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Method for extracting microalgae grease by using supercritical carbon dioxide entraining ethanol

A technology of carbon dioxide and microalgae oil, which is applied in the direction of fat oil/fat production and fat production, can solve the problems of weakening the influence of solvent solubility and mass transfer performance, high puffing temperature, high oil recovery rate, etc., and achieve green extraction process Environmental protection, simple operation, and stable composition

Pending Publication Date: 2019-07-19
ZHEJIANG NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Chinese patent CN106635405 discloses a method for supercritically extracting DHA oil from microalgae powder, using an extruder to expand the microalgae powder to break the wall of the microalgae powder, and then extracting oil through supercritical carbon dioxide; the oil recovery rate of the invention High, but the puffing temperature is as high as 40-100°C, which has a negative impact on heat-sensitive and easily oxidized long-chain polyunsaturated fatty acids
However, during the extraction process, ethanol as a co-solvent will gradually lose as the extraction proceeds, and the influence of the co-solvent on the solubility and mass transfer properties of the supercritical fluid will be weakened, and the co-solvent cannot be fully utilized in the oil recovery process. role in

Method used

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  • Method for extracting microalgae grease by using supercritical carbon dioxide entraining ethanol
  • Method for extracting microalgae grease by using supercritical carbon dioxide entraining ethanol
  • Method for extracting microalgae grease by using supercritical carbon dioxide entraining ethanol

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Effect test

example 1

[0057] Device example 1, a kind of supercritical carbon dioxide entrained ethanol extraction device, such as image 3 As stated, by CO 2 Feed module A, ethanol feed module B, extraction module C, separation module D, CO 2 Composed of a flow measurement module E and a sample collection module F;

[0058] CO 2 Feed module A includes CO 2 Steel cylinder 1, low-temperature water tank 2, plunger pump 3, ethanol feeding module B includes reagent bottle 4, high-efficiency liquid phase pump 5, check valve 6, extraction module C includes mixer 7, preheating coil 8, extraction kettle 9, Pressure gauge 10, thermometer 11, expansion valve 12, separation module D includes separation kettle 13, pressure gauge 14, CO 2 The flow measurement module E includes a rotameter 15 (the rotameter 15 has a valve), and the sample collection module F includes a valve 16 , a peristaltic pump 17 , and a sample collection bottle 18 .

[0059] CO 2 Steel cylinder 1, low-temperature water tank 2, and pl...

Embodiment 1

[0064] Embodiment 1, a kind of technology that supercritical carbon dioxide entrains ethanol to extract microalgae oil, carries out following steps successively:

[0065] 1) Pretreatment of raw materials:

[0066] Centrifuge the microalgae fermentation broth at 4°C and 8000r / min for 20 minutes to collect the microalgae cells, then freeze-dry them at -53°C and 0.1mbar to constant weight, grind them, and pass through an 80-mesh sieve. The freeze-dried powder of microalgae is prepared.

[0067] 2), extraction:

[0068] Weigh 20.0g microalgae freeze-dried powder, mix with equal mass (20g) glass microspheres (the particle diameter of glass microspheres is about 2-3mm), place in the extraction kettle 9 of the supercritical extraction system, set the extraction kettle The temperature in 9 is 50-52°C, the pressure is 37-39MPa, and the plunger pump 3 is used to supply CO 2 Pressurize, control the flow rate to 5L / min (CO 2 At 25°C, the flow rate under 0.1MPa), the expansion valve 12...

Embodiment 2

[0075] Embodiment 2, a kind of technique of supercritical carbon dioxide extraction microalgae oil,

[0076] With respect to step 2) of embodiment 1, make the following changes: control the flow rate of entrainer ethanol (about 0.62mL / min) by high-efficiency liquid phase pump 5, so that the molar fraction of ethanol in the fluid is 0.05mol / mol, and all the other are equivalent In Example 1. The extraction time remains unchanged at 3 hours.

[0077] A total of 4.24g of microalgae oil was obtained; the recovery rate was 85.1%.

[0078] After the above-mentioned microalgae oil was methylated with 10% (w / w) acetyl chloride methanol solution, gas chromatography analysis was carried out, and its composition and content were as follows: myristic acid 6.1%, palmitic acid 40.3%, stearic acid 1.3% %, hexadecenoic acid 2.5%, oleic acid 2.7%, docosapentaenoic acid (DPA) 7.4%, docosahexaenoic acid (DHA) 38.2%.

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Abstract

The invention discloses a method for extracting microalgae grease by using supercritical carbon dioxide entraining ethanol. The method comprises the following steps: preparing a microalgae fermentation liquid into microalgae freeze-dry powder; uniformly mixing the microalgae freeze-dry powder with glass beads of which the diameter is 2-5mm, and putting into an extraction kettle as a material; extracting the material in the extraction kettle by using a supercritical CO2 entrained ethanol fluid prepared from an entrainment agent ethanol and CO2, wherein the extraction time is 2.5-3 hours; discharging and collecting ethanol-containing microalgae grease from the outlet in the bottom of a separation kettle. Due to the adoption of the ethanol supercritical carbon dioxide entrained ethanol fluid,the method disclosed by the invention has the advantages of being non-toxic, good in selectivity, green and environmental-friendly, adjustable in polarity, possible to recycle and reuse, and the like, and compared with a conventional organic solvent extraction method, the method has the advantages of being safe and non-toxic.

Description

technical field [0001] The invention relates to a process for extracting oil from microalgae by entraining ethanol with supercritical carbon dioxide. Background technique [0002] Schizochytrium sp. is a common microalgae whose growth cycle is much lower than that of animals. Therefore, it is very easy to scale up culture through fermentation regulation. The total oil content in the fermented algal cells can be higher than 70%. Among them, the content of omega-3 long-chain polyunsaturated fatty acids, especially docosahexaenoic acid (DHA), is about 30-50% of the total oil, and is an ideal raw material for DHA production that can replace deep-sea fish oil. With the implementation and deepening of my country's energy-saving and emission-reduction policies, environmentally friendly green oil extraction technology has become a research and development hotspot. Among them, supercritical carbon dioxide (scCO 2 ) extraction process is very suitable for the extraction of easily ox...

Claims

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Application Information

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IPC IPC(8): C11B1/10
CPCC11B1/104
Inventor 邓刚李佩雷李红娜大卫·安德列亚林洁茹
Owner ZHEJIANG NORMAL UNIVERSITY
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