CN104449788A - Method for preparing micro-algal oil by microalgae hydro-thermal liquefaction - Google Patents
Method for preparing micro-algal oil by microalgae hydro-thermal liquefaction Download PDFInfo
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- CN104449788A CN104449788A CN201310418953.5A CN201310418953A CN104449788A CN 104449788 A CN104449788 A CN 104449788A CN 201310418953 A CN201310418953 A CN 201310418953A CN 104449788 A CN104449788 A CN 104449788A
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- micro
- algae
- microalgae
- hydro
- algal oil
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Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1011—Biomass
- C10G2300/1014—Biomass of vegetal origin
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a method for preparing micro-algal oil by microalgae hydro-thermal liquefaction. The method comprises the following steps of 1, culturing and collecting microalgae, adding the microalgae into a hydro-thermal reactor and mixing the microalgae and deionized water to obtain a microalgae liquid with a solid-liquid ratio of 1-50g: 100ml, 2, sealing the hydro-thermal reactor, completely removing air in the reactor, carrying out heating to a temperature of 180-450 DEG C with stirring and keeping the temperature for 10-180min, and 3, cooling and collecting the reaction products, carrying out extraction and suction extraction, separating and filtering an organic phase, removing the organic solvent and collecting the micro-algal oil. The method utilizes microalgae as a raw material, utilizes a mild and controllable hydro-thermal reaction system to prepare the micro-algal oil, reduces energy consumption and a cost of the reaction system, improves a calorific value and a yield of the micro-algal oil and realizes resource utilization of algae waste causing water eutrophication.
Description
Technical field
The present invention relates to biomass energy technology field, particularly relate to a kind of method micro-algae oil being prepared by micro-algae hydrothermal liquefaction.
Background technology
Along with the raising of expanding economy and living standards of the people, the demand of the mankind to the energy increases day by day, meanwhile, day by day exhausted with the fossil oil that coal, oil are representative, and a large amount of uses of fossil oil certainly will bring the environmental problems such as such as Greenhouse effect, how cracking lack of energy and environmental pollution bottleneck is the key subjects of pendulum in face of the universe, is that the renewable energy source of representative is because of its environmental friendliness and reproducible feature causes extensive concern day by day with biomass energy.
Biomass energy is as a kind of clean reproducible energy, and it utilizes process can realize the closed circulation of carbon, thus reduces to airborne release CO
2, effectively reduce greenhouse gases effect.Current biomass energy develops and focuses mostly in terrestrial organism matter, and the mainly lignocellulose raw material such as stalk, wood type, biomass material is converted into liquid fuel bio oil by reaction process many employings high temperature (>500 DEG C) pyrolysis.But, Wooden Biomass raw material exist growth cycle slow, take up an area large, biomass is lower and by the larger shortcoming of seasonal effect, and pyrolytic process requires very high temperature and raw material need shift to an earlier date drying, and the bio oil oxygen level of gained is high and character unstable.
Micro-algae is a kind of waterplant, has the characteristic of the aspects such as short, the solid carbon efficiencies of growth cycle is high, fecundity strong, easily cultivation, tolerance extreme environment.Containing abundant carbohydrate, protein, fat etc. in micro-algae, not containing xylogen, just can realize pyrolysis at a lower temperature, micro-algae oil of gained has more advantage compared with the bio oil prepared with lignocellulose raw material in stability, calorific value etc.
Publication number is that the Chinese invention patent of CN1446883A proposes the micro-algae of a kind of fast pyrogenation to prepare the method for biofuel, application number be 01136699.0 Chinese invention patent application also with micro-algae for raw material carries out pyrolysis to prepare Oil/gas Fuels, these patents all adopt the transform mode of high temperature pyrolysis, because the water content of micro-algae is all more than 90%, algae all needs to carry out drying treatment after collection, micro-algae is prepared as algae powder, and therefore energy consumption is larger.Application number is a kind of method that the Chinese invention patent application of 200910054288.X proposes micro-algae preparing liquid fuel by hydrothermal liquification, but this method need pour high pressure N
2, higher to equipment requirements.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method that micro-algae hydrothermal liquefaction prepares micro-algae oil, and its energy consumption is low, low for equipment requirements, and the micro-algae oil-proofness, calorific value and the productive rate that prepare are high.
For solving the problems of the technologies described above, micro-algae hydrothermal liquefaction of the present invention prepares the method for micro-algae oil, and step comprises:
1) cultivate and collect micro-algae, adding in hydrothermal reaction kettle, being mixed to form micro-algae liquid of solid-to-liquid ratio 1 ~ 50g:100ml with deionized water;
2) seal hydrothermal reaction kettle, the air side by side in clean hydrothermal reaction kettle, is then under agitation warming up to 180 ~ 450 DEG C, keeps 10 ~ 180min;
3) cooling water heat reactor, collecting reaction product, and carry out extracting and extracting with organic solvent, be then separated and filter organic phase, removing organic solvent, obtaining micro-algae oil.
Described micro-algae is seawater or the freshwater microalgae of high-moisture percentage, comprises chlorella, spirulina, blue-green algae, salt algae, Enteromorpha etc.
Step 1), can add NaOH, KOH, K in reaction system
2cO
3, Na
2cO
3in one or more as additive, the solution quality percentage concentration of additive is 0 ~ 10.0%.
Step 3), the organic solvent for extracting can use in the organic solvents such as methylene dichloride, chloroform, tetracol phenixin one or more.
The present invention for raw material with micro-algae, adopts gentle controlled hydro-thermal reaction system to prepare micro-algae oil, compared with the existing preparation method of micro-algae oil, has the following advantages and beneficial effect:
1. raw material is without the need to drying, and micro-algae just can directly be liquefied after simple concentrated collection, and water-heat process temperature is very low, and therefore energy consumption is less, gained micro-algae oil calorific value and productive rate high.
2. the micro-algae that can be used as raw material is wide in variety, and micro-algae itself have growth and breeding speed fast, be easy to the advantages such as possession, land seizure area are little, pond, coastal marine site, beach, wetland etc. can be made full use of propagate artificially on a large scale, thus the cost of raw material can be reduced.
3. effectively can process the algae pollutant waste causing body eutrophication, realize its recycling.Meanwhile, micro-algae propagation process can also realize CO
2high-performance bio fix, chemical conversion and closed carbon cycle.
4. react gained liquid product, solid residue and gaseous component (mainly CO
2) can realize circulating and fully utilizing.Wherein, liquid product and gaseous component capable of circulation for microdisk electrode, solid phase residue be rich in the elements such as C, N can be used for lean soil improvement.
Accompanying drawing explanation
Fig. 1 is the method flow schematic diagram that micro-algae hydrothermal liquefaction of the present invention prepares micro-algae oil.
Embodiment
Understand more specifically for having technology contents of the present invention, feature and effect, now by reference to the accompanying drawings, to the present invention, details are as follows:
Embodiment 1
With the micro-algae of bead for raw material, get the micro-algae of 20g bead and 150ml distilled water loading 300ml autoclave, stir and be prepared into micro-algae slurries.Reactor is sealed, uses N
2air in emptying still, opens heater switch, determines stirring velocity 200r/min, starts with the ramp to 300 DEG C of about 4 DEG C/min, keep 30min, close heater switch immediately, be cooled to room temperature, collect the gas produced, drive still and take out reaction mixture, utilize CH
2cl
2cleaning reaction still inwall and agitator, and mixture is extracted.Separating and extracting liquid, uses filtered on buchner funnel CH
2cl
2phase, then CH is reclaimed in underpressure distillation
2cl
2, obtain micro-algae oil.
The productive rate of micro-algae oil is 23.00%, and calorific value is 35.81KJ/g.Water-dissolving phase product is capable of circulation again for microdisk electrode after certain process, and remaining solid phase algae-residue can be used for soil improvement after drying, the CO in the gas produced in hydrothermal liquefaction process
2, can both culturing microalgae be cycled to used in.
Embodiment 2
With the micro-algae of bead for raw material, get the micro-algae of 20g bead and 200ml distilled water loading 300ml autoclave, stir and be prepared into micro-algae slurries.Reactor is sealed, uses N
2air in emptying still, opens heater switch, determines stirring velocity 200r/min, starts with the ramp to 320 DEG C of about 4 DEG C/min, keep 30min, close heater switch immediately, be cooled to room temperature, collect the gas produced, drive still and take out reaction mixture, utilize CH
2cl
2cleaning reaction still inwall and agitator, and mixture is extracted.Separating and extracting liquid, uses filtered on buchner funnel CH
2cl
2phase, then CH is reclaimed in underpressure distillation
2cl
2, obtain micro-algae oil.
The productive rate of micro-algae oil is 30.62%, and calorific value is 32.34KJ/g.Water-dissolving phase product is capable of circulation again for microdisk electrode after certain process, and remaining solid phase algae-residue can be used for soil improvement after drying, the CO in the gas produced in hydrothermal liquefaction process
2, can both culturing microalgae be cycled to used in.
Embodiment 3
With the micro-algae of bead for raw material, get the micro-algae of 20g bead and concentration be 5.0% 200ml NaOH solution load 300ml autoclave, stir and be prepared into micro-algae slurries.Reactor is sealed, uses N
2air in emptying still, opens heater switch, determines stirring velocity 200r/min, starts with about 4 DEG C/min ramp to 300 DEG C, keeps 30min, closes heater switch immediately, be cooled to room temperature, collects the gas produced, and drives still and takes out reaction mixture, utilize CH
2cl
2cleaning reaction still inwall and agitator, and mixture is extracted.Separating and extracting liquid, uses filtered on buchner funnel CH
2cl
2phase, then CH is reclaimed in underpressure distillation
2cl
2, obtain micro-algae oil.
The productive rate of micro-algae oil is 32.83%, and calorific value is 30.53KJ/g.Water-dissolving phase product is capable of circulation again for microdisk electrode after certain process, and remaining solid phase algae-residue can be used for soil improvement after drying, the CO in the gas produced in hydrothermal liquefaction process
2, can both culturing microalgae be cycled to used in.
Claims (5)
1. micro-algae hydrothermal liquefaction prepares the method for micro-algae oil, and it is characterized in that, step comprises:
1) cultivate and collect micro-algae, adding in hydrothermal reaction kettle, being mixed to form micro-algae liquid of solid-to-liquid ratio 1 ~ 50g:100ml with deionized water;
2) seal hydrothermal reaction kettle, the air side by side in clean hydrothermal reaction kettle, is then under agitation warming up to 180 ~ 450 DEG C, keeps 10 ~ 180min;
3) cooling water heat reactor, collecting reaction product, and carry out extracting and extracting with organic solvent, be then separated and filter organic phase, removing organic solvent, obtaining micro-algae oil.
2. the method for claim 1, is characterized in that, described micro-algae is seawater or the freshwater microalgae of high-moisture percentage, comprises chlorella, spirulina, blue-green algae, salt algae, Enteromorpha.
3. the method for claim 1, is characterized in that, step 1), in reaction system, add NaOH, KOH, K
2cO
3, Na
2cO
3in one or more as additive.
4. method as claimed in claim 3, it is characterized in that, the solution quality percentage concentration of described additive is 0 ~ 10.0%.
5. the method for claim 1, is characterized in that, step 3), and the organic solvent for extracting comprises one or more the mixing solutions in methylene dichloride, chloroform, tetracol phenixin.
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|---|---|---|---|
| CN201310418953.5A CN104449788A (en) | 2013-09-13 | 2013-09-13 | Method for preparing micro-algal oil by microalgae hydro-thermal liquefaction |
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|---|---|---|---|
| CN201310418953.5A CN104449788A (en) | 2013-09-13 | 2013-09-13 | Method for preparing micro-algal oil by microalgae hydro-thermal liquefaction |
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| Publication Number | Publication Date |
|---|---|
| CN104449788A true CN104449788A (en) | 2015-03-25 |
Family
ID=52896551
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310418953.5A Pending CN104449788A (en) | 2013-09-13 | 2013-09-13 | Method for preparing micro-algal oil by microalgae hydro-thermal liquefaction |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105001971A (en) * | 2015-06-26 | 2015-10-28 | 新奥科技发展有限公司 | Two-step production method for microalgae bio-oil |
| CN105080939A (en) * | 2015-09-07 | 2015-11-25 | 中国科学院烟台海岸带研究所 | Emergency rapid reduction method of ashore green tide algae |
| CN107151055A (en) * | 2017-06-01 | 2017-09-12 | 中国农业大学 | A kind of method that waste water of livestock poultry environment increment is utilized |
| CN107159679A (en) * | 2017-05-17 | 2017-09-15 | 浙江大学 | A kind of method that fuel oil is produced in Kitchen waste hydrothermal liquefaction |
| CN108671928A (en) * | 2018-05-04 | 2018-10-19 | 中国人民大学 | A kind of catalyst and the preparation method and application thereof for microalgae hydrothermal liquefaction deoxidation |
| CN109569476A (en) * | 2018-10-24 | 2019-04-05 | 浙江海洋大学 | The method that fresh-water fishes waste prepares bio-oil |
| CN110194981A (en) * | 2019-05-07 | 2019-09-03 | 江苏大学 | Sludge, microalgae are total to hydro-thermal liquefaction and waste liquid culture microalgae integration cyclic utilization system |
| RU2701372C1 (en) * | 2018-12-26 | 2019-09-26 | федеральное государственное автономное образовательное учреждение высшего образования "Российский государственный университет нефти и газа (национальный исследовательский университет) имени И.М. Губкина" | Method of producing biofuel |
| CN110467945A (en) * | 2019-06-27 | 2019-11-19 | 江苏大学 | A kind of method that the voluminous object of microalgae liquefaction participates in the copyrolysis upgrading of kitchen abandoned oil |
| CN110591919A (en) * | 2019-09-10 | 2019-12-20 | 江苏大学 | Method for cultivating microalgae and preparing bio-oil by using kitchen waste water |
| CN110819370A (en) * | 2019-10-24 | 2020-02-21 | 华南农业大学 | Method for promoting quality improvement of microalgae hydrothermal heavy oil by virtue of synergy of acid and surfactant and application of method |
| CN111205883A (en) * | 2020-01-21 | 2020-05-29 | 安徽大学 | Method for preparing low-nitrogen biomass oil by microalgae hydrothermal liquefaction |
| CN111253966A (en) * | 2020-03-19 | 2020-06-09 | 浙江昌丽家居有限公司 | Environment-friendly wood leftover material recycling and harmless treatment method |
| RU2787537C1 (en) * | 2022-09-21 | 2023-01-10 | Федеральное государственное автономное образовательное учреждение высшего образования "Балтийский федеральный университет имени Иммануила Канта" (БФУ им. И. Канта) | Method for producing a biofuel from macroalgae |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105001971A (en) * | 2015-06-26 | 2015-10-28 | 新奥科技发展有限公司 | Two-step production method for microalgae bio-oil |
| CN105080939A (en) * | 2015-09-07 | 2015-11-25 | 中国科学院烟台海岸带研究所 | Emergency rapid reduction method of ashore green tide algae |
| CN107159679A (en) * | 2017-05-17 | 2017-09-15 | 浙江大学 | A kind of method that fuel oil is produced in Kitchen waste hydrothermal liquefaction |
| CN107159679B (en) * | 2017-05-17 | 2019-12-03 | 浙江大学 | A kind of method that fuel oil is produced in Kitchen waste hydrothermal liquefaction |
| CN107151055A (en) * | 2017-06-01 | 2017-09-12 | 中国农业大学 | A kind of method that waste water of livestock poultry environment increment is utilized |
| CN108671928B (en) * | 2018-05-04 | 2021-05-18 | 中国人民大学 | Catalyst for microalgae hydrothermal liquefaction and deoxidation and preparation method and application thereof |
| CN108671928A (en) * | 2018-05-04 | 2018-10-19 | 中国人民大学 | A kind of catalyst and the preparation method and application thereof for microalgae hydrothermal liquefaction deoxidation |
| CN109569476A (en) * | 2018-10-24 | 2019-04-05 | 浙江海洋大学 | The method that fresh-water fishes waste prepares bio-oil |
| RU2701372C1 (en) * | 2018-12-26 | 2019-09-26 | федеральное государственное автономное образовательное учреждение высшего образования "Российский государственный университет нефти и газа (национальный исследовательский университет) имени И.М. Губкина" | Method of producing biofuel |
| CN110194981A (en) * | 2019-05-07 | 2019-09-03 | 江苏大学 | Sludge, microalgae are total to hydro-thermal liquefaction and waste liquid culture microalgae integration cyclic utilization system |
| CN110467945A (en) * | 2019-06-27 | 2019-11-19 | 江苏大学 | A kind of method that the voluminous object of microalgae liquefaction participates in the copyrolysis upgrading of kitchen abandoned oil |
| CN110591919A (en) * | 2019-09-10 | 2019-12-20 | 江苏大学 | Method for cultivating microalgae and preparing bio-oil by using kitchen waste water |
| CN110819370A (en) * | 2019-10-24 | 2020-02-21 | 华南农业大学 | Method for promoting quality improvement of microalgae hydrothermal heavy oil by virtue of synergy of acid and surfactant and application of method |
| CN111205883A (en) * | 2020-01-21 | 2020-05-29 | 安徽大学 | Method for preparing low-nitrogen biomass oil by microalgae hydrothermal liquefaction |
| CN111253966A (en) * | 2020-03-19 | 2020-06-09 | 浙江昌丽家居有限公司 | Environment-friendly wood leftover material recycling and harmless treatment method |
| RU2794959C1 (en) * | 2022-05-16 | 2023-04-26 | федеральное государственное автономное образовательное учреждение высшего образования "Российский университет дружбы народов" (РУДН) | Method for obtaining biofuel |
| RU2787537C1 (en) * | 2022-09-21 | 2023-01-10 | Федеральное государственное автономное образовательное учреждение высшего образования "Балтийский федеральный университет имени Иммануила Канта" (БФУ им. И. Канта) | Method for producing a biofuel from macroalgae |
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