CN106191143A - A kind of method preparing biodiesel for raw material with Dunaliella salina - Google Patents
A kind of method preparing biodiesel for raw material with Dunaliella salina Download PDFInfo
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- CN106191143A CN106191143A CN201610766706.8A CN201610766706A CN106191143A CN 106191143 A CN106191143 A CN 106191143A CN 201610766706 A CN201610766706 A CN 201610766706A CN 106191143 A CN106191143 A CN 106191143A
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P7/00—Preparation of oxygen-containing organic compounds
- C12P7/64—Fats; Fatty oils; Ester-type waxes; Higher fatty acids, i.e. having at least seven carbon atoms in an unbroken chain bound to a carboxyl group; Oxidised oils or fats
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- C12P7/649—Biodiesel, i.e. fatty acid alkyl esters
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- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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Abstract
The invention discloses a kind of method preparing biodiesel for raw material with Dunaliella salina, comprise the following steps: Dunaliella salina is seeded to culture medium, irradiate 16 20h/ days with red blue dual-colored LED light compensating lamp, cultivate 10 12 days at 25 27 DEG C, Dunaliella salina cell can be collected；The Dunaliella salina cell collected adds high speed ball mill and crushes, 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 1:3 5:0.03 0.05 and carry out esterification, obtain esterification products, esterification products through separating, purifying, i.e. can get biodiesel again.The inventive method, with Dunaliella salina 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
Technical field
The invention belongs to biomass energy technology field, a kind of with Dunaliella salina for the biological bavin of raw material preparation specifically
The method of oil.
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.
Dunaliella salina (Dunaliella salina) is a kind of green microalgae, belongs to Chlorophyceae volvocales, and Dunaliella salina contains
Abundant oils and fats, beta-carotene, protein, polysaccharide etc., simultaneously containing mineral such as higher Ca, P, Zn, the glycerol of accumulation is dry
The 40% of weight, mainly contains C in lubricant component18、C16The fatty glyceride of carbochain, with the biological bavin extracted from vegetable oil
Oil ingredient is close, is the class bioenergy material with potentiality to be exploited.
Summary of the invention
The present invention is directed to the problem that Vegetable oil lipoprotein limits throughput and existing biodiesel oil preparing process exist, it is provided that a kind of with
Dunaliella salina is the method that biodiesel prepared by raw material.The inventive method has that raw material sources are extensive, catalytic efficiency is high, power consumption
The advantage such as low, biodiesel production rate is high, preparation technology is simple, lays a good foundation for biodiesel industrialization, scale,
Can effective alleviating energy crisis problem.
In order to realize object above, the present invention is to be achieved through the following technical solutions:
A kind of method preparing biodiesel for raw material with Dunaliella salina, comprises the following steps:
S1. Dunaliella salina is cultivated: with Dunaliella salina as raw material, then inoculates with the inoculum density of ten thousand cell/mL of 400-600
To culture medium, irradiate 16-20h/ days with red blue dual-colored LED light compensating lamp, control intensity of illumination in 3500-4000LX, cultivation temperature
Controlling at 25-27 DEG C, cultivate 10-12 days, the density of Dunaliella salina reaches concentration and reaches 90,000,000 cell/mL, collects Du Shi
Dunaliella salina cell；Described culture medium is composed of the following components: glucose 20-30mg/L, NaNO3 1.8-2.4mg/L、
KH2PO41.0-1.2mg/L、Na2SiO31.0-1.5mg/L, chitosan 0.6-0.8mg/L, biogas slurry 6-10mg/L, f2 vitamin 1-
3mL and sea water 1L；
S2. oils and fats extracts: step S1 is collected Dunaliella salina cell concentration after drying, adds high speed ball mill and crushes,
Dunaliella salina powder, adding in Dunaliella salina powder with its mass ratio is the petroleum ether of 1:6-9, and mixing stands 2-5h, and upper liquid is i.e.
For oils and fats extracting solution, then by extracting solution 70-80 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 0.03-0.05 adds in reactor, at temperature is 50-55 DEG C, carries out esterification 80-100min, is esterified
Product；
S4. standing separation；By esterification products centrifugal 15-20min, stratification under rotating speed is 350-500r/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 75-80 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, the high speed ball mill described in above step S2 crushes is to control rotating speed to crush under 500-800r/min
20-25min。。
Compared with prior art, the beneficial effect that the present invention obtains:
1, the present invention prepares biodiesel with Dunaliella salina for raw material, can effectively alleviate current energy crisis and environment is dirty
Dye problem, Dunaliella salina has that distribution is wide, Biomass high, photosynthetic efficiency is high, adaptive capacity to environment is strong, growth cycle is short, oils and fats
The significant advantages such as content height, low cost and environmental friendliness, it is possible to solve the Vegetable oil lipoprotein insufficient raw material in biodiesel exploitation, one-tenth
This crosses 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 Du Shi salt
The photosynthesis of algae, accelerates Dunaliella salina and produces and improve yield, can also improve the oils and fats productivity of Dunaliella salina, with often simultaneously
Electric filament lamp, fluorescent lamp or monochromatic LED lamp compare, the oils and fats productivity of Dunaliella salina improves about 5%.
4, the present invention uses high speed ball mill crushing microalgae cells, has low cost, efficiency height, environmentally safe, consumption
The advantages such as energy is low, are one processing methods cost-effectively.
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 Dunaliella salina culture medium: glucose 20mg/L, NaNO3 2.4mg/L、KH2PO41.0mg/L、
Na2SiO31.0mg/L, chitosan 0.6mg/L, biogas slurry 10mg/L, f2 vitamin 1mL and sea water 1L；
A kind of method preparing biodiesel for raw material with Dunaliella salina, comprises the following steps:
S1. Dunaliella salina is cultivated: with Dunaliella salina as raw material, then is seeded to training with the inoculum density of 4,000,000 cell/mL
Supporting base, irradiate 16h/ days with red blue dual-colored LED light compensating lamp, wherein HONGGUANG and blue light proportioning are that 1:1 control intensity of illumination exists
3500LX, cultivation temperature controls at 25 DEG C, cultivates 12 days, and the density of Dunaliella salina reaches concentration and reaches 90,000,000 cell/mL,
Collect Dunaliella salina cell；
S2. oils and fats extracts: step S1 is collected Dunaliella salina cell concentration after drying, adds high speed ball mill and at rotating speed is
Under 500r/min, broken 25min, obtains Dunaliella salina powder, and adding in Dunaliella salina powder with its mass ratio is the petroleum ether of 1:6, mixed
Even standing 2h, upper liquid is oils and fats extracting solution, then by extracting solution 70 DEG C of distillations, i.e. can get microalgae grease；
S3. ester exchange reaction: be 1:3:0.03'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 80min, obtains esterification products；
S4. standing separation；By esterification products centrifugal 20min, 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 75 DEG C,
To biodiesel.
Embodiment 2
The preparation of Dunaliella salina culture medium: glucose 25mg/L, NaNO3 2.0mg/L、KH2PO41.1mg/L、
Na2SiO31.2mg/L, chitosan 0.7mg/L, biogas slurry 8mg/L, f2 vitamin 3mL and sea water 1L；
A kind of method preparing biodiesel for raw material with Dunaliella salina, comprises the following steps:
S1. Dunaliella salina is cultivated: with Dunaliella salina as raw material, then is seeded to training with the inoculum density of 5,000,000 cell/mL
Supporting base, irradiate 18h/ days with red blue dual-colored LED light compensating lamp, wherein HONGGUANG and blue light proportioning are that 2:1 control intensity of illumination exists
3700LX, cultivation temperature controls at 26 DEG C, cultivates 10 days, and the density of Dunaliella salina reaches concentration and reaches 90,000,000 cell/mL,
Collect Dunaliella salina cell；
S2. oils and fats extracts: step S1 is collected Dunaliella salina cell concentration after drying, adds high speed ball mill and at rotating speed is
Under 600r/min, broken 23min, obtains Dunaliella salina powder, and adding in Dunaliella salina powder with its mass ratio is the petroleum ether of 1:7, mixed
Even standing 3h, upper liquid is oils and fats extracting solution, then by extracting solution 80 DEG C of distillations, i.e. can get microalgae grease；
S3. ester exchange reaction: be 1:4:0.05'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 90min, obtains esterification products；
S4. standing separation；By esterification products centrifugal 18min, 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 78 DEG C,
To biodiesel.
Embodiment 3
The preparation of Dunaliella salina culture medium: glucose 30mg/L, NaNO3 1.8mg/L、KH2PO41.2mg/L、
Na2SiO31.5mg/L, chitosan 0.8mg/L, biogas slurry 6mg/L, f2 vitamin 2mL and sea water 1L；
A kind of method preparing biodiesel for raw material with Dunaliella salina, comprises the following steps:
S1. Dunaliella salina is cultivated: with Dunaliella salina as raw material, then is seeded to training with the inoculum density of 6,000,000 cell/mL
Supporting base, irradiate 20h/ days with red blue dual-colored LED light compensating lamp, wherein HONGGUANG and blue light proportioning are that 3:1 control intensity of illumination exists
4000LX, cultivation temperature controls at 27 DEG C, cultivates 12 days, and the density of Dunaliella salina reaches concentration and reaches 90,000,000 cell/mL,
Collect Dunaliella salina cell；
S2. oils and fats extracts: step S1 is collected Dunaliella salina cell concentration after drying, adds high speed ball mill and at rotating speed is
Under 800r/min, broken 20min, obtains Dunaliella salina powder, and adding in Dunaliella salina powder with its mass ratio is the petroleum ether of 1:9, mixed
Even standing 5h, upper liquid is oils and fats extracting solution, then by extracting solution 75 DEG C of distillations, i.e. can get microalgae grease；
S3. ester exchange reaction: be 1:5:0.04'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 100min, obtains esterification products；
S4. standing separation；By esterification products centrifugal 15min, stratification under rotating speed is 500r/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.
The Dunaliella salina utilizing oils and fats extraction weight method to collect above example carries out fat content mensuration, and result is such as
Shown in table 1.Wherein oils and fats total content=(microalgae grease/Dunaliella salina powder) × 100%.
Table 1. Dunaliella salina fat content
| Oils and fats total content (%) | |
| Embodiment 1 | 42 |
| Embodiment 2 | 48 |
| Embodiment 3 | 44 |
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 | 0.86 | 5.56 | 0.62 | 151 | 63 |
| Embodiment 2 | 0.85 | 4.78 | 0.56 | 159 | 67 |
| Embodiment 3 | 0.83 | 5.33 | 0.54 | 163 | 52 |
| 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. a kind of method preparing biodiesel for raw material with Dunaliella salina, it is characterised in that comprise the following steps:
S1. Dunaliella salina is cultivated: with Dunaliella salina as raw material, then is seeded to training with the inoculum density of ten thousand cell/mL of 400-600
Support base, irradiate 16-20h/ days with red blue dual-colored LED light compensating lamp, control intensity of illumination and control in 3500-4000LX, cultivation temperature
At 25-27 DEG C, cultivating 10-12 days, the density of Dunaliella salina reaches concentration and reaches 90,000,000 cell/mL, collects Dunaliella salina
Cell；Described culture medium is composed of the following components: glucose 20-30mg/L, NaNO3 1.8-2.4mg/L、KH2PO41.0-
1.2mg/L、Na2SiO31.0-1.5mg/L, chitosan 0.6-0.8mg/L, biogas slurry 6-10mg/L, f2 vitamin 1-3mL and sea water
1L；
S2. oils and fats extracts: step S1 is collected Dunaliella salina cell concentration after drying, adds high speed ball mill and crushes, obtains Du Shi
Salt alga powder, adding in Dunaliella salina powder with its mass ratio is the petroleum ether of 1:6-9, and mixing stands 2-5h, and upper liquid is oil
Fat extracting solution, then by extracting solution 70-80 DEG C of distillation, i.e. can get microalgae grease；
S3. ester exchange reaction: be 1:3-5:0.03-according to mass ratio by microalgae grease, methanol and zeolite molecular sieve catalyst
The ratio of 0.05 adds in reactor, at temperature is 50-55 DEG C, carries out esterification 80-100min, obtains esterification products；
S4. standing separation；By esterification products centrifugal 15-20min, stratification under rotating speed is 350-500r/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 75-80 DEG C, the most available
Biodiesel.
A kind of method preparing biodiesel for raw material with Dunaliella salina the most according to claim 1, its feature exists
In: the described HONGGUANG in red blue dual-colored LED light compensating lamp is 1-3:1 with blue light proportioning.
A kind of method preparing biodiesel for raw material with Dunaliella salina the most according to claim 1, its feature exists
In: described high speed ball mill broken be control rotating speed at 500-800r/min under broken 20-25min.
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Citations (1)
| 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 |
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Patent Citations (1)
| 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 |
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Application publication date: 20161207 |