Supercritical fluid extraction, rectification and chromatography preparation device and control method thereof
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A technology for supercritical fluid and preparation device, applied in the field of chromatography devices, can solve the problem of high cost consumption, and achieve the effects of reducing labor intensity, saving labor costs, and ensuring safe operation.
Active Publication Date: 2016-07-06
DALIAN POLYTECHNIC UNIVERSITY
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[0005] In order to solve the problems of high-efficiency, high-quality, automatic separation of compounds and high cost consumption, the present invention provides a supercritical fluid extraction, rectification, and chromatographic preparation device, which can perform efficient, high-quality, automatic separation of compounds, and reduce energy consumption few
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Embodiment 1
[0052] The raw material is the deodorized distillate of soybean oil, which has been methylated, and the natural vitamin E content is 6.27%.
[0053] The single-column mode of the rectification tower is used to open the first stop valve T1, the third stop valve T3, the tenth stop valve T10, the sixth stop valve T6, and the seventh stop valve T7 to form the flow direction of the liquid path; the soybean oil deodorization distillate is obtained by Feed pump 9 is transported to the first rectification tower 10 through the first feed branch pipe 9a, the first feed inlet 9c, rectification sample and supercritical CO 2 Dissolved, the dissolved part is subjected to rectification treatment on the sample through the temperature gradient of the rectification tower, and then the first CO at the upper end of the first rectification tower 10 2 The output branch pipe 10g, the rectifying tower pipeline 10b, enter the first separation kettle 7 and the second separation kettle 8 in turn, and di...
Embodiment 2
[0059] The raw material is fish oil, which has been ethyl-esterified, and the content of EPA and DHA is 30%.
[0060] The conditions of supercritical fluid distillation are as follows: temperature gradient of rectification tower (from bottom to top): 40-90°C; first separation tank: 45°C; second separation tank: 45°C; feeding port: feeding port in Section 3; Feeding speed: 1mL / min; CO 2 Flow rate: 100mL / min; pressure: 15MPa, keep for 5h.
[0061] Supercritical fluid chromatography conditions are as follows: Chromatographic column packing: silica gel (300-400 mesh); extraction kettle, first separation kettle, 2 temperature: 40°C; extraction kettle, first separation kettle pressure: 15MPa; second separation kettle pressure: 1 MPa; CO 2 Flow rate: 100mL / min, hold for 30min, enrich EPA and DHA.
[0062] After product analysis, the natural vitamin E content increased from 30% to 96%, and the recovery rate was 90.44%.
[0063] The invention has the advantages of no reagent consum...
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Abstract
The invention discloses a supercritical fluid extraction, rectification and chromatography preparation device and belongs to the technical field of chromatography devices. The supercritical fluid extraction part of the device comprises an extraction kettle, a first separation kettle, a second separation kettle, a CO2 conveying pump and a feeding pump; the supercritical fluid rectification part of the device comprises a rectification tower, the first separation kettle, the second separation kettle, the CO2 conveying pump and the feeding pump; the supercritical fluid chromatography part of the device comprises a chromatography column, the first separation kettle, the second separation kettle, the CO2 conveying pump and the feeding pump. The three parts control and monitor various indexes of the device through programmable logic controllers (PLCs), and an automatic control system capable of separating natural products is formed. The device has the advantages that operating manners of the device are regulated by changing the opening and closing states of valves and flow path directions, and the device is efficient and continuous in process, low in manpower and time costs, low in labor intensity of workers, capable of continuously, intelligently and efficiently separating the natural products, free of waste generation in the whole process, and environmental friendly.
Description
technical field [0001] The invention relates to a supercritical fluid extraction, rectification, chromatographic preparation device and a control method thereof, belonging to the technical field of chromatographic devices. Background technique [0002] The traditional compound separation method has a long period, high operating temperature, and a fixed value of solvent solubility, which can only be changed by changing the type or proportion of the solvent. After the test, additional operations are required to remove excess reagents, resulting in increased costs and a large amount of waste reagents, causing environmental pollution. The problem of solvent residue in the sample is unavoidable, and it is easy to cause unknown influence on the test results. Therefore, the development of efficient and energy-saving separation and preparation devices has always been the focus of the separation field. [0003] Supercritical fluid has many unique properties, such as low viscosity, ...
Claims
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