CN114507561B - Method for extracting grease from microalgae - Google Patents
Method for extracting grease from microalgae Download PDFInfo
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- CN114507561B CN114507561B CN202011286917.4A CN202011286917A CN114507561B CN 114507561 B CN114507561 B CN 114507561B CN 202011286917 A CN202011286917 A CN 202011286917A CN 114507561 B CN114507561 B CN 114507561B
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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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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/02—Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
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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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- Preparation Of Compounds By Using Micro-Organisms (AREA)
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Abstract
The invention discloses a method for extracting grease from microalgae, which comprises the following steps: 1) Extruding, puffing and granulating: extruding and puffing the microalgae powder to obtain puffed algae powder particles composed of wall-broken microalgae powder; 2) Solvent extraction: extracting the puffed algae powder particles obtained in the step 1) by using a solvent to obtain mixed oil containing the solvent and microalgae grease and microalgae meal; 3) And removing the solvent from the mixed oil and the microalgae meal through evaporation respectively to obtain microalgae grease and microalgae meal. The method has simple process and low energy consumption.
Description
Technical Field
The invention belongs to the field of deep processing of microalgae, and relates to a method for efficiently extracting microalgae grease from microalgae. In particular to a method for processing microalgae powder by extrusion and puffing and realizing granulation at the same time, which is convenient for microalgae grease extraction, effectively improves the extraction rate of the microalgae grease and obtains high-quality microalgae meal.
Background
Microalgae can utilize sunlight, water and CO 2 Synthesizing the self-substance. The microalgae has the characteristics of short cell cycle, easiness for large-scale culture, adaptability to various growth environments, extremely high grease content and the like. In recent years, a plurality of microalgae varieties rich in fatty acid, in particular EPA and DHA rich in highly unsaturated fatty acid, such as chlorella, pseudomicroalgae, scenedesmus and the like, are reported successively, and the development of algae-based edible oil resources is possible. It is counted that the oil produced by microalgae per hectare is about 20 times that produced by oil-rich plants such as palm and jatropha, so that the oil production by microalgae has a wide application prospect.
Microalgae grease mainly contains glyceride, has a fatty acid composition similar to that of vegetable oil, and contains polyunsaturated fatty acid with great health value. The microalgae cells are small, the cell walls are tough, the oil is wrapped in the cells, and the traditional oil squeezing method is not suitable for microalgae oil extraction. Microalgae grease is mainly composed of triglyceride, glycolipid and phospholipid, wherein the triglyceride is generally present in cytoplasm, while the glycolipid and phospholipid are generally present in membrane structure, and if solvent extraction is adopted, solvent penetration into cells is required to extract (extract) the grease. However, the presence of a hard cell wall on the outer layer of microalgae prevents penetration of the solvent and dissolution of microalgae intracellular material. For example, without damaging the cell wall, the extraction rate of about 40% can be obtained by soaking nannochloropsis with a nonpolar solvent for 12 hours. Therefore, various methods are needed to perform the wall breaking pretreatment, so as to promote the infiltration of the solvent and the dissolution or release of intracellular grease and other substances.
The algae meal obtained after the microalgae is extracted by grease contains rich proteins, has complete amino acid types and balanced proportion, and can be used as an ideal protein source for people. Therefore, the pretreatment and extraction processes should fully consider the quality of the microalgae meal.
In chinese patent applications CN200810240949, 201010110577, 200610130601, 200910225296 and 201910908237 for breaking wall of microalgae, physical methods such as steam wall breaking, ultra-high voltage pulse electric field, ultrasonic, high-pressure homogenization and high-pressure jet flow are adopted to break wall of microalgae respectively, but the problems of high cost, high energy consumption, difficulty in industrial amplification and the like exist. The chemical method generally refers to breaking the wall by strong acid and alkali, and a large amount of waste liquid is inevitably brought, for example, 0.5mol/L nitric acid is adopted in the extraction of the pseudo-microalgae grease, and the good wall breaking effect is obtained only by heating at 120 ℃ for 30min (Bioresource Technology 172 (2014) 138-142). The enzymolysis method has good effect, but causes serious emulsification, needs demulsification treatment and is difficult to industrialize (J. Agric. Food chem.2012,60, 11771-11776).
The Chinese patent with the application number of CN200910085128.1 refers to an extrusion method for oil crops, adopts an extrusion mode to pretreat oil-producing rhodotorula glutinis, oil-producing chlorella, oil-producing spiral seaweed, oil-producing oleaginous yeast, rhodotorula gracilis, cryptococcus albus, candida albicans and the like, and is characterized in that: tempering is carried out in a drying link before puffing the microbial raw material, namely, the moisture is adjusted to 7-12%, and the temperature of the raw material in the tempering process is 80-90 ℃; heating the material in the puffing process, wherein the temperature of the material in the puffing process is 110-145 ℃; the whole pretreatment process has high energy consumption. Even so, the raw materials are leached out by No. 6 solvent after puffing, and the extraction time is still about 1 hour. The algae meal after oil extraction has high protein content, but the protein solubility is questionable (not described in the original application, according to common sense, the protein is inactivated under the action of the temperature and time).
The Chinese patent with the application number of CN201110375595 is characterized in that the algae powder is granulated by adding an adhesive, and further stir-fried to break the wall, but the stir-frying process needs higher temperature, so that the surface of the algae powder is easy to carbonize, and the quality of the leached oil is affected. On the other hand, the frying temperature is high, the time is long, the protein in the algae meal is seriously denatured, and the energy consumption in the frying process is high.
In summary, the extraction of oil from microalgae generally requires a variety of methods to perform wall breaking pretreatment and promote release of intracellular compounds. The existing mature methods such as high-pressure homogenization and the like have large treatment capacity but high energy consumption, and the enzymolysis method and the like have good effects but difficult industrialization. Therefore, a wall breaking pretreatment method which has low energy consumption and is easy to be applied industrially needs to be developed. Other methods of extraction of oils, e.g. supercritical CO 2 The extraction method, subcritical extraction method, ultrasonic wave or microwave assisted extraction method and the like can avoid the cell wall breaking step, but the new problems are high extraction operation pressure, high equipment requirement or high energy consumption.
Disclosure of Invention
The invention aims to provide a method for extracting grease from microalgae, which has simple process and low energy consumption.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a method of extracting grease from microalgae, the method comprising the steps of:
1) Extruding, puffing and granulating:
extruding and puffing the microalgae powder with the water content less than or equal to 6% to obtain puffed algae powder particles composed of wall-broken microalgae powder;
2) Solvent extraction:
extracting the puffed algae powder particles obtained in the step 1) by using a solvent to obtain mixed oil containing the solvent and microalgae grease and microalgae meal;
3) And removing the solvent from the mixed oil and the microalgae meal through evaporation respectively to obtain microalgae grease and microalgae meal.
Preferably, the microalgae species include one or more of Phaeodactylum, chaetoceros, chlorella, nannochloropsis, scenedesmus, crypthecodinium, golden algae, schizochytrium, haematococcus and Dunaliella.
Preferably, the extrusion conditions are: the puffing pressure is 2-8 MPa, heating is not carried out in the extrusion puffing process, and the residence time of the microalgae powder is less than or equal to 10 seconds.
Preferably, the length of the puffed algae powder particles is 2-10mm.
Preferably, the solvent is one or more of n-hexane, ethanol and isopropanol.
Preferably, in step 2), the solvent extraction temperature is from room temperature to 60 ℃, the total extraction time is from 5 to 20 minutes, and the extraction times are from 3 to 5 times.
Preferably, in the step 2), the weight ratio of the puffed algae powder particles to the solvent is 1:1-1:3.
preferably, in step 3), the evaporation conditions are: the absolute pressure is 100Pa, and the evaporation temperature is 40-60 ℃.
Specifically, the method for extracting grease from microalgae comprises the following steps.
(1) Extruding, puffing and granulating: puffing microalgae powder by extrusion puffing equipment to obtain porous and molded puffed algae powder particles composed of broken wall algae powder.
(2) Solvent extraction (leaching): extracting the puffed algae powder particles obtained in the step (1) by using a solvent to obtain mixed oil containing the solvent and the microalgae grease and microalgae meal containing the solvent.
The microalgae powder is prepared by concentrating and dehydrating microalgae liquid to obtain wet algae mud, and further drying the wet algae mud to obtain the microalgae powder with the water content of less than 6%.
The mixed oil containing the solvent and the microalgae grease can be used for removing the solvent in the mixed oil by evaporation to obtain the microalgae grease. Wherein the solvent removed by evaporation can be recovered and recycled.
The solvent in the microalgae meal can be removed by evaporation, so that the solvent-free microalgae meal is obtained. The microalgae meal can be further used for preparing feed or extracting proteins and other compounds.
The microalgae provided by the invention comprise microalgae cultivated in a photoautotrophic or heterotrophic or photoautotrophic-heterotrophic mixed cultivation mode; the microalgae species include Phaeodactylum, chaetoceros, chlorella pseudomicrocystis, scenedesmus, crypthecodinium, golden algae, schizochytrium, haematococcus and Dunaliella; the microalgae powder is one or a mixture of more than two of the algae species.
The extrusion equipment comprises, but is not limited to, a screw extrusion machine; the operation conditions are as follows: the puffing pressure is 2-8 MPa, the whole extrusion puffing process is not heated, and the residence time of the microalgae powder is not more than 10 seconds. The microalgae powder is extruded and puffed to naturally form porous and molded puffed algae powder particles with the length of 2-10mm.
In the solvent extraction step, the solvent is a mixed solvent formed by combining one or more of normal hexane, ethanol, isopropanol and the like, the solvent extraction step is carried out at the room temperature to 60 ℃, and the contact time of the puffed algae powder particles and the solvent is 5-20min.
In the solvent extraction step of the present invention, the extraction process is repeated 3-5 times, said "times" being re-leaching with new solvent.
The method for extracting grease from microalgae powder provided by the invention has the following conditions that the solvent in the mixed oil is removed by evaporation: absolute pressure 100Pa,40-60 ℃; removing solvent to obtain algae crude oil, collecting and condensing solvent, and reusing.
The general principle of extrusion puffing pretreatment oil is as follows: the oil is extruded, sheared, rubbed and the like in the cylinder barrel of the extrusion bulking machine, so that oil cells are destroyed, mechanical friction is converted into heat energy, the temperature of the material in front of the die head is quickly increased, water vapor is evaporated, the pressure is suddenly reduced at the die plate outlet of the oil extrusion bulking machine, and the water vapor is evaporated, thereby obtaining moderately bulked material. The mechanical extrusion, friction and puffing effect can fully expose the grease in the cells, so that the leaching and desolventizing efficiency is improved. Meanwhile, the oil is not heated and cured at the front end, so that the retention time in the oil extrusion and puffing machine is shorter, and the method is very beneficial to protecting the quality of raw materials.
The proper water content of the material which is generally puffed is generally more than 10%, for example, the water content of the material is 17% in the research on the extrusion puffing characteristics of different varieties of corns in the literature, the extraction rate of rice bran oil in the research on the test of extracting rice bran oil by an extrusion pretreatment aqueous enzymatic method shows the trend of rising and then falling along with the increase of the water content of the material, when the water content is about 16%, the oil extraction rate is obviously higher, and when the water content is too high or too low, the extraction rate is lower, so the water content level is 11-19%. The water content of the materials in Chinese patent CN101560440A, a preparation method of microbial oil, is 7-12%. The reason why it is generally required to maintain a high moisture content (higher than 10%) of the material is that when the moisture content of the material is too low, the power of instantaneous evaporation of the water vapor in the extruded blasting stage is insufficient, so that the puffing effect is low, and even caking occurs due to difficult discharging.
However, the invention discovers that although the microalgae raw material has low water content, the material is not easy to agglomerate and gelatinize due to low starch substance content. In the puffing process, water in cells can be gasified instantly, the cell walls of microalgae are hard, and water vapor can be sealed in the cells, so that the water vapor is accumulated in the cells and causes the cell walls to crack, and a good wall breaking effect is achieved. Compared with the conventional puffing method in the literature, the puffing process of the low-water-content raw material is short in time, low in required energy consumption and low in protein denaturation degree.
Compared with the prior art in the field, the invention has the following advantages:
(1) The invention realizes that the low-moisture algae powder can be puffed without tempering by adjusting the water content, and greatly simplifies the process of extrusion puffing pretreatment of the microalgae powder.
(2) The invention realizes the granulation of microalgae powder while breaking the wall. The individual algae powder cells are very small, and separation of the extraction solvent from the algae cells is difficult to realize by adopting a traditional method. In the invention, after extrusion and puffing, the microalgae powder is changed into porous and molded puffed algae powder particles composed of broken microalgae cells. After the extraction is finished, the separation of algae powder particles and the solvent can be realized by adopting a common screen (more than 400 meshes), so that the content of algae powder residues in the mixed oil is reduced.
(3) According to the invention, after extrusion and puffing, the microalgae powder is changed into porous and molded puffed algae powder particles composed of wall-broken algae powder, so that the flow of a solvent among particles, the diffusion in the pores of the particles and the infiltration in cells are facilitated, the extraction process of microalgae grease is greatly accelerated, and the high extraction rate is obtained. The extraction rate of the total lipid in the wall-broken parachloropsis is 60% in 5min by taking the n-hexane ethanol as an extraction solvent, and the extraction rate of the total lipid in the wall-broken spray-dried parachloropsis powder in 5min is only 10% and can reach 40% in 360 min.
(4) The microalgae powder has low wall breaking energy consumption. The energy consumption is less than 1kWh/kg, and is lower than that of various microalgae wall breaking methods summarized in the literature, for example, the ultrasonic wall breaking energy consumption is 132MJ/kg (about 36 kWh/kg), the energy consumption of a hydrodynamic cavitation method and a microwave method which are relatively low in energy consumption is about 33MJ/kg and 9.6MJ/kg, and the nuclear power consumption is about 9.2kWh/kg and 2.7kWh/kg (Biomass and bioenergy (2012) 89-101).
(5) The invention uses the extrusion puffing pretreatment thought of the traditional oil crops, not only fully utilizes the instant pressure reduction in the puffing process and has good wall breaking effect, but also avoids the degradation of the quality of grease and meal caused by the cooking and curing processes in the traditional oil puffing process, and obtains the microalgae meal with good quality. The algae meal has high content of soluble protein and the nitrogen solubility index of the algae meal is 0.7-0.8.
Detailed Description
The present invention will be described in more detail with reference to examples. It should be noted that the description and examples are intended to facilitate an understanding of the invention and are not intended to limit the invention. The protection scope of the invention is subject to the claims.
In the present invention, percent "%" is by weight unless otherwise specified.
The drying equipment used in the examples was a spray dryer model MDR-600 and the manufacturer was modern drying equipment Co.Ltd. The chemical reagents used in the examples are all commercially available.
The method for evaluating the extraction rate of the microalgae grease comprises the following steps:
in the present invention, "oil extraction rate" is used to indicate the efficiency of oil extraction from microalgae. Specifically, the extraction rate is calculated by the following formula:
oil extraction rate= (amount of oil extracted/total amount of oil in microalgae) ×100%;
wherein the amount of extracted oil is the amount of oil extracted from the mixed oil by evaporation in step (c). The total amount of oil is the amount of oil originally present in the microalgae. They all measured their fatty acid content by gas chromatography and further converted to the amount of oil in terms of triglycerides.
The process is as follows:
about 50mg of sample was taken and 2mL of 2% NaOH/CH was added 3 OH solution, 0.1mL of 1 mg/mL undecyl triglyceride was added as an internal standard, and the mixture was water-bath at 80℃for 2h. Then 1.75ml of 14% BF was added 3 /CH 3 The OH solution was cooled rapidly to room temperature after continuing the water bath for 10min. Then 1mL of chromatographically pure hexane was added, followed by shaking, and 2mL of saturated NaCl solution was added. The mixture was centrifuged to separate the phases, and the n-hexane phase was filtered through a 0.22 μm membrane and loaded. The method is used for measuring the oil content in microalgae by using a gas chromatograph and an Agilent 7890GC-FID gas chromatograph. The oil content in the crude oil is multiplied by the weight of the crude oil to obtain the extracted oil content.
Gas chromatography conditions: the Agilent 7820A gas chromatograph is equipped with a chromatographic column DB-23, the temperature of a sample injector is 250 ℃, the temperature of an FID detector is 280 ℃, the carrier gas is nitrogen, the flow rate is 1mL/min, the tail blowing flow rate is 25mL/min, the hydrogen flow rate is 40mL/min, and the air flow rate is 400mL/min. The temperature program was maintained from 70℃for 1min, then 4℃per min to 185℃and then 1.5℃per min to 230℃and for 1min. The content of each fatty acid methyl ester was calculated from the ratio of Fatty Acid Methyl Ester (FAME) peak area to internal standard peak area. The absolute content of each component is calculated by the lipid conversion coefficient. The oil content in microalgae is calculated based on triglyceride content.
Example 1
The method of the invention is used for processing the algae powder obtained after harvesting and drying the pseudo-microcystis (Nannochloropsis sp.) and sequentially comprises the following steps:
(1) Spray drying to obtain microalgae powder with water content of 5%;
(2) The dry microalgae powder is directly fed into a double-screw extrusion and puffing machine through a feeding device, the temperature of the three sections of the puffing machine is controlled, the extrusion and puffing process is not heated, the model of the double-screw extrusion and puffing machine is adopted, and the manufacturer is Jinan Lin Yang mechanical Co.
(3) Leaching, cooling the puffed oil to 60 ℃, and spraying and soaking with n-hexane solvent. The leaching time is 10min. Separating the mixed oil and the leached algae meal.
(4) Removing impurities, and filtering and removing impurities from the mixed oil.
(5) The mixed oil is vacuum desolventized at 60 ℃ to obtain the microalgae grease, and the grease extraction rate is 85%.
(6) The algae meal is desolventized, the algae meal is desolventized in vacuum at 60 ℃ to obtain the microalgae meal with residual solution less than 0.05wt% and nitrogen dissolution index of 0.78.
Example 2
The method of the invention is used for processing the algae powder obtained after harvesting and drying the pseudo-microcystis (Nannochloropsis sp.) and sequentially comprises the following steps:
(1) Spray drying to obtain microalgae powder with water content of 2%.
(2) The dry microalgae powder is directly fed into a double-screw extrusion puffing machine through a feeding device, the temperature of the three sections of the puffing machine is controlled, and the puffing machine is not heated, the model of the double-screw extrusion puffing machine is LY32-II, and the manufacturer is Jinan Lin Yang mechanical Co.
(3) Leaching, cooling the puffed oil to 60 ℃, and spraying and soaking with n-hexane solvent. The leaching time is 10min. Separating the mixed oil and the leached algae meal.
(4) Removing impurities, and filtering and removing impurities from the mixed oil.
(5) The mixed oil is vacuum desolventized at 60 ℃ to obtain the microalgae grease, and the grease extraction rate is 87%.
(6) The algae meal is desolventized, the algae meal is desolventized in vacuum at 60 ℃ to obtain the microalgae meal with residual solution less than 0.05wt% and nitrogen dissolution index of 0.79.
Example 3
The method of the invention processes the algae powder obtained after harvesting and drying Chlorella (Chlorella sp.) as follows:
(1) Spray drying to obtain microalgae powder with water content of 4%.
(2) The dry microalgae powder is directly fed into a double-screw extrusion and puffing machine through a feeding device, the temperature of the three sections of the puffing machine is controlled, the extrusion and puffing process is not carried out, the model of the double-screw extrusion and puffing machine is LY32-II, and the manufacturer is Jinan Lin Yang mechanical Co.
(3) Leaching, cooling the puffed oil to 60 ℃, and spraying and soaking with n-hexane solvent. The leaching time is 30min. Separating the mixed oil and the leached algae meal.
(4) Removing impurities, and filtering and removing impurities from the mixed oil.
(5) The mixed oil is vacuum desolventized at 60 ℃ to obtain the microalgae grease, and the grease extraction rate is 88%.
(6) The algae meal is desolventized, the algae meal is desolventized in vacuum at 60 ℃ to obtain the microalgae meal with residual solution less than 0.05wt% and nitrogen dissolution index of 0.76.
Example 4
The method of the invention is used for processing the algae powder obtained after the Schizochytrium sp is collected and dried, and the steps are as follows:
(1) Spray drying to obtain microalgae powder with water content of 3%.
(2) Extruding and puffing, namely feeding the dry microalgae powder into a double-screw extruding and puffing machine directly through a feeding device, controlling the temperature of the three sections of the puffing machine, and heating in the extruding and puffing process. The model of the twin-screw extrusion bulking machine is LY32-II, and the manufacturer is Jinan Lin Yang mechanical Co.
(3) Leaching, cooling the puffed oil to 60 ℃, and spraying and soaking with a mixed solvent of n-hexane and ethanol. The leaching time is 10min. Separating the mixed oil and the leached algae meal.
(4) Removing impurities, and filtering and removing impurities from the mixed oil.
(5) The mixed oil is vacuum desolventized at 60 ℃ to obtain the microalgae grease, and the grease extraction rate is 92%.
(6) Desolventizing, vacuum desolventizing at 60 ℃ to obtain microalgae meal with residual solution lower than 0.05wt% and nitrogen dissolution index of 0.70.
Example 5
The method of the invention is used for processing the algae powder obtained after harvesting and drying the pseudo-microcystis (Nannochloropsis sp.) and sequentially comprises the following steps:
(1) Spray drying to obtain microalgae powder with water content of 6%.
(2) Extruding and puffing, namely feeding the dry microalgae powder into a double-screw extruding and puffing machine directly through a feeding device, controlling the temperature of the three sections of the puffing machine, and heating in the extruding and puffing process. The model of the twin-screw extrusion bulking machine is LY32-II, and the manufacturer is Jinan Lin Yang mechanical Co.
(3) Leaching, cooling the puffed oil to 60 ℃, and spraying and soaking with a mixed solvent of n-hexane and ethanol. The leaching time is 10min. Separating the mixed oil and the leached algae meal.
(4) Removing impurities, and filtering and removing impurities from the mixed oil.
(5) The mixed oil is vacuum desolventized at 60 ℃ to obtain the microalgae grease, and the grease extraction rate is 93%.
(6) Desolventizing, vacuum desolventizing at 60 ℃ to obtain microalgae meal with residual solution lower than 0.05wt% and nitrogen dissolution index of 0.72.
Comparative example 1
(1) Spray drying to obtain microalgae powder with water content of 15%.
(2) Extruding and puffing, namely feeding the dry microalgae powder into a double-screw extruding and puffing machine directly through a feeding device, wherein the temperature of the puffing machine is controlled in three sections, the temperature of the first section is 50 ℃, the temperature of the second section is 80 ℃, and the temperature of the third section is 110 ℃. The model of the twin-screw extrusion bulking machine is LY32-II, and the manufacturer is Jinan Lin Yang mechanical Co.
(3) Leaching, cooling the puffed oil to 60 ℃, and spraying and soaking with n-hexane solvent. The leaching time is 10min. Separating the mixed oil and the leached algae meal.
(4) Removing impurities, and filtering and removing impurities from the mixed oil.
(5) The mixed oil is vacuum desolventized at 60 ℃ to obtain the microalgae grease, and the grease extraction rate is 15%.
(6) Desolventizing, vacuum desolventizing at 60 ℃ to obtain microalgae meal with residual solution lower than 0.05wt% and nitrogen dissolution index of 0.65.
Comparative example 2
(1) Spray drying to obtain microalgae powder with water content of 12%.
(2) Extruding and puffing, namely feeding the dry microalgae powder into a double-screw extruding and puffing machine directly through a feeding device, wherein the temperature of the puffing machine is controlled in three sections, the temperature of the first section is 50 ℃, the temperature of the second section is 80 ℃, and the temperature of the third section is 110 ℃. The model of the twin-screw extrusion bulking machine is LY32-II, and the manufacturer is Jinan Lin Yang mechanical Co.
(3) Leaching, cooling the puffed oil to 60 ℃, and spraying and soaking with n-hexane solvent. Leaching time is 1h. Separating the mixed oil and the leached algae meal.
(4) Removing impurities, and filtering and removing impurities from the mixed oil.
(5) The mixed oil is vacuum desolventized at 60 ℃ to obtain the microalgae grease, and the grease extraction rate is 21%.
(6) Desolventizing, vacuum desolventizing at 60 ℃ to obtain microalgae meal with residual solution lower than 0.05wt% and nitrogen dissolution index of 0.68.
Comparative example 3
(1) Spray drying to obtain microalgae powder with water content of 10%.
(2) Extruding and puffing, namely feeding the dry microalgae powder into a double-screw extruding and puffing machine directly through a feeding device, wherein the temperature of the puffing machine is controlled in three sections, the temperature of the first section is 50 ℃, the temperature of the second section is 80 ℃, and the temperature of the third section is 110 ℃. The model of the twin-screw extrusion bulking machine is LY32-II, and the manufacturer is Jinan Lin Yang mechanical Co.
(3) Leaching, cooling the puffed oil to 60 ℃, and spraying and soaking with n-hexane ethanol solvent. Leaching time is 1h. Separating the mixed oil and the leached algae meal.
(4) Removing impurities, and filtering and removing impurities from the mixed oil.
(5) The mixed oil is vacuum desolventized at 60 ℃ to obtain the microalgae grease, and the grease extraction rate is 40%.
(6) Desolventizing, vacuum desolventizing the algae-containing meal at 60 ℃ to obtain microalgae grease, and obtaining microalgae meal with residual solution lower than 0.05wt% and nitrogen dissolution index of 0.51.
As can be seen from the above examples, compared with the microalgae raw material obtained by extrusion and puffing in the prior art, the microalgae cake obtained by the extrusion and puffing method has the advantages of no tempering and heating in the puffing process, greatly shortened microalgae oil extraction process, improved oil rate, low energy consumption, good quality of the obtained microalgae cake and high utilization value.
The method can be realized by the upper and lower limit values of the interval and the interval value of the process parameters (such as temperature, time and the like), and the examples are not necessarily listed here.
The invention may be practiced without these specific details, using any knowledge known in the art.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and are not limiting. Although the present invention has been described in detail with reference to the embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the present invention, which is intended to be covered by the appended claims.
Claims (7)
1. A method of extracting grease from microalgae, the method comprising the steps of:
1) Extruding, puffing and granulating:
extruding and puffing the microalgae powder with the water content less than or equal to 6% to obtain puffed algae powder particles composed of wall-broken microalgae powder;
2) Solvent extraction:
extracting the puffed algae powder particles obtained in the step 1) by using a solvent to obtain mixed oil containing the solvent and microalgae grease and microalgae meal; the solvent is one or more of n-hexane, ethanol and isopropanol;
3) And removing the solvent from the mixed oil and the microalgae meal through evaporation respectively to obtain microalgae grease and microalgae meal.
2. The method of extracting oil from microalgae according to claim 1, characterized in that the algae species of the microalgae comprise one or more of phaeodactylum algae, chaetoceros, chlorella, pseudomicrocystis, scenedesmus, cryptodinoflagellate, chrysophyte, schizochytrium, rhodococcus and dunaliella.
3. The method for extracting oil from microalgae according to claim 1, characterized in that the extrusion conditions are as follows: the puffing pressure is 2-8 MPa, and the residence time of the microalgae powder is less than or equal to 10 seconds.
4. The method of extracting oil from microalgae according to claim 1, characterized in that the length of the puffed algae powder particles is 2-10mm.
5. The method for extracting oil from microalgae according to claim 1, wherein in the step 2), the solvent extraction temperature is room temperature to 60 ℃, the total extraction time is 5-20min, and the extraction times are 3-5 times.
6. The method for extracting oil from microalgae according to claim 1, characterized in that in step 2), the weight ratio of the puffed algae powder particles to the solvent is 1:1-1:3.
7. the method for extracting oil from microalgae according to claim 1, wherein in the step 3), the evaporation conditions are as follows: the absolute pressure is 100Pa, and the evaporation temperature is 40-60 ℃.
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