CN114507561A - Method for extracting grease from microalgae - Google Patents
Method for extracting grease from microalgae Download PDFInfo
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- CN114507561A CN114507561A CN202011286917.4A CN202011286917A CN114507561A CN 114507561 A CN114507561 A CN 114507561A CN 202011286917 A CN202011286917 A CN 202011286917A CN 114507561 A CN114507561 A CN 114507561A
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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
-
- 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
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 consisting 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 (3) respectively evaporating the mixed oil and the microalgae meal to remove the solvent to obtain microalgae oil 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 oil from microalgae. In particular to a method for treating microalgae powder by extrusion and puffing and realizing granulation, which is convenient for extracting microalgae grease, effectively improves the extraction rate of the microalgae grease and simultaneously obtains high-quality microalgae meal.
Background
The microalgae can utilize sunlight, water and CO2Synthesizing the self substance. The microalgae has the characteristics of short cell cycle, easy large-scale culture, adaptability to various growth environments, extremely high oil content and the like. In recent years, a plurality of microalgae varieties rich in fatty acid are successively reported, particularly microalgae varieties rich in high unsaturated fatty acid EPA and DHA and the like, such as chlorella, microspheric algae, scenedesmus and the like, which are used as algae-based edible oil resourcesDevelopment is possible. According to statistics, the oil produced by microalgae per hectare per year is about 20 times of that of oil-rich plants such as palm and jatropha curcas, so that the oil produced by microalgae has wide application prospect.
The microalgae oil and fat mainly comprises glyceride, the fatty acid composition is similar to that of vegetable oil, and some microalgae oil and fat also contain polyunsaturated fatty acid with high health value. Microalgae cells are small, cell walls are tough, oil is wrapped in the cells, and the traditional oil squeezing method is not suitable for extracting the microalgae oil. Microalgae oil is mainly composed of triglyceride, glycolipid and phospholipid, triglyceride is generally present in cytoplasm, glycolipid and phospholipid are mostly present in membrane structure, and if solvent extraction is adopted, solvent permeation into cells is required to extract (extract) oil. However, the outer layer of microalgae has a hard cell wall, which prevents penetration of the solvent and dissolution of microalgae intracellular material. For example, about 40% extraction can be obtained by soaking nannochloropsis with a nonpolar solvent for 12 hours without damaging the cell walls. Therefore, various methods are required for wall-breaking pretreatment to promote the penetration of solvents and the dissolution or release of intracellular lipids and other substances.
The algae meal obtained after the microalgae is extracted by the grease contains rich protein, has complete amino acid types and balanced proportion, and can be used as an ideal protein source for people. Therefore, the quality of the microalgae meal should be fully considered in the pretreatment and extraction processes.
In chinese patent applications CN200810240949, 201010110577, 200610130601, 200910225296, and 201910908237 relating to wall breaking of microalgae, physical methods such as steam wall breaking, ultra-high voltage pulsed electric field, ultrasound, high-pressure homogenization, and high-pressure jet are respectively adopted to wall breaking of microalgae, but all have the problems of high cost, high energy consumption, and difficulty in industrial amplification. The chemical method generally refers to breaking walls with strong acid and strong alkali, which inevitably brings a large amount of waste liquid, for example, extraction of Micrococcus sp grease adopts 0.5mol/L nitric acid, and heating is performed at 120 ℃ for 30min to obtain a better wall-breaking effect (Bioresource Technology 172(2014) 138-. The enzymolysis method and the like have good effects, but cause serious emulsification, require demulsification treatment and are difficult to industrialize (J.Agric.food chem.2012,60, 11771-11776).
Chinese patent with application number CN200910085128.1 refers to an extrusion method for oil crops, which uses an extrusion method to pretreat oil-producing rhodotorula glutinis, oil-producing chlorella, oil-producing spirulina platensis, oil-producing yeast, grease yeast sdalei, torulopsis pinicola, cryptococcus albidus, candida albicans, etc., and is characterized in that: tempering is carried out in a drying link before the microbial raw material is puffed, namely, the water content is adjusted to 7-12%, and the raw material temperature in the tempering process is 80-90 ℃; heating the materials in the expansion process, wherein the temperature of the materials in the expansion process is 110-; the energy consumption of the whole pretreatment process is high. Even if the raw material is puffed and then leached by the No. 6 solvent, the extraction time still needs about 1 hour. The protein content of the algae meal after the oil extraction is higher, but the solubility of the protein is uncertain (not explained in the original application, the protein is inactivated under the action of the temperature and the time according to the common knowledge).
Chinese patent with application number CN201110375595 granulates algae powder by adding adhesive, and further fries to break the wall, but the process of frying requires higher temperature, resulting in easy carbonization of the surface of algae particles, affecting the quality of the oil. On the other hand, the stir-frying temperature is high, the stir-frying time is long, protein in the algae meal is seriously denatured, and the energy consumption in the stir-frying process is high.
In summary, extraction of oil from microalgae usually requires wall-breaking pretreatment by various methods to promote release of intracellular compounds. However, 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, the development of a wall-breaking pretreatment method with low energy consumption and easy industrial application is required. Other methods of extracting fats and oils, e.g. supercritical CO2The extraction method, the subcritical extraction method, the ultrasonic or microwave-assisted extraction method and the like can avoid the cell wall breaking step, but introduce new problems of high extraction operation pressure, high requirements on equipment or high energy consumption.
Disclosure of Invention
The invention aims to provide a method for extracting oil from microalgae, which has simple process and low energy consumption.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method of extracting oil from microalgae, the method comprising the steps of:
1) extruding, puffing and granulating:
extruding and puffing microalgae powder with the water content of less than or equal to 6% to obtain puffed algae powder granules consisting 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 (3) respectively evaporating the mixed oil and the microalgae meal to remove the solvent to obtain microalgae oil and microalgae meal.
Preferably, the algal species of the microalgae comprise one or more of phaeodactylum, chaetoceros, chlorella, nannochloropsis, scenedesmus, crypthecodinium, chrysophyceae, schizochytrium, haematococcus and dunaliella.
Preferably, the extrusion puffing conditions are: the puffing pressure is 2-8 MPa, heating is not carried out in the extrusion puffing process, and the retention time of the microalgae powder is less than or equal to 10 seconds.
Preferably, the length of the expanded algae powder particles is 2-10 mm.
Preferably, the solvent is one or more of n-hexane, ethanol and isopropanol.
Preferably, in the step 2), the solvent extraction temperature is between room temperature and 60 ℃, the total extraction time is 5-20min, and the extraction times are 3-5.
Preferably, in the step 2), the weight ratio of the expanded algae powder particles to the solvent is 1: 1-1: 3.
preferably, in step 3), the evaporation conditions are as follows: absolute pressure 100Pa and evaporating temperature 40-60 deg.C.
Specifically, the method for extracting the grease from the microalgae comprises the following steps.
(1) Extruding, puffing and granulating: puffing the microalgae powder by an extrusion puffing device to obtain porous and molded puffed algae powder particles consisting of wall-broken 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 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 below 6%.
The mixed oil containing the solvent and the microalgae grease can remove the solvent in the mixed oil through 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 through evaporation, and solvent-free microalgae meal is obtained. The microalgae meal can be further used for preparing feed or extracting protein and other compounds.
The microalgae comprises microalgae obtained by photoautotrophic, heterotrophic or photoautotrophic-heterotrophic mixed culture; the microalgae species include Phaeodactylum, Chaetoceros, Chlorella, Chlorococcus, Scenedesmus, Crypthecodinium, Chrysophytum, Schizochytrium, Haematococcus, and Dunaliella; the microalgae powder is one or a mixture of more than two of the algae.
The extrusion puffing equipment comprises but is not limited to a screw extrusion puffing machine; the operating conditions are as follows: the puffing pressure is 2-8 MPa, the whole extrusion and puffing process is not heated, and the retention 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 2-10 mm.
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 room temperature to 60 ℃, and the contact time of the expanded algae powder particles and the solvent is 5-20 min.
In the solvent extraction step of the invention, the extraction process is repeated 3-5 times, wherein the extraction process is repeated for 'times' by using new solvent for secondary extraction.
The method for extracting the grease from the microalgae powder comprises the following conditions of evaporating and removing the solvent in the mixed oil: absolute pressure 100Pa, 40-60 ℃; removing solvent to obtain crude algae oil, and collecting and condensing the solvent for reuse.
The general principle of the extrusion and expansion pretreatment of oil materials is as follows: the oil material is extruded, sheared, kneaded and the like in the cylinder barrel of the extrusion puffing machine, so that oil material cells are destroyed, mechanical friction is converted into heat energy, the material in front of a die head is rapidly heated, water vapor is evaporated, pressure is suddenly reduced at the outlet of a template of the oil material extrusion puffing machine, and the water vapor is evaporated, so that the properly puffed material is obtained. Because the mechanical extrusion, friction and expansion function fully expose intracellular grease, the leaching and desolventizing efficiency is improved. Meanwhile, as the oil is not heated and cured at the front end, the retention time in the oil extrusion-expansion machine is short, which is very favorable for protecting the quality of the raw materials.
The proper water content of materials subjected to puffing is generally more than 10%, for example, the feed water content in the literature, namely the research on the extrusion and puffing characteristics of different varieties of corns, is 17%, the extraction rate of rice bran oil in the research on the experimental study on the extraction of the rice bran oil by the water enzyme method for the extrusion and puffing pretreatment shows a trend of rising firstly and then falling along with the increase of the water content of the materials, 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 that the water content level is selected from 11% to 19%. In Chinese patent CN101560440A, a preparation method of microbial oil, the water content of the material is 7-12%. The reason why the higher water content (higher than 10%) of the material is generally needed is that when the water content of the material is too low, the power of the instantaneous evaporation of water vapor in the extrusion blasting section is not enough, so that the puffing effect is lower, and even the material is hard to discharge and is blocked.
However, the invention finds that although the microalgae raw material has low water content, the material is not easy to agglomerate and gelatinize due to the low content of starch substances. During the expansion process, water in the cells can be instantly gasified, and the cell walls of the microalgae are hard, so that water vapor can be just sealed in the cells, the water vapor is accumulated in the cells, the cell walls are cracked, and a good wall breaking effect is achieved. Compared with the conventional puffing method in the literature, the puffing process time of the raw material with low water content is short, the required energy consumption is low, and the protein denaturation degree is low.
Compared with the prior art in the field, the invention has the advantages that:
(1) the invention realizes the puffing of the low-moisture algae powder without conditioning by adjusting the water content, and greatly simplifies the process of pretreating the microalgae algae powder by extrusion puffing.
(2) The invention realizes the granulation of the microalgae powder while breaking the wall. The individual algae powder cells are very small, and the separation of the extraction solvent and the algae cells is difficult to realize by adopting the traditional method. In the invention, microalgae powder is extruded and puffed to form porous and molded puffed algae powder particles consisting of wall-broken microalgae cells. After extraction, the separation of algae powder particles and a solvent can be realized by adopting a common screen (larger than 400 meshes), and the content of algae powder residues in the mixed oil is reduced.
(3) In the invention, the microalgae powder is extruded and puffed to form porous and molded puffed algae powder particles formed by wall-broken algae powder, so that the flowing of a solvent among the particles, the diffusion in particle pores and the infiltration in cells are facilitated, the extraction process of microalgae grease is greatly accelerated, and high extraction rate is obtained. The extraction yield of the total lipids extracted from the wall-broken nannochloropsis is 60% in 5min by using normal hexane ethanol as an extraction solvent, while the extraction yield of the total lipids extracted from the wall-broken nannochloropsis sprayed and dried nannochloropsis is only 10% in 5min, and can reach 40% in 360 min.
(4) The wall breaking energy consumption of the microalgae powder is low. The energy consumption is less than 1kWh/kg, and is lower than that of various microalgae wall breaking methods summarized in the literature, such as the ultrasonic wall breaking energy consumption is 132MJ/kg (approximately equal to 36kWh/kg), the energy consumption of a hydrodynamic cavitation method and a microwave method with relatively low energy consumption is about 33MJ/kg and 9.6MJ/kg, and the accounting power consumption is about 9.2kWh/kg and 2.7kWh/kg (Biomass and bioenergy 46(2012) 89-101).
(5) The invention uses the traditional oil crop extrusion and puffing pretreatment thought for reference, not only makes full use of the instant reduction of pressure in the puffing process and has good wall breaking effect, but also avoids the reduction of the quality of grease and meal brought by the cooking and curing processes in the traditional oil puffing process, and obtains the microalgae meal with good quality. The content of soluble protein in the algae meal is high, 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 is to be understood that the description and examples are intended to facilitate the 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, percentages "%" are by weight unless otherwise specified.
The drying equipment used in the examples was a spray dryer model MDR-600, the manufacturer being modern drying equipment Co., Ltd. The chemicals used in the examples are all commercially available.
The microalgae oil extraction rate evaluation method comprises the following steps:
in the present invention, "oil extraction rate" is used to indicate the efficiency of extracting oil from microalgae. Specifically, the extraction rate is calculated by the following formula:
the oil extraction rate is (amount of extracted oil/total oil in microalgae) × 100%;
wherein the amount of extracted oil and fat is the amount of oil and fat 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 the fatty acid content by gas chromatography and further converted the amount of the oil or fat in terms of triglyceride.
The process is as follows:
about 50mg of sample was taken and 2mL of 2% NaOH/CH was added3OH solution, 0.1mL of 1 mg/mL undecane triglyceride was added as an internal standard, and water bath was carried out at 80 ℃ for 2 h. Then 1.75mL of 14% BF was added3/CH3And (5) continuing the water bath for 10min, and quickly cooling the OH solution to room temperature. Then 1mL of chromatographically pure n-hexane was added, shaking was carried out, and 2mL of saturated NaCl solution was added. Centrifuging, taking n-hexane phase, and filtering and loading the n-hexane phase by using a 0.22 mu m membrane. The method is used for Agilent 7890GC-FID gas chromatograph determination on gas chromatograph determination, and the oil content in the microalgae is calculated by triglyceride content. The oil content in the crude oil is multiplied by the weight of the crude oil to obtain the oilThe amount of grease taken out.
Gas chromatography conditions: an Agilent 7820A gas chromatographic analyzer is provided with a chromatographic column DB-23, a sample injector with the temperature of 250 ℃, an FID detector with the temperature of 280 ℃, a carrier gas with nitrogen, the flow rate of 1mL/min, the flow rate of a tail gas flow of 25mL/min, the flow rate of hydrogen of 40mL/min and the flow rate of air of 400 mL/min. The temperature raising program is kept for 1min from 70 ℃, then raised to 185 ℃ at 4 ℃/min, then raised to 230 ℃ at 1.5 ℃/min, and kept for 1 min. The content of each fatty acid methyl ester was calculated from the ratio of the Fatty Acid Methyl Ester (FAME) peak area to the internal standard peak area. And calculating the absolute content of each component through a lipid conversion coefficient. The oil content in the microalgae is calculated by the content of triglyceride.
Example 1
The method is used for processing the algae powder obtained after the Nannochloropsis sp is collected and dried, and the steps are as follows in sequence:
(1) spray drying to obtain microalgae powder with water content of 5%;
(2) and (3) extruding and puffing, namely directly feeding the dry microalgae powder into a double-screw extruding and puffing machine through a feeding device, controlling the temperature of the puffing machine in three sections, and not heating in the extruding and puffing process, wherein the type of the used double-screw extruding and puffing machine is that the manufacturer is Jinan forest machinery Co., Ltd.
(3) Leaching, cooling the expanded oil to 60 ℃, and spraying and soaking the expanded oil by using a normal hexane solvent. The leaching time is 10 min. Separating the mixed oil and leaching the algae meal.
(4) Removing impurities, filtering the mixed oil to remove impurities.
(5) And (3) carrying out vacuum desolventizing on the mixed oil at the temperature of 60 ℃ to obtain the microalgae oil, wherein the oil extraction rate is 85%.
(6) Desolventizing the algae meal, and vacuum desolventizing the algae meal containing the dissolved algae at 60 ℃ to obtain the microalgae meal with residual solubility of less than 0.05 wt%, wherein the nitrogen solubility index is 0.78.
Example 2
The method is used for processing the algae powder obtained after the Nannochloropsis sp is collected and dried, and the steps are as follows in sequence:
(1) spray drying to obtain microalgae powder with water content of 2%.
(2) And (3) extruding and puffing, namely directly feeding the dry microalgae powder into a double-screw extruding and puffing machine through a feeding device, controlling the temperature of the three sections of the puffing machine without heating, wherein the model of the used double-screw extruding and puffing machine is LY32-II, and the manufacturer is Jinan mechanical Limited company.
(3) Leaching, cooling the expanded oil to 60 ℃, and spraying and soaking the expanded oil by using a normal hexane solvent. The leaching time is 10 min. Separating the mixed oil and leaching the algae meal.
(4) Removing impurities, filtering the mixed oil to remove impurities.
(5) And (3) carrying out vacuum desolventizing on the mixed oil at the temperature of 60 ℃ to obtain the microalgae oil, wherein the oil extraction rate is 87%.
(6) Desolventizing the algae meal, and vacuum desolventizing the algae meal containing the dissolved algae at 60 ℃ to obtain the microalgae meal with residual solubility of less than 0.05 wt%, wherein the nitrogen solubility index is 0.79.
Example 3
The method comprises the following steps of processing the algae powder obtained after the Chlorella (Chlorella sp.) is collected and dried according to the method of the invention:
(1) spray drying to obtain microalgae powder with water content of 4%.
(2) And (3) extruding and puffing, namely directly feeding the dry microalgae powder into a double-screw extruding and puffing machine through a feeding device, controlling the temperature of the puffing machine in three sections, wherein the extruding and puffing process is not heated, the model of the used double-screw extruding and puffing machine is LY32-II, and the manufacturer is Jinan mechanical company Limited.
(3) Leaching, cooling the expanded oil to 60 ℃, and spraying and soaking the expanded oil by using a normal hexane solvent. The leaching time is 30 min. Separating the mixed oil and leaching the algae meal.
(4) Removing impurities, filtering the mixed oil to remove impurities.
(5) And (3) carrying out vacuum desolventizing on the mixed oil at 60 ℃ to obtain the microalgae oil, wherein the oil extraction rate is 88%.
(6) Desolventizing the algae meal, and vacuum desolventizing the algae meal containing the dissolved algae at 60 ℃ to obtain the microalgae meal with residual solubility of less than 0.05 wt%, wherein the nitrogen solubility index is 0.76.
Example 4
The method for processing the algae powder obtained after harvesting and drying Schizochytrium sp comprises the following steps:
(1) spray drying to obtain microalgae powder with water content of 3%.
(2) And (3) extruding and puffing, namely directly feeding the dry microalgae powder into a double-screw extruding and puffing machine through a feeding device, controlling the temperature of the three sections of the puffing machine, and not heating in the extruding and puffing process. The model of the double-screw extrusion puffing machine is LY32-II, and the manufacturer is Jinan Linyang machinery Co.
(3) Leaching, cooling the expanded oil material to 60 ℃, and spraying and soaking the expanded oil material by using a mixed solvent of n-hexane and ethanol. The leaching time is 10 min. Separating the mixed oil and leaching the algae meal.
(4) Removing impurities, filtering the mixed oil to remove impurities.
(5) And (3) carrying out vacuum desolventizing on the mixed oil at the temperature of 60 ℃ to obtain the microalgae oil, wherein the oil extraction rate is 92%.
(6) Desolventizing the dissolved algae-containing meal at 60 ℃, and performing vacuum desolventizing to obtain microalgae meal with residual solubility of less than 0.05 wt%, wherein the nitrogen solubility index is 0.70.
Example 5
The method is used for processing the algae powder obtained after the Nannochloropsis sp is collected and dried, and the steps are as follows in sequence:
(1) spray drying to obtain microalgae powder with water content of 6%.
(2) And (3) extruding and puffing, namely directly feeding the dry microalgae powder into a double-screw extruding and puffing machine through a feeding device, controlling the temperature of three sections of the puffing machine, and not heating in the extruding and puffing process. The model of the double-screw extrusion bulking machine is LY32-II, and the manufacturer is Jinan Linyang machinery Co.
(3) Leaching, cooling the expanded oil material to 60 ℃, and spraying and soaking the expanded oil material by using a mixed solvent of n-hexane and ethanol. The leaching time is 10 min. Separating the mixed oil and leaching the algae meal.
(4) Removing impurities, filtering the mixed oil to remove impurities.
(5) And (3) carrying out vacuum desolventizing on the mixed oil at the temperature of 60 ℃ to obtain the microalgae oil, wherein the oil extraction rate is 93%.
(6) Desolventizing the dissolved algae-containing meal at 60 ℃, and performing vacuum desolventizing to obtain microalgae meal with residual solubility of less than 0.05 wt%, wherein the nitrogen solubility index is 0.72.
Comparative example 1
(1) Spray drying to obtain microalgae powder with water content of 15%.
(2) Extruding and puffing, namely directly feeding the dry microalgae powder into a double-screw extruding and puffing machine 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 double-screw extrusion puffing machine is LY32-II, and the manufacturer is Jinan Linyang machinery Co.
(3) Leaching, cooling the expanded oil to 60 ℃, and spraying and soaking the expanded oil by using a normal hexane solvent. The leaching time is 10 min. Separating the mixed oil and leaching the algae meal.
(4) Removing impurities, filtering the mixed oil to remove impurities.
(5) And (3) carrying out vacuum desolventizing on the mixed oil at the temperature of 60 ℃ to obtain the microalgae oil, wherein the oil extraction rate is 15%.
(6) Desolventizing the dissolved algae-containing meal at 60 ℃, and performing vacuum desolventizing to obtain microalgae meal with residual solubility of less than 0.05 wt%, wherein the nitrogen solubility index is 0.65.
Comparative example 2
(1) Spray drying to obtain microalgae powder with water content of 12%.
(2) Extruding and puffing, namely directly feeding the dry microalgae powder into a double-screw extruding and puffing machine 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 double-screw extrusion puffing machine is LY32-II, and the manufacturer is Jinan Linyang machinery Co.
(3) Leaching, cooling the expanded oil to 60 ℃, and spraying and soaking the expanded oil by using a normal hexane solvent. The leaching time is 1 h. Separating the mixed oil and leaching the algae meal.
(4) Removing impurities, filtering the mixed oil to remove impurities.
(5) And (3) carrying out vacuum desolventizing on the mixed oil at the temperature of 60 ℃ to obtain the microalgae oil, wherein the oil extraction rate is 21%.
(6) Desolventizing the dissolved algae-containing meal at 60 ℃, and performing vacuum desolventizing to obtain microalgae meal with residual solubility of less than 0.05 wt%, wherein the nitrogen solubility index is 0.68.
Comparative example 3
(1) Spray drying to obtain microalgae powder with water content of 10%.
(2) Extruding and puffing, namely directly feeding the dry microalgae powder into a double-screw extruding and puffing machine 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 double-screw extrusion puffing machine is LY32-II, and the manufacturer is Jinan Linyang machinery Co.
(3) Leaching, cooling the expanded oil material to 60 ℃, and spraying and soaking the expanded oil material by using a normal hexane ethanol solvent. The leaching time is 1 h. Separating the mixed oil and leaching the algae meal.
(4) Removing impurities, filtering the mixed oil to remove impurities.
(5) And (3) carrying out vacuum desolventizing on the mixed oil at the temperature of 60 ℃ to obtain the microalgae oil, wherein the oil extraction rate is 40%.
(6) And (3) performing desolventizing, namely performing vacuum desolventizing on the microalgae-containing meal at the temperature of 60 ℃ to obtain microalgae oil, so as to obtain microalgae meal with residual solvent of less than 0.05 wt%, wherein the nitrogen solubility index is 0.51.
According to the embodiments, compared with the microalgae raw material obtained by adopting an extrusion puffing method in the prior art, the method disclosed by the invention has the advantages that the tempering is not carried out before the puffing, the puffing process is not heated, the microalgae oil extraction process is greatly shortened, the oil rate is improved, the energy consumption is low, and the obtained microalgae meal has good quality and high utilization value.
The method can be realized by upper and lower limit values and interval values of intervals of process parameters (such as temperature, time and the like), and embodiments are not listed.
Conventional technical knowledge in the art can be used for the details which are not described in the present invention.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and are not limited. Although the present invention has been described in detail with reference to the embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (8)
1. A method of extracting oil from microalgae, the method comprising the steps of:
1) extruding, puffing and granulating:
extruding and puffing microalgae powder with the water content of less than or equal to 6% to obtain puffed algae powder granules consisting 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 (3) respectively evaporating the mixed oil and the microalgae meal to remove the solvent to obtain microalgae oil and microalgae meal.
2. The method of claim 1, wherein the algal species of the microalgae comprise one or more of Phaeodactylum, Chaetoceros, Chlorella, Scenedesmus, Crypthecodinium, Chrysophytum, Schizochytum, Haematococcus, and Dunaliella.
3. The method for extracting oil from microalgae according to claim 1, wherein the extrusion puffing conditions are: the puffing pressure is 2-8 MPa, and the retention time of the microalgae powder is less than or equal to 10 seconds.
4. The method for extracting oil from microalgae according to claim 1, wherein the expanded algae meal particles have a length of 2-10 mm.
5. The method for extracting oil from microalgae according to claim 1, wherein the solvent is one or more of n-hexane, ethanol and isopropanol.
6. The method for extracting oil from microalgae according to claim 1, wherein in the step 2), the solvent extraction temperature is between room temperature and 60 ℃, the total extraction time is 5-20min, and the extraction times are 3-5.
7. The method for extracting grease from microalgae according to claim 1, wherein in the step 2), the weight ratio of the expanded algae powder particles to the solvent is 1: 1-1: 3.
8. the method for extracting oil from microalgae according to claim 1, wherein in step 3), the evaporation conditions are as follows: absolute pressure 100Pa and evaporating temperature 40-60 deg.C.
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