CN104293474A - Method for extracting oil from oil production microbes - Google Patents
Method for extracting oil from oil production microbes Download PDFInfo
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- CN104293474A CN104293474A CN201310306523.4A CN201310306523A CN104293474A CN 104293474 A CN104293474 A CN 104293474A CN 201310306523 A CN201310306523 A CN 201310306523A CN 104293474 A CN104293474 A CN 104293474A
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- oleaginous microorganism
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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
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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
- C11B1/12—Production of fats or fatty oils from raw materials by melting out
- C11B1/14—Production of fats or fatty oils from raw materials by melting out with hot water or aqueous solutions
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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- Organic Chemistry (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
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Abstract
The invention discloses a method for extracting oil from oil production microbes. The method is characterized in that the method comprises the following steps: 1, adjusting the pH value of a water slurry containing the oil production microbes to 7.5-14; 2, stirring under hydrothermal conditions to dissolve out oil in the cells of the oil production microbes in order to obtain an oil production microbes dissolved slurry containing oil; and 3, adjusting the pH value of the oil production microbes dissolved slurry to 6.8-7.2 by using an acidic flocculating agent under stirring, allowing the obtained slurry to stand for layering, and separating the obtained upper layer oil, wherein the acidic flocculating agent is a flocculating agent which is acidic after dissolved in water. The method for extracting oil from oil production microbes allows the pH value of the oil production microbes dissolved slurry to 6.8-7.2 by using the acidic flocculating agent to successfully realize the demulsification of the oil production microbes dissolved slurry in order to thoroughly flocculate microbe residues, so an oil phase and a water phase can be well separate, the oil extraction rate is high, and the energy consumption is low.
Description
Technical field
The present invention relates to oleaginous microorganism field of engineering technology, particularly, relate to a kind of method extracting grease from oleaginous microorganism.
Background technology
Because microorganism cells propagation is fast; with short production cycle; microorganism growth desired raw material wide material sources; low price, and microorganism growth does not limit by season, climate change, energy scale operation continuously; production cost is low; and oil length is high in oleaginous microorganism, therefore, utilize oleaginous microorganism to produce grease and become a kind of important means alleviating global energy crisis.
Split kettle algae and micro-algae due to fat content in cell high, can be used as the important glyceride stock source of biological liquid fuel.Particularly along with world energy sources is as the day by day shortage of oil, with animal-plant oil (comprise and split kettle algae grease, microalgae grease) for raw material production biofuel is subject to extensive concern, and competitively carry out the research of biofuel.
The extraction of oleaginous microorganism grease is the gordian technique of biological diesel oil refining always.Usually hydrothermal method is adopted at present.Hydrothermal method normally carries out cell wall breaking, grease stripping by High Temperature High Pressure in the basic conditions, general temperature is 100-300 DEG C, the molten slurry of gained oleaginous microorganism carries out oily water separation by centrifugal, as CN100460513C, but due to the milk sap that the molten slurry of the oleaginous microorganism obtained is containing microorganism slag, oil phase and aqueous phase mix, and are difficult to be separated, and are undertaken that oily water separation energy consumption is higher, grease extraction efficiency is lower by centrifugal.
Therefore, the efficient and technology extracting grease from oleaginous microorganism of economy becomes the emphasis of research.
Summary of the invention
The object of the invention is to overcome in prior art from oleaginous microorganism, extract the defect that grease extraction efficiency is low, energy consumption is high, a kind of efficient and method extracting grease from oleaginous microorganism of economy is provided.
The present inventor surprisingly finds under study for action, hydrothermal method is utilized to extract grease from oleaginous microorganism, the molten slurry of oleaginous microorganism to the pH value obtained is regulated to be 6.8-7.2 with acid flocculation agent, successfully can realize the breakdown of emulsion of the molten slurry of oleaginous microorganism, thus microorganism slag is flocculated, oil phase, aqueous phase separation.Not only extraction yield is high, and energy consumption is low.
Therefore, to achieve these goals, the invention provides a kind of method extracting grease from oleaginous microorganism, it is characterized in that, described method comprises the steps:
(1) aqueous slurry to the pH value containing oleaginous microorganism is regulated to be 7.5-14;
(2) stir under hydrothermal conditions, make the grease stripping in oleaginous microorganism cell, obtain the molten slurry of oleaginous microorganism containing grease;
(3) under agitation regulate the molten slurry of described oleaginous microorganism to be 6.8-7.2, then stratification to pH value with acid flocculation agent, isolate upper strata grease, described acid flocculation agent be water-soluble after in acid flocculation agent.
Preferably, described acid flocculation agent is selected from one or more in molysite, aluminium salt and ammonium salt; More preferably, described acid flocculation agent is selected from one or more in iron trichloride, ferric sulfate, aluminum chloride, Tai-Ace S 150 and ammonium chloride.
Preferably, in step (3), the condition of described stirring comprises: temperature is 40-90 DEG C, the material be stirred relative to every cubic metre, and power of agitator is 0.15-1.5kW, and the time is 5-60 minute.
Preferably, described oleaginous microorganism is for splitting kettle algae.
Preferably, described oleaginous microorganism is micro-algae.
The method extracting grease from oleaginous microorganism provided by the invention, the molten slurry of oleaginous microorganism is regulated to be 6.8-7.2 to pH value with acid flocculation agent, successfully can realize the breakdown of emulsion of the molten slurry of oleaginous microorganism, thus microorganism slag is flocculated more up hill and dale, oil phase, aqueous phase are separated better, grease extraction efficiency is high, and energy consumption is low.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Embodiment
Below the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
The invention provides a kind of method extracting grease from oleaginous microorganism, the method comprises the steps:
(1) aqueous slurry to the pH value containing oleaginous microorganism is regulated to be 7.5-14;
(2) stir under hydrothermal conditions, make the grease stripping in oleaginous microorganism cell, obtain the molten slurry of oleaginous microorganism containing grease;
(3) under agitation regulate the molten slurry of oleaginous microorganism to be 6.8-7.2, then stratification to pH value with acid flocculation agent, isolate upper strata grease, acid flocculation agent be water-soluble after in acid flocculation agent.
In the present invention, the aqueous slurry containing oleaginous microorganism refers to the liquid containing oleaginous microorganism collected oleaginous microorganism and obtain from oleaginous microorganism nutrient solution.With the dry weight basis of oleaginous microorganism, be preferably 2-40 % by weight containing the content of oleaginous microorganism in the aqueous slurry of oleaginous microorganism, be more preferably 7-15 % by weight.
In the present invention, in step (1), aqueous slurry to the pH value containing oleaginous microorganism is regulated to be 7.5-14, for pH value condition, alkali can be added regulate, for alkali without particular requirement, the alkali that this area is conventional can be adopted, such as, alkali can be selected from one or more in oxyhydroxide, carbonate, supercarbonate and phosphoric acid salt.
In the present invention, pH value is recorded by pH meter.
In the present invention, hydrothermal condition refers to and keeps liquid condition at a certain temperature.In step of the present invention (2), hydrothermal condition preferably includes: temperature is 100-180 DEG C; More preferably comprise: temperature is 120-150 DEG C.
It will be understood by those skilled in the art that in step (2), as long as the pressure of hydrothermal condition makes water can keep liquid at the temperature disclosed above.
In step of the present invention (2), for the condition stirred, as long as make the grease stripping in oleaginous microorganism cell.Such as, the condition of stirring can comprise: the material be stirred relative to every cubic metre, and power of agitator is 0.15-1.5kW; Churning time is 2-30 minute; Preferably, the condition of stirring can comprise: the material be stirred relative to every cubic metre, and power of agitator is 0.2-1kW; Churning time is 15-30 minute.Under above-mentioned agitation condition, the grease stripping in oleaginous microorganism cell can be made.
In the present invention, namely the molten slurry of oleaginous microorganism refers to containing the oleaginous microorganism cell wall damage in the aqueous slurry of oleaginous microorganism, and born of the same parents' inner structure is disintegrated, the mixture that the stripping of oleaginous microorganism grease obtains.Namely microorganism slag refers to the solid matter in the molten slurry of oleaginous microorganism.
In the present invention, namely acid flocculation agent refers to water-soluble rear in acid flocculation agent.The molten slurry of oleaginous microorganism is regulated to be 6.8-7.2 to pH value, as long as the consumption of acid flocculation agent meets above-mentioned pH value condition with acid flocculation agent.
In the present invention, acid flocculation agent be preferably selected from molysite, aluminium salt and ammonium salt one or more; More preferably, acid flocculation agent is selected from one or more in iron trichloride, ferric sulfate, aluminum chloride, Tai-Ace S 150 and ammonium chloride.
In step of the present invention (3), the condition optimization stirred is comprised: temperature is 40-90 DEG C, the material be stirred relative to every cubic metre, and power of agitator is 0.15-1.5kW, and the time is 5-60 minute; More preferably comprise: temperature is 70-90 DEG C, the material be stirred relative to every cubic metre, power of agitator is 0.2-1kW, and the time is 10-30 minute.
In the present invention, oleaginous microorganism can be heterotrophic microorganism, can be also autotrophic microorganism, include but not limited to bacterium, fungi, actinomycetes and micro-algae, and be preferably schizochytrium limacinum or micro-algae, schizochytrium limacinum is also known as splitting kettle algae.In the present invention, kind for micro-algae has no particular limits, and is preferably oil-producing microalgae, is more preferably the produce oil engineering microalgae with larger industrial utilization, such as, micro-algae can be selected from least one in chlorella, grid algae, spirulina, chrysophyceae or Phaeodactylum tricornutum.
Embodiment
The present invention is further illustrated for following embodiment, but therefore do not limit the present invention.
In following embodiment and comparative example:
With the dry algae powder and deionized water that split kettle algae be mixed with 9 % by weight, 11 % by weight and 14 % by weight containing the aqueous slurry splitting kettle algae.
The aqueous slurry containing chlorella of 7.7 % by weight and 10.4 % by weight is mixed with the dry algae powder of chlorella and deionized water.
The weight of the weight/dry algae powder of the grease of grease extraction efficiency=extraction.
PH value is recorded by pH meter (Beijing Technew SA of Ge Le regular senior middle school, PH-9701).
Embodiment 1
This embodiment is for illustration of the method extracting grease from oleaginous microorganism of the present invention.
(1) take 11 % by weight containing the aqueous slurry 45g splitting kettle algae, regulate pH value containing the aqueous slurry splitting kettle algae to be 8 with NaOH;
(2) mechanic whirl-nett reaction still is placed in by containing the aqueous slurry splitting kettle algae, be under the hydrothermal condition of 130 DEG C in temperature, the material be stirred relative to every cubic metre, power of agitator is that 0.6kW(adopts Juancheng, Shandong Province Yongxing instrument plant YXMD type simulated reinforcement electric mixer to stir, lower same), stir 20 minutes, obtain splitting the molten slurry of kettle algae;
(3) splitting the molten slurry of kettle algae to pH value with iron trichloride adjustment is 7.0, at 90 DEG C, and the material be stirred relative to every cubic metre, power of agitator is 0.6kW, stirs 20 minutes, then stratification, collect upper oil phase and obtain grease 2.06g, calculating grease extraction efficiency is 41.6%.
Embodiment 2
This embodiment is for illustration of the method extracting grease from oleaginous microorganism of the present invention.
(1) take 14 % by weight containing the aqueous slurry 35g splitting kettle algae, regulate pH value containing the aqueous slurry splitting kettle algae to be 10 with NaOH;
(2) being placed in mechanic whirl-nett reaction still by containing the aqueous slurry splitting kettle algae, is under the hydrothermal condition of 120 DEG C in temperature, the material be stirred relative to every cubic metre, and power of agitator is 0.2kW, stirs 30 minutes, obtains splitting the molten slurry of kettle algae;
(3) splitting the molten slurry of kettle algae to pH value with Tai-Ace S 150 adjustment is 6.8, at 80 DEG C, and the material be stirred relative to every cubic metre, power of agitator is 0.2kW, stirs 30 minutes, then stratification, collect upper oil phase and obtain grease 2.26g, calculating grease extraction efficiency is 46.1%.
Embodiment 3
This embodiment is for illustration of the method extracting grease from oleaginous microorganism of the present invention.
(1) take 9 % by weight containing the aqueous slurry 55g splitting kettle algae, regulate pH value containing the aqueous slurry splitting kettle algae to be 12 with NaOH;
(2) being placed in mechanic whirl-nett reaction still by containing the aqueous slurry splitting kettle algae, is under the hydrothermal condition of 150 DEG C in temperature, the material be stirred relative to every cubic metre, and power of agitator is 0.3kW, stirs 15 minutes, obtains splitting the molten slurry of kettle algae;
(3) splitting the molten slurry of kettle algae to pH value with ammonium chloride adjustment is 7.2, at 70 DEG C, and the material be stirred relative to every cubic metre, power of agitator is 0.3kW, stirs 10 minutes, then stratification, collect upper oil phase and obtain grease 1.95g, calculating grease extraction efficiency is 39.4%.
Embodiment 4
This embodiment is for illustration of the method extracting grease from oleaginous microorganism of the present invention.
(1) take the aqueous slurry 40g containing chlorella of 7.7 % by weight, the pH value of the aqueous slurry regulated containing chlorella with NaOH is 14;
(2) aqueous slurry containing chlorella being placed in mechanic whirl-nett reaction still, is under the hydrothermal condition of 130 DEG C in temperature, the material be stirred relative to every cubic metre, and power of agitator is 0.6kW, stirs 25 minutes, obtains the molten slurry of chlorella;
(3) chlorella molten slurry is regulated to be 7.0 to pH value with ferric sulfate, at 90 DEG C, the material be stirred relative to every cubic metre, power of agitator is 0.6kW, stirs 25 minutes, then stratification, collect upper oil phase and obtain grease 0.87g, calculating grease extraction efficiency is 28.2%.
Embodiment 5
This embodiment is for illustration of the method extracting grease from oleaginous microorganism of the present invention.
(1) take the aqueous slurry 35g containing chlorella of 10.4 % by weight, the pH value of the aqueous slurry regulated containing chlorella with NaOH is 10;
(2) aqueous slurry containing chlorella being placed in mechanic whirl-nett reaction still, is under the hydrothermal condition of 150 DEG C in temperature, the material be stirred relative to every cubic metre, and power of agitator is 0.3kW, stirs 18 minutes, obtains the molten slurry of chlorella;
(3) chlorella molten slurry is regulated to be 6.9 to pH value with aluminum chloride, at 80 DEG C, the material be stirred relative to every cubic metre, power of agitator is 0.3kW, stirs 15 minutes, then stratification, collect upper oil phase and obtain grease 0.96g, calculating grease extraction efficiency is 26.4%.
Comparative example 1
(1) take 11 % by weight containing the aqueous slurry 45g splitting kettle algae, regulate pH value containing the aqueous slurry splitting kettle algae to be 8 with NaOH;
(2) being placed in mechanic whirl-nett reaction still by containing the aqueous slurry splitting kettle algae, is under the hydrothermal condition of 200 DEG C in temperature, the material be stirred relative to every cubic metre, and power of agitator is 0.6kW, stirs 60 minutes, obtains splitting the molten slurry of kettle algae;
(3) will split the centrifugation 10 minutes under 5000rpm of the molten slurry of kettle algae, collect upper oil phase and obtain grease 1.86g, calculating grease extraction efficiency is 37.6%.
Comparative example 2
Grease is extracted from containing the aqueous slurry splitting kettle algae according to the method for embodiment 1, unlike, in step (3), adjust ph to 7.5.Collect upper oil phase and obtain grease 1.84g, calculating grease extraction efficiency is 37.2%.
Comparative example 3
Grease is extracted from containing the aqueous slurry splitting kettle algae according to the method for embodiment 1, unlike, in step (3), adjust ph is 6.5.Collect upper oil phase and obtain grease 1.74g, calculating grease extraction efficiency is 35.2%.
Embodiment 1 and comparative example 1 are compared and can be found out, the inventive method, compared with traditional hydrothermal method, can improve grease extraction efficiency, can save the energy consumption of centrifugation.Embodiment 1 is compared can find out with comparative example 2 and comparative example 3 respectively, only under the condition of pH value 6.8-7.2, just can realize the successful breakdown of emulsion of the molten slurry of oleaginous microorganism, microorganism slag just can flocculate more up hill and dale, and aqueous phase, oil phase just can be separated preferably.
The method extracting grease from oleaginous microorganism provided by the invention, the molten slurry of oleaginous microorganism is regulated to be 6.8-7.2 to pH value with acid flocculation agent, successfully can realize the breakdown of emulsion of the molten slurry of oleaginous microorganism, thus microorganism slag is flocculated more up hill and dale, oil phase, aqueous phase are separated better, grease extraction efficiency is high, and energy consumption is low.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out arbitrary combination between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. from oleaginous microorganism, extract a method for grease, it is characterized in that, described method comprises the steps:
(1) aqueous slurry to the pH value containing oleaginous microorganism is regulated to be 7.5-14;
(2) stir under hydrothermal conditions, make the grease stripping in oleaginous microorganism cell, obtain the molten slurry of oleaginous microorganism containing grease;
(3) under agitation regulate the molten slurry of described oleaginous microorganism to be 6.8-7.2, then stratification to pH value with acid flocculation agent, isolate upper strata grease, described acid flocculation agent be water-soluble after in acid flocculation agent.
2. method according to claim 1, wherein, with the dry weight basis of oleaginous microorganism, described is 2-40 % by weight containing the content of oleaginous microorganism in the aqueous slurry of oleaginous microorganism.
3. method according to claim 1, wherein, in step (2), hydrothermal condition comprises: temperature is 100-180 DEG C.
4. method according to claim 1, wherein, in step (2), the condition of stirring comprises: the material be stirred relative to every cubic metre, and power of agitator is 0.15-1.5kW; Churning time is 2-30 minute.
5. method according to claim 1, wherein, described acid flocculation agent be selected from molysite, aluminium salt and ammonium salt one or more.
6. method according to claim 5, wherein, described acid flocculation agent be selected from iron trichloride, ferric sulfate, aluminum chloride, Tai-Ace S 150 and ammonium chloride one or more.
7. method according to claim 1, wherein, in step (3), the condition of described stirring comprises: temperature is 40-90 DEG C, the material be stirred relative to every cubic metre, and power of agitator is 0.15-1.5kW, and the time is 5-60 minute.
8. method according to claim 1, wherein, described oleaginous microorganism is for splitting kettle algae.
9. method according to claim 1, wherein, described oleaginous microorganism is micro-algae.
10. method according to claim 9, wherein, described micro-algae is selected from least one in chlorella, grid algae, spirulina, chrysophyceae and Phaeodactylum tricornutum.
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| CN105296137A (en) * | 2015-10-15 | 2016-02-03 | 中国科学院水生生物研究所 | Method for extracting microalgae lipid through biological enzyme catalysis wall breaking |
| CN109609261A (en) * | 2018-11-16 | 2019-04-12 | 水母娘娘海洋生物科技有限公司 | A kind of aurelia extractive liquid oleosa and the preparation method and application thereof |
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| CN109609261A (en) * | 2018-11-16 | 2019-04-12 | 水母娘娘海洋生物科技有限公司 | A kind of aurelia extractive liquid oleosa and the preparation method and application thereof |
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