CN106190536A - A kind of preparation method of microalgae biodiesel - Google Patents

A kind of preparation method of microalgae biodiesel Download PDF

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Publication number
CN106190536A
CN106190536A CN201610766858.8A CN201610766858A CN106190536A CN 106190536 A CN106190536 A CN 106190536A CN 201610766858 A CN201610766858 A CN 201610766858A CN 106190536 A CN106190536 A CN 106190536A
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biodiesel
algae
intestinal
single intestinal
microalgae
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CN201610766858.8A
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黄健峻
其他发明人请求不公开姓名
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Nanning Overseas Chinese Investment Zone Sun Trading Co Ltd
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Nanning Overseas Chinese Investment Zone Sun Trading Co Ltd
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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
    • C11B1/02—Pretreatment
    • C11B1/04—Pretreatment of vegetable raw material
    • 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
    • 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
    • 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
    • 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

Abstract

The invention discloses the preparation method of a kind of microalgae biodiesel, comprise the following steps: list intestinal algae is seeded to culture medium, irradiate 10 15h/ days with red blue dual-colored LED light compensating lamp, cultivate 10 11 days at 25 28 DEG C, single intestinal frustule can be collected；The single intestinal frustule ultrasound wave collected carries out broken wall treatment, again with organic solvent extraction, obtain microalgae grease, again microalgae grease, methanol and zeolite molecular sieve catalyst are added in reactor according to the ratio that mass ratio is 1:4 6:0.01 0.03 and carry out esterification, obtain esterification products, esterification products through separating, purifying, i.e. can get biodiesel again.The inventive method, with single intestinal algae with short production cycle, widely distributed, that photosynthesis is strong, fat content is high as raw material, solves the problem that the Vegetable oil lipoprotein raw material in biodiesel exploitation exists.The most also have that preparation technology is simple, catalytic efficiency is high, grease extraction efficiency is high, product yield advantages of higher, lay a good foundation for biodiesel industrialization, scale.

Description

A kind of preparation method of microalgae biodiesel
Technical field
The invention belongs to biomass energy technology field, the preparation method of a kind of microalgae biodiesel.
Background technology
Along with the exhaustion day by day of fossil fuel, oil price persistently sharp rises, and seeking regenerative resource has become solution Human survival and the needs of holding World Economics sustainable development, the biodiesel as novel alternative energy source is sent out in countries in the world Exhibition is rapidly.Biodiesel refers to oil crop such as Semen sojae atricolor, Brassica campestris L, cotton, Petiolus Trachycarpi etc., the water such as Wild oil plant and engineering microalgae Raw vegetable oil fat and animal oil, food garbage oil etc. for raw oil by replacing that ester exchange or thermochemical processes are made The reproducibility diesel fuel of petrifaction diesel.The advantage of biodiesel is not limited only to recyclability, compared with existing diesel oil, also has Following advantage: Cetane number is high so that combustibility is more preferable；Preferably wettability, makes injection pump, engine cylinder-body and connecting rod Abrasion reduce, increase the service life；In biodiesel, sulfur content is low, and the discharge of sulfur dioxide and sulfide is low, reduces environment Pollute；Biodiesel flash-point is high, is not belonging to dangerous materials, all has superiority in transport, storage, use etc..
At present, China's industrialized production biodiesel is mainly with Oleum Brassicae campestris, Oleum Gossypii semen, Chinese tallow, shinyleaf yellowhorn oil, Oleum Camelliae It is raw material with waste oil etc..But the limits throughput of these raw materials, the biodiesel of production can only meet current vehicle demand for fuel The 0.3% of amount.And a large amount of Vegetable oil lipoprotein produces biodiesel, anxiety and the crops price of land resource will certainly be caused Rise, especially in the case of China has a large population and a few land, these are particularly problematic.In this case, microalgae biodiesel The concern of more and more people has been attracted with the advantage of its uniqueness.Microalgae, as a kind of important biodiesel raw material, is planted with oil plant Thing is compared, and has that distribution is wide, Biomass high, photosynthetic efficiency is high, adaptive capacity to environment is strong, growth cycle is short, fat content is high, becomes The significant advantages such as this lowest and environmental friendliness.
In recent years, research prepared by relevant biodiesel is concentrated mainly on the aspect such as woody oleiferous plants and disposed waste oil, from Microalgae extracts oils and fats little for the research report preparing biodiesel.Wherein, biodiesel one is prepared with microalgae for raw material As comprise the following steps that: Strain selection, pilot scale culture, extraction oils and fats, esterification prepare biodiesel coarse product, warp Cross refine and i.e. can get biodiesel.The microalgae kind selecting fat content high is to prepare the key of biodiesel, cultivates simultaneously Base and envirment factor also have important impact to the fat content of microalgae.Therefore, how to improve the nutritional labeling of culture medium and change The changing environment factor is one of approach improving algae oils and fats productivity.Although improving microalgae fat content can be that biodiesel is laid well Basis, but the production technology of biodiesel is most important to its yield effect.The production technology of existing biodiesel is general There is problems in that catalytic efficiency is low, yield of biodiesel is low, response time length, etching apparatus, complex process, energy consumption are relatively big, Relatively costly deficiency such as grade.
Single intestinal algae (Monallanthus salina), owing to speed of production is fast, fat content is up to 25-30%, and oils and fats becomes C is mainly contained in Fen18、C16The fatty glyceride of carbochain, close with the biodiesel fuel component extracted from vegetable oil, it is one Class has the bioenergy material of potentiality to be exploited.
Summary of the invention
The present invention is directed to Vegetable oil lipoprotein limits throughput and the problem of existing biodiesel oil preparing process existence, it is provided that Yi Zhongwei The preparation method of algae biodiesel.The inventive method has that raw material sources are extensive, catalytic efficiency is high, it is low to consume energy, biodiesel is produced The advantages such as rate is high, preparation technology is simple, lay a good foundation for biodiesel industrialization, scale, can effectively alleviate energy Source crises problem.
In order to realize object above, the present invention is to be achieved through the following technical solutions:
The preparation method of a kind of microalgae biodiesel, comprises the following steps:
S1. single intestinal algae is cultivated: with single intestinal algae as raw material, then be seeded to training with the inoculum density of ten thousand cell/mL of 500-700 Support base, irradiate 12-16h/ days with red blue dual-colored LED light compensating lamp, control intensity of illumination and control in 2500-3500LX, cultivation temperature At 25-28 DEG C, cultivating 10-11 days, the density of single intestinal algae reaches concentration and reaches 80,000,000 cell/mL, collects single intestinal frustule； Described culture medium is composed of the following components: glucose 20-30mg/L, NaNO3 1.8-2.4mg/L、KH2PO41.5-2.0mg/ L, chitosan 0.5-0.7mg/L, biogas slurry 5-8mg/L, f2 vitamin 3-4mL and sea water 1L；
S2. oils and fats extracts: after step S1 is collected single intestinal frustule concentrate drying, uses ultrasound wave to break single intestinal algae Wall processes, and obtains single intestinal algae powder, and adding in single intestinal algae powder with its mass ratio is the petroleum ether of 1:5-7, and mixing stands 2-5h, upper strata Liquid is oils and fats extracting solution, then by extracting solution 80-85 DEG C of distillation, i.e. can get microalgae grease；
S3. ester exchange reaction: be 1:3-5 according to mass ratio by microalgae grease, methanol and zeolite molecular sieve catalyst: The ratio of 0.02-0.04 adds in reactor, at temperature is 50-55 DEG C, carries out esterification 75-80min, obtains esterification and produces Thing；
S4. standing separation；By esterification products centrifugal 15-20min, stratification under rotating speed is 300-400r/min, divide Separating out upper strata glycerol, lower floor is biodiesel crude product；
S5. distilation: biodiesel crude product is added to distillation column, is distilled off unnecessary methanol at 80-85 DEG C, Obtain biodiesel.
Further, the compound method of the f2 vitamin described in above step S1 is as follows: 0.5mg vitamin B12、0.5mg Biotin, 100mL vitamin B1 and pure water 1000mL.
Further, the HONGGUANG in above-described red blue dual-colored LED light compensating lamp is 1-3:1 with blue light proportioning, preferably joins Ratio is 2:1.
Further, using ultrasound wave that single intestinal algae is carried out broken wall treatment described in above step S2, ultrasonic power is 200- 250W, ultrasonic time are 45-55min.
Compared with prior art, the beneficial effect that the present invention obtains:
1, the present invention prepares biodiesel with single intestinal algae for raw material, can effectively alleviate current energy crisis and environmental pollution Problem, single intestinal algae has that distribution is wide, Biomass is high, photosynthetic efficiency is high, adaptive capacity to environment is strong, growth cycle is short, fat content The significant advantages such as height, low cost and environmental friendliness, it is possible to solve the Vegetable oil lipoprotein insufficient raw material in biodiesel exploitation, cost mistake The problems such as height.
2, the present invention adds in the medium chitosan and biogas slurry, containing nutrition such as substantial amounts of trace element, Organic substances Composition, can accelerate microalgae speed of production and improve the oils and fats productivity of microalgae.
3, the inventive method is by using red blue dual-colored LED light compensating lamp to change illumination condition, is possible not only to improve single intestinal algae Photosynthesis, accelerate single intestinal algae and produce and improve yield, the oils and fats productivity of single intestinal algae can also be improved simultaneously, white with conventional Vehement lamp, fluorescent lamp or monochromatic LED lamp are compared, and the oils and fats productivity of single intestinal algae improves about 5%.
4, the inventive method uses supersonic wave wall breaking method, and ultrasound wave can produce unique mechanical vibration to microalgae cell Effect and cavitation, advantages such as having that sporoderm-broken rate is high, process the time period, environmentally safe, power consumption are low, improve oils and fats Extraction ratio.
5, the inventive method uses zeolite molecular sieve as catalyst, possesses that reaction interface is big, surface area big, resistance to mass tranfer Little, reaction condition is gentle, active height, pollution-free, the not feature such as etching apparatus, improve catalytic efficiency, shorten esterification Time, catalytic effect is notable, improves the yield of biodiesel.
6, the inventive method have that preparation technology is simple, catalytic efficiency is high, grease extraction efficiency is high, biodiesel production rate is high, Product purity is high, raw material sources extensively, the advantage such as low cost, power consumption be low, there is good society, ecology and economic benefit, for Microalgae biodiesel industrialization, scale are laid a good foundation.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further described, but is not limited to protection scope of the present invention.
Embodiment 1
The preparation of single intestinal algae culture medium: glucose 20mg/L, NaNO3 2.4mg/L、KH2PO41.5mg/L, chitosan 0.5mg/L, biogas slurry 5mg/L, f2 vitamin 3mL and sea water 1L；
The preparation method of a kind of microalgae biodiesel, comprises the following steps:
S1. single intestinal algae is cultivated: with single intestinal algae as raw material, then is seeded to cultivate with the inoculum density of 7,000,000 cell/mL Base, irradiates 12h/ days with red blue dual-colored LED light compensating lamp, and in LED light supplement lamp, HONGGUANG and blue light proportioning are 1:1, control intensity of illumination At 3500LX, cultivation temperature controls at 25 DEG C, cultivates 11 days, and the density of single intestinal algae reaches concentration and reaches 80,000,000 cell/mL, Collect single intestinal frustule；
S2. oils and fats extracts: after step S1 is collected single intestinal frustule concentrate drying, uses ultrasound wave to break single intestinal algae Wall processes, and control ultrasonic power is 200W, ultrasonic reaction 48min, obtains single intestinal algae powder, adds and its mass ratio in single intestinal algae powder For the petroleum ether of 1:5, mixing stands 2h, and upper liquid is oils and fats extracting solution, then by extracting solution 80 DEG C of distillations, i.e. can get micro- Algae oils and fats；
S3. ester exchange reaction: be 1:3:0.04's according to mass ratio by microalgae grease, methanol and zeolite molecular sieve catalyst Ratio adds in reactor, at temperature is 50 DEG C, carries out esterification 75min, obtains esterification products；
S4. standing separation；By esterification products centrifugal 20min, stratification under rotating speed is 300r/min, isolate upper strata Glycerol, lower floor is biodiesel crude product；
S5. distilation: biodiesel crude product is added to distillation column, is distilled off unnecessary methanol at 80 DEG C, To biodiesel.
Embodiment 2
The preparation of single intestinal algae culture medium: glucose 25mg/L, NaNO3 2.0mg/L、KH2PO41.7mg/L, chitosan 0.6mg/L, biogas slurry 7mg/L, f2 vitamin 4mL and sea water 1L；
The preparation method of a kind of microalgae biodiesel, comprises the following steps:
S1. single intestinal algae is cultivated: with single intestinal algae as raw material, then is seeded to cultivate with the inoculum density of 5,000,000 cell/mL Base, irradiates 14h/ days with red blue dual-colored LED light compensating lamp, and in LED light supplement lamp, HONGGUANG and blue light proportioning are 2:1, control intensity of illumination At 3000LX, cultivation temperature controls at 26 DEG C, cultivates 10 days, and the density of single intestinal algae reaches concentration and reaches 80,000,000 cell/mL, Collect single intestinal frustule；
S2. oils and fats extracts: after step S1 is collected single intestinal frustule concentrate drying, uses ultrasound wave to break single intestinal algae Wall processes, and control ultrasonic power is 220W, ultrasonic reaction 50min, obtains single intestinal algae powder, adds and its mass ratio in single intestinal algae powder For the petroleum ether of 1:6, mixing stands 3h, and upper liquid is oils and fats extracting solution, then by extracting solution 85 DEG C of distillations, i.e. can get micro- Algae oils and fats；
S3. ester exchange reaction: be 1:4:0.03's according to mass ratio by microalgae grease, methanol and zeolite molecular sieve catalyst Ratio adds in reactor, at temperature is 52 DEG C, carries out esterification 78min, obtains esterification products；
S4. standing separation；By esterification products centrifugal 18min, stratification under rotating speed is 350r/min, isolate upper strata Glycerol, lower floor is biodiesel crude product；
S5. distilation: biodiesel crude product is added to distillation column, is distilled off unnecessary methanol at 82 DEG C, To biodiesel.
Embodiment 3
The preparation of single intestinal algae culture medium: glucose 30mg/L, NaNO31.8mg/L、KH2PO42.0mg/L, chitosan 0.7mg/L, biogas slurry 8mg/L, f2 vitamin 3mL and sea water 1L；
The preparation method of a kind of microalgae biodiesel, comprises the following steps:
S1. single intestinal algae is cultivated: with single intestinal algae as raw material, then is seeded to cultivate with the inoculum density of 6,000,000 cell/mL Base, irradiates 16h/ days with red blue dual-colored LED light compensating lamp, and in LED light supplement lamp, HONGGUANG and blue light proportioning are 3:1, control intensity of illumination At 2500LX, cultivation temperature controls at 28 DEG C, cultivates 11 days, and the density of single intestinal algae reaches concentration and reaches 80,000,000 cell/mL, Collect single intestinal frustule；
S2. oils and fats extracts: after step S1 is collected single intestinal frustule concentrate drying, uses ultrasound wave to break single intestinal algae Wall processes, and control ultrasonic power is 250W, ultrasonic reaction 55min, obtains single intestinal algae powder, adds and its mass ratio in single intestinal algae powder For the petroleum ether of 1:7, mixing stands 5h, and upper liquid is oils and fats extracting solution, then by extracting solution 82 DEG C of distillations, i.e. can get micro- Algae oils and fats；
S3. ester exchange reaction: be 1:5:0.02's according to mass ratio by microalgae grease, methanol and zeolite molecular sieve catalyst Ratio adds in reactor, at temperature is 55 DEG C, carries out esterification 80min, obtains esterification products；
S4. standing separation；By esterification products centrifugal 15min, stratification under rotating speed is 400r/min, isolate upper strata Glycerol, lower floor is biodiesel crude product；
S5. distilation: biodiesel crude product is added to distillation column, is distilled off unnecessary methanol at 85 DEG C, To biodiesel.
The single intestinal algae utilizing oils and fats extraction weight method to collect above example carries out fat content mensuration, result such as table Shown in 1.Wherein oils and fats total content=(microalgae grease/mono-intestinal algae powder) × 100%.
The single intestinal algae fat content of table 1.
Oils and fats total content (%)
Embodiment 1 33
Embodiment 2 34
Embodiment 3 36
Biodiesel prepared by above example is according to GB/T20828-2007 (diesel fuel blending biodiesel) The performance of standard detection product, testing result is as shown in table 2.
The properties of product of the biodiesel of table 2. the present embodiment
Density (g/cm3) Viscosity (40 DEG C of mm2/s) Acid number (mgKOH/g) Flash-point (DEG C) Cetane number
Embodiment 1 0.83 3.98 0.57 148 56
Embodiment 2 0.86 4.82 0.62 152 53
Embodiment 3 0.82 4.17 0.60 154 54
Standard value 0.82-0.9 1.9-6.0 ≤0.8 ≥130℃ ＞ 49
As can be seen from the above table, the indices of biodiesel prepared by the present invention is above diesel fuel blending life The standard of thing diesel oil, good market prospects.
Above content is to combine concrete/the most made for the present invention further description, it is impossible to Assert the present invention be embodied as be confined to these explanations.General technical staff of the technical field of the invention is come Saying, without departing from the inventive concept of the premise, these embodiments having described that can also be made some replacements or modification by it, And these substitute or variant all should be considered as belonging to protection scope of the present invention.

Claims (3)

1. the preparation method of a microalgae biodiesel, it is characterised in that comprise the following steps:
S1. single intestinal algae is cultivated: with single intestinal algae as raw material, then is seeded to cultivate with the inoculum density of ten thousand cell/mL of 500-700 Base, irradiates 12-16h/ days with red blue dual-colored LED light compensating lamp, controls intensity of illumination and control in 2500-3500LX, cultivation temperature 25-28 DEG C, cultivating 10-11 days, the density of single intestinal algae reaches concentration and reaches 80,000,000 cell/mL, collects single intestinal frustule；Institute The culture medium stated is composed of the following components: glucose 20-30mg/L, NaNO3 1.8-2.4mg/L、KH2PO4 1.5-2.0mg/L、 Chitosan 0.5-0.7mg/L, biogas slurry 5-8mg/L, f2 vitamin 3-4mL and sea water 1L；
S2. oils and fats extracts: after step S1 is collected single intestinal frustule concentrate drying, uses ultrasound wave to carry out single intestinal algae at breaking cellular wall Reason, obtains single intestinal algae powder, and adding in single intestinal algae powder with its mass ratio is the petroleum ether of 1:5-7, and mixing stands 2-5h, and upper liquid is i.e. For oils and fats extracting solution, then by extracting solution 80-85 DEG C of distillation, i.e. can get microalgae grease；
S3. ester exchange reaction: be 1:3-5:0.02-according to mass ratio by microalgae grease, methanol and zeolite molecular sieve catalyst The ratio of 0.04 adds in reactor, at temperature is 50-55 DEG C, carries out esterification 75-80min, obtains esterification products；
S4. standing separation；By esterification products centrifugal 15-20min, stratification under rotating speed is 300-400r/min, isolate Upper strata glycerol, lower floor is biodiesel crude product；
S5. distilation: biodiesel crude product is added to distillation column, is distilled off unnecessary methanol at 80-85 DEG C, the most available Biodiesel.
The preparation method of a kind of microalgae biodiesel the most according to claim 1, it is characterised in that: described red indigo plant is double-colored HONGGUANG in LED light supplement lamp and blue light proportioning are 1-3:1.
The preparation method of a kind of microalgae biodiesel the most according to claim 1 and 2, it is characterised in that: described in step S2 Using ultrasound wave that single intestinal algae is carried out broken wall treatment, ultrasonic power is 200-250W, ultrasonic time is 45-55min.
CN201610766858.8A 2016-08-30 2016-08-30 A kind of preparation method of microalgae biodiesel Pending CN106190536A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101649332A (en) * 2008-08-15 2010-02-17 上海高技企业发展公司 Production method of biodiesel
CN101767893A (en) * 2010-02-11 2010-07-07 清华大学 Device and method for coupling producing biological oil by utilizing microalgae to deeply treating wastewater
CN103045352A (en) * 2011-10-17 2013-04-17 中国石油化工股份有限公司 Extraction method of microalga grease

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101649332A (en) * 2008-08-15 2010-02-17 上海高技企业发展公司 Production method of biodiesel
CN101767893A (en) * 2010-02-11 2010-07-07 清华大学 Device and method for coupling producing biological oil by utilizing microalgae to deeply treating wastewater
CN103045352A (en) * 2011-10-17 2013-04-17 中国石油化工股份有限公司 Extraction method of microalga grease

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Application publication date: 20161207