CN100453629C - Method for extracting safflower seed oil with supercritical carbon dioxide - Google Patents

Abstract

A method for extracting safflower seed oil with supercritical carbon dioxide is to place safflower seeds crushed to a particle size of 0.3-0.5 mm in an extraction tank of a supercritical extraction device, use supercritical carbon dioxide as an extraction agent, and use supercritical carbon dioxide as an extraction agent at a pressure of 20 -28MPa, the temperature is 35-60°C for extraction; separation after extraction, the primary separation pressure is 9-14MPa, the temperature is 35-50°C, and the separation is safflower seed oil; the secondary separation pressure is 5-8MPa , the temperature is 30-40°C to obtain water and safflower seed oil. The invention has the advantages of fast extraction speed, no residual extractant in the product, high purity of safflower seed oil, unsaturated fatty acid content of over 90%, and linoleic acid content of about 85%.

Description

Method for extracting safflower seed oil with supercritical carbon dioxide

technical field

The invention relates to a method for extracting safflower seed oil, in particular to a method for extracting linoleic acid-based oil from safflower seeds by using carbon dioxide fluid in a supercritical state as an extractant.

Background technique

Safflower seeds are the seeds of Compositae safflower. The cultivated area of safflower in my country is 30,000 to 40,000 hectares, mainly concentrated in Xinjiang, followed by Sichuan, Yunnan and other provinces. Safflower seed oil is a vegetable oil extracted from safflower seeds. Its linoleic acid content is the highest among all vegetable oils, and it also contains active substances such as flavonoids and vitamin E. Linoleic acid is the only fatty acid that is necessary for the human body but cannot be synthesized in the body itself. It is an essential factor for maintaining brain and nerve functions. Long-term consumption of linoleic acid can soften blood vessels, reduce the absorption of cholesterol in the gastrointestinal tract, and excrete it from the body; at the same time, it can resist thrombosis, lower blood lipids, and prevent atherosclerosis; in addition, it can prevent cancer and inhibit tumor cell metastasis. Inhibit allergies, enhance immunity and prolong life. Therefore safflower oil is considered as one of the best cooking oils in the world.

At present, the safflower seed oil production process is mainly based on shelling, pre-pressing and leaching. During the pressing process, even if the cold pressing method is used, the seeds will inevitably be heated during the extrusion process, which will oxidize and deteriorate the biologically active flavonoids, vitamin E and other nutrients; during the leaching process, due to organic extractants such as ethanol, With the introduction of petroleum ether, n-hexane, etc., a small amount of organic extractant will inevitably remain in the leached oil, causing the product to be polluted by organic matter. It can be seen from the above factors that the current extraction methods of safflower seed oil have problems such as destroying nutrients and producing extractant residues.

When the temperature T and pressure P of carbon dioxide are higher than its critical temperature Tc (31.1°C) and critical pressure Pc (7.39MPa) respectively, it is called supercritical carbon dioxide. Supercritical carbon dioxide has a strong dissolving ability, which can be easily adjusted by changing operating parameters to improve product purity and increase yield. Carbon dioxide has a low critical temperature and is especially suitable for the separation of thermally sensitive and chemically unstable natural products. In addition, carbon dioxide is cheap, inert and has no residue, and it also has the functions of preventing oxidation and inhibiting bacteria.

Sun Chuanjing et al. (CN 1102646C) reported the results of supercritical carbon dioxide reverse extraction of some medicinal vegetable oils, but did not involve the raw material safflower seeds, nor did they produce examples in industrial devices. There is no method for extracting safflower seed oil with supercritical carbon dioxide in practical application.

Contents of the invention

The purpose of the present invention is to provide a method for preparing safflower seed oil with simple process flow, convenient operation, high product quality and high yield in view of the shortcomings of the above-mentioned traditional process.

The main technical feature of the present invention is to use non-toxic, easy to obtain and cheap carbon dioxide as an extraction agent to extract safflower seed oil in a supercritical state, and at the same time reduce the pressure step by step to realize the self-separation of safflower seed oil and carbon dioxide. recycle.

The method for extracting safflower seed oil of the present invention, comprises the steps:

(1) Taking safflower seeds as raw material, pulverizing it to a particle size of 0.3-0.5mm;

(2) placing the pulverized safflower seeds in an extraction tank of a supercritical extraction device, using supercritical carbon dioxide as an extraction agent, and extracting at a pressure of 20-28MPa and a temperature of 35-60°C;

(3) Carry out two-stage decompression separation, the first-stage separation pressure is 9-14MPa, and the temperature is 35-50°C, and the separation obtains safflower seed oil; the second-stage separation pressure is 5-8MPa, and the temperature is 30-40°C, and the obtained Water and Safflower Oil.

The protein and amino acid rich in the extracted residue have not changed during the extraction process, and can be made into feed through further processing.

The invention has been verified from the laboratory to the industrial extraction device

Advantages of the present invention:

1. The safflower seed oil obtained by supercritical carbon dioxide extraction has high purity, and the content of unsaturated fatty acids can reach more than 90%, including about 85% of linoleic acid;

2. The extraction speed of the present invention is fast, and the extraction and separation process can be completed in a relatively short period of time;

3. No organic extractant is used in production, and there is no extractant residue in the product;

4. The product of the present invention can soften blood vessels, prevent and treat diseases such as heart disease, cerebrovascular disease and liver cirrhosis.

Description of drawings

Fig. 1 is a process flow diagram of the present invention.

As shown in the figure, 1. Gas tank 2. Condensation tank 3. High pressure pump 4. Preheater 5. Extraction tank a 6. Extraction tank b 7. Back pressure valve 8. Separation tank I 9. Separation tank II 10. Release material valve

The carbon dioxide enters the carbon dioxide condensation tank 2 from the gas tank 1 to condense into a liquid, which is injected from the bottom into the extraction tank 5 or extraction tank 6 which is pre-installed with crushed safflower seeds by a high-pressure pump, and the safflower seeds are extracted, and the pressure controller gradually extracts the safflower seeds. The pressure is lowered step by step, and the carbon dioxide fluid carrying safflower seed oil is sent to the separation tank 8 for separation, the density of supercritical carbon dioxide is reduced, and the solute and the extractant are separated step by step. The temperature of extraction tank 5, 6 and separation tank 8, 9 is controlled by the thermal circulation water heating of its jacket. The safflower oil is discharged from the bottom of the separation tank 8 and the separation tank 9, and the carbon dioxide enters the condensation tank 2 from the upper part of the separation tank 9, returns to the pump cavity after becoming a liquid, and is recycled.

Detailed ways

Embodiment 1: Take 50 grams of safflower seeds, grind them to an average particle size of 0.4 mm, put them in an extraction tank after drying and seal them. Open the gas tank, carbon dioxide reaches the extraction tank through the condensation tank and high-pressure pump, and extracts at 28MPa, 50°C, and a flow rate of 4.5L/h; the extract enters the primary separation tank, and performs primary separation at 10MPa, 45°C to obtain yellow Transparent safflower oil; carbon dioxide continues to enter the secondary separation tank, and a little water and safflower oil are separated in the secondary separation tank at 6MPa and 40°C. The carbon dioxide separated from the separation tank returns to the condensation tank. After 2 hours of dynamic operation, 12.22 grams of safflower seed oil was obtained from the separation tank, with an extraction rate of 24.4%, accounting for 90.5% of the oil content. The content of linoleic acid in the obtained oil was 85.6%.

Embodiment 2: Take 50 grams of safflower seeds, grind them to an average particle size of 0.4 mm, put them in an extraction tank after drying and seal them. Open the gas tank, carbon dioxide reaches the extraction tank through the condensation tank and high-pressure pump, and extracts at 24MPa, 45°C, and a flow rate of 4.5L/h; the extract enters the primary separation tank, and performs primary separation at 10MPa, 50°C to obtain yellow Transparent safflower seed oil; carbon dioxide continues to enter the secondary separation tank, and a little water and safflower seed oil are separated in the secondary separation tank at 5MPa and 30°C. The carbon dioxide separated from the separation tank returns to the condensation tank. After 2 hours of dynamic operation, 11.9 grams of safflower seed oil was obtained from the separation tank, with an extraction rate of 23.8%, accounting for 88.2% of the oil content. The content of linoleic acid in the obtained oil was 84.9%.

Embodiment 3: Take 50 grams of safflower seeds, grind them to an average particle size of 0.5 mm, put them in an extraction tank after drying and seal them. Open the gas tank, carbon dioxide reaches the extraction tank through the condensation tank and high-pressure pump, and extracts at 20MPa, 35°C, and a flow rate of 4.5L/h; the extract enters the primary separation tank, and performs primary separation at 12MPa, 35°C to obtain yellow Transparent safflower oil; carbon dioxide continues to enter the secondary separation tank, and a little water and safflower oil are separated in the secondary separation tank at 6MPa and 35°C. The carbon dioxide separated from the separation tank returns to the condensation tank. After 2 hours of dynamic operation, 7.1 grams of safflower seed oil was obtained from the separation tank, with an extraction rate of 14.2%, accounting for 52.6% of the oil content. The content of linoleic acid in the obtained oil was 84.8%.

Embodiment 4: Take 50 grams of safflower seeds, grind them to an average particle size of 0.4 mm, put them in an extraction tank after drying and seal them. Open the gas tank, carbon dioxide reaches the extraction tank through the condensation tank and high-pressure pump, and extracts at 28MPa, 60°C, and a flow rate of 4.5L/h; the extract enters the primary separation tank, and performs primary separation at 10MPa, 60°C to obtain yellow Transparent safflower oil; carbon dioxide continues to enter the secondary separation tank, and a little water and safflower oil are separated in the secondary separation tank at 5MPa and 35°C. The carbon dioxide separated from the separation tank returns to the condensation tank. After 2 hours of dynamic operation, 10.4 grams of safflower seed oil was obtained from the separation tank, with an extraction rate of 20.8%, accounting for 77.0% of the oil content. The content of linoleic acid in the obtained oil was 86.2%.

Example 5: 70 grams of safflower seeds were taken, crushed to an average particle size of 0.4 mm, dried, placed in an extraction tank and sealed. Open the gas tank, carbon dioxide reaches the extraction tank through the condensation tank and high-pressure pump, and extracts at 28MPa, 40°C, and a flow rate of 4.5L/h; the extract enters the primary separation tank, and performs primary separation at 14MPa, 45°C to obtain yellow Transparent safflower oil; carbon dioxide continues to enter the secondary separation tank, and some water and safflower oil are separated in the secondary separation tank at 5MPa and 40°C. The carbon dioxide separated from the separation tank returns to the condensation tank. After 2 hours of dynamic operation, 13.3 grams of safflower seed oil was obtained from the separation tank, with an extraction rate of 19.0%, accounting for 70.3% of the oil content. The content of linoleic acid in the obtained oil was 84.7%.

Example 6: Another 50 kg of safflower seeds were taken, crushed to an average particle size of 0.3 mm, placed in an extraction tank and sealed. Open the gas tank, carbon dioxide reaches the extraction tank through the condensation tank and high-pressure pump, and extracts at 25MPa, 50°C, and a flow rate of 0.46m ³ /h; the extract enters the primary separation tank, and performs primary separation at 9MPa, 40°C to obtain Yellow and transparent safflower oil; carbon dioxide continues to enter the secondary separation tank, and a little water and safflower oil are separated in the secondary separation tank at 8MPa and 40°C. The carbon dioxide separated from the separation tank returns to the condensation tank. After 6 hours of dynamic operation, 10.2 kg of safflower seed oil was obtained from the separation tank, with an extraction rate of 20.4%, accounting for 75.6% of the oil content. The content of linoleic acid in the obtained oil was 84.9%.

Example 7: Another 50 kg of safflower seeds were taken, crushed to an average particle size of 0.3 mm, placed in an extraction tank and sealed. Open the gas tank, carbon dioxide reaches the extraction tank through the condensation tank and high-pressure pump, and extracts at 28MPa, 50°C, and a flow rate of 0.46m ³ /h; the extract enters the primary separation tank, and performs primary separation at 9MPa, 40°C to obtain Yellow transparent vegetable oil; carbon dioxide continues to enter the secondary separation tank, and a little water and oil samples are separated in the secondary separation tank at 8MPa and 40°C. The carbon dioxide separated from the separation tank returns to the condensation tank. After 6 hours of dynamic operation, 11.3 kg of safflower seed oil was obtained from the separation tank, with an extraction rate of 22.6%, accounting for 77.9% of the oil content. The content of linoleic acid in the obtained oil was 85.6%.

Claims (1)

1, a kind of method for supercritical carbon dioxide extraction safflower seed oil, is characterized in that comprising the steps: (1) Taking safflower seeds as raw material, pulverizing it to a particle size of 0.3-0.5mm; (2) placing the pulverized safflower seeds in an extraction tank of a supercritical extraction device, using supercritical carbon dioxide as an extraction agent, and extracting at a pressure of 20-28MPa and a temperature of 35-60°C; (3) Carry out two-stage decompression separation, the first-stage separation pressure is 9-14MPa, and the temperature is 35-50°C, and the separation obtains safflower seed oil; the second-stage separation pressure is 5-8MPa, and the temperature is 30-40°C, and the obtained Water and Safflower Oil.

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