Method for extracting xanthoceras sorbifolia bunge oil by using subcritical fluid

Abstract

The invention relates to the technical field of vegetable oil extraction, and provides a method for extracting xanthoceras sorbifolia bunge oil by using subcritical fluid, and the method comprises the following steps: S1, taking xanthoceras sorbifolia bunge seed kernels, crushing, and drying to obtain xanthoceras sorbifolia bunge seed kernel powder; s2, extracting the xanthoceras sorbifolia bunge kernel powder by using an extracting agent, concentrating and drying to obtain a xanthoceras sorbifolia bunge oil crude product; s3, performing subcritical fluid extraction, separation and concentration on the xanthoceras sorbifolia bunge oil crude product by using an extracting agent to obtain xanthoceras sorbifolia bunge oil; the extracting agent comprises petroleum ether and o-dimethoxybenzene; the extraction agent comprises tetrafluoroethane and an entrainer; the entrainer comprises ethanol. Through the technical scheme, the problem of low extraction rate of xanthoceras sorbifolia bunge oil in related technologies is solved.

Description

Technical Field

[0001] The invention relates to the technical field of plant oil extraction, and in particular to a method for extracting Xanthoceras sorbifolia oil by using a subcritical fluid. Background Art

[0002] Xanthoceras sorbifolia oil is rich in unsaturated fatty acids, such as oleic acid and linoleic acid, which have many benefits to human health and have potential application prospects in the fields of health care and medicine. At the same time, due to its good combustion properties, it has also attracted much attention in industrial fields such as biodiesel preparation. It is crucial to develop efficient Xanthoceras sorbifolia oil extraction technology.

[0003] Traditional Xanthoceras sorbifolia oil extraction processes, such as pressing, are easy to operate, but have a low oil yield, and a large amount of oil remains in the cake, causing a waste of resources; the solvent extraction method also performs poorly in improving the extraction rate.

[0004] The emergence of subcritical extraction technology has brought new opportunities for the extraction of Xanthoceras sorbifolia oil. With its advantages of high extraction efficiency, mild operating conditions, and solvent recyclability, it has solved some of the problems of traditional processes to a certain extent. However, there is still room for improvement in the past subcritical extraction process in the extraction of Xanthoceras sorbifolia oil. For example, the equipment requirements are high, and some Xanthoceras sorbifolia oil components will be lost during the extraction process due to reactions with residual impurities, resulting in the extraction rate being difficult to achieve the expected.

[0005] Nowadays, as the demand for Xanthoceras sorbifolia oil in various industries continues to grow, the requirements for extraction efficiency and oil quality are becoming more and more stringent. In this context, the development of a subcritical extraction process for Xanthoceras sorbifolia oil to improve the extraction rate of Xanthoceras sorbifolia oil is of vital importance. Summary of the invention

[0006] The invention provides a method for extracting Xanthoceras sorbifolia oil by using a subcritical fluid, which solves the problem of low extraction rate of Xanthoceras sorbifolia oil in the related art.

[0007] The technical solution of the present invention is as follows: The present invention provides a method for extracting Xanthoceras sorbifolia oil using a subcritical fluid, comprising the following steps: S1. Taking Xanthoceras sorbifolia seed kernels, crushing and drying them to obtain Xanthoceras sorbifolia seed kernel powder; S2, extracting the Xanthoceras sorbifolia seed kernel powder using an extractant, concentrating, and drying to obtain a crude Xanthoceras sorbifolia oil; S3, subjecting the crude Xanthoceras sorbifolia oil to subcritical fluid extraction using an extractant, separating, and concentrating to obtain Xanthoceras sorbifolia oil; The extractant includes petroleum ether and o-phenyl dimethyl ether; The extractant comprises tetrafluoroethane and an entrainer; The entrainer includes ethanol.

[0008] As a further technical solution, the mass volume ratio of the Xanthoceras sorbifolia seed kernel powder to the extractant is 1g:15~20mL.

[0009] As a further technical solution, the volume ratio of the extractant petroleum ether to dimethyl ether is 15-17:1.

[0010] In the present invention, the volume ratio of the extractant petroleum ether to phthalate is adjusted to 15-17:1, thereby further improving the extraction rate of Xanthoceras sorbifolia oil.

[0011] As a further technical solution, the extraction temperature is 30-40°C and the extraction time is 8-10 hours.

[0012] As a further technical solution, the mass ratio of the crude Xanthoceras sorbifolia oil to the extractant is 1:10~13.

[0013] As a further technical solution, during the subcritical fluid extraction, the temperature is 30-50°C, the air pressure is 0.8-1MPa, and the time is 0.5-1h.

[0014] As a further technical solution, the mass ratio of tetrafluoroethane to entrainer is 25-30:1.

[0015] As a further technical solution, the particle size of the Xanthoceras sorbifolia seed kernel powder is 100-200 meshes.

[0016] As a further technical solution, the entrainer also includes isopentenol.

[0017] In the present invention, when isopentenol is added to the entrainer, the content of nervonic acid in Xanthoceras sorbifolia oil is increased. As an unsaturated fatty acid, nervonic acid is an important component of nerve cell membranes, can provide the necessary material basis for the growth and repair of nerve cells, is conducive to the regeneration and repair of damaged nerve cells, and has a certain effect on treating nerve damage and preventing neurodegenerative diseases such as Alzheimer's disease and Parkinson's disease.

[0018] As a further technical solution, the mass ratio of ethanol to isopentenol is 10:2-3.

[0019] In the present invention, the content of nervonic acid in Xanthoceras sorbifolia oil is further increased by adjusting the mass ratio of ethanol to isopentenol to 10:2-3.

[0020] The working principle and beneficial effects of the present invention are: 1. In the present invention, a mixed solvent of petroleum ether and o-phthalic dimethyl ether is used as an extractant. The petroleum ether and o-phthalic dimethyl ether act synergistically to improve the extraction rate.

[0021] 2. In the present invention, tetrafluoroethane is used as the extractant for subcritical fluid extraction. Tetrafluoroethane has a high diffusion coefficient in the subcritical state, can quickly penetrate into the material, fully contact with the extracted material, accelerate the extraction process, shorten the extraction time, and improve production efficiency.

[0022] 3. In the present invention, an entrainer is added to the extractant of the subcritical fluid. The entrainer can reduce the interfacial tension between the subcritical fluid and the extracted substance, making it easier for the subcritical fluid to penetrate into the material and fully contact the extracted substance, thereby accelerating the mass transfer process and improving the extraction rate. When subcritically extracting oils and fats, adding an appropriate amount of entrainer can make the solvent diffuse into the oil cells faster, accelerate the dissolution of oils and fats, and shorten the extraction time. When ethanol is used as an entrainer, ethanol has a certain antioxidant capacity. During the extraction process, it can protect some easily oxidized target components, such as unsaturated fatty acids, from being oxidized and deteriorated, thereby ensuring the activity of the extracted product. DETAILED DESCRIPTION

[0023] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0024] Example 1 A method for extracting Xanthoceras sorbifolia oil using a subcritical fluid comprises the following steps: S1. Take 100 g of Xanthoceras sorbifolia seed kernels, crush them into a particle size of 200 mesh, and dry them to obtain Xanthoceras sorbifolia seed kernel powder; S2, extracting the Xanthoceras sorbifolia seed kernel powder with an extractant at 40° C. for 8 h, concentrating, and drying to obtain a crude Xanthoceras sorbifolia oil; S3, using an extractant to perform subcritical fluid extraction on the crude Xanthoceras sorbifolia oil, separating, and concentrating to obtain Xanthoceras sorbifolia oil; Extraction agents include petroleum ether and phthalic acid; The extractant includes tetrafluoroethane and an entrainer in a mass ratio of 30:1; The entrainer is ethanol; The mass volume ratio of Xanthoceras sorbifolia seed kernel powder to the extractant is 1g:20mL; The volume ratio of petroleum ether to dimethyl ether in the extractant is 20:1; The mass ratio of crude Xanthoceras sorbifolia oil to the extractant was 1:13; During subcritical fluid extraction, the temperature is 50°C, the gas pressure is 1MPa, and the time is 0.5h.

[0025] Example 2 A method for extracting Xanthoceras sorbifolia oil using a subcritical fluid comprises the following steps: S1. Take 100 g of Xanthoceras sorbifolia seed kernels, crush them into a particle size of 100 mesh, and dry them to obtain Xanthoceras sorbifolia seed kernel powder; S2, extracting the Xanthoceras sorbifolia seed kernel powder with an extractant at 30° C. for 10 h, concentrating, and drying to obtain a crude Xanthoceras sorbifolia oil; S3, using an extractant to perform subcritical fluid extraction on the crude Xanthoceras sorbifolia oil, separating, and concentrating to obtain Xanthoceras sorbifolia oil; Extraction agents include petroleum ether and phthalic acid; The extractant includes tetrafluoroethane and an entrainer in a mass ratio of 25:1; The entrainer is ethanol; The mass volume ratio of Xanthoceras sorbifolia seed kernel powder to the extractant is 1g:15mL; The volume ratio of petroleum ether to dimethyl ether in the extractant is 12:1; The mass ratio of crude Xanthoceras sorbifolia oil to the extractant is 1:10; During subcritical fluid extraction, the temperature was 30°C, the gas pressure was 0.8 MPa, and the time was 1 h.

[0026] Example 3 A method for extracting Xanthoceras sorbifolia oil using a subcritical fluid comprises the following steps: S1. Take 100 g of Xanthoceras sorbifolia seed kernels, crush them to a particle size of 150 mesh, and dry them to obtain Xanthoceras sorbifolia seed kernel powder; S2, extracting the Xanthoceras sorbifolia seed kernel powder with an extractant at 35° C. for 9 hours, concentrating, and drying to obtain a crude Xanthoceras sorbifolia oil; S3, using an extractant to perform subcritical fluid extraction on the crude Xanthoceras sorbifolia oil, separating, and concentrating to obtain Xanthoceras sorbifolia oil; Extraction agents include petroleum ether and phthalic acid; The extractant includes tetrafluoroethane and an entrainer in a mass ratio of 27:1; The entrainer is ethanol; The mass volume ratio of Xanthoceras sorbifolia seed kernel powder to the extractant is 1g:18mL; The volume ratio of petroleum ether to dimethyl ether in the extractant is 14:1; The mass ratio of crude Xanthoceras sorbifolia oil to the extractant was 1:12; During subcritical fluid extraction, the temperature was 40°C, the gas pressure was 0.9 MPa, and the time was 0.8 h.

[0027] Example 4 The only difference between this embodiment and embodiment 3 is that the volume ratio of petroleum ether to dimethyl ether in the extracting agent of this embodiment is 18:1.

[0028] Example 5 The only difference between this embodiment and embodiment 3 is that the volume ratio of petroleum ether to dimethyl ether in the extracting agent of this embodiment is 15:1.

[0029] Example 6 The only difference between this embodiment and embodiment 3 is that the volume ratio of petroleum ether to dimethyl ether in the extracting agent of this embodiment is 17:1.

[0030] Example 7 The only difference between this embodiment and embodiment 3 is that the entrainer in this embodiment is ethanol and isopentenol, and the mass ratio of ethanol to isopentenol is 5:2.

[0031] Example 8 The only difference between this embodiment and embodiment 3 is that the entrainer in this embodiment is ethanol and isopentenol, and the mass ratio of ethanol to isopentenol is 10:1.

[0032] Example 9 The only difference between this embodiment and embodiment 3 is that the entrainer in this embodiment is ethanol and isopentenol, and the mass ratio of ethanol to isopentenol is 5:1.

[0033] Example 10 The only difference between this embodiment and embodiment 3 is that the entrainer in this embodiment is ethanol and isopentenol, and the mass ratio of ethanol to isopentenol is 10:3.

[0034] Comparative Example 1 The difference between this comparative example and Example 2 is that the extracting agent in this comparative example is petroleum ether.

[0035] Comparative Example 2 The difference between this comparative example and Example 2 is that the extractant in this comparative example is o-phenylenedimethyl ether.

[0036] Comparative Example 3 A method for extracting Xanthoceras sorbifolia oil using a subcritical fluid comprises the following steps: S1. Take 100 g of Xanthoceras sorbifolia seed kernels, crush them into a particle size of 100 mesh, and dry them to obtain Xanthoceras sorbifolia seed kernel powder; S2, using an extractant to perform subcritical fluid extraction on the Xanthoceras sorbifolia seed kernel powder, separating and concentrating the powder to obtain Xanthoceras sorbifolia oil; The extractant includes tetrafluoroethane and an entrainer in a mass ratio of 25:1; The entrainer is ethanol; The mass ratio of Xanthoceras sorbifolia seed kernel powder to the extractant is 1:10; During subcritical fluid extraction, the temperature was 30°C, the gas pressure was 0.8 MPa, and the time was 1 h.

[0037] Experimental Example 1 The Xanthoceras sorbifolia oils prepared in Examples 1 to 6 and Comparative Examples 1 to 3 were tested according to the following method.

[0038] Extraction rate A (%) = m1 / m; m1 is the mass of Xanthoceras sorbifolia oil; m is the mass of Xanthoceras sorbifolia kernel; The test results are shown in Table 1.

[0039]

[0040] Comparing Example 2 with Comparative Examples 1 to 3, it is shown that the mixed solvent of petroleum ether and phthalic acid is used as the extractant in the present invention, and the petroleum ether and phthalic acid act synergistically to improve the extraction rate of Xanthoceras sorbifolia oil.

[0041] Comparing Examples 5-6 with Examples 3-4, it is shown that when the volume ratio of petroleum ether to phthalic dimethyl ether is 15-17:1, the extraction rate of Xanthoceras sorbifolia oil is further improved.

[0042] Experimental Example 2 The Xanthoceras sorbifolia oil obtained in Examples 3 and 7 to 10 was tested for nervonic acid content according to the following method.

[0043] GC-MS / MS was used for analysis, with an HP-23 column, an injection port temperature of 230°C, a column oven temperature program of 50°C at 15°C / min to 200°C, held for 15 min, 3°C / min to 215°C, held for 10 min, 3°C / min to 230°C, held for 5 min, a carrier gas flow rate of 1 mL / min, an injection volume of 1 μL, and a split ratio of 40:1. The ion source (EI) temperature was 230°C, the transfer line temperature was 245°C, the detection voltage was 1700 V, the solvent delay was 5 min, and the mass scan range (m / z) was 45~400u.

[0044] The test results are shown in Table 2.

[0045]

[0046] Comparing Examples 7 to 10 with Example 3, it is shown that the use of ethanol and prenol as entrainers at the same time increases the content of nervonic acid in Xanthoceras sorbifolia oil. Comparing Examples 9 to 10 with Examples 7 to 8, it is shown that when the mass ratio of ethanol to prenol is 10:2 to 3, the content of nervonic acid in Xanthoceras sorbifolia oil is further increased.

[0047] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for extracting Xanthoceras sorbifolia oil using a subcritical fluid, characterized in that: The following steps are involved: S1. Taking Xanthoceras sorbifolia seed kernels, crushing and drying them to obtain Xanthoceras sorbifolia seed kernel powder; S2, extracting the Xanthoceras sorbifolia seed kernel powder using an extractant, concentrating, and drying to obtain a crude Xanthoceras sorbifolia oil; S3, subjecting the crude Xanthoceras sorbifolia oil to subcritical fluid extraction using an extractant, separating, and concentrating to obtain Xanthoceras sorbifolia oil; The extractant includes petroleum ether and o-phenyl dimethyl ether; The extractant comprises tetrafluoroethane and an entrainer; The entrainer includes ethanol.

2. A method for extracting Xanthoceras sorbifolia oil using a subcritical fluid according to claim 1, characterized in that: The mass volume ratio of the Xanthoceras sorbifolia seed kernel powder to the extractant is 1g:15-20mL.

3. A method for extracting Xanthoceras sorbifolia oil using a subcritical fluid according to claim 1, characterized in that: The volume ratio of petroleum ether to phthalate in the extractant is 15-17:

1.

4. A method for extracting Xanthoceras sorbifolia oil using a subcritical fluid according to claim 1, characterized in that: The extraction temperature is 30-40°C and the extraction time is 8-10 hours.

5. A method for extracting Xanthoceras sorbifolia oil using a subcritical fluid according to claim 1, characterized in that: The mass ratio of the crude Xanthoceras sorbifolia oil to the extractant is 1:10-13.

6. A method for extracting Xanthoceras sorbifolia oil using a subcritical fluid according to claim 1, characterized in that: During the subcritical fluid extraction, the temperature is 30-50° C., the air pressure is 0.8-1 MPa, and the time is 0.5-1 h.

7. The method for extracting Xanthoceras sorbifolia oil using a subcritical fluid according to claim 1, characterized in that: The mass ratio of tetrafluoroethane to entrainer is 25-30:

1.

8. The method for extracting Xanthoceras sorbifolia oil using a subcritical fluid according to claim 1, characterized in that: The particle size of the Xanthoceras sorbifolia seed kernel powder is 100-200 meshes.

9. A method for extracting Xanthoceras sorbifolia oil using a subcritical fluid according to claim 1, characterized in that: The entrainer also includes prenol.

10. The method for extracting Xanthoceras sorbifolia oil using a subcritical fluid according to claim 9, characterized in that: The mass ratio of the ethanol to isopentenol is 10:2-3.

Images