CN110643421A - Preparation method for producing three kinds of microalgae oil by three-step solvent method - Google Patents
Preparation method for producing three kinds of microalgae oil by three-step solvent method Download PDFInfo
- Publication number
- CN110643421A CN110643421A CN201910825620.1A CN201910825620A CN110643421A CN 110643421 A CN110643421 A CN 110643421A CN 201910825620 A CN201910825620 A CN 201910825620A CN 110643421 A CN110643421 A CN 110643421A
- Authority
- CN
- China
- Prior art keywords
- algae powder
- extracted
- freeze
- microalgae
- butane
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
-
- 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
- C11B3/00—Refining fats or fatty oils
- C11B3/008—Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
-
- 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
- C11B3/00—Refining fats or fatty oils
- C11B3/12—Refining fats or fatty oils by distillation
Abstract
The invention discloses a preparation method for producing three kinds of microalgae oil by a three-step solvent method, which comprises the following steps: uniformly spreading powdery nannochloropsis oculata in a culture dish for pre-freezing, and freeze-drying after the pre-freezing is finished to obtain freeze-dried algae powder; mixing the freeze-dried algae powder with water, and extruding and puffing to obtain puffed algae powder; mixing the puffed algae powder with acetone for extraction, evaporating the acetone from the primary extracting solution by using an evaporator, and obtaining residues after evaporation, namely the microalgae oil extracted by the acetone; mixing the primary dried algae powder and butane for extraction, evaporating the butane from the secondary extracting solution by using an evaporator, and obtaining residue after evaporation, namely the butane-extracted microalgae oil; mixing the secondary dried algae powder with ethanol for extraction, evaporating the ethanol from the tertiary extract by using an evaporator, and obtaining the residue after evaporation, namely the microalgae oil extracted by the ethanol. The preparation method for producing the three microalgae oils by the three-step solvent method has safe process and convenient preparation.
Description
Technical Field
The invention relates to the technical field of microalgae oil, in particular to a preparation method for producing three types of microalgae oil by a three-step solvent method.
Background
Unsaturated fatty acid is essential fatty acid for human growth and development, and is mainly extracted from fish oil at present, but the processing is complex and the pollution is serious. Microalgae has great potential as another main source of unsaturated fatty acid, has rich microalgae resources, has the advantages of short growth cycle, quick harvest and the like, contains polar lipids which form various membrane structures and comprise glycolipids, phospholipids, triglycerides and the like, and the lipids contain a large amount of polyunsaturated fatty acid, such as alpha-linolenic acid (ALA), eicosapentaenoic acid (EPA), docosahexaenoic acid (DHA) and the like; a large number of researches show that polyunsaturated fatty acid plays an important role in maintaining cardiovascular health of human bodies, resisting tumors and infection, and different solvents are used for extracting lipid, so that the influence on the content of each component in the lipid is huge.
Disclosure of Invention
Aiming at the defects in the technology, the invention provides a preparation method for producing three kinds of microalgae oil by a three-step solvent method with safe process and convenient preparation.
The technical scheme includes that the preparation method for producing three kinds of microalgae oil through a three-step solvent method comprises the following steps of uniformly spreading powdery nannochloropsis oculata in a culture dish for pre-freezing, after the pre-freezing is finished, putting the pre-frozen nannochloropsis oculata into freeze drying equipment for freeze drying, crushing the powder and then sieving the powder through a 40 ~ -60-mesh sieve to obtain freeze-dried algae powder, wherein the water content range of the freeze-dried algae powder is 3 ~%, secondly, uniformly mixing the freeze-dried algae powder and water according to a material-liquid ratio of 8 ~ g to 1mL, adding the mixture into an extruder for extrusion and expansion to obtain expanded algae powder, thirdly, mixing the expanded algae powder with acetone, extracting at a certain temperature, filtering to obtain primary extracting solution and primary extracting algae powder, drying the primary extracting solution and the primary extracting algae powder at a constant temperature of 60 5980 ℃ to obtain constant weight, obtaining primary dried algae powder, extracting solution and secondary extracting the butane extracting solution after the primary extracting solution and the butane are extracted by a vacuum evaporator at a constant temperature of ~ ℃, evaporating the primary extracting solution and the butane to obtain secondary extracting solution, evaporating the butane, drying the butane, evaporating the secondary extracting solution and the butane to obtain secondary extracting solution, evaporating the butane and drying the butane to obtain the butane, and drying the residue after the secondary extracting solution, evaporating the secondary extracting solution, and the butane, wherein the residue after the secondary extracting solution is the secondary extracting solution, the butane, the secondary extracting solution is obtained by the secondary extracting solution, the butane, the secondary extracting solution is obtained by the secondary extracting step 3, the butane, the step 35.
Preferably, the tiling thickness in the step one is 4 ~ 8mm, the pre-freezing temperature is-30 ~ -20 ℃, and the pre-freezing time is 8 ~ 12 hours.
Preferably, the freeze-drying conditions in the step one are that the freeze-drying pressure is 20 ~ 45Pa, the freeze-drying temperature is-65 ~ -60 ℃, and the freeze-drying time is 8 ~ 10 hours.
Preferably, the extrusion puffing conditions in the second step are that the rotating speed of a screw is 300 ~ 500r/min, and the barrel temperatures of the feeding end, the middle section and the discharging end are respectively 70 ~ 90 ℃, 90 ~ 110 ℃ and 120 ~ 140 ℃.
Preferably, in the third step, the puffed algae powder and acetone are mixed according to the ratio of 1g to 2 ~ 4mL, and the mixture is extracted for 15 ~ 20min at the temperature of 4 ~ 8 ℃.
Preferably, the extraction rate of lipid in the microalgae oil extracted by acetone is 9.3 ~ 9.5.5%, the content of phospholipid is 3.0 ~ 3.5.5%, the content of neutral ester is 83.7 ~ 85.1.1%, and the content of glycolipid is 10.2 ~ 12.7.7%.
Preferably, in the fourth step, the primary dried algae powder and butane are mixed according to the feed-liquid ratio of 1g to 2 ~ 4ml, and the mixture is extracted for 15 ~ 20min at the temperature of 25 ~ 30 ℃.
Preferably, the butane-extracted microalgae oil has a lipid extraction rate of 6.2 ~ 6.5.5%, a phospholipid content of 10.5 ~ 12.3.3%, a neutral ester content of 75.7% ~ 80.2.2%, and a glycolipid content of 9.8% ~ 10.5.5%.
Preferably, in the fifth step, the secondary dried algae powder is mixed with ethanol according to the feed-liquid ratio of 1g to 3 ~ 6ml, and the mixture is extracted for 15 ~ 20min at the temperature of 25 ~ 30 ℃.
Preferably, the ethanol-extracted microalgae oil has a lipid extraction rate of 15.8 ~ 18.9.9%, a phospholipid content of 20.3 ~ 22.4.4%, a neutral ester content of 70.2% ~ 73.0%, and a glycolipid content of 5.8% ~ 6.5.5%.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a preparation method for producing three kinds of microalgae oil by a three-step solvent method, which adopts the three-step solvent method to replace the traditional one-step solvent method, greatly improves the extraction efficiency of lipid, and the solvent combination of acetone, butane and ethanol maximizes the extraction efficiency of the lipid; by extruding and puffing the freeze-dried algae powder, the wall breaking rate of the algae powder is effectively improved, the yield of grease can be increased, the dissolution of free fatty acid is increased, and enzymes with adverse effects are passivated; the three microalgae oils obtained by the three-step solvent method have obvious difference in lipid content and components, and the chemical components and functional characteristics of the microalgae oils are found to be greatly related by comparing the antioxidant capacity of the three microalgae oils, so that the method is beneficial to later development of the customized microalgae oil with target functionality.
Detailed Description
The present invention is described in further detail below to enable those skilled in the art to practice the invention with reference to the description.
The invention provides a preparation method for producing three kinds of microalgae oil by a three-step solvent method, which comprises the following steps:
uniformly spreading powdery nannochloropsis oculata in a culture dish for pre-freezing with the spreading thickness of 4 ~ 8mm, the pre-freezing temperature of-30 ~ -20 ℃ and the pre-freezing time of 8 ~ 12 hours, after the pre-freezing is finished, putting the pre-frozen nannochloropsis oculata into freeze drying equipment for freeze drying under the freeze drying pressure of 20 ~ 45Pa, the freeze drying temperature of-65 ~ -60 ℃ and the freeze drying time of 8 ~ 10 hours, crushing the nannochloropsis oculata and sieving the crushed nannochloropsis oculata with a 40 ~ 60-mesh sieve to obtain freeze-dried algae powder, wherein the water content range of the freeze-dried algae powder is 3 ~ 5%;
step two, uniformly mixing the freeze-dried algae powder and water according to a material-liquid ratio of 8 ~ 10g to 1mL, adding the mixture into a double-screw extruder for extrusion and expansion, wherein the rotating speed of a screw is 300 ~ 500r/min, and the barrel temperatures of a feeding end, a middle section and a discharging end are respectively 70 ~ 90 ℃, 90 ~ 110 ℃ and 120 ~ 140 ℃ to obtain expanded algae powder;
step three, mixing the puffed algae powder with acetone according to a material-liquid ratio of 1g to 2 ~ 4mL, extracting at the temperature of 4 ~ 8 ℃ for 15 ~ 20min, filtering to obtain a primary extracting solution and a primary extracted algae powder, drying the primary extracted algae powder at the constant temperature of 60 ~ 80 ℃ to constant weight to obtain primary dried algae powder, evaporating the acetone from the primary extracting solution at the temperature of 30 ~ 35 ℃ by using a vacuum rotary evaporator, and obtaining the residue after evaporation, namely the microalgae oil extracted by the acetone, wherein the extraction rate of lipid in the microalgae oil extracted by the acetone is 9.3 ~ 9.5.5%, the content of phospholipid is 3.0 ~ 3.5.5%, the content of neutral ester is 83.7 ~ 85.1.1%, and the content of glycolipid is 10.2 ~ 12.7.7%;
step four, mixing the primary dried algae powder and butane according to a material-liquid ratio of 1g to 2 ~ 4ml, extracting for 15 ~ 20min at the temperature of 25 ~ 30 ℃, filtering to obtain a secondary extracting solution and secondary extracted algae powder, drying the secondary extracted algae powder at the constant temperature of 65 ~ 75 ℃ to constant weight to obtain secondary dried algae powder, evaporating butane from the secondary extracting solution at the temperature of 30 ~ 35 ℃ by using a vacuum rotary evaporator, and obtaining the residue after evaporation, wherein the lipid extraction rate of the butane-extracted microalgae oil is 6.2 ~ 6.5.5%, the phospholipid content is 10.5 ~ 12.3.3%, the neutral ester content is 75.7% ~ 80.2.2%, and the glycolipid content is 9.8% ~ 10.5.5%;
step five, mixing the secondary dried algae powder with ethanol according to a material-liquid ratio of 1g to 3 ~ 6ml, extracting for 15 ~ 20min at the temperature of 25 ~ 30 ℃, filtering to obtain a third extracting solution, evaporating the third extracting solution with ethanol by using a vacuum rotary evaporator at the temperature of 30 ~ 35 ℃, wherein the residue obtained after evaporation is the microalgae oil extracted with ethanol, the lipid extraction rate of the microalgae oil extracted with ethanol is 15.8 ~ 18.9.9%, the phospholipid content is 20.3 ~ 22.4.4%, the neutral ester content is 70.2% ~ 73.0.0%, and the glycolipid content is 5.8% ~ 6.5.5%.
Example 1
Uniformly spreading powdery nannochloropsis oculata in a culture dish for pre-freezing, wherein the spreading thickness is 4mm, the pre-freezing temperature is-30 ℃, the pre-freezing time is 8 hours, after the pre-freezing is finished, putting the nannochloropsis oculata subjected to pre-freezing treatment into a freeze drying device for freeze drying, the freeze drying pressure is 20Pa, the freeze drying temperature is-65 ℃, the freeze drying time is 8 hours, crushing the nannochloropsis oculata, and sieving the crushed nannochloropsis oculata with a 40-mesh sieve to obtain freeze-dried algae powder, wherein the water content range of the freeze-dried algae powder is 5%; uniformly mixing the freeze-dried algae powder and water according to a material-liquid ratio of 8g to 1mL, adding the mixture into a double-screw extruder for extrusion and expansion, wherein the rotating speed of a screw is 300r/min, and the barrel temperatures of a feeding end, a middle section and a discharging end are respectively 70 ℃, 90 ℃ and 120 ℃, so as to obtain expanded algae powder; mixing the puffed algae powder with acetone according to a material-liquid ratio of 1g to 2mL, extracting at 4 ℃ for 15min, filtering to obtain a primary extracting solution and a primary extracted algae powder, drying the primary extracted algae powder at a constant temperature of 60 ℃ to constant weight to obtain primary dried algae powder, evaporating the acetone from the primary extracting solution at 30 ℃ by using a vacuum rotary evaporator to obtain an evaporated residue, namely the microalgae oil extracted by the acetone, wherein the extraction rate of lipid in the microalgae oil extracted by the acetone is 9.5%, the phospholipid content is 3.5%, the neutral ester content is 83.7%, and the glycolipid content is 10.2%; mixing the primary dried algae powder and butane according to a material-liquid ratio of 1g to 2ml, extracting for 15min at the temperature of 25 ℃, filtering to obtain a secondary extracting solution and secondary extracted algae powder, drying the secondary extracted algae powder at the constant temperature of 65 ℃ to constant weight to obtain secondary dried algae powder, evaporating butane from the secondary extracting solution at the temperature of 30 ℃ by using a vacuum rotary evaporator, and obtaining a residue after evaporation, namely the butane-extracted microalgae oil, wherein the lipid extraction rate of the butane-extracted microalgae oil is 6.2%, the phospholipid content is 10.5%, the neutral ester content is 75.7%, and the glycolipid content is 9.8%; mixing the secondary dried algae powder with ethanol according to a feed-liquid ratio of 1g to 3ml, extracting for 15min at the temperature of 25 ℃, filtering to obtain a third extracting solution, evaporating the ethanol from the third extracting solution at the temperature of 30 ℃ by using a vacuum rotary evaporator, and obtaining residues after evaporation, namely the microalgae oil extracted by the ethanol, wherein the extraction rate of lipid in the microalgae oil extracted by the ethanol is 15.8%, the content of phospholipid is 20.3%, the content of neutral ester is 70.2%, and the content of glycolipid is 5.8%.
Example 2
Uniformly spreading powdery nannochloropsis oculata in a culture dish for pre-freezing, wherein the spreading thickness is 6mm, the pre-freezing temperature is-25 ℃, the pre-freezing time is 10 hours, after the pre-freezing is finished, putting the nannochloropsis oculata subjected to pre-freezing treatment into a freeze drying device for freeze drying, the freeze drying pressure is 32.5Pa, the freeze drying temperature is-62.5 ℃, the freeze drying time is 9 hours, crushing the nannochloropsis oculata, and sieving the crushed nannochloropsis oculata with a 50-mesh sieve to obtain freeze-dried algae powder, wherein the water content range of the freeze-dried algae powder is 4%; uniformly mixing the freeze-dried algae powder and water according to a material-liquid ratio of 9g to 1mL, adding the mixture into a double-screw extruder for extrusion and expansion, wherein the rotating speed of a screw is 400r/min, and the barrel temperatures of a feeding end, a middle section and a discharging end are respectively 80 ℃, 100 ℃ and 130 ℃, so as to obtain expanded algae powder; mixing the puffed algae powder with acetone according to a material-liquid ratio of 1g to 3mL, extracting at 6 ℃ for 18min, filtering to obtain a primary extracting solution and a primary extracted algae powder, drying the primary extracted algae powder at 70 ℃ to constant weight to obtain primary dried algae powder, evaporating the acetone from the primary extracting solution at 32 ℃ by using a vacuum rotary evaporator to obtain an evaporated residue, namely the acetone-extracted microalgae oil, wherein the acetone-extracted microalgae oil has a lipid extraction rate of 9.4%, a phospholipid content of 3.2%, a neutral ester content of 84.4% and a glycolipid content of 11.4%; mixing the primary dried algae powder and butane according to a material-liquid ratio of 1g:3ml, extracting at 28 ℃ for 18min, filtering to obtain a secondary extracting solution and secondary extracted algae powder, drying the secondary extracted algae powder at a constant temperature of 70 ℃ to constant weight to obtain secondary dried algae powder, evaporating butane from the secondary extracting solution at 32 ℃ by using a vacuum rotary evaporator, and obtaining a residue after evaporation, namely the butane-extracted microalgae oil, wherein the lipid extraction rate, the phospholipid content, the neutral ester content and the glycolipid content in the butane-extracted microalgae oil are respectively 6.3%, 11.4%, 78% and 10.2%; mixing the secondary dried algae powder with ethanol according to a feed-liquid ratio of 1g to 4.5ml, extracting at 28 ℃ for 18min, filtering to obtain a third extracting solution, evaporating the ethanol from the third extracting solution at 32 ℃ by using a vacuum rotary evaporator, and obtaining residues after evaporation, namely the microalgae oil extracted by the ethanol, wherein the lipid extraction rate of the microalgae oil extracted by the ethanol is 17.4%, the phospholipid content is 21.3%, the neutral ester content is 71.6%, and the glycolipid content is 6.1%.
Example 3
Uniformly spreading powdery nannochloropsis oculata in a culture dish for pre-freezing, wherein the spreading thickness is 8mm, the pre-freezing temperature is-20 ℃, the pre-freezing time is 12 hours, after the pre-freezing is finished, putting the nannochloropsis oculata subjected to pre-freezing treatment into a freeze drying device for freeze drying, the freeze drying pressure is 45Pa, the freeze drying temperature is-60 ℃, the freeze drying time is 10 hours, crushing the nannochloropsis oculata, and then sieving the crushed nannochloropsis oculata with a 60-mesh sieve to obtain freeze-dried algae powder, wherein the water content range of the freeze-dried algae powder is 3%; uniformly mixing the freeze-dried algae powder and water according to a material-liquid ratio of 10g to 1mL, adding the mixture into a double-screw extruder for extrusion and expansion, wherein the rotating speed of a screw is 500r/min, and the barrel temperatures of a feeding end, a middle section and a discharging end are respectively 90 ℃, 110 ℃ and 140 ℃, so as to obtain expanded algae powder; mixing the puffed algae powder with acetone according to a material-liquid ratio of 1g to 4mL, extracting at the temperature of 8 ℃ for 20min, filtering to obtain a primary extracting solution and a primary extracted algae powder, drying the primary extracted algae powder at the constant temperature of 80 ℃ to constant weight to obtain primary dried algae powder, evaporating the acetone from the primary extracting solution at the temperature of 35 ℃ by using a vacuum rotary evaporator to obtain a residue, namely the microalgae oil extracted by the acetone, wherein the extraction rate of lipid in the microalgae oil extracted by the acetone is 9.5%, the phospholipid content is 3.5%, the neutral ester content is 83.7%, and the glycolipid content is 12.7%; mixing the primary dried algae powder and butane according to a material-liquid ratio of 1g: 4ml, extracting at 30 ℃ for 20min, filtering to obtain a secondary extracting solution and secondary extracted algae powder, drying the secondary extracted algae powder at 75 ℃ to constant weight to obtain secondary dried algae powder, evaporating butane from the secondary extracting solution at 35 ℃ by using a vacuum rotary evaporator, and obtaining a residue after evaporation, namely the butane-extracted microalgae oil, wherein the lipid extraction rate, the phospholipid content and the neutral ester content in the butane-extracted microalgae oil are 6.5%, 12.3%, 75.7% and 10.5%; mixing the secondary dried algae powder with ethanol according to a feed-liquid ratio of 1g to 6ml, extracting for 20min at the temperature of 30 ℃, filtering to obtain a third extracting solution, evaporating the ethanol from the third extracting solution at the temperature of 35 ℃ by using a vacuum rotary evaporator, and obtaining residues after evaporation, namely the microalgae oil extracted by the ethanol, wherein the microalgae oil extracted by the ethanol has the lipid extraction rate of 18.9%, the phospholipid content of 22.4%, the neutral ester content of 70.2% and the glycolipid content of 6.5%.
While embodiments of the invention have been described above, it is not limited to the applications set out in the description and embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described without departing from the generic concept as defined by the claims and their equivalents.
Claims (10)
1. A preparation method for producing three kinds of microalgae oil by a three-step solvent method is characterized by comprising the following steps:
uniformly spreading powdery nannochloropsis oculata in a culture dish for pre-freezing, after the pre-freezing is finished, putting the pre-frozen nannochloropsis oculata into freeze drying equipment for freeze drying, crushing the powder, and sieving the crushed powder with a 40 ~ 60-mesh sieve to obtain freeze-dried algae powder, wherein the water content range of the freeze-dried algae powder is 3 ~ 5%;
step two, uniformly mixing the freeze-dried algae powder with water according to a material-liquid ratio of 8 ~ 10g to 1mL, and adding the mixture into a double-screw extruder for extrusion and expansion to obtain expanded algae powder;
mixing the puffed algae powder with acetone, extracting at a certain temperature, filtering to obtain a primary extracting solution and a primary extracted algae powder, drying the primary extracted algae powder at a constant temperature of 60 ~ 80 ℃ to constant weight to obtain a primary dried algae powder, evaporating the acetone from the primary extracting solution at a temperature of 30 ~ 35 ℃ by using a vacuum rotary evaporator, and obtaining a remainder which is the microalgae oil extracted by the acetone after evaporation;
step four, mixing the primary dried algae powder and butane, extracting at a certain temperature, filtering to obtain a secondary extracting solution and secondary extracted algae powder, drying the secondary extracted algae powder at the constant temperature of 65 ~ 75 ℃ to constant weight to obtain secondary dried algae powder, evaporating the butane from the secondary extracting solution at the temperature of 30 ~ 35 ℃ by using a vacuum rotary evaporator, and obtaining a remainder which is the butane-extracted microalgae oil after evaporation;
and step five, mixing the secondary dried algae powder with ethanol, extracting at a certain temperature, filtering to obtain a third extracting solution, evaporating the ethanol from the third extracting solution at the temperature of 30 ~ 35 ℃ by using a vacuum rotary evaporator, and obtaining residues after evaporation, namely the microalgae oil extracted by the ethanol.
2. The method of claim 1, wherein the first step comprises a flat thickness of 4 ~ 8mm, a pre-freezing temperature of-30 ~ -20 ℃, and a pre-freezing time of 8 ~ 12 hours.
3. The method for preparing three microalgae oils according to claim 1, wherein the freeze-drying conditions in the first step are a freeze-drying pressure of 20 ~ 45Pa, a freeze-drying temperature of-65 ~ -60 ℃, and a freeze-drying time of 8 ~ 10 hours.
4. The method for preparing three microalgae oils according to claim 1, wherein the extrusion-expansion conditions in the second step are that the screw speed is 300 ~ 500r/min, and the barrel temperatures at the feeding end, the middle section and the discharging end are 70 ~ 90 ℃, 90 ~ 110 ℃ and 120 ~ 140 ℃ respectively.
5. The preparation method for producing three microalgae oils according to claim 1, wherein the expanded algae powder and acetone are mixed according to the feed-liquid ratio of 1g:2 ~ 4mL, and extracted at 4 ~ 8 ℃ for 15 ~ 20 min.
6. The method of claim 1, wherein the acetone-extracted microalgae oil has a lipid extraction rate of 9.3 ~ 9.5.5%, a phospholipid content of 3.0 ~ 3.5.5%, a neutral ester content of 83.7 ~ 85.1.1%, and a glycolipid content of 10.2 ~ 12.7.7%.
7. The method for preparing three microalgae oils according to claim 1, wherein the first dry algae powder and butane are mixed according to a feed-liquid ratio of 1g:2 ~ 4ml, and extracted at 25-25 ~ 30 ℃ for 15 ~ 20 min.
8. The method of claim 1, wherein the butane-extracted microalgae oil has lipid extraction rate of 6.2 ~ 6.5.5%, phospholipid content of 10.5 ~ 12.3.3%, neutral ester content of 75.7% ~ 80.2.2%, and glycolipid content of 9.8% ~ 10.5.5%.
9. The preparation method of three microalgae oils according to claim 1, wherein in step five, the secondary dried algae powder is mixed with ethanol according to the feed-liquid ratio of 1g to 3 ~ 6ml, and extracted at 25-25 ~ 30 ℃ for 15 ~ 20 min.
10. The method of claim 1, wherein the ethanol-extracted microalgae oil has a lipid extraction rate of 15.8 ~ 18.9.9%, a phospholipid content of 20.3 ~ 22.4.4%, a neutral ester content of 70.2% ~ 73.0.0%, and a glycolipid content of 5.8% ~ 6.5.5%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910825620.1A CN110643421A (en) | 2019-09-03 | 2019-09-03 | Preparation method for producing three kinds of microalgae oil by three-step solvent method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910825620.1A CN110643421A (en) | 2019-09-03 | 2019-09-03 | Preparation method for producing three kinds of microalgae oil by three-step solvent method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110643421A true CN110643421A (en) | 2020-01-03 |
Family
ID=69010032
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910825620.1A Pending CN110643421A (en) | 2019-09-03 | 2019-09-03 | Preparation method for producing three kinds of microalgae oil by three-step solvent method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110643421A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102533430A (en) * | 2010-12-28 | 2012-07-04 | 中国科学院大连化学物理研究所 | Extraction method of micro-algae oil |
| CN102559375A (en) * | 2010-11-30 | 2012-07-11 | 新奥科技发展有限公司 | Method for extracting greasy from microalgae |
| CN103582694A (en) * | 2011-04-06 | 2014-02-12 | 赫里开发公司 | Extraction of polar lipids by a two solvent method |
| CN107129860A (en) * | 2017-05-11 | 2017-09-05 | 韶关学院 | A kind of extracting method of microalgae grease |
| CN107384585A (en) * | 2017-09-21 | 2017-11-24 | 江南大学 | A kind of grading system for antarctic krill oil method |
-
2019
- 2019-09-03 CN CN201910825620.1A patent/CN110643421A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102559375A (en) * | 2010-11-30 | 2012-07-11 | 新奥科技发展有限公司 | Method for extracting greasy from microalgae |
| CN102533430A (en) * | 2010-12-28 | 2012-07-04 | 中国科学院大连化学物理研究所 | Extraction method of micro-algae oil |
| CN103582694A (en) * | 2011-04-06 | 2014-02-12 | 赫里开发公司 | Extraction of polar lipids by a two solvent method |
| CN107129860A (en) * | 2017-05-11 | 2017-09-05 | 韶关学院 | A kind of extracting method of microalgae grease |
| CN107384585A (en) * | 2017-09-21 | 2017-11-24 | 江南大学 | A kind of grading system for antarctic krill oil method |
Non-Patent Citations (2)
| Title |
|---|
| 杜彦山等: ""微藻油脂提取技术进展"", 《粮食与油脂》 * |
| 黄远星等: ""水生微藻制备生物燃料的方法综述"", 《水资源与水工程学报》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103859067B (en) | A kind of nutrition Rice oil and production method thereof | |
| AU2012360885A1 (en) | Use of whole soft avocados for preparing avocado oil rich in unsaponifiables | |
| CN102099452A (en) | Method for isolating oils from cells and biomasses | |
| Wang et al. | Microalgal cell disruption via extrusion for the production of intracellular valuables | |
| CN103305335A (en) | Low-temperature countercurrent extraction method of euphausia superba sauce | |
| NZ549432A (en) | Solvent extraction of lipids such from green-lipped mussel Perna canaliculus | |
| CN101785789B (en) | Method for preparing animal gall powder | |
| CN110643421A (en) | Preparation method for producing three kinds of microalgae oil by three-step solvent method | |
| AU2013208886B2 (en) | Use of avocado pit for obtaining an avocado oil enriched with alkyl polyols and/or acetylated derivatives thereof | |
| KR101100120B1 (en) | Edible Oil Comprising Ginseng Oil extracted from Ginseng or its Residue Extract and Preparation Method The Same | |
| Balacuit et al. | Comparison of Microwave-Assisted Extraction to Soxhlet Extraction of Mango Seed Kernel Oil using Ethanol and n-Hexane as Solvents | |
| CN107904023B (en) | Method for extracting residual grease from degreased dried shrimp residues of Antarctic krill | |
| CN111387477A (en) | Microcapsule embedding technology for improving digestion stability of lotus leaf flavone | |
| CA3108999A1 (en) | Oilseed extraction method | |
| RU2372095C1 (en) | Method for making native form of dihydroquercetin | |
| CN110540896A (en) | Preparation method of EPA-containing nannochloropsis oculata oil | |
| RU2632111C2 (en) | Application of avocado peel for receiving unsaponifiable avocado product enriched with saturated aliphatic hydrocarbons and sterols | |
| Ariff et al. | Effect of CO2 flow rate, co-solvent and pressure behavior to yield by supercritical CO2 extraction of Mariposa Christia Vespertilionis leaves | |
| WO2017203498A1 (en) | Processes for extracting cynaropicrin from leaves of cynara cardunculus l. | |
| CN114507561B (en) | Method for extracting grease from microalgae | |
| Kuk et al. | The potential of soapstock-derived film: cottonseed and safflower | |
| CN108130193B (en) | Method for improving extraction rate of oil from euphausia superba | |
| CN107964453B (en) | Method for preparing grease from degreased dried euphausia superba residues | |
| JPH0677505B2 (en) | Method for producing phospholipid containing a large amount of docosahexaenoic acid | |
| CN103614232A (en) | Method for extracting dogwood kernel oil |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200103 |
|
| RJ01 | Rejection of invention patent application after publication |