CN103361166A - Method for preparing bio-oil from microalgae through direct liquidation - Google Patents
Method for preparing bio-oil from microalgae through direct liquidation Download PDFInfo
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Abstract
The invention relates to a method for preparing a bio-oil from microalgae through direct liquidation. The method comprises the following steps of: mixing microalgae with an alcohol-water mixed solution and putting the mixture into a reaction kettle, and heating for reacting, wherein the reaction conditions are as follows: temperature is 260-360 DEG C, and the pressure is 7-22 MPa; the reaction time ranges from 15 to 45 min; the ratio of the microalgae to the alcohol-water mixed solution is 1:(5-20), and the unit of the mixture is g/mL; the volume percentage content of the alcohol in the alcohol-water mixed solution is 20-80%; after the reaction is ended, adding an organic solvent for extracting the reaction liquid, wherein the reaction liquid is divided into an organic solvent phase, an alcohol-water phase and solid residues; after the extraction is finished, separating out the solid residues through suction filtration, and obtaining the organic solvent phase through separation after standing and layering of the liquid phase; removing the organic solvent from the organic solvent phase through reduced pressure distillation, thereby obtaining an oily liquid, namely, the bio-oil product, wherein the conditions of reduced pressure distillation are as follows: the gauge pressure is 0.085-0.095 MPa, and the temperature is 20-40 DEG C. The method provided by the invention is simple in process flow and low in energy consumption; the process of the method is environmentally-friendly.
Description
Technical field
The invention belongs to the biomass energy technology field, particularly the little algae of direct liquefaction prepares the method for bio-fuel-oil under a kind of Asia/supercritical water-pure condition.
Background technology
Along with the fast development of modern industry with science and technology, the problem of environmental pollution in short supply and that use fossil resource to bring of fossil resource has become two hang-ups of restriction human kind sustainable development.That biomass energy has is renewable, without CO
2Clean discharging and SO
x, NO
xThe advantages such as quantity discharged is few become the new forms of energy of people's common concern.At present, how fully effectively utilizing biomass resource has become people and has fallen over each other the focus studying and pay close attention to.The research that begins to consider to prepare take biomass as raw material the bio-fuel-oil aspect both at home and abroad mainly is that material take lignin and Mierocrystalline cellulose or hemicellulose class is as main, but because the temperature that lignin and Mierocrystalline cellulose or hemicellulose class need in pyrolytic process is high, processing condition are comparatively harsh, cause production cost to improve.Simultaneously, lignin and Mierocrystalline cellulose or hemicellulose are owing to self chemical composition and structure characteristic, and the bad of cracking gained bio-fuel-oil is compared with gasoline or diesel oil and still had larger difference, have therefore limited its development.
At present, little algae prepares biofuel and has obtained showing great attention to of countries in the world government and investigator.Little algae biofuel is considered to the third generation biofuel behind grain and the biological fuel of Mierocrystalline cellulose, algae is about to become one of most important biofuel source, be widely used little algae energy and can significantly alleviate fossil energy to the negative impact that social and environment bring, will become the trend of following bioenergy exploitation.The U.S. started " the miniature manhattan project " of obtaining energy fuel from little algae in 2007, and USDOE was issued again " national little algae bioenergy Technology Roadmap " draft in 2009.China also progressively strengthens the strategic understanding of seaweed bio fuel, the marine alga energy is being classified as the important component part of following biomass fuel industry.
Little algae is that a class formation is simple, the rapidly lower plant that grows, and it is wide at the distributed pole in the whole world, and having slightly, algae is the potential high quality raw material of preparation bioenergy owing to containing abundant grease.Compare with other higher plants, little algae has many advantages as the raw material of producing bioenergy: photosynthetic efficiency is high, growth cycle is short, adaptive capacity to environment is strong, easily cultivate, lipid content is high and process of growth in the efficient advantage such as stabilizing carbon dioxide.In addition, algal grown and procreation all are in water, do not strive ground with agricultural, do not affect agriculture production and process and can realize automatization and mass-producing.Therefore, research and develop little algal biomass energy conversion utilisation technology and have extremely important strategic importance.
Little algae recovery energy the earliest is to adopt the extracting, esterifying method, first lipid out is converted into biofuel through transesterification reaction again from the microalgae cell extracting and separating.Yet little algae is made of biochemical components such as protein, polysaccharide and lipids, and the extracting, esterifying method can only be utilized lipidic component wherein, and is high to the lipid content requirement of raw material, and the lipid composition is subjected to the lipid composition to affect very large on product property.In order to take full advantage of all components of little algae, people begin to adopt thermochemical techniques algae to be changed into the liquefied product-bio oil (bio-oil) of high-quality.Bio oil has low, the easy storage of sulphur nitrogen content, easily transportation and energy density advantages of higher, can be directly use as boiler oil, after also can promoting through upgrading as power with oil, also can be used to refine the chemical of processing high added value.
The liquefaction of little algae mainly comprises Rapid Thermal solution and direct liquefaction method etc.The Rapid Thermal solution is under the secluding air condition, adopts superelevation heating rate and ultra short contact time that little algae pyrolysis is converted into bio oil.The Rapid Thermal solution need to be carried out drying to raw material, so energy consumption is large; Next severe reaction conditions, equipment requirements is high.The direct liquefaction method claims again pressurized liquefied, refers to the method that biomass liquefy under suitable ambient condition.Wherein the direct liquefying method take water as medium claims again the hydro-thermal liquefaction process, and water medium is in Asia/supercritical state usually in little algae hydro-thermal liquefaction process.Compare with the pyrolysis liquefaction method, the hydro-thermal liquefaction process has following advantage: (1) raw material need not drying, energy consumption reduces greatly.This point is even more important (little algae water content generally surpasses 80%) to the great little algae of water content; (2) gained bio oil oxygen level and moisture obviously are better than quick cracking process; (3) the wet contained moisture of algae can provide hydrogenation liquefaction required hydrogen, is conducive to the generation of liquefaction reaction and the generation of short hydrocarbon; (4) Asia/supercritical water have macroion long-pending, to organic superpower solvability, the characteristic such as viscosity is low, resistance to mass transfer is little and diffusion is good, the liquefaction oil that hydro-thermal liquefaction produces can dissolve rapidly and spread, and has reduced the generation of condensation or the side reaction such as coking.The hydro-thermal liquefaction process of algae is subject to various countries investigator's extensive concern at present, becomes gradually the mainstream research direction in this field.Yet also there are many weak points in the liquefaction of algae hydro-thermal: (1) oily productive rate is low; (2) quality of bio-oil is undesirable.These shortcomings have seriously restricted the mass-producing of little algae hydro-thermal liquefaction process and have used.Except water as the medium, adopt the stronger solvent of other hydrogen supply capacities can improve liquefaction effect.Part alcohol also can with liquefaction intermediate lipid acid generation esterification, thereby improve bio oil productive rate and calorific value.Alcohols is cheap and easy to get, and wherein part alcohol can be obtained by biomass ferment, also has recyclability.
Mention a kind of method that from little algae, prepares biofuel in the patent of invention 200910148494.7.This patent is extracted microalgae grease and one step of production of biodiesel finishes, and simplifies processing step and equipment, saves cost; Produce used sulfuric acid and low-carbon alcohol recyclable after, the again drying recycling of anhydrating reduces the cost, and the finished product are neutrality and need not washing, alleviates aftertreatment pressure.But this patent has two deficiencies: 1. in little algae except lipid, also have the compositions such as a large amount of protein, polysaccharide not take full advantage of, caused the huge waste of resource.2. this technological process adopts the liquid sulfur acid as catalyst, and catalyzer is not easy to be recycled.If do not carry out aftertreatment, directly discharging then can cause serious environmental pollution.
Mention a kind of method of from Dunaliella salina, extracting carotenoid and liquefaction bio-fuel-oil in the patent of invention 200910238784.0.This patent extracts carotenoid first under the supercritical co condition, the algae-residue that obtains is liquefaction bio-fuel-oil processed under the condition of super/near-critical water.Raw material need not drying, energy consumption is low, and whole process environment is friendly, technique is simple; Plant factor is high.But the described algae-residue liquefaction process of this patent is to carry out under the condition of super/near-critical water, because emergent pressure and the critical temperature relatively high (Tc:374.15 ℃ and Pc:22.12Mpa) of supercritical water, the liquefaction reaction of little algae is higher to equipment requirements in Asia/supercritical water medium, and reaction conditions is relatively harsh; Simultaneously, the liquefaction process of little algae in Asia/supercritical water exists oil yield rate relatively on the low side, causes the shortcomings such as its quality is undesirable in the product bio-fuel-oil because acid number is higher.
Summary of the invention
The purpose of this invention is to provide the method that a kind of little algae direct liquefaction prepares bio-fuel-oil, for the worsening shortages of current fossil resource, and the Application and Development of biomass resource has environmental protection and reproducible characteristics.
To achieve these goals, little algae provided by the invention prepares the method for bio-fuel-oil, take little algae as raw material, (supercritical water refers to that temperature and pressure is higher than the water of stagnation point (374.2 ℃ and 22.1MPa) at Asia/supercritical water, and subcritical water refers to that temperature and pressure does not reach near the water of stagnation point, general temperature should be greater than 200 ℃)-pure condition under the little algae of direct liquefaction prepare bio-fuel-oil, it is characterized in that, the method is carried out as follows:
(1) a certain amount of little algae sample is placed reactor from the aqueous solution of different percentage composition alcohol, heat to certain temperature and react;
(2) after reaction finishes, add organic solvent extracting and extract reaction solution, reaction solution is divided into organic solvent phase, pure water and solid residue;
(3) after extraction finished, suction filtration was isolated solid residue, separated obtaining organic phase behind the liquid phase standing demix;
(4) organic solvent is removed in the organic phase underpressure distillation, obtained oily liquids and be the bio-fuel-oil product.
In the method for the present invention, described little algae is selected from one or more the mixture in Dunaliella salina, chlorella and the blue-green algae.
In the method for the present invention, the solid-liquid ratio of described little algae and Asia/supercritical water-pure blending agent is 1: 5～1: 20 (g/mL).
In the method for the present invention, in described Asia/supercritical water-pure blending agent, the volumn concentration of alcohol is 20%～80%.
In the method for the present invention, described alcohol is selected from and is one or more the mixture in methyl alcohol, ethanol, propyl alcohol, the butanols.
In the method for the present invention, the reaction conditions of the little algae of direct liquefaction is under Asia/supercritical water-pure condition: liquefaction temperature is 260 ℃～360 ℃; Pressure is 7～22MPa; Reaction times is 15～45min.
In the method for the present invention, described organic solvent is selected from and is one or more the mixture in normal hexane, chloroform, the tetrahydrofuran (THF).
In the method for the present invention, distillation condition is under the reduced pressure described in the step (4), and pressure is 0.085～0.095MPa (gauge pressure), and temperature is 20～40 ℃.
In the method for the present invention, the liquefied fraction of the little algae of direct liquefaction is higher than 90% under described Asia/supercritical water-pure condition, and oil yield rate is 40%～70%.
Beneficial effect of the present invention is:
(1) uses little algae to be raw material, can overcome and alleviate the in short supply and problem of environmental pollution of fossil energy, also do not need raw material is carried out drying treatment simultaneously, reduced the energy consumption of process, reduced production cost;
(2) Asia/supercritical water-pure mixed solvent unique properties, the cheap environmental protection of safety.Little algae raw material does not need drying, and energy consumption reduces greatly;
(3) whole technological process is simple, energy consumption is low, easy to operate, have the industrial applications prospect;
(4) rate of the liquefied fraction of little algae and bio-fuel-oil is high, and the bio-fuel-oil water content is little, ash content is low, acid number is low, calorific value is high.
(5) three effects of introducing alcohols in the water medium: Asia/supercritical water solvent is carried out the performance regulation and control, reduce stagnation point; Little algae required hydrogen that liquefies is provided; Carry out esterification with little algae liquefaction intermediate organic acid and improve bio oil productive rate and quality.
Description of drawings
Fig. 1 is the present invention prepares bio-fuel-oil in the little algae of direct liquefaction process flow sheet
Embodiment:
Describe the present invention in detail below in conjunction with Fig. 1.Be that 1: 5～1: 20 (g/mL) takes by weighing the algae sample and water-alcohol mixture joins in the reactor according to solid-liquid ratio at first, the volumn concentration of alcohol is 20%～80% in the water-alcohol mixture medium, after the sealing reactor is transferred in the process furnace, then react under suitable reaction conditions, reaction conditions is: liquefaction temperature is 260 ℃～360 ℃; Pressure is 7～22MPa; Reaction times is 15～45min.After reaction finishes, take out reactor, be cooled to room temperature.Take out reaction product, add organic solvent and extract, the product mixed solution that obtains is divided into three parts: organic phase, pure water and solid residue; Isolate solid residue behind the mixture suction filtration, after the drying, weigh in the solid residue baking oven, calculate liquefied fraction; Filtrate is used the separating funnel standing demix, isolates pure water and organic phase, after wherein pure water is removed alcohol, obtains water soluble ingredient; Organic phase is the Distillation recovery organic solvent under the condition of underpressure distillation, obtains bio oil, weighs, and calculates oil yield rate.
Embodiment 1
Be that 1: 10 (g/mL) takes by weighing the little algae sample of 4g and the 40mL water-alcohol mixture joins in the reactor according to solid-liquid ratio, the volumn concentration of alcohol is 40% in the water-alcohol mixture medium, and liquefaction temperature is 260 ℃; Pressure is 8.45MPa; Reaction times is 30min, and the liquefied fraction of the little algae of gained is 92.84%, and oil yield rate is 47.11%.
Embodiment 2
Be that 1: 10 (g/mL) takes by weighing the little algae sample of 4g and the 40mL water-alcohol mixture joins in the reactor according to solid-liquid ratio, the volumn concentration of alcohol is 40% in the water-alcohol mixture medium, and liquefaction temperature is 340 ℃; Pressure is 14.52MPa; Reaction times is 30min, and the liquefied fraction of the little algae of gained is 99.35%, and oil yield rate is 60.56%.
Embodiment 3
Be that 1: 10 (g/mL) takes by weighing the little algae sample of 4g and the 40mL water-alcohol mixture joins in the reactor according to solid-liquid ratio, the volumn concentration of alcohol is 0% in the water-alcohol mixture medium, and liquefaction temperature is 320 ℃; Pressure is 11.27MPa; Reaction times is 30min, and the liquefied fraction of the little algae of gained is 95.39%, and oil yield rate is 48.93%.
Embodiment 4
Be that 1: 10 (g/mL) takes by weighing the little algae sample of 4g and the 40mL water-alcohol mixture joins in the reactor according to solid-liquid ratio, the volumn concentration of alcohol is 40% in the water-alcohol mixture medium, and liquefaction temperature is 320 ℃; Pressure is 13.80MPa; Reaction times is 33min, and the liquefied fraction of the little algae of gained is 98.24%, and oil yield rate is 64.68%.
Embodiment 5
Be that 1: 10 (g/mL) takes by weighing the little algae sample of 4g and the 40mL water-alcohol mixture joins in the reactor according to solid-liquid ratio, the volumn concentration of alcohol is 100% in the water-alcohol mixture medium, and liquefaction temperature is 320 ℃; Pressure is 11.30MPa; Reaction times is 33min, and the liquefied fraction of the little algae of gained is 91.81%, and oil yield rate is 49.89%.
Claims (4)
1. a little algae direct liquefaction prepares the method for bio-fuel-oil, it is characterized in that:
(1) little algae is mixed with pure water mixed solution place reactor, heating is reacted; Reaction conditions is: temperature is 260～360 ℃; Pressure is 7～22MPa; Reaction times is 15～45min;
Little algae is 1: 5～20 with pure water mixed solution ratio, the g/mL of unit;
In the alcohol water mixed solution, the volumn concentration of alcohol is 20～80%;
(2) after reaction finishes, add organic solvent extracting and extract reaction solution, reaction solution is divided into organic solvent phase, pure water and solid residue;
(3) after extraction finished, suction filtration was isolated solid residue, separated obtaining the organic solvent phase behind the liquid phase standing demix;
(4) organic solvent is removed in the underpressure distillation of organic solvent phase, obtained oily liquids and be the bio-fuel-oil product; The condition of underpressure distillation is: gauge pressure 0.085～0.095Mpa, 20～40 ℃ of temperature.
2. the preparation method of described bio-fuel-oil according to claim 1 is characterized in that: described little algae is selected from one or more the mixture in Dunaliella salina, chlorella and the blue-green algae.
3. the preparation method of described bio-fuel-oil according to claim 1 is characterized in that: described alcohol is selected from one or more the mixture in methyl alcohol, ethanol, propyl alcohol, the butanols.
4. the preparation method of described bio-fuel-oil according to claim 1 is characterized in that: described organic solvent can be one or more the mixture in normal hexane, chloroform, the tetrahydrofuran (THF).
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| CN103589501A (en) * | 2013-11-20 | 2014-02-19 | 江苏理工学院 | Extraction method of microalgae oil and content detecting method for triglyceride in microalgae |
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| CN105018211A (en) * | 2015-07-13 | 2015-11-04 | 上海婉静纺织科技有限公司 | Cyanobacteria extract oil for biological fuel and preparation method of cyanobacteria extract oil |
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| CN105132043A (en) * | 2015-07-15 | 2015-12-09 | 广西南宁高斯特科贸有限公司 | Bio-fuel oil and preparation method thereof |
| CN105176601A (en) * | 2015-07-13 | 2015-12-23 | 上海婉静纺织科技有限公司 | High-calorific value environmental-friendly biodiesel, and preparation method thereof |
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| CN112322384A (en) * | 2020-09-22 | 2021-02-05 | 天津大学 | Multistage reduced pressure distillation separation device and method for photovoltaic biological oil |
| CN112522034A (en) * | 2020-11-09 | 2021-03-19 | 中国林业科学研究院林产化学工业研究所 | Method for preparing biofuel from rhodosporidium toruloides |
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| CN104730161A (en) * | 2013-11-20 | 2015-06-24 | 江苏理工学院 | Detection method for content of triglyceride in microalgae |
| CN103589501A (en) * | 2013-11-20 | 2014-02-19 | 江苏理工学院 | Extraction method of microalgae oil and content detecting method for triglyceride in microalgae |
| CN104730161B (en) * | 2013-11-20 | 2016-10-26 | 江苏理工学院 | The detection method of content of triglyceride in microalgae |
| CN105176601B (en) * | 2015-07-13 | 2018-01-05 | 上海婉静纺织科技有限公司 | High heating value environment-protective biodiesel and preparation method thereof |
| CN105018211A (en) * | 2015-07-13 | 2015-11-04 | 上海婉静纺织科技有限公司 | Cyanobacteria extract oil for biological fuel and preparation method of cyanobacteria extract oil |
| CN105176601A (en) * | 2015-07-13 | 2015-12-23 | 上海婉静纺织科技有限公司 | High-calorific value environmental-friendly biodiesel, and preparation method thereof |
| CN105132043A (en) * | 2015-07-15 | 2015-12-09 | 广西南宁高斯特科贸有限公司 | Bio-fuel oil and preparation method thereof |
| CN105062576A (en) * | 2015-07-20 | 2015-11-18 | 肖宏阳 | Method for extracting liquid fuel from green algae |
| CN106520171A (en) * | 2016-11-02 | 2017-03-22 | 中国林业科学研究院林产化学工业研究所 | Method for liquefaction of bamboo powder in water/n-butyl alcohol solvent system and separation of product thereof |
| CN108315075A (en) * | 2018-02-11 | 2018-07-24 | 北京欧美中科学技术研究院 | A kind of high-capacity environment-protecting type biomass fuel and preparation method thereof |
| CN108315075B (en) * | 2018-02-11 | 2020-04-21 | 北京欧美中科学技术研究院 | High-energy environment-friendly biomass fuel and preparation method thereof |
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