CN108893185B - Method for preparing microalgae grease by magnetic hydrophobic eutectic solvent assisted flash extraction - Google Patents
Method for preparing microalgae grease by magnetic hydrophobic eutectic solvent assisted flash extraction Download PDFInfo
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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
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
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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
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
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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
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/108—Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
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Abstract
The invention provides a method for preparing microalgae grease by magnetic hydrophobic eutectic solvent assisted flash extraction, which comprises the steps of adding microalgae mud with certain water content into a flash extractor, extracting for a certain time under certain extraction voltage to obtain microalgae slurry containing the microalgae grease, fully mixing the microalgae slurry and the magnetic hydrophobic eutectic solvent, standing, separating a magnetic hydrophobic eutectic solvent phase, adding a magnetic rod into the magnetic hydrophobic eutectic solvent phase, and recovering the magnetic hydrophobic eutectic solvent to obtain the microalgae grease, wherein the method has the advantages of short extraction time, high efficiency, low energy consumption and the like; the magnetic hydrophobic eutectic solvent can realize effective extraction of the microalgae grease, and under the action of an external magnetic field, the separation purpose of the magnetic hydrophobic eutectic solvent and the grease is achieved, so that the cyclic utilization of the magnetic hydrophobic eutectic solvent is realized.
Description
Technical Field
The invention belongs to the technical field of microalgae oil separation, and particularly relates to a method for preparing microalgae oil through magnetic hydrophobic eutectic solvent assisted flash extraction.
Background
Microalgae have become good biomass resource research objects due to the advantages of high oil content, short culture period, easily controlled culture conditions, sustainable production and the like. However, the cultivation, harvesting, extraction and conversion of microalgae into biodiesel is a high-cost input process, and has become an important obstacle to research and development of microalgae. In the oil extraction process, organic solvent and energy are continuously consumed for cell disruption and extraction, so that an effective extraction method is adopted to shorten the extraction time, reduce the consumption of the organic solvent and reduce the energy output, and meanwhile, the effective extraction effect is ensured to become an important cost-reducing input link.
The flash extraction method is a new extraction method in recent years, can rapidly crush materials to proper granularity at room temperature, and enables effective components to permeate and release by rapid stirring and vibration, and has the characteristics of short extraction time, high efficiency, low energy consumption and the like.
Compared with the traditional organic solvent and ionic liquid, the eutectic solvent is formed by combining a hydrogen bond acceptor and a hydrogen bond donor in a certain stoichiometric ratio, and has the advantages of low melting point, low cost, low toxicity, easy preparation, regeneration, biodegradability and the like. The hydrophilic eutectic solvent is used as an extraction medium and is widely applied to extraction and separation of flavone, polyphenol and other active ingredients in biomass; at present, relatively few research on the application of the hydrophobic eutectic solvent is carried out, and the method is mainly applied to the extraction of model molecules; the prior art discloses that polyprenyl acetate in ginkgo leaves is extracted by using a hydrophobic eutectic solvent, and a target product is recovered by using macroporous resin, but the defects of low recovery rate of the target product, complex operation and the like exist; the prior art has reports of extracting microalgae grease by using a eutectic solvent, but the extraction rate of the eutectic solvent is low, and the separation process of the eutectic solvent and a target product is complex.
Disclosure of Invention
In order to solve the technical problems, the invention provides a novel method for preparing microalgae oil by magnetic hydrophobic eutectic solvent assisted flash extraction, which is convenient to operate and good in extraction effect, and a green solvent can be recycled.
The specific technical scheme of the invention is as follows:
the invention provides a method for preparing microalgae grease by magnetic hydrophobic eutectic solvent assisted flash extraction, which comprises the following steps:
1) adding microalgae mud with a certain water content into a flash extractor, and extracting for a certain time at a certain extraction voltage to obtain microalgae slurry containing microalgae grease;
2) fully and uniformly mixing the microalgae slurry containing the microalgae grease prepared in the step 1) with the magnetic hydrophobic eutectic solvent, standing, and separating a magnetic hydrophobic eutectic solvent phase;
3) adding a magnetic rod into the magnetic hydrophobic eutectic solvent phase separated in the step 2), and recovering the magnetic hydrophobic eutectic solvent to obtain the microalgae grease.
Preferably, the method for preparing the microalgae bathing mud with certain water content comprises the following steps: and (3) filtering the microalgae in the logarithmic phase of growth to obtain algae mud, adding water, oscillating and suspending until the water content reaches the specified content.
The further improvement is that the microalgae is chlorella, chrysophyceae, nannochloropsis, scenedesmus, etc.
In a further improvement, the magnetic hydrophobic eutectic solvent in the step 2) is a mixture of DL-menthol, organic acid and anhydrous ferric trichloride in a molar ratio of 1:1-2: 1.
In a further refinement, the organic acid is selected from one or more of acetic acid, pyruvic acid, levulinic acid, or lactic acid; preferably, the magnetic hydrophobic eutectic solvent is a mixture of DL-menthol, acetic acid and anhydrous ferric chloride in a molar ratio of 1:1:1, or a mixture of DL-menthol, pyruvic acid and anhydrous ferric chloride in a molar ratio of 1:2:1, or a mixture of DL-menthol, levulinic acid and anhydrous ferric chloride in a molar ratio of 1:1:1, or a mixture of DL-menthol, lactic acid and anhydrous ferric chloride in a molar ratio of 1:2: 1.
In a further improvement, the water content of the microalgae bathing mud in the step 1) is 20-85%, and preferably, the water content is 40-75%.
In a further improvement, the extraction voltage in the step 1) is 40-80V, preferably 50-70V.
In a further improvement, the extraction time in the step 1) is 0.5-3min, preferably, the extraction time is 1-2.5 min.
In a further improvement, the volume ratio of the microalgae slurry containing microalgae grease to the magnetic hydrophobic eutectic solvent in the step 2) is 1:0.3-1, preferably 1:0.5-1: 1.
In a further improvement, the standing time is 0.5-2h, preferably 0.7-1.5 h.
In a further improvement, the magnetism of the magnetic rod in the step 3) is 0.5-1.5T.
Compared with the prior art, the method for preparing the microalgae grease by the magnetic hydrophobic eutectic solvent assisted flash extraction has the advantages that: the flash extraction adopted by the invention has the advantages of quickly crushing materials to proper granularity, accelerating the permeation and release of the microalgae grease through quick stirring and vibration, short extraction time, high efficiency, low energy consumption and the like; the magnetic hydrophobic eutectic solvent is adopted to realize effective extraction of the microalgae grease, and under the action of an external magnetic field, the separation purpose of the magnetic hydrophobic eutectic solvent and the grease is achieved, so that the recycling of the magnetic hydrophobic eutectic solvent is realized, and the extraction rate of the microalgae grease is obviously improved by combining the magnetic hydrophobic eutectic solvent with a flash extraction method.
Detailed Description
Example 1
A magnetic hydrophobic eutectic solvent assisted flash extraction method for preparing microalgae oil comprises the following steps:
1) adding microalgae mud with water content of 50% into a flash extractor, and extracting at 50V for 1min to obtain microalgae slurry containing microalgae oil;
2) mixing the algae slurry containing microalgae grease with a magnetic hydrophobic eutectic solvent according to a volume ratio of 1:0.5, fully and uniformly mixing, standing for 0.7h, and separating a magnetic hydrophobic eutectic solvent phase, wherein the magnetic hydrophobic eutectic solvent is a mixture of DL-menthol, acetic acid and anhydrous ferric trichloride according to a molar ratio of 1:1: 1;
3) and adding a magnetic rod with the magnetism of 0.6T into the separated magnetic hydrophobic eutectic solvent phase, and recovering the magnetic hydrophobic eutectic solvent to obtain the microalgae grease with the extraction rate of 98.42%.
The extraction rate is the weight of extracted microalgae oil/theoretical weight of microalgae oil contained in microalgae mud.
Example 2
A magnetic hydrophobic eutectic solvent assisted flash extraction method for preparing microalgae oil comprises the following steps:
1) adding microalgae mud with water content of 75% into a flash extractor, extracting at 60V for 2.5min to obtain microalgae slurry containing microalgae oil;
2) mixing algae slurry containing microalgae grease with a magnetic hydrophobic eutectic solvent according to a volume ratio of 1:0.7, fully and uniformly mixing, standing for 1h, and separating a magnetic hydrophobic eutectic solvent phase, wherein the magnetic hydrophobic eutectic solvent is a mixture of DL-menthol, pyruvic acid and anhydrous ferric trichloride according to a molar ratio of 1:2: 1;
3) adding a magnetic rod with the magnetism of 1.0T into the separated magnetic hydrophobic eutectic solvent phase, and recovering the magnetic hydrophobic eutectic solvent to obtain the microalgae grease with the extraction rate of 97.85%.
Example 3
A magnetic hydrophobic eutectic solvent assisted flash extraction method for preparing microalgae oil comprises the following steps:
1) adding microalgae mud with water content of 40% into a flash extractor, extracting at 70V for 1.5min to obtain microalgae slurry containing microalgae oil;
2) mixing algae slurry containing microalgae grease with a magnetic hydrophobic eutectic solvent according to a volume ratio of 1:1, fully and uniformly mixing, standing for 1.5h, and separating a magnetic hydrophobic eutectic solvent phase, wherein the magnetic hydrophobic eutectic solvent is a mixture of DL-menthol, lactic acid and anhydrous ferric trichloride according to a molar ratio of 1:2: 1;
3) adding a magnetic rod with the magnetism of 1.0T into the separated magnetic hydrophobic eutectic solvent phase, and recovering the magnetic hydrophobic eutectic solvent to obtain the microalgae grease with the extraction rate of 98.90 percent.
Example 4
A magnetic hydrophobic eutectic solvent assisted flash extraction method for preparing microalgae oil comprises the following steps:
1) adding microalgae mud with water content of 60% into a flash extractor, and extracting at 50V for 2min to obtain microalgae slurry containing microalgae oil;
2) mixing algae slurry containing microalgae grease with a magnetic hydrophobic eutectic solvent according to a volume ratio of 1:0.6, fully and uniformly mixing, standing for 1.2h, and separating a magnetic hydrophobic eutectic solvent phase, wherein the magnetic hydrophobic eutectic solvent is a mixture of DL-menthol, levulinic acid and anhydrous ferric trichloride according to a molar ratio of 1:1: 1;
3) and adding a magnetic rod with the magnetism of 0.7T into the separated magnetic hydrophobic eutectic solvent phase, and recovering the magnetic hydrophobic eutectic solvent to obtain the microalgae grease with the extraction rate of 97.34%.
Example 5
A magnetic hydrophobic eutectic solvent assisted flash extraction method for preparing microalgae oil comprises the following steps:
1) adding microalgae mud with water content of 55% into a flash extractor, extracting at 55V extraction voltage for 2min to obtain microalgae slurry containing microalgae oil;
2) mixing the algae slurry containing microalgae grease with a magnetic hydrophobic eutectic solvent according to a volume ratio of 1:0.6, fully and uniformly mixing, standing for 0.9h, and separating a magnetic hydrophobic eutectic solvent phase, wherein the magnetic hydrophobic eutectic solvent is a mixture of DL-menthol, acetic acid and anhydrous ferric trichloride according to a molar ratio of 1:1: 1;
3) and adding a magnetic rod with the magnetism of 0.9T into the separated magnetic hydrophobic eutectic solvent phase, and recovering the magnetic hydrophobic eutectic solvent to obtain the microalgae grease with the extraction rate of 97.88%.
Example 6
A magnetic hydrophobic eutectic solvent assisted flash extraction method for preparing microalgae oil comprises the following steps:
1) adding microalgae mud with water content of 65% into a flash extractor, extracting at 65V extraction voltage for 1.7min to obtain microalgae slurry containing microalgae oil;
2) mixing the algae slurry containing microalgae grease with a magnetic hydrophobic eutectic solvent according to a volume ratio of 1:0.8, fully and uniformly mixing, standing for 1.2h, and separating a magnetic hydrophobic eutectic solvent phase, wherein the magnetic hydrophobic eutectic solvent is a mixture of DL-menthol, lactic acid and anhydrous ferric trichloride according to a molar ratio of 1:2: 1;
3) and adding a magnetic rod with the magnetism of 0.7T into the separated magnetic hydrophobic eutectic solvent phase, and recovering the magnetic hydrophobic eutectic solvent to obtain the microalgae grease with the extraction rate of 98.03%.
Example 7
A magnetic hydrophobic eutectic solvent assisted flash extraction method for preparing microalgae oil comprises the following steps:
1) adding microalgae mud with water content of 55% into a flash extractor, extracting at 65V for 1.5min to obtain microalgae slurry containing microalgae oil;
2) mixing the algae slurry containing microalgae grease with a magnetic hydrophobic eutectic solvent according to a volume ratio of 1:0.8, fully and uniformly mixing, standing for 0.8h, and separating a magnetic hydrophobic eutectic solvent phase, wherein the magnetic hydrophobic eutectic solvent is a mixture of DL-menthol, lactic acid and anhydrous ferric trichloride according to a molar ratio of 1:1: 1;
3) and adding a magnetic rod with the magnetism of 0.8T into the separated magnetic hydrophobic eutectic solvent phase, and recovering the magnetic hydrophobic eutectic solvent to obtain the microalgae grease with the extraction rate of 94.18%.
Example 8
A magnetic hydrophobic eutectic solvent assisted flash extraction method for preparing microalgae oil comprises the following steps:
1) adding microalgae mud with water content of 65% into a flash extractor, extracting at 55V for 1.5min to obtain microalgae slurry containing microalgae oil;
2) mixing algae slurry containing microalgae grease with a magnetic hydrophobic eutectic solvent according to a volume ratio of 1:0.9, fully and uniformly mixing, standing for 1h, and separating a magnetic hydrophobic eutectic solvent phase, wherein the magnetic hydrophobic eutectic solvent is a mixture of DL-menthol, acetic acid and anhydrous ferric trichloride according to a molar ratio of 1:2: 1;
3) and adding a magnetic rod with the magnetism of 0.6T into the separated magnetic hydrophobic eutectic solvent phase, and recovering the magnetic hydrophobic eutectic solvent to obtain the microalgae grease with the extraction rate of 95.75%.
Example 9
A magnetic hydrophobic eutectic solvent assisted flash extraction method for preparing microalgae oil comprises the following steps:
1) adding microalgae mud with water content of 45% into a flash extractor, extracting at 50V for 2.2min to obtain microalgae slurry containing microalgae oil;
2) mixing algae slurry containing microalgae grease with a magnetic hydrophobic eutectic solvent according to a volume ratio of 1:0.7, fully and uniformly mixing, standing for 1h, and separating a magnetic hydrophobic eutectic solvent phase, wherein the magnetic hydrophobic eutectic solvent is a mixture of DL-menthol, pyruvic acid and anhydrous ferric trichloride according to a molar ratio of 1:1: 1;
3) and adding a magnetic rod with the magnetism of 0.9T into the separated magnetic hydrophobic eutectic solvent phase, and recovering the magnetic hydrophobic eutectic solvent to obtain the microalgae grease with the extraction rate of 93.67%.
Example 10
A magnetic hydrophobic eutectic solvent assisted flash extraction method for preparing microalgae oil comprises the following steps:
1) adding microalgae mud with water content of 85% into a flash extractor, extracting at 75V for 3min to obtain microalgae slurry containing microalgae oil;
2) mixing algae slurry containing microalgae grease with a magnetic hydrophobic eutectic solvent according to a volume ratio of 1:0.3, fully and uniformly mixing, standing for 2 hours, and separating a magnetic hydrophobic eutectic solvent phase, wherein the magnetic hydrophobic eutectic solvent is a mixture of DL-menthol, lactic acid and anhydrous ferric trichloride according to a molar ratio of 1:2: 1;
3) and adding a magnetic rod with the magnetism of 0.5T into the separated magnetic hydrophobic eutectic solvent phase, and recovering the magnetic hydrophobic eutectic solvent to obtain the microalgae grease with the extraction rate of 92.17%.
Example 11
A magnetic hydrophobic eutectic solvent assisted flash extraction method for preparing microalgae oil comprises the following steps:
1) adding microalgae mud with water content of 30% into a flash extractor, and extracting at 40V extraction voltage for 0.7min to obtain microalgae slurry containing microalgae oil;
2) mixing the algae slurry containing microalgae grease with a magnetic hydrophobic eutectic solvent according to a volume ratio of 1:0.5, fully and uniformly mixing, standing for 0.5h, and separating a magnetic hydrophobic eutectic solvent phase, wherein the magnetic hydrophobic eutectic solvent is a mixture of DL-menthol, lactic acid and anhydrous ferric trichloride according to a molar ratio of 1:2: 1;
3) and adding a magnetic rod with the magnetism of 1.2T into the separated magnetic hydrophobic eutectic solvent phase, and recovering the magnetic hydrophobic eutectic solvent to obtain the microalgae grease with the extraction rate of 95.34%.
Example 12
A magnetic hydrophobic eutectic solvent assisted flash extraction method for preparing microalgae oil comprises the following steps:
1) adding microalgae mud with water content of 20% into a flash extractor, and extracting at 80V extraction voltage for 0.5min to obtain microalgae slurry containing microalgae oil;
2) mixing the algae slurry containing microalgae grease with a magnetic hydrophobic eutectic solvent according to a volume ratio of 1:0.4, fully and uniformly mixing, standing for 1.7h, and separating a magnetic hydrophobic eutectic solvent phase, wherein the magnetic hydrophobic eutectic solvent is a mixture of DL-menthol, lactic acid and anhydrous ferric trichloride according to a molar ratio of 1:1: 1;
3) adding a magnetic rod with the magnetism of 1.5T into the separated magnetic hydrophobic eutectic solvent phase, and recovering the magnetic hydrophobic eutectic solvent to obtain the microalgae grease with the extraction rate of 92.23%.
Parameter investigation
The parameters in the steps 1) to 3) of the invention are respectively examined, the extraction rate of the microalgae oil under different parameters is measured, the result of examining a certain parameter is shown in table 1, and the unchanged parameters are the same as the parameters in the example 1.
TABLE 1 examination of various parameters in step S1
The table shows that the water content, the extraction voltage, the extraction time and the like have obvious influence on the extraction rate of the microalgae grease, and when the water content is not in the range of 20-80% and the volume ratio of the algae slurry to the magnetic hydrophobic eutectic solvent is not in the range of 1:0.3-1, the extraction rate of the microalgae grease is low due to the fact that the magnetic hydrophobic eutectic solvent is not well separated from the algae slurry or the water content greatly influences the content of the microalgae grease in the magnetic hydrophobic eutectic solvent; according to the data, the selection of the magnetic hydrophobic eutectic solvent has a remarkable influence on the extraction rate of the microalgae grease; the voltage and the extraction time of flash extraction both have obvious influence on the extraction rate, when the extraction voltage is low or the extraction time is short, the extraction rate is low due to insufficient extraction, and when the extraction voltage is too high or the extraction time is too long, the oil components in the microalgae bath mud can be broken, so that the extraction rate is influenced; the standing time also influences the extraction rate, when the standing time is short, the microalgae grease does not completely enter the magnetic hydrophobic low eutectic solvent, and when the standing time is too long, the magnetic hydrophobic low eutectic solvent is insufficiently separated from the microalgae grease, so that the extraction rate is reduced; when the magnetism of the magnetic rod is too high or too low, the extraction rate of the microalgae grease can be influenced.
Claims (1)
1. A magnetic hydrophobic eutectic solvent assisted flash extraction method for preparing microalgae oil is characterized by comprising the following steps:
1) adding microalgae mud with a certain water content into a flash extractor, and extracting for a certain time at a certain extraction voltage to obtain microalgae slurry containing microalgae grease;
2) fully and uniformly mixing the microalgae slurry containing the microalgae grease prepared in the step 1) with the magnetic hydrophobic eutectic solvent, standing, and separating a magnetic hydrophobic eutectic solvent phase;
3) adding a magnetic rod into the magnetic hydrophobic eutectic solvent phase separated in the step 2), and recovering the magnetic hydrophobic eutectic solvent to obtain microalgae grease;
the magnetic hydrophobic eutectic solvent is a mixture of DL-menthol, acetic acid and anhydrous ferric chloride in a molar ratio of 1:1:1, or a mixture of DL-menthol, pyruvic acid and anhydrous ferric chloride in a molar ratio of 1:2:1, or a mixture of DL-menthol, levulinic acid and anhydrous ferric chloride in a molar ratio of 1:1:1, or a mixture of DL-menthol, lactic acid and anhydrous ferric chloride in a molar ratio of 1:2: 1;
in the step 1), the water content of the microalgae bathing mud is 20-85 percent;
the extraction voltage in the step 1) is 40-80V;
the extraction time in the step 1) is 0.5-3 min;
the volume ratio of the microalgae slurry containing the microalgae grease to the magnetic hydrophobic eutectic solvent in the step 2) is 1: 0.3-1;
standing for 0.5-2 h;
the magnetism of the magnetic rod in the step 3) is 0.5-1.5T.
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