mass percent concentration is 6:1(L:kg with micro-algae Botryococcus sp. by liquid-solid ratio) mix, add organic solvents, chloroform/methyl alcohol (volume ratio 1:1) simultaneously, the liquid-solid ratio of organic solvent and micro-algae is that (L:kg) is 3:1, stir process 2 hours under atmospheric boiling point, can obtain yield and be 94% grease in centrifugal rear organic phase.
The extracting method of embodiment 3 microalgae greases
The acetic acid solution that is 80% with mass percent concentration with micro-algae Chlorella vulgaris by liquid-solid ratio 8:1(L:kg) mix after, stir process 3 hours under atmospheric boiling point, use again organic solvents, chloroform/ethanol (volume ratio 1:1) to carry out grease extracting, the liquid-solid ratio (L:kg) of organic solvent and micro-algae is 10:1, can obtain yield and be 95% grease in centrifugal rear organic phase.
The extracting method of embodiment 4 microalgae greases
In the propionic acid solution that is 70% to mass percent concentration, add mass percent concentration (based on micro-algae dry weight) and be 0.3% sulfuric acid, gained mixed solution with micro-algae Botryococcus sp. by liquid-solid ratio 10:1(L:kg) mix after, stir process 3.0 hours under atmospheric boiling point, use again organic solvent-normal hexane (volume ratio 1:1) to carry out grease extracting, the liquid-solid ratio (L:kg) of organic solvent and micro-algae is 4:1, can obtain yield and be 90% grease in centrifugal rear organic phase.
The extracting method of embodiment 5 microalgae greases
In the acetic acid solution that is 70% to mass percent concentration, add mass percent concentration (based on micro-algae dry weight) and be 0.2% sulfuric acid, gained mixed solution is 4:1(L:kg with micro-algae C.vulgaris by liquid-solid ratio) mix, add normal hexane simultaneously, the liquid-solid ratio (L:kg) of organic solvent and micro-algae is 6:1, stir process 3.0 hours under atmospheric boiling point, can obtain yield and be 90% grease in centrifugal rear organic phase.
The extracting method of embodiment 6 microalgae greases
Be 0.5% hydrochloric acid to adding mass percent concentration (based on micro-algae dry weight) in the formic acid solution of massfraction 30%, gained mixed solution and micro-algae C.vulgaris, be 10:1(L:kg by liquid-solid ratio) mix after, stir process 3.0 hours under atmospheric boiling point, use again organic solvents, chloroform/ethanol (volume ratio 1:1) to carry out grease extracting, the liquid-solid ratio (L:kg) of organic solvent and micro-algae is 8:1, can obtain yield and be 95% grease in centrifugal rear organic phase.
The extracting method of embodiment 7 microalgae greases
The formic acid solution that is 70% by mass percent concentration with micro-algae C.minutissima by liquid-solid ratio 10:1(L:kg) mix after, stir process 0.25 hour under atmospheric boiling point, use again organic solvent sherwood oil/methyl alcohol (volume ratio 1:1) to carry out grease extracting, the liquid-solid ratio (L:kg) of organic solvent and micro-algae is 3:1, can obtain yield and be 92% grease in centrifugal rear organic phase.The extracting method of embodiment 8 microalgae greases
The acetic acid solution that is 70% by mass percent concentration is 10:1(L:kg with micro-algae T.fluviatilis by liquid-solid ratio) mix after, stir process 2 hours under atmospheric boiling point, use again organic solvent sherwood oil/methyl alcohol (volume ratio 2:1) to carry out grease extracting, the liquid-solid ratio (L:kg) of organic solvent and micro-algae is 10:1, can obtain yield and be 95% grease in centrifugal rear organic phase.
The extracting method of embodiment 9 microalgae greases
The acetic acid solution that is 30% at mass percent concentration interpolation mass percent concentration (based on micro-algae dry weight) is 2% hydrochloric acid, gained mixed solution is 10:1(L:kg with micro-algae T.fluviatilis by liquid-solid ratio) mix after, stir process 2 hours under atmospheric boiling point, use again organic solvents, chloroform/ethanol alcohol (volume ratio 3:1) to carry out grease extracting, the liquid-solid ratio (L:kg) of organic solvent and micro-algae is 5:1, can obtain yield and be 98% grease in centrifugal rear organic phase.
The extracting method of embodiment 10 microalgae greases
The propionic acid solution that is 30% at mass percent concentration interpolation mass percent concentration (based on micro-algae dry weight) is 3% sulfuric acid, gained mixed solution is 5:1(L:kg with micro-algae T.pseudonana by liquid-solid ratio) mix after, stir process 3 hours under atmospheric boiling point, use again organic solvents, chloroform/methyl alcohol (volume ratio 1:1) to carry out grease extracting, the liquid-solid ratio (L:kg) of organic solvent and micro-algae is 2:1, can obtain yield and be 94% grease in centrifugal rear organic phase.
The extracting method of embodiment 11 microalgae greases
The formic acid solution that is 70% by mass percent concentration is 8:1(L:kg with micro-algae T.pseudonana by liquid-solid ratio) mix after, stir process 5 hours under atmospheric boiling point, use again organic solvents, chloroform/methyl alcohol (volume ratio 2:1) to carry out grease extracting, the liquid-solid ratio (L:kg) of organic solvent and micro-algae is 3:1, can obtain yield and be 96% grease in centrifugal rear organic phase.
The extracting method of embodiment 12 microalgae greases
In the acetic acid solution that is 50% at mass percent concentration, add mass percent concentration (based on micro-algae dry weight) and be 2% phosphoric acid, gained mixed solution is 5:1(L:kg with micro-algae Botryococcus sp. by liquid-solid ratio) mix after, stir process 4.0 hours under atmospheric boiling point, carry out grease extracting with organic solvent sherwood oil again, the liquid-solid ratio (L:kg) of organic solvent and micro-algae is 3:1, can obtain yield and be 92% grease in centrifugal rear organic phase.
The extracting method of embodiment 13 microalgae greases
The formic acid solution that is 60% by mass percent concentration is 9:1(L:kg with micro-algae T.pseudonana by liquid-solid ratio) mix after, stir process 2.0 hours under atmospheric boiling point, carry out grease extracting with organic solvents, chloroform again, the liquid-solid ratio (L:kg) of organic solvent and micro-algae is 6:1, can obtain yield and be 92% grease in centrifugal rear organic phase.
The extracting method of embodiment 14 microalgae greases
The acetic acid solution that is 80% by mass percent concentration is 7:1(L:kg with micro-algae T.fluviatilis by liquid-solid ratio) mix after, stir process 5.0 hours under atmospheric boiling point, carry out grease extracting with organic solvent-normal hexane again, the liquid-solid ratio (L:kg) of organic solvent and micro-algae is 7:1, can obtain yield and be 93% grease in centrifugal rear organic phase.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (8)
1. the extracting method of microalgae grease, it is characterized in that, the solid-to-liquid ratio that is 1:3-20 by kg:L adds the organic acid of mass percent concentration 30%-100% and the mineral acid of mass percent concentration 0%-3% in micro-algae, processes after 0.25-5.0h, adds organic solvent to carry out the extraction of grease.
2. method according to claim 1, is characterized in that, described organic solvent and organic acid add in a subtle way in algae simultaneously.
3. method according to claim 1 and 2, is characterized in that, the solid-to-liquid ratio that is 1:2-10 by kg:L adds organic solvent in micro-algae.
4. method according to claim 1 and 2, is characterized in that, described organic acid is aliphatics organic acid.
5. method according to claim 4, is characterized in that, described organic acid includes but not limited to formic acid, acetic acid and/or propionic acid.
6. method according to claim 1 and 2, is characterized in that, described mineral acid includes but not limited to sulfuric acid, hydrochloric acid, phosphoric acid and/or nitric acid.
7. method according to claim 1 and 2, is characterized in that, described organic solvent includes but not limited to chloroform, sherwood oil and/or normal hexane, and the mixed solution of they and methyl alcohol or ethanol.
8. method according to claim 1 and 2, is characterized in that, described micro-algae includes but not limited to Chlorella vulgaris, Botryococcus sp., C.vulgaris, C.minutissima, T.fluviatilis, T.pseudonana.
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| CN201410108480.3A CN103849458B (en) | 2014-03-21 | 2014-03-21 | The extracting method of microalgae grease |
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| CN201410108480.3A CN103849458B (en) | 2014-03-21 | 2014-03-21 | The extracting method of microalgae grease |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105623831A (en) * | 2014-10-28 | 2016-06-01 | 中国石油化工股份有限公司 | Method for extracting 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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| CN105623831A (en) * | 2014-10-28 | 2016-06-01 | 中国石油化工股份有限公司 | Method for extracting microalgae grease |
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| CN109111987A (en) * | 2018-08-30 | 2019-01-01 | 中国海洋大学 | A kind of oil extracting methods |
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| CN103849458B (en) | 2016-08-10 |
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Effective date of registration: 20190729 Address after: 100084 Beijing Haidian District Tsinghua Science and Technology Park Innovation Building B Block 10 Floor 1001 Patentee after: Beijing Kaidi Deqing Bioenergy Technology Co., Ltd. Address before: 100084 Beijing Haidian District Tsinghua Yuan 100084-82 mailbox Patentee before: Tsinghua University |