Preparation device of high-purity quercetagetin

Abstract

The utility model belongs to the technical field of natural active substance separation devices, and particularly relates to a preparation device of high-purity quercetagetin. The preparation device of the high-purity quercetagetin comprises the crude extraction system, the solvent recovery system, the crude product separation system and the recrystallization separation system, the purpose of combining and optimizing unit operation can be achieved, key links for preparing the high-purity quercetagetin are completed in series connection, the one-time investment cost of equipment is low, and the equipment is suitable for large-scale production. And continuous operation can be realized, and the production efficiency can be improved.

Description

Technical Field

[0001] The utility model belongs to the technical field of natural active substance separation devices, and particularly relates to a preparation device for high-purity quercetin. Background Art

[0002] Marigold (Tagetes erecta L.) is an annual herb of the genus Tagetes in the Asteraceae family. It mainly contains flavonoids, carotenoids, terpenes, glycosides, essential oils and other substances. Quercetin is a flavonoid compound that can be extracted and separated from it.

[0003] Obtaining high-purity quercetin from marigold requires a series of process flows. In the early stages, the main parts of marigold containing quercetin are subjected to crude extraction processes such as extraction, concentration, and filtration. In order to obtain a product with higher purity, a refining process is usually required in the later stages to improve the product purity.

[0004] The prior art disclosed in publication number CN105541775A mixes marigold residue with alcohol, extracts it using ultrasound, and then centrifuges, concentrates, centrifuges, and purifies it to obtain a quercetin product. However, the purity of the quercetin product extracted and prepared by this method is only 80-85%, with a yield of 2.5-3.8%. The prior art CN102190646B (a method for preparing high-purity quercetin) uses a 5-90% ethanol aqueous solution to extract a crude quercetin extract from the residue after extracting marigold lutein lipids. The extract is then concentrated under reduced pressure to a paste. The quercetin is then separated and purified from the quercetin-containing solution using a preparative high-speed countercurrent chromatograph to obtain quercetin. HPLC analysis shows a purity of over 95%. However, this separation method has a low yield and is difficult to achieve continuous production, which is easily limited in industrialization. In addition, the prior art CN110776449B (an industrial method for extracting lutein and quercetin) uses an acetone solution to fully extract lutein and quercetin from marigold flowers, and separates them by extraction with a low-grade alcohol solution to obtain two products. However, the acetone concentration and concentration level must be strictly controlled throughout the entire process to achieve a good refining effect, making it difficult to control the product quality of each batch of products.

[0005] Therefore, it is of great significance to provide a preparation device for high-purity quercetin. Utility Model Content

[0006] The present invention aims to solve one or more technical problems existing in the above-mentioned prior art and at least provide a beneficial alternative or create conditions. Specifically, the present invention aims to provide a high-purity quercetin preparation device, focusing on improving preparation efficiency and ensuring product purity. The device can complete the key steps in the preparation of high-purity quercetin, has a low one-time investment cost, can achieve continuous operation, and helps improve production efficiency.

[0007] To achieve the above objectives, the present invention is implemented through the following technical solutions:

[0008] A device for preparing high-purity quercetin comprises a crude extraction system, a solvent recovery system, a crude product separation system and a recrystallization separation system. The crude extraction system consists of a first heater 1, a jacketed extraction kettle 2, a stirring paddle with a hanging basket 3 and an extraction solvent delivery pump 4; the solvent recovery system consists of a second heater 5, an evaporation chamber 6, a condenser 7, a cooler 8 and a liquid collector 9; the crude product separation system consists of a first buffer tank 10, a centrifugal liquid storage device 11 and a spray liquid storage tank 12; the recrystallization separation system consists of a second buffer tank 13, a jacketed vertical crystallization device 14, a stirring paddle 14-1, a stirring paddle transmission device 14-2, a centrifugal frame 14-3, a centrifugal frame transmission device 14-4, a crystallization solvent storage tank 14-5, a mother liquor pump 14-6, a mother liquor tank 14-7 and a mother liquor solvent recovery pump 14-8.

[0009] In the crude extraction system, the first heater 1 provides a heat source for the jacketed extraction kettle 2, the hanging basket is used to place the extract raw materials, and the extraction solvent inlet of the extraction kettle is connected to the liquid collector 9 of the solvent recovery system through the extraction solvent delivery pump.

[0010] In the solvent recovery system, the material inlet of the second heater 5 is connected to the extract outlet of the extraction crude extraction system, the second heater 5 and the evaporation chamber 6 are connected via a liquid reflux pipe with a valve, the top of the evaporation chamber 6 is connected to a condenser 7, the condenser 7 is connected to a liquid collector 9 via a cooler 8, and the bottom of the liquid collector 9 is connected to the extraction kettle 2 of the extraction crude extraction system via an extraction solvent delivery pump 4.

[0011] In the coarse product separation system, the lower part of the first buffer tank 10 is a conical structure; the centrifugal liquid storage device 11 is a square structure, and the centrifugal liquid storage device 11 is composed of a top spray pipe 11-1, an upper centrifugal assembly and a bottom liquid storage tank 11-4. The inlet of the centrifugal liquid storage device 11 is connected to the lower outlet of the first buffer tank 10, and a solenoid valve 11-5 is arranged between the connected pipes; the top spray pipe 11-1 is connected to the spray liquid storage tank 12.

[0012] In the coarse product separation system, the upper centrifugal assembly in the centrifugal liquid storage device 11 includes a drying drum 11-2 and a motor 11-3 for driving the drying drum to rotate.

[0013] In the recrystallization separation system, the inlet of the second buffer tank 13 is connected to the bottom liquid storage tank 11-4 of the centrifugal liquid storage device 11 of the coarse product separation system, and the outlet of the second buffer tank 13 is connected to the jacketed vertical crystallization device 14. The jacket inlet and outlet of the jacketed vertical crystallization device 14 are connected to the refrigeration circulating liquid; its liquid discharge port forms two branches after passing through the mother liquid pump 14-6, which are the first transport pipeline F1 connected to the liquid inlet of the jacketed vertical crystallization device and the second transport pipeline F2 connected to the mother liquid tank 14-7.

[0014] Compared with the prior art, the present invention can achieve the following beneficial effects:

[0015] The utility model can increase the separation capacity through dynamic monitoring and flexible control, can realize continuous and automated production, can greatly improve the output and efficiency, and ensure the stability and reliability of product quality.

[0016] The utility model can quickly and effectively recover the solvent in the purified extract, concentrate the quercetin purified liquid with low loss, and efficiently transition to the next unit operation, thereby realizing continuous serial connection of the process flow and jointly completing the process flow for preparing high-purity quercetin.

[0017] The utility model can further precipitate the purified quercetin in the form of crystals, quickly realize solid-liquid separation, and ensure the recovery and reuse of the crystallization solvent, thereby realizing continuous serial connection of the process flow and jointly completing the process flow for preparing high-purity quercetin.

[0018] In general, the utility model can complete the key steps of preparing high-purity quercetin, the one-time investment cost of the equipment is relatively low, continuous operation can be achieved, and production efficiency is improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 This is a schematic diagram of the serial connection of the various block system processes of the present utility model;

[0020] Figure 2 It is a schematic diagram of the device of the present utility model.

[0021] Figure 2In: 1- the first heater of the crude extraction system, 2- the jacketed extraction kettle of the crude extraction system, 3- the stirring paddle with hanging basket of the crude extraction system, 4- the extraction solvent delivery pump of the crude extraction system; 5- the second heater of the solvent recovery system, 6- the evaporation chamber of the solvent recovery system, 7- the condenser of the solvent recovery system, 8- the cooler of the solvent recovery system, 9- the liquid collector of the solvent recovery system; 10- the first buffer tank of the crude product separation system, 11- the centrifugal liquid storage device of the crude product separation system, 11-1- the top spray pipe, 11-2- the spin drying drum, 11-3- the motor driving the spin drying drum to rotate, 11-4- the bottom liquid storage tank and 11-5- the electromagnetic valve, 12- the spray liquid storage tank of the crude product separation system, 13-the second buffer tank of the recrystallization separation system, 14-the jacketed vertical crystallization equipment of the recrystallization separation system, 14-1-the stirring paddle of the jacketed vertical crystallization equipment, 14-2-the stirring paddle transmission equipment of the jacketed vertical crystallization equipment, 14-3-the centrifugal frame of the jacketed vertical crystallization equipment, 14-4-the centrifugal frame transmission equipment of the jacketed vertical crystallization equipment, 14-5-the crystallization solvent storage tank of the jacketed vertical crystallization equipment, 14-6-the mother liquor pump of the jacketed vertical crystallization equipment, 14-7-the mother liquor tank of the jacketed vertical crystallization equipment, 14-8-the mother liquor solvent recovery pump, F1-the first transport pipeline connecting the access liquid inlet of the jacketed vertical crystallization equipment, F2-the second transport pipeline connecting the mother liquor tank. DETAILED DESCRIPTION

[0022] In order to make the technical solution of the present invention more clearly understood by those skilled in the art, the following examples are given for illustration. It should be noted that the following examples do not limit the scope of protection claimed by the present invention.

[0023] Unless otherwise specified, the raw materials, reagents, or devices used in the following examples can be obtained from conventional commercial sources or by existing known methods.

[0024] Reference Figure 1 As shown, in this embodiment, the crude extraction system, the solvent recovery system, the crude product separation system and the recrystallization separation system are connected in sequence.

[0025] Reference Figure 2As shown, the preparation device of high-purity quercetin includes an extraction crude extraction system, a solvent recovery system, a crude product separation system and a recrystallization separation system. The extraction crude extraction system consists of a first heater 1, a jacketed extraction kettle 2, a stirring paddle with a hanging basket 3 and an extraction solvent delivery pump 4; the solvent recovery system consists of a second heater 5, an evaporation chamber 6, a condenser 7, a cooler 8 and a liquid collector 9; the crude product separation system consists of a first buffer tank 10, a centrifugal liquid storage device 11 and a spray liquid storage tank 12; the recrystallization separation system consists of a second buffer tank 13, a jacketed vertical crystallization device 14, a stirring paddle 14-1, a stirring paddle transmission device 14-2, a centrifugal frame 14-3, a centrifugal frame transmission device 14-4, a crystallization solvent storage tank 14-5, a mother liquor pump 14-6, a mother liquor tank 14-7 and a mother liquor solvent recovery pump 14-8. The jacket inlet and outlet of the jacketed vertical crystallization equipment 14 are connected to the refrigeration circulating liquid; its liquid discharge port forms two branches after passing through the mother liquid pump 14-6, which are the first transport pipeline F1 connected to the liquid inlet of the jacketed vertical crystallization equipment and the second transport pipeline F2 connected to the mother liquid tank 14-7.

[0026] The marigold residue after lutein extraction is used as raw material and placed in the hanging basket of the extraction crude extraction system. The extraction solvent is introduced into the extraction solvent inlet of the jacketed extraction kettle 2 through the extraction solvent delivery pump 4. The first heater 1 provides a heat source for the jacketed extraction kettle 2. A certain extraction time is set to extract quercetin.

[0027] The extracted liquid is transported to the second heater 5 of the solvent recovery system, and evaporated and concentrated by the evaporation chamber 6, condenser 7, and cooler 8. The evaporated solvent is stored in the liquid collector 9 for testing.

[0028] Solvent is added to the extraction solvent inlet of jacketed extraction kettle 2 to form a crude liquid to be separated. The crude liquid to be separated passes through first buffer tank 10 for buffering and sedimentation, then waits in an orderly manner. After solenoid valve 11-5 opens according to the operating procedure, the crude liquid enters the spin-drying drum 11-2 according to the set weight. Solenoid valve 11-5 closes, and motor 11-3, which drives the spin-drying drum, begins to operate. The spin-drying drum then rotates at high speed, removing the solvent and achieving solid-liquid separation. Spray liquid from spray liquid storage tank 12 is sprayed and washed through spray pipe 11-1 to obtain crude quercetin. The crude product in the spin-drying drum is discharged, and solvent is added to form a liquid to be recrystallized.

[0029] The liquid to be recrystallized is transferred to the second buffer tank 13 of the recrystallization separation system and placed in a jacketed vertical crystallization device 14. The cooling speed is controlled by the jacketed freezing liquid, and the temperature is slowly lowered to 5°C for freezing precipitation. The above-mentioned crystallization mother liquor is transferred to the centrifugal frame through the mother liquor pump 14-6, and the crystallized material is centrifuged by the centrifugal frame transmission device 14-4 until no filtrate flows out to obtain a filter cake. The mother liquor is transported to the mother liquor tank 14-7 via the mother liquor pump 14-6. The quercetin obtained by centrifugation needs to meet the purity requirements before it can be sent to the drying equipment for drying. Otherwise, it is transferred to the vertical crystallization equipment again through the mother liquor pump and the above operation is repeated to ensure that each batch of products can meet the high purity requirements. The solvent in the mother liquor tank is connected to the heater pipeline of the solvent recovery system through a pipeline to achieve solvent reuse.

[0030] As described above, the utility model provides a useful preparation device for obtaining high-purity quercetin, which can complete the key steps of preparing high-purity quercetin, has a low one-time investment cost, can realize continuous operation, and helps to improve production efficiency.

[0031] The above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present invention may be modified or replaced by equivalents without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. A preparation device for high-purity quercetin, comprising a crude extraction system, a solvent recovery system, a crude product separation system, and a recrystallization separation system, characterized in that: The crude extraction system is composed of a first heater (1), a jacketed extraction kettle (2), a stirring blade with a hanging basket (3), and an extraction solvent delivery pump (4); the solvent recovery system is composed of a second heater (5), an evaporation chamber (6), a condenser (7), a cooler (8), and a liquid collector (9); the crude product separation system is composed of a first buffer tank (10), a centrifugal liquid storage device (11), and a spray liquid storage tank (12); the recrystallization separation system is composed of a second buffer tank (13), a jacketed vertical crystallization device (14), a stirring blade (14-1), a stirring blade transmission device (14-2), a centrifugal frame (14-3), a centrifugal frame transmission device (14-4), a crystallization solvent storage tank (14-5), a mother liquor pump (14-6), a mother liquor tank (14-7), and a mother liquor solvent recovery pump (14-8); In the solvent recovery system, the material inlet of the second heater (5) is connected to the extract outlet of the crude extraction system; The extraction solvent inlet of the jacketed extraction kettle (2) is connected to the liquid collector (9) of the solvent recovery system through the extraction solvent delivery pump (4); The inlet at the top of the first buffer tank (10) is connected to the outlet at the bottom of the evaporation chamber (6); The inlet of the second buffer tank (13) is connected to the bottom liquid storage tank (11-4) of the centrifugal liquid storage device (11) of the coarse product separation system.

2. The preparation device according to claim 1, characterized in that: In the crude extraction system, the first heater (1) provides a heat source for the jacketed extraction kettle (2), and the hanging basket is used to place the extract raw material.

3. The preparation device according to claim 1, characterized in that: In the solvent recovery system, the material inlet of the second heater (5) is connected to the extract outlet of the crude extraction system, the second heater (5) and the evaporation chamber (6) are connected via a liquid reflux pipe with a valve, the top of the evaporation chamber (6) is connected to a condenser (7), and the condenser (7) is connected to a liquid collector (9) via a cooler (8).

4. The preparation device according to claim 1, characterized in that: In the crude product separation system, the lower portion of the first buffer tank (10) is a conical structure; the centrifugal liquid storage device (11) is a square structure, and the centrifugal liquid storage device (11) is composed of a top spray pipe (11-1), an upper centrifugal assembly and a bottom liquid storage tank (11-4); the inlet of the centrifugal liquid storage device (11) is connected to the lower outlet of the first buffer tank (10), and a solenoid valve (11-5) is provided between the connected pipes; the top spray pipe (11-1) is connected to the spray liquid storage tank (12).

5. The preparation device according to claim 4, characterized in that: In the crude product separation system, the upper centrifugal assembly in the centrifugal liquid storage device (11) includes a spin-drying drum (11-2) and a motor (11-3) for driving the spin-drying drum to rotate.

6. The preparation device according to claim 1, characterized in that: In the recrystallization separation system, the outlet of the second buffer tank (13) is connected to the jacketed vertical crystallization device (14), and the jacket inlet and outlet of the jacketed vertical crystallization device (14) are connected to the refrigeration circulating liquid; Its liquid discharge port forms two branches after passing through the mother liquid pump (14-6), namely a first transport pipeline (F1) connected to the liquid inlet of the jacketed vertical crystallization equipment (14) and a second transport pipeline (F2) connected to the mother liquid tank (14-7).

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