CN101368193A - Process for preparing fine algae cultivation coupling biological diesel oil refining - Google Patents
Process for preparing fine algae cultivation coupling biological diesel oil refining Download PDFInfo
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- CN101368193A CN101368193A CNA2008102011166A CN200810201116A CN101368193A CN 101368193 A CN101368193 A CN 101368193A CN A2008102011166 A CNA2008102011166 A CN A2008102011166A CN 200810201116 A CN200810201116 A CN 200810201116A CN 101368193 A CN101368193 A CN 101368193A
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Classifications
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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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
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- Liquid Carbonaceous Fuels (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Micro-Organisms Or Cultivation Processes Thereof (AREA)
Abstract
The invention relates to the fields of microalgae culturing project, biodiesel refining and environment protection, in particular to a production method for refining the biodiesel through microalgae culturing and coupling. In the method, carbon dioxide industrial waste water and eutrophicated surface water or industrial waste water is used as main material to extensively culture the microalgae containing oil, and microalgae oil is used as the material to refine the biodiesel and simultaneously realize the drainage reducing of carbon dioxide, the control of polluted water and the cleaning production of biodiesel. The method is characterized in that the waste gas of carbon dioxide and the eutrophicated water are firstly used to culture and collect the microalgae; and then extraction, pre-processing and interchange esterification reaction of microalgae is carried out. In the invention, the two processing of culturing the microalgae and refining the biodiesel are coupled together; the ''three wastes'' and waste heat generated during the reefing process of the biodiesel and the unsalable outgrowth of crude glycerine are used as the materials and the heat source for culturing the microalgae; therefore, not only the production cost is reduced, but also the discharge of the ''three wastes'' is eliminated.
Description
[technical field]
The present invention relates to little algae culturing engineering field, biological diesel oil refining field and environmental protection field, is a kind of production method of fine algae cultivation coupling biological diesel oil refining specifically.
[background technology]
Along with the fast development of world economy, fossil fuel can not satisfy the needs of development of world economy.Especially in recent years international oil price is unprecedentedly soaring, and is increasing to the influence of various countries' economy.Diesel oil is as a kind of important refining of petroleum product, and the share in various countries' fuel structure improves year by year.Quickening along with vehicle diesel oil trend in the world wide, the demand of following diesel oil can be more and more big, world energy sources shortage and diesel-fuel price rises steadily in addition, and various countries' environmental regulation is perfect day by day, raw material is easy to get, biofuel material cheap, the high-quality cleaning is shown one's talent, the exploitation upsurge constantly heats up, and technical progress obtains breakthrough repeatly.
Biofuel is a fatty acid methyl ester, it is the renewable energy source of cleaning, it is the liquid fuel that raw material is made with oil plant waterplant and animal grease such as oil-yielding shrubs fruits such as oil crops such as soybean and Semen Brassicae campestris, oil palm, Cortex jatrophae and Chinese pistache, " engineering microalgae ", the food and drink oil that gives up, cottonseed wet goods, is fine petrifaction diesel surrogate.Biofuel is typical " green energy resource ", have good environmental-protecting performance, good safety performance, good combustionproperty, lubricity etc. preferably, and biofuel itself still is a kind of excellent solvent and important chemical material.Therefore, greatly develop biofuel to sustainable economic development, advance energy substitution, alleviate environmental stress, the control urban atmospheric pollution has the important strategic meaning.But because higher raw materials cost makes the price of biofuel be higher than petrifaction diesel, raw material supply has become the most thorny issue with price.The key of development biofuel is the supply of raw oil material, in general, grease character and composition decision work flow and products scheme, the oil plant per mu yield influences the production equipment scale, and oil plant collection, transportation, logistics radius and oil product market clout plant site selection.According to statistics; 70～80% of production of biodiesel cost, raw materials cost; the basic factor that influences the biofuel cost is a raw oil material; all more important than equipment amortization, labour cost, energy consumption, methyl alcohol, catalyzer; therefore; thereby adopt cheap glyceride stock and raising grease transformation efficiency to reduce cost, be biofuel whether can mass-producing, the key of industrialization, choose suitable, oil resource produces the general trend that thing diesel oil is development next life cheaply.
Characteristics such as algae has the photosynthetic efficiency height, adaptive capacity to environment is strong, growth cycle is short, biological yield height, so the oil-containing algae is the good raw material of preparation biofuel.With " engineering microalgae,, the production biofuel is for diesel production has been opened up a new technological approaches." engineering microalgae " that cultivate by modern biotechnology in the renewable laboratory of American National, can make under laboratory condition that lipid content is increased to more than 60% in " engineering microalgae ", outdoor production also can reach more than 40%, can produce biofuel more than 2 tons for every mu.Utilize " engineering microalgae " to produce diesel oil and have important economic implications and ecological significance, its superiority is: little algae throughput height exceeds tens times than terrestrial plant per unit area yield grease; Can utilize marginality soils such as seabeach, saltings, sandy bare land to carry out little algae and cultivate, save cultivated land resource; As micro-algae culture medium, can save agricultural resource with seawater, enriched surface water or trade effluent; The biofuel of producing is sulfur-bearing not, does not discharge toxic gas during burning; Biofuel can be degraded by microorganisms, and is free from environmental pollution.Therefore, development be rich in butyrous little algae or " engineering microalgae,, be a megatrend of production biofuel, in case industrialization is succeeded in developing and realized to high produce oil algae, can reach tens million of tons by the scale of algae refining biofuel.
From present state of the art both domestic and external, realize the industrialization of little algae oil refining, also need solve following technical barrier:
Little algae of 1. seed selection oil yield rate height, fast growth;
2. develop the low cost production device that little algae is cultivated in industrialization;
3. reduce the cultivation of little algae, the cost of gathering;
4. solve the waste water handling problem in the biological diesel oil refining process.
[summary of the invention]
The present invention adopts the oil length height that domestic and international each scientific research institution provides, little algae algae kind of fast growth, the production technique and the equipment of fine algae cultivation coupling biological diesel oil refining are proposed, realize the reduction of discharging of carbonic acid gas, the improvement of polluted-water simultaneously, and the cleaner production of biofuel.
The production method of fine algae cultivation coupling biological diesel oil refining, comprise the algae kind, Erlenmeyer flask, airlift photobioreactor, small-sized gas push type photobioreactor, large-scale gas push type photobioreactor, air flotation tank, the nutrient solution blend tank, high pressure homogenizer, extraction kettle, horizontal spiral centrifuge, water-and-oil separator, multifunctional reaction still, skimmer, methanol distillation column, the methyl alcohol basin, water washing tank, distillation tower, the biofuel basin, oil-firing boiler, methyl alcohol, the vitriol oil, sodium hydroxide, nutrient solution, carbonic acid gas and nitrogen mixture, the carbonic acid gas industrial gaseous waste, filtrated air is characterized in that:
A. utilize CO 2 waste gas, eutrophication water cultivation and gather little algae
At first the algae kind is inoculated in the Erlenmeyer flask that nutrient solution is housed, these Erlenmeyer flasks is put into carries out the cultivation of one-level expanding species in the shaking table, culture temperature is 25 ℃, and incubation time is 3～6 days, makes secondary algae kind; In airlift photobioreactor earlier add nutrient solution thereafter, inoculate above-mentioned secondary algae kind immediately and carry out the cultivation of secondary expanding species, culture temperature is 25 ℃, and feed the gas mixture of carbonic acid gas and nitrogen in the airlift photobioreactor, and gas concentration lwevel is 3～6% in the gas mixture, pressure is decompressed to normal pressure, air flow is 50～150 liters/minute, incubation time is 3～6 days, and little algae enters logarithmic phase, makes three grades of algae kinds; Adding nutrient solution then in small-sized gas push type photobioreactor makes liquid level reach 10 centimetres, the main body of starting the breather generation nutrient solution in the small-sized gas push type photobioreactor flows, inoculate above-mentioned three grades of algae kinds subsequently and carry out three grades of expanding species cultivations, small-sized gas push type photobioreactor places outdoor, feed the stack gas of oil-firing boiler discharging by day continuously, the carbon dioxide content of stack gas air after filtration is diluted to 1～5%, to guarantee the growth of little algae, feed filtrated air at night and keep the breathing of little algae, adopt logical hot/cold wind, hot/cold water temperature adjustment means are controlled at 20～25 ℃ with the temperature of nutrient solution, progressively adding nutrient solution then makes liquid level reach 35 centimetres, continue to cultivate little algae after 4～6 days, little algae enters logarithmic phase, makes the industrial production algae kind as industrial production device; Industrial production device is to place the outdoor large-scale gas push type photobioreactor that is arranged in parallel by row and row, adding nutrient solution earlier in reactor makes liquid level reach 10 centimetres, the main body of starting breather generation nutrient solution then flows, inoculate above-mentioned industrial production algae kind subsequently, and progressively add nutrient solution and make liquid level reach 20 centimetres, feed continuously by day carbon dioxide content after filtration air be diluted to 1～5% carbonic acid gas industrial gaseous waste, to guarantee the growth of little algae, feed filtrated air at night and keep the breathing of little algae, adopt logical hot/cold wind, ventilation puts in a skylight, shading temperature adjustment means are controlled at 15～35 ℃ with the temperature of nutrient solution; After detecting the nutrient minimizing or the decline of algae liquid liquid level in the nutritive medium, carry out fluid infusion by liquid supplementation pipe, the highest liquid level after the fluid infusion is 30 centimetres; Look micro algae culturing liquid concentration little algae of irregularly gathering, promptly open the liquid discharge pipe valve and discharge algae liquid, when the liquid level of large-scale gas push type photobioreactor is reduced to 15～20 centimetres, stop discharge opeing, to control each recovery ratio 10～30%; Gathering of little algae adopts the aerating collecting method that feeds CO 2 waste gas in air flotation tank to carry out, and realizes the carbonic acid gas of complement lysis in micro algae culturing liquid simultaneously;
The extraction of b. little algae oil, pre-treatment and transesterification reaction
Little algae (slurry) that aerating collecting obtains is behind the high pressure homogenizer broken wall, extract little algae oil through extraction kettle with fatty acid methyl ester (biofuel), the extraction ratio is 1～4:1, adopt horizontal spiral centrifuge to carry out liquid-solid separation to the material after the extraction, isolated liquid phase is added to and is separated into oil phase and water in the water-and-oil separator, and oil phase is little algae oil (being dissolved in the biofuel); The equipment of the pre-treatment of little algae oil and refining biofuel thereof adopts multifunctional reaction still, in multifunctional reaction still, add algae oil in a subtle way, carry out vacuum hydro-extraction earlier, add the methyl alcohol and the vitriol oil then and carry out pre-esterification reactor, make the free fatty acids in the stock oil turn to fatty acid methyl ester, after pre-esterification reactor finishes, according to added vitriol oil amount, calculate the amount of the required sodium hydroxide that just in time neutralizes fully, in reactor, add the sodium hydroxide saturated solution for preparing and carry out neutralization reaction, after reaction finishes, under the situation that the multifunctional reaction still kettle is continued thermostatically heating, vacuumize dehydration, separating methanol, methyl alcohol by rectifying and water sepn after reuse; After the pre-treatment of little algae oil finishes, in multifunctional reaction still, add methyl alcohol and alkaline catalysts sodium hydroxide, carry out transesterification reaction, make the glycerin fatty acid ester reaction in the stock oil generate fatty acid methyl ester, after transesterification reaction finishes, under the situation that the multifunctional reaction still kettle is continued thermostatically heating, vacuumize separating methanol, direct reuse after methyl alcohol is condensed; Behind the vacuum separating methanol, from multifunctional reaction still, discharge the mixture of product fatty acid methyl ester and by-product glycerin, then by after standing demix or the centrifugation, crude fatty acid methyl ester is washed and distilled, make the biofuel of national standards such as meeting China or Germany; One of carbon source that in the isolated raw glycerine 10～70% cultivated as little algae is added in the micro algae culturing liquid blend tank, and remaining raw glycerine is further refining; To the sodium hydroxide waste water that produces in the coarse biodiesel water washing process absorption agent, absorb the nutritive salt that sodium bicarbonate that the back produces is cultivated as little algae as carbonic acid gas; Sodium hydroxide waste water is added in the air flotation tank, heightens the pH value of algae liquid, helps flocculation and the air supporting of little algae; Sodium hydroxide waste water is added in the nutrient solution blend tank, regulates the pH value of nutrient solution, makes it to be more suitable for the growth of little algae; The waste salt that in the vitriol oil and the sodium hydroxide and back generates is added in the nutrient solution blend tank, becomes salinity source and nutritive salt that the little algae of salt water is cultivated; Effusive low-temperature water heating is as the thermal source medium of regulating the gas push type photobioreactor culture-liquid temp in the multifunctional reaction still chuck.
Little algae described in the present invention is adopted freshwater microalgae or little algae of salty lake water or the little algae of seawater, and classification is chrysophyceae or green alga or diatom or blue-green algae or red algae, is preferably to contain the high grape algae of fat or chlorella or Isochrysis galbana 3011 or pavlova viridis.
With little algae oil is this chemical process of raw material production biofuel, must be accompanied by the generation of waste water, waste residue, waste gas, used heat.These " three wastes " can only be as waste discharge in the process of independent little algae oil refining biofuel, but, after little algae cultivation and biological diesel oil refining two PROCESS COUPLING, both reduce the material consumption and the energy consumption of little algae culturing process, eliminated " three wastes " discharging in the biological diesel oil refining process again.
In addition, extract grease in little algae with the coarse biodiesel produced of the little algae oil of refining, the pollution of having avoided petrochemical industry solvent extraction microalgae greases such as common employing sherwood oil, normal hexane and having produced to biofuel product and environment, and gasification is reclaimed the required a large amount of energy consumptions of solvent, the purchase cost of also having saved extraction agent simultaneously.One of carbon source that the by product raw glycerine of refining little algae oil is cultivated as little algae is added in the micro algae culturing liquid blend tank, has so both reduced the cost of nutrient solution, has solved the problem of outlet (present glycerine market saturation, sales difficulty) of partial glycerol again.And with the fuel of coarse biodiesel, both reduced the purchase cost of oil fuel as oil-firing boiler, and also guaranteed to enter the purity of the CO 2 waste gas of small-sized gas push type photobioreactor, avoided in the conventional stack gas element such as sulphur to the infringement of algae kind.In addition, little algae is cultivated and biological diesel oil refining coupled production method, has also saved the transportation cost of stock oil production unit to biological diesel oil refining enterprise.
[description of drawings]
Fig. 1 is the production scheme of fine algae cultivation coupling biological diesel oil refining.
[embodiment]
The invention will be further described below in conjunction with embodiment that accompanying drawing and accompanying drawing provide.Manufacturing technology of the present invention is to implement easily to this professional people.
Referring to Fig. 1, the key equipment of fine algae cultivation coupling biological diesel oil refining adopt the applicant applied for patent of invention gas push type photobioreactor (gas push type photobioreactor. Chinese invention patent, application number: 200810039168.8; A kind of little algae industrialization production equipment and produce the method for little algae. Chinese invention patent, application number: 200810038075.3), biological diesel oil refining equipment (multifunctional reaction still of production biofuel and working method thereof. Chinese invention patent, application number: 200810039167.3), wherein, the making method of small-sized gas push type photobioreactor be applicant first to file " gas push type photobioreactor. Chinese invention patent; application number: 200810039168.8 ", the making method of large-scale gas push type photobioreactor be applicant first to file " a kind of little algae industrialization production equipment and produce the method for little algae. Chinese invention patent; application number: 200810038075.3 ", the making method of multifunctional reaction still be applicant first to file " multifunctional reaction still of production biofuel and working method thereof. Chinese invention patent, application number: 200810039167.3 ".
At first taking out pavlova viridis algae kind from algae kind storehouse, to be inoculated into 10 capacity that nutrient solution is housed be in 1000 milliliters the Erlenmeyer flask, these Erlenmeyer flasks are put into carry out the one-level expanding species in the good shaking table of illumination condition and cultivate, culture temperature is 25 ℃, incubation time is 5 days, therefrom select 6 bottles of little algaes that upgrowth situation is good then, as the algae kind of secondary cultivation.The secondary culture apparatus is an airlift photobioreactor, and the diameter of this reactor urceolus is 30 centimetres, highly is 100 centimetres; The diameter of inner core is 20 centimetres, highly is 50 centimetres; The periphery of reactor is thrown light on 8 40 watts perpendicular Liege light modulation.In airlift photobioreactor, add 45 liters of nutrient solutions earlier, inoculate above-mentioned 6 bottles of secondary algae kinds then and carry out the cultivation of secondary expanding species.Reactor places illumination condition preferably in the air-conditioned room, and culture temperature is 25 ℃, and the gas that is led to is for from the carbonic acid gas of steel cylinder and the gas mixture of nitrogen, and gas concentration lwevel is 5% in the gas mixture, and pressure is decompressed to normal pressure, and air flow is 100 liters/minute.Incubation time is 4 days, and little algae enters logarithmic phase, can be used as the algae kind of three grades of cultivations this moment.Three grades of culture apparatuses are that width is that 1 meter, length are that 6 meters, the degree of depth are 45 centimetres small-sized gas push type photobioreactor, adding nutrient solution earlier in small-sized gas push type photobioreactor makes liquid level reach 10 centimetres, start the main body that breather produces nutrient solution then and flow, inoculate whole three grades of algae kinds that above-mentioned airlift photobioreactor cultivates subsequently and carry out three grades of expanding species and cultivate.Small-sized gas push type photobioreactor places outdoor, feeds the stack gas of oil-firing boiler discharging by day continuously, and carbon dioxide content air after filtration is diluted to 4%, to guarantee the growth of little algae, suitably feeds the breathing that filtrated air is kept little algae at night.Adopt temperature adjustment means such as logical hot/cold wind, hot/cold water, make the temperature of nutrient solution remain on 20～25 ℃ of suitable micro algae growth.Cultivate after 1 day, add nutrient solution again and make liquid level reach 20 centimetres, cultivate 1 day again after, add nutrient solution again and make liquid level reach 35 centimetres, continue to cultivate 2 days, little algae enters logarithmic phase, this moment is as the industrial production algae kind of industrial production device.Above-mentioned to pavlova viridis algae kind step by step in the expanding species culturing process prescription of used nutrient solution all adopt the f/2 prescription.
Industrial production device is to place the outdoor large-scale gas push type photobioreactor that is arranged in parallel by row and row; The width of each reactor is 3 meters, and length is 60 meters, and the degree of depth is 40 centimetres; The water surface total area that little algae is cultivated is 300 mu.Adding nutrient solution during production earlier in large-scale gas push type photobioreactor makes liquid level reach 10 centimetres, the main body of starting breather generation nutrient solution then flows, inoculate whole industrial production algae kinds that above-mentioned small-sized gas push type photobioreactor is cultivated subsequently, progressively add nutrient solution then and make liquid level reach 20 centimetres.Feed the power plant flue gas that is rich in carbonic acid gas by day continuously, carbon dioxide content air after filtration is diluted to 3%, to guarantee the growth of little algae, suitably feeds the breathing that filtrated air is kept little algae at night.With logical hot/cold wind, the ventilation that puts in a skylight, shading temperature adjustment means, make the temperature of nutrient solution remain on 15～35 ℃ of suitable micro algae growth.Behind minimizing of the nutrient in the nutritive medium or moisture evaporation, carry out fluid infusion by liquid supplementation pipe, the highest liquid level after the fluid infusion is 30 centimetres.Look micro algae culturing liquid concentration little algae of irregularly gathering, promptly open the liquid discharge pipe valve and discharge algae liquid, when reducing to 15～20 centimetres, the reactor liquid level stops discharge opeing, to control each recovery ratio 10～30%, at little frond long-pending little, with the more approaching characteristic of density of water, employing feeds the aerating collecting method of CO 2 waste gas and carries out gathering of little algae in air flotation tank, realize the carbonic acid gas of complement lysis in micro algae culturing liquid simultaneously.The sewage after sterilization that the nutrient solution that is added in the large-scale gas push type photobioreactor is discharged by seawater shrimps plant, water quality is IV class water, concentration by 3 gram/cubic meters is added ironic citrate, concentration by 0.1 gram/cubic meter is added VITMAIN B1, sneak into the waste water and the 50% raw glycerine by product that produce in the process of rare algae liquid that air flotation tank comes out, little algae oil refining biofuel again, in the nutrient solution blend tank, mix and form.
Little algae (slurry) that aerating collecting obtains is behind the high pressure homogenizer broken wall, and with the little algae oil of crude fatty acid methyl ester (biofuel) extraction, the extraction ratio is 2:1.Adopt horizontal spiral centrifuge to carry out liquid-solid separation to the material after the extraction, isolated liquid phase is added to and is separated into oil phase and water in the water-and-oil separator, and oil phase is little algae oil (being dissolved in the biofuel).Here be the base-catalyzed transesterification method with little algae oil production method of bio-diesel oil,, must remove in advance because little algae oil contains moisture content and free fatty acids.
10m with 3 parallel connections
3Multifunctional reaction still production biofuel, handle 4 batches of little algae oil every day, every batch adds 20 tons of little algae oil.The pre-treatment of little algae oil is to carry out vacuum hydro-extraction earlier, adds the methyl alcohol and the vitriol oil then and carries out pre-esterification reactor, makes the free fatty acids in the stock oil turn to fatty acid methyl ester.After pre-esterification reactor finishes,, calculate the amount of the required sodium hydroxide that just in time neutralizes fully, in reactor, add the sodium hydroxide saturated solution for preparing and carry out neutralization reaction according to added vitriol oil amount.After reaction finishes, under the situation that kettle is continued thermostatically heating, vacuumize dehydration, separating methanol, methyl alcohol by rectifying and water sepn after reuse.After the pre-treatment of little algae oil finishes, in reactor, add methyl alcohol and alkaline catalysts sodium hydroxide, carry out transesterification reaction, make the glycerin fatty acid ester reaction in the stock oil generate fatty acid methyl ester.After transesterification reaction finishes, under the situation that kettle is continued thermostatically heating, vacuumize separating methanol, direct reuse after methyl alcohol is condensed.Behind the vacuum separating methanol, discharge the mixture of product fatty acid methyl ester and by-product glycerin from reactor, mixture enters in the skimmer settlement separate.Because glycerine, methyl esters proportion differ bigger, two-layer about being divided into very soon in skimmer, glycerine is than the great lower floor that occupies, and methyl esters occupies the upper strata.Raw glycerine after the separation is emitted by the bottom, and wherein one of 50% carbon source of cultivating as little algae is added in the micro algae culturing liquid blend tank, and remaining raw glycerine is delivered to the glycerine workshop and handled.The coarse biodiesel on skimmer top obtains the purified biofuel again after the distillation tower distillation after the water washing tank washing.
In above-mentioned production process, the waste water that produces in the biological diesel oil refining, waste residue, waste gas, used heat all are used as raw material and the thermal source that little algae is cultivated, one of carbon source that the by product raw glycerine is cultivated as little algae, add in the micro algae culturing liquid blend tank, realized that little algae is cultivated and the coupling of biological diesel oil refining, seen Fig. 1 for details.
The density (20 ℃) of little algae biofuel that the present invention produces is 0.868kg/m
3, kinematic viscosity (40 ℃) is 3.8mm
2/ s, water-content (massfraction) are 0.02%, acid number is 0.58mgKOH/g, and calorific value is up to 42MJ/kg, meet China's " diesel-fuel blending with biofuel (BD100) " national standard.
Claims (2)
1. the production method of fine algae cultivation coupling biological diesel oil refining, comprise the algae kind, Erlenmeyer flask, airlift photobioreactor, small-sized gas push type photobioreactor, large-scale gas push type photobioreactor, air flotation tank, the nutrient solution blend tank, high pressure homogenizer, extraction kettle, horizontal spiral centrifuge, water-and-oil separator, multifunctional reaction still, skimmer, methanol distillation column, the methyl alcohol basin, water washing tank, distillation tower, the biofuel basin, oil-firing boiler, methyl alcohol, the vitriol oil, sodium hydroxide, nutrient solution, carbonic acid gas and nitrogen mixture, the carbonic acid gas industrial gaseous waste, filtrated air is characterized in that:
A. utilize CO 2 waste gas, eutrophication water cultivation and gather little algae
At first the algae kind is inoculated in the Erlenmeyer flask that nutrient solution is housed, these Erlenmeyer flasks is put into carries out the cultivation of one-level expanding species in the shaking table, culture temperature is 25 ℃, and incubation time is 3～6 days, makes secondary algae kind; In airlift photobioreactor earlier add nutrient solution thereafter, inoculate above-mentioned secondary algae kind immediately and carry out the cultivation of secondary expanding species, culture temperature is 25 ℃, and feed the gas mixture of carbonic acid gas and nitrogen in the airlift photobioreactor, and gas concentration lwevel is 3～6% in the gas mixture, pressure is decompressed to normal pressure, air flow is 50～150 liters/minute, incubation time is 3～6 days, and little algae enters logarithmic phase, makes three grades of algae kinds; Adding nutrient solution then in small-sized gas push type photobioreactor makes liquid level reach 10 centimetres, the main body of starting the breather generation nutrient solution in the small-sized gas push type photobioreactor flows, inoculate above-mentioned three grades of algae kinds subsequently and carry out three grades of expanding species cultivations, small-sized gas push type photobioreactor places outdoor, feed the stack gas of oil-firing boiler discharging by day continuously, the carbon dioxide content of stack gas air after filtration is diluted to 1～5%, to guarantee the growth of little algae, feed filtrated air at night and keep the breathing of little algae, adopt logical hot/cold wind, hot/cold water temperature adjustment means are controlled at 20～25 ℃ with the temperature of nutrient solution, progressively adding nutrient solution then makes liquid level reach 35 centimetres, continue to cultivate little algae after 4～6 days, little algae enters logarithmic phase, makes the industrial production algae kind as industrial production device; Industrial production device is to place the outdoor large-scale gas push type photobioreactor that is arranged in parallel by row and row, adding nutrient solution earlier in reactor makes liquid level reach 10 centimetres, the main body of starting breather generation nutrient solution then flows, inoculate above-mentioned industrial production algae kind subsequently, and progressively add nutrient solution and make liquid level reach 20 centimetres, feed continuously by day carbon dioxide content after filtration air be diluted to 1～5% carbonic acid gas industrial gaseous waste, to guarantee the growth of little algae, feed filtrated air at night and keep the breathing of little algae, adopt logical hot/cold wind, ventilation puts in a skylight, shading temperature adjustment means are controlled at 15～35 ℃ with the temperature of nutrient solution; After detecting the nutrient minimizing or the decline of algae liquid liquid level in the nutritive medium, carry out fluid infusion by liquid supplementation pipe, the highest liquid level after the fluid infusion is 30 centimetres; Look micro algae culturing liquid concentration little algae of irregularly gathering, promptly open the liquid discharge pipe valve and discharge algae liquid, when the liquid level of large-scale gas push type photobioreactor is reduced to 15～20 centimetres, stop discharge opeing, to control each recovery ratio 10～30%; Gathering of little algae adopts the aerating collecting method that feeds CO 2 waste gas in air flotation tank to carry out, and realizes the carbonic acid gas of complement lysis in micro algae culturing liquid simultaneously;
The extraction of b. little algae oil, pre-treatment and transesterification reaction
Little algae that aerating collecting obtains is behind the high pressure homogenizer broken wall, extract little algae oil through extraction kettle with fatty acid methyl ester, the extraction ratio is 1～4:1, adopt horizontal spiral centrifuge to carry out liquid-solid separation to the material after the extraction, isolated liquid phase is added to and is separated into oil phase and water in the water-and-oil separator, and oil phase is little algae oil; The equipment of the pre-treatment of little algae oil and refining biofuel thereof adopts multifunctional reaction still, in multifunctional reaction still, add algae oil in a subtle way, carry out vacuum hydro-extraction earlier, add the methyl alcohol and the vitriol oil then and carry out pre-esterification reactor, make the free fatty acids in the stock oil turn to fatty acid methyl ester, after pre-esterification reactor finishes, according to added vitriol oil amount, calculate the amount of the required sodium hydroxide that just in time neutralizes fully, in reactor, add the sodium hydroxide saturated solution for preparing and carry out neutralization reaction, after reaction finishes, under the situation that the multifunctional reaction still kettle is continued thermostatically heating, vacuumize dehydration, separating methanol, methyl alcohol by rectifying and water sepn after reuse; After the pre-treatment of little algae oil finishes, in multifunctional reaction still, add methyl alcohol and alkaline catalysts sodium hydroxide, carry out transesterification reaction, make the glycerin fatty acid ester reaction in the stock oil generate fatty acid methyl ester, after transesterification reaction finishes, under the situation that the multifunctional reaction still kettle is continued thermostatically heating, vacuumize separating methanol, direct reuse after methyl alcohol is condensed; Behind the vacuum separating methanol, from multifunctional reaction still, discharge the mixture of product fatty acid methyl ester and by-product glycerin, then by after standing demix or the centrifugation, crude fatty acid methyl ester is washed and distilled, make the biofuel that meets China or DIN; One of carbon source that in the isolated raw glycerine 10～70% cultivated as little algae is added in the micro algae culturing liquid blend tank, and remaining raw glycerine is further refining; To the sodium hydroxide waste water that produces in the coarse biodiesel water washing process absorption agent, absorb the nutritive salt that sodium bicarbonate that the back produces is cultivated as little algae as carbonic acid gas; Sodium hydroxide waste water is added in the air flotation tank, heightens the pH value of algae liquid; Sodium hydroxide waste water is added in the nutrient solution blend tank, regulates the pH value of nutrient solution; The waste salt that in the vitriol oil and the sodium hydroxide and back generates is added in the nutrient solution blend tank, becomes salinity source and nutritive salt that the little algae of salt water is cultivated; Effusive low-temperature water heating is as the thermal source medium of regulating the gas push type photobioreactor culture-liquid temp in the multifunctional reaction still chuck.
2. the production method of a kind of fine algae cultivation coupling biological diesel oil refining according to claim 1, it is characterized in that described little algae employing freshwater microalgae or little algae of salty lake water or the little algae of seawater, classification is chrysophyceae or green alga or diatom or blue-green algae or red algae, is preferably to contain the high grape algae of fat or chlorella or Isochrysis galbana 3011 or pavlova viridis.
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