CN104745298A - Method for preparing biodiesel by directly performing ester exchange by oleaginous microorganisms - Google Patents
Method for preparing biodiesel by directly performing ester exchange by oleaginous microorganisms Download PDFInfo
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- CN104745298A CN104745298A CN201510148399.2A CN201510148399A CN104745298A CN 104745298 A CN104745298 A CN 104745298A CN 201510148399 A CN201510148399 A CN 201510148399A CN 104745298 A CN104745298 A CN 104745298A
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- Prior art keywords
- ester exchange
- oleaginous microorganism
- biodiesel
- preparing biodiesel
- method utilizing
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Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
-
- C—CHEMISTRY; METALLURGY
- 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
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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
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
- C11C3/10—Ester interchange
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Wood Science & Technology (AREA)
- Microbiology (AREA)
- General Chemical & Material Sciences (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Liquid Carbonaceous Fuels (AREA)
Abstract
The invention discloses a method for preparing biodiesel by directly performing ester exchange by oleaginous microorganisms. The method is used for preparing biodiesel by directly performing ester exchange by taking oleaginous microorganisms as raw materials. The method comprises the following steps: mixing a mixed solvent comprising dried biomass with normal hexane and alcohol with certain concentration with a catalyst concentrated sulfuric acid, and performing reaction under reflux condensation and stirring for a certain time in a constant-temperature oil bath at a certain temperature; after the reaction is ended, filtering to remove filter residues, extracting filtrate, and distilling solvent under reduced pressure to obtain a biodiesel crude product. According to the method disclosed by the invention, a low-toxicity organic solvent is utilized to directly prepare the biodiesel by taking the biomass as a raw material through extraction-ester exchange one step. Assistance of microwaves, ultrasonic sounds and the like is not required in the reaction process, so that the energy consumption is reduced; the solvents are low-toxicity organic solvents, clean and environmentally friendly. The process is simple and easy to operate.
Description
Technical field
The invention belongs to field of biological energy source, be specifically related to take oleaginous microorganism as raw material, adopt the vitriol oil as catalyzer, in organic solvent system, extraction-ester exchanges the method that a step prepares biofuel.
Background technology
Along with the day by day exhausted of fossil oil and the pollution of burning to environment thereof, seek sustainable extremely urgent with renewable energy source.
Biofuel (biodiesel) refers to animal-plant oil, microbial oil, food garbage wet goods to be the liquid fuel of the replaced petrifaction diesel that stock oil is made by ester exchange process, splendid with diesel oil intermiscibility, and can mix with GB diesel oil or be used alone, being typical clean, renewable " green energy resource ", is the ideal substitute of the Nonrenewable resources such as oil.
Along with the development of Modern microbiological technology, take microbial oil as raw material, the research of production biofuel also makes some progress.Microorganism has the features such as reproduction speed is fast, growth cycle is short, grease yield is high, adaptive capacity to environment is strong, compared with other oil crops, utilize the floor space needed for microorganism culturing production biofuel few, microorganism can utilize carbonic acid gas as raw material, can also grow in various weather, environment, even comprise the area of the unsuitable agro-farming such as desert, wasteland and beach beach.
Be at present that the method for the direct preparing biodiesel by ester exchange of raw material has a lot with oleaginous microorganism, but in order to make microorganism, intracellular grease is discharged, general all with ultrasonic or microwave for subsidiary conditions, destroy the cell walls of oleaginous microorganism and accelerate transesterification reaction speed; Or with strong polar organic solvent as chloroform extracts-ester permutoid reaction under the high temperature conditions.But aforesaid method all has weak point, use energy consumption that is ultrasonic, microwave very large, be not easy to industrialization; Although the shell-broken effect of chloroform is fine, toxicity is very large, has a certain impact to environment.
Therefore, the preparation method developing the biofuel that a kind of efficiency is high, energy consumption is low, technique is simple, cost is low is needed.
Summary of the invention
The object of the present invention is to provide a kind of take oleaginous microorganism as the method for raw material, direct preparing biodiesel by ester exchange, and described method utilizes low toxicity mixed organic solvents, can realize being directly raw material with biomass, extracts-ester and exchanges a step and prepare biofuel.Reaction process is assisted without the need to microwave, ultrasonic etc., energy efficient; Solvent is low-toxic organic solvent, clean environment firendly; Technical process is simple, easy to operate.
For achieving the above object, the technical scheme that present invention employs is a kind of method utilizing the direct preparing biodiesel by ester exchange of oleaginous microorganism, and specifically, the method comprises the steps,
The mixed solvent that the oleaginous microorganism of drying forms with normal hexane and ethanol by S1, the catalyzer vitriol oil mix, condensing reflux stirring reaction in thermostatical oil bath under the high temperature conditions.
After S2 has reacted, the solution reacted is taken out, under room temperature condition, leaves standstill cooling 1-1.5 hour, cross and filter filter residue, filtrate n-hexane extraction, add saturated NaCl solution, after stratification, collect upper strata normal hexane phase, repeatedly extract 3-4 time, merge organic phase, underpressure distillation, namely obtains biodiesel coarse product.
Described oleaginous microorganism is one or more in chlorella, grape ball algae, grid algae, Dunaliella salina, plan Nannochloropsis oceanica, rhodotorula glutinis, ocean rhodotorula.
The biomass of described oleaginous microorganism and the solid-liquid ratio of mixed solvent are 1:10 ~ 1:30g/mL.
In described mixed solvent, the volume ratio of normal hexane and ethanol is 1:3 ~ 3:1, and the concentration of ethanol is 70% ~ 80% (v/v).
The concentration of the described catalyzer vitriol oil is 5 ~ 25mL/g biomass.
The temperature of described reaction condensing reflux in constant temperature oil bath is 60 ~ 100 DEG C.
The time that described mixed solvent and biomass are reacted is 30 ~ 120min.
Compared with prior art, the present invention has following beneficial effect.
According to method of the present invention, utilize the mixed organic solvents of low toxicity, can realize taking oleaginous microorganism as raw material, extract-ester exchange single stage method and prepare biofuel.Reaction process is assisted without the need to microwave, ultrasonic etc., energy efficient; Solvent is low-toxic organic solvent, clean environment firendly; Technical process is simple, easy to operate.
Embodiment
Essentiality content for a better understanding of the present invention, elaborates in conjunction with example, but does not limit the present invention with this.Protection scope of the present invention is as the criterion with appending claims.
Embodiment 1
Take the dry algae powder 0.3g of chlorella in 50mL round-bottomed flask, add the normal hexane of 6mL and the mixing solutions (normal hexane: 75% ethanol=1:2 (v/v) of 75% ethanol, the vitriol oil of 0.8mL, round-bottomed flask is placed at condensing reflux in the constant temperature oil bath of 90 DEG C, stirring reaction 120min.After having reacted, the solution reacted is taken out, under room temperature condition, leaves standstill cooling 1 hour, cross and filter algae powder, filtrate is transferred in separating funnel, uses 4mL n-hexane extraction, add the saturated NaCl solution of 4mL, after stratification, collect upper strata normal hexane phase, repeatedly extract 3 times, merge organic phase, underpressure distillation, namely obtains biodiesel coarse product, and the conversion yield of biofuel is 90.61%.
Embodiment 2
Take the dry algae powder 0.3g of chlorella in 50mL round-bottomed flask, add the normal hexane of 4.5mL and the mixing solutions (normal hexane: 75% ethanol=1:2 (v/v) of 75% ethanol, the vitriol oil of 0.6mL, round-bottomed flask is placed at condensing reflux in the constant temperature oil bath of 90 DEG C, stirring reaction 120min.After having reacted, the solution reacted is taken out, under room temperature condition, leaves standstill cooling 1 hour, cross and filter algae powder, filtrate is transferred in separating funnel, uses 3mL n-hexane extraction, add the saturated NaCl solution of 3mL, after stratification, collect upper strata normal hexane phase, repeatedly extract 4 times, merge organic phase, underpressure distillation, namely obtains biodiesel coarse product, and the conversion yield of biofuel is 84.46%.
Embodiment 3
Take the dry algae powder 0.3g of chlorella in 50mL round-bottomed flask, add the normal hexane of 6mL and the mixing solutions (normal hexane: 75% ethanol=1:2 (v/v) of 75% ethanol, the vitriol oil of 0.4mL, round-bottomed flask is placed at condensing reflux in the constant temperature oil bath of 100 DEG C, stirring reaction 120min.After having reacted, the solution reacted is taken out, under room temperature condition, leaves standstill cooling 1 hour, cross and filter algae powder, filtrate is transferred in separating funnel, uses 4mL n-hexane extraction, add the saturated NaCl solution of 4mL, after stratification, collect upper strata normal hexane phase, repeatedly extract 3 times, merge organic phase, underpressure distillation, namely obtains biodiesel coarse product, and the conversion yield of biofuel is 89.13%.
In above embodiment, oleaginous microorganism used is replaced with grape ball algae, grid algae, Dunaliella salina, plan Nannochloropsis oceanica, rhodotorula glutinis, ocean rhodotorula, repeat above-mentioned experiment, acquired results is similar.
Claims (7)
1. utilize a method for the direct preparing biodiesel by ester exchange of oleaginous microorganism, it is characterized in that: the method comprises the steps,
The mixed solvent that the oleaginous microorganism of drying forms with normal hexane and ethanol by S1, the catalyzer vitriol oil mix, condensing reflux stirring reaction in thermostatical oil bath under the high temperature conditions;
After S2 has reacted, the solution reacted is taken out, under room temperature condition, leaves standstill cooling 1-1.5 hour, cross and filter filter residue, filtrate n-hexane extraction, add saturated NaCl solution, after stratification, collect upper strata normal hexane phase, repeatedly extract 3-4 time, merge organic phase, underpressure distillation, namely obtains biodiesel coarse product.
2. a kind of method utilizing the direct preparing biodiesel by ester exchange of oleaginous microorganism according to claim 1, is characterized in that: described oleaginous microorganism is one or more in chlorella, grape ball algae, grid algae, Dunaliella salina, plan Nannochloropsis oceanica, rhodotorula glutinis, ocean rhodotorula.
3. a kind of method utilizing the direct preparing biodiesel by ester exchange of oleaginous microorganism according to claim 1, is characterized in that: the biomass of described oleaginous microorganism and the solid-liquid ratio of mixed solvent are 1:10 ~ 1:30g/mL.
4. a kind of method utilizing the direct preparing biodiesel by ester exchange of oleaginous microorganism according to claim 1, it is characterized in that: in described mixed solvent, the volume ratio of normal hexane and ethanol is 1:3 ~ 3:1, the concentration of ethanol is 70% ~ 80% (v/v).
5. a kind of method utilizing the direct preparing biodiesel by ester exchange of oleaginous microorganism according to claim 1, is characterized in that: the concentration of the described catalyzer vitriol oil is 5 ~ 25mL/g biomass.
6. a kind of method utilizing the direct preparing biodiesel by ester exchange of oleaginous microorganism according to claim 1, is characterized in that: the temperature of described reaction condensing reflux in constant temperature oil bath is 60 ~ 100 DEG C.
7. a kind of method utilizing the direct preparing biodiesel by ester exchange of oleaginous microorganism according to claim 1, is characterized in that: the time that described mixed solvent and biomass are reacted is 30 ~ 120min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510148399.2A CN104745298A (en) | 2015-03-31 | 2015-03-31 | Method for preparing biodiesel by directly performing ester exchange by oleaginous microorganisms |
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| CN201510148399.2A CN104745298A (en) | 2015-03-31 | 2015-03-31 | Method for preparing biodiesel by directly performing ester exchange by oleaginous microorganisms |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108102790A (en) * | 2016-11-24 | 2018-06-01 | 中国科学院大连化学物理研究所 | A kind of aquatic byproducts fatty-acid ethyl ester preparation method |
| CN108774581A (en) * | 2018-07-06 | 2018-11-09 | 中国林业科学研究院林产化学工业研究所 | A kind of method and device directly preparing biodiesel from yeast |
| CN109722313A (en) * | 2019-02-25 | 2019-05-07 | 电子科技大学中山学院 | Oil refining technology by pressure reduction explosion of oil-containing microalgae |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101580857A (en) * | 2009-07-01 | 2009-11-18 | 新奥科技发展有限公司 | Biomass energy prepared by one-step method of microalgae |
| CN102071100A (en) * | 2011-01-17 | 2011-05-25 | 中国科学院青岛生物能源与过程研究所 | Method for extracting grease from wet alga mud by using mixed organic solvent |
| US20120094339A1 (en) * | 2009-04-10 | 2012-04-19 | Electric Power Development Co., Ltd. | Micro-alga belonging to genus navicula, process for production of oil by culture of the micro-alga, and oil collected from the micro-alga |
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2015
- 2015-03-31 CN CN201510148399.2A patent/CN104745298A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20120094339A1 (en) * | 2009-04-10 | 2012-04-19 | Electric Power Development Co., Ltd. | Micro-alga belonging to genus navicula, process for production of oil by culture of the micro-alga, and oil collected from the micro-alga |
| CN101580857A (en) * | 2009-07-01 | 2009-11-18 | 新奥科技发展有限公司 | Biomass energy prepared by one-step method of microalgae |
| CN102071100A (en) * | 2011-01-17 | 2011-05-25 | 中国科学院青岛生物能源与过程研究所 | Method for extracting grease from wet alga mud by using mixed organic solvent |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108102790A (en) * | 2016-11-24 | 2018-06-01 | 中国科学院大连化学物理研究所 | A kind of aquatic byproducts fatty-acid ethyl ester preparation method |
| CN108774581A (en) * | 2018-07-06 | 2018-11-09 | 中国林业科学研究院林产化学工业研究所 | A kind of method and device directly preparing biodiesel from yeast |
| CN109722313A (en) * | 2019-02-25 | 2019-05-07 | 电子科技大学中山学院 | Oil refining technology by pressure reduction explosion of oil-containing microalgae |
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