Separation and purification device for a new chlorogenic acid

Abstract

The utility model discloses a kind of separation and purification devices of new chlorogenic acid, including dissolving tank, reaction tank, buffer tank one, macroporous adsorption resin system, buffer tank two, drying tank one, crystallization tank one, plate and frame filter one, crystallization tank two, plate and frame filter two, drying tank two, new chlorogenic acid storage tank;Dissolving tank is connected with ethanol solution storage tank one and pH regulator storage tank one;Buffer tank one is connected with pH regulator storage tank two;Macroporous adsorption resin system includes first resin column, second resin column, third resin column;The liquid inlet of first resin column is connected with acid solution storage tank, and the liquid inlet of first resin column, second resin column is all connected with ethanol solution storage tank two;Buffer tank two is connected with pH regulator storage tank three.This device uses stevia chlorogenic acid crude product as raw material, through isomerization, macroporous resin separation, crystallization treatment improves the purity and yield of new chlorogenic acid, waste liquid in recovery process is recycled, and it is economic and environmental protection.

Description

Technical Field

[0001] This utility model relates to the field of neochlorogenic acid preparation technology, specifically to a neochlorogenic acid separation and purification device. Background Technology

[0002] Neochlorogenic acid, an important isomer of chlorogenic acid, is a phenylpropanoid active compound found in various plants such as stevia, honeysuckle, eucommia, and photinia. Modern pharmacological studies have shown that this component possesses a variety of biological activities, including antioxidant, antitumor, antibacterial, antiviral, blood pressure lowering, uric acid lowering, and cardiovascular system protection, demonstrating broad application prospects in the fields of medicine, health food, and cosmetics.

[0003] Currently, the extraction and purification of neochlorogenic acid from plants faces numerous challenges. Firstly, the content of neochlorogenic acid in plant tissues is far lower than that of chlorogenic acid, and its physicochemical properties are very similar to many structural analogs, making the efficient separation of high-purity neochlorogenic acid monomers extremely difficult. Furthermore, traditional methods for extraction and preliminary enrichment often rely on solvent extraction processes, generating large amounts of organic waste. While advanced technologies such as high-pressure preparative chromatography can also be used for the purification of neochlorogenic acid, they involve high equipment maintenance and operating costs, and require extremely stringent separation conditions. Therefore, providing a separation and purification device for neochlorogenic acid to achieve efficient separation and reduce the generation of waste is of great significance. Utility Model Content

[0004] The technical problem to be solved by this utility model is to provide a separation and purification device for chlorogenic acid, which addresses the shortcomings of the existing technology. The device uses crude chlorogenic acid from stevia as raw material and effectively improves the purity and yield of chlorogenic acid by combining isomerization, macroporous resin adsorption, separate analysis and multiple crystallization. All waste liquid in the recovery process is recycled, which is economical and environmentally friendly.

[0005] To solve the above-mentioned technical problems, the technical solution of this utility model is as follows:

[0006] A new chlorogenic acid separation and purification device includes a dissolving tank, a reaction tank, a buffer tank 1, a macroporous adsorption resin system, a buffer tank 2, a drying tank 1, a crystallization tank 1, a plate and frame filter 1, a crystallization tank 2, a plate and frame filter 2, a drying tank 2, and a new chlorogenic acid storage tank connected in sequence.

[0007] The dissolving tank is connected to an ethanol solution storage tank and a pH adjuster storage tank; the reaction tank is connected to a vacuum pump and a nitrogen storage tank; the buffer tank is connected to a pH adjuster storage tank; the macroporous adsorption resin system includes a first resin column, a second resin column, and a third resin column connected in series; the inlet of the first resin column is connected to an acid storage tank, and the inlets of both the first and second resin columns are connected to an ethanol solution storage tank; the buffer tank is connected to a pH adjuster storage tank; the crystallization tank is connected to an acetone storage tank and a chlorogenic acid seed crystal storage tank; the crystallization tank is connected to a purified water storage tank and a pH adjuster storage tank.

[0008] Preferably, the outlet of the eluent from the first resin column is connected to the dissolving tank.

[0009] Preferably, the filtrate outlet of the plate and frame filter press is connected to the buffer tank via a concentration tank.

[0010] Preferably, the jackets of the dissolving tank, reaction tank, buffer tank 1, buffer tank 2, crystallizing tank 2, drying tank 1, drying tank 2, and concentration tank are all equipped with baffles.

[0011] Preferably, the filtrate outlet of the second plate and frame filter press is connected to the second buffer tank.

[0012] Preferably, the reaction vessel is equipped with a pressure sensor and a temperature sensor.

[0013] Preferably, the dissolving tank, buffer tank one, buffer tank two, and crystallizing tank two are all equipped with pH sensors.

[0014] By adopting the above technical solution, this utility model has at least the following beneficial effects:

[0015] This invention provides a device for separating and purifying neochlorogenic acid. The device first dissolves crude stevia chlorogenic acid containing neochlorogenic acid, and then performs isomerization, adsorption, desorption, and crystallization treatments to recover high-purity neochlorogenic acid from the crude stevia chlorogenic acid.

[0016] The macroporous adsorption resin system of this device uses three resin columns connected in series. This series connection of multiple resin columns can achieve highly selective adsorption of the target product neochlorogenic acid and deeply remove impurities, thereby effectively separating neochlorogenic acid from other components in the feed solution, which is convenient for subsequent crystallization and purification.

[0017] This device employs stepwise crystallization in crystallizer tank one and crystallizer tank two, effectively removing specific impurities that are difficult to separate in a single crystallizer, thereby improving product purity. All waste liquid generated during the separation and purification process is recycled, increasing raw material utilization and reducing production costs.

[0018] This device uses multiple pH adjustment tanks to precisely control the pH in each processing step, ensuring the smooth separation and purification of neochlorogenic acid and improving product yield and purity.

[0019] This device incorporates baffles within the jackets of multiple tanks, significantly enhancing the turbulence of the heat exchange medium within the jackets and disrupting the laminar boundary layer. This substantially increases heat exchange efficiency, ensuring that the material within the tanks can quickly and uniformly reach and maintain the target temperature, thereby improving the separation and purification efficiency of chlorogenic acid. Attached Figure Description

[0020] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0021] Figure 1 This is a schematic diagram of the structure of Embodiment 1 of this utility model;

[0022] Figure 2 yes Figure 1 Enlarged structural diagram at point A;

[0023] In the diagram, 1. Dissolving tank; 2. Reaction tank; 3. Buffer tank one; 4. Macroporous adsorption resin system; 401. First resin column; 402. Second resin column; 403. Third resin column; 5. Buffer tank two; 6. Crystallization tank one; 7. Plate and frame filter one; 8. Crystallization tank two; 9. Plate and frame filter two; 10. Drying tank two; 11. New chlorogenic acid storage tank; 12. Ethanol solution storage tank one; 13. pH adjuster storage tank one; 14. 15. Vacuum pump; 16. Nitrogen storage tank; 17. pH adjuster storage tank II; 18. Acid storage tank; 19. Ethanol solution storage tank II; 20. pH adjuster storage tank III; 21. Acetone storage tank; 22. Neochlorogenic acid seed crystal storage tank; 23. Purified water storage tank; 24. pH adjuster storage tank IV; 25. Concentrator; 26. Baffle plate; 27. Pressure sensor; 28. Temperature sensor; 29. ​​pH sensor; 20. Drying tank I. Detailed Implementation

[0024] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present utility model.

[0025] Example 1

[0026] like Figure 1-2 As shown in the figure, a new chlorogenic acid separation and purification device includes a dissolving tank 1, a reaction tank 2, a buffer tank 3, a macroporous adsorption resin system 4, a buffer tank 2 5, a drying tank 29, a crystallization tank 6, a plate and frame filter 7, a crystallization tank 2 8, a plate and frame filter 2 9, a drying tank 2 10, and a new chlorogenic acid storage tank 11, which are connected in sequence.

[0027] The dissolving tank 1 is connected to an ethanol solution storage tank 12 and a pH adjuster storage tank 13; the reaction tank 2 is connected to a vacuum pump 14 and a nitrogen storage tank 15; the buffer tank 3 is connected to a pH adjuster storage tank 16; the macroporous adsorption resin system 4 includes a first resin column 401, a second resin column 402, and a third resin column 403 connected in series; the inlet of the first resin column 401 is connected to an acid storage tank 17, and the inlets of the first resin column 401 and the second resin column 402 are both connected to an ethanol solution storage tank 18; the buffer tank 5 is connected to a pH adjuster storage tank 19; the crystallization tank 6 is connected to an acetone storage tank 20 and a chlorogenic acid seed crystal storage tank 21; the crystallization tank 8 is connected to a purified water storage tank 22 and a pH adjuster storage tank 23.

[0028] This device first converts other isomers of crude stevia chlorogenic acid into neochlorogenic acid through an isomerization reaction. Then, it uses a multi-stage series macroporous adsorption resin system 4 to initially separate and enrich the neochlorogenic acid. Finally, it combines two-step crystallization treatment to obtain high-purity neochlorogenic acid.

[0029] In this embodiment, the outlet of the eluent from the first resin column 401 is connected to the dissolving tank 1. The outlet of the filtrate from the plate and frame filter 7 is connected to the buffer tank 3 via the concentration tank 24. The outlet of the filtrate from the second plate and frame filter 9 is connected to the second buffer tank 5. This arrangement allows for the recycling of waste liquid during the separation process, thereby improving raw material utilization and reducing waste emissions.

[0030] In this embodiment, baffles 25 are provided inside the jackets of the dissolving tank 1, reaction tank 2, buffer tank 3, buffer tank 5, crystallizing tank 8, drying tank 29, drying tank 10, and concentration tank 24. The baffles 25 enhance heat transfer efficiency, thereby improving the separation and purification efficiency of chlorogenic acid.

[0031] In this embodiment, the reaction vessel 2 is equipped with a pressure sensor 26 and a temperature sensor 27; the dissolving vessel 1, buffer vessel 3, buffer vessel 5, and crystallizing vessel 8 are all equipped with pH sensors 28. These features enable precise monitoring and control of conditions in each step, ensuring the stability of each process and thus improving product quality.

[0032] The working principle of this device is as follows:

[0033] Crude stevia chlorogenic acid is added to dissolving tank 1. A certain concentration of ethanol solution is added to dissolving tank 1 through ethanol solution storage tank 12, and the mixture is stirred to dissolve. The pH is adjusted by adding pH adjuster through pH adjuster storage tank 13, and then the mixture is introduced into reaction tank 2. A vacuum pump 14 is used to create a negative pressure to a certain value, and then nitrogen is added through nitrogen storage tank 15 to bring the pressure to atmospheric pressure. This process is repeated 3-5 times. The mixture is then heated to carry out an isomerization reaction. After the reaction, the solution is introduced into buffer tank 3, cooled to room temperature, and the pH is adjusted. It is then pumped into macroporous adsorption resin system 4 for adsorption treatment. The solution in acid storage tank 17 is used for top-feeding, and then ethanol solution in ethanol solution storage tank 18 is used to precipitate the first resin column 401. The precipitate is recovered back to dissolving tank 1 and then discharged through ethanol solution storage tank 18. The ethanol solution of column 18 is used to elute the second resin column 402 and the third resin column 403. The elution solution enters the buffer tank 25, and after pH adjustment, it is dried in the drying tank 29. The dried material enters the crystallization tank 6. Acetone is added to the crystallization tank 6 through the acetone storage tank 20, and after stirring and dissolving, chlorogenic acid seed crystals are added. The crystallization is carried out at room temperature with stirring. The crystallization solution is filtered through the plate and frame filter press 7. The filtrate is desolvated in the concentration tank 24 and recovered into the buffer tank 3. The filter cake is pumped into the crystallization tank 28, purified water is added, the pH is adjusted, and the temperature is raised and stirred until the solid dissolves. The pH is adjusted again, and the temperature is slowly lowered for crystallization. Finally, the crystallization solution is filtered through the plate and frame filter press 29. The filtrates are combined into the buffer tank 25, and the filter cake is dried in the drying tank 210 and then enters the chlorogenic acid storage tank 11.

[0034] The above description of the disclosed embodiments enables those skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A new chlorogenic acid separation and purification device, characterized in that: It includes, in sequence, a dissolving tank, a reaction tank, a buffer tank 1, a macroporous adsorption resin system, a buffer tank 2, a drying tank 1, a crystallizing tank 1, a plate and frame filter 1, a crystallizing tank 2, a plate and frame filter 2, a drying tank 2, and a chlorogenic acid storage tank; The dissolving tank is connected to an ethanol solution storage tank and a pH adjuster storage tank; the reaction tank is connected to a vacuum pump and a nitrogen storage tank; the buffer tank is connected to a pH adjuster storage tank; the macroporous adsorption resin system includes a first resin column, a second resin column, and a third resin column connected in series; the inlet of the first resin column is connected to an acid storage tank, and the inlets of both the first and second resin columns are connected to an ethanol solution storage tank; the buffer tank is connected to a pH adjuster storage tank; the crystallization tank is connected to an acetone storage tank and a chlorogenic acid seed crystal storage tank; the crystallization tank is connected to a purified water storage tank and a pH adjuster storage tank.

2. The separation and purification apparatus for neochlorogenic acid according to claim 1, characterized in that: The outlet of the first resin column is connected to the dissolving tank.

3. The apparatus for separating and purifying neochlorogenic acid according to claim 1, characterized in that: The filtrate outlet of plate and frame filter press one is connected to buffer tank one through a concentration tank.

4. The apparatus for separating and purifying neochlorogenic acid according to claim 3, characterized in that: The jackets of the dissolving tank, reaction tank, buffer tank 1, buffer tank 2, crystallizing tank 2, drying tank 1, drying tank 2, and concentration tank are all equipped with baffles.

5. The apparatus for separating and purifying neochlorogenic acid according to claim 1, characterized in that: The filtrate outlet of the second plate and frame filter press is connected to the second buffer tank.

6. The apparatus for separating and purifying neochlorogenic acid according to claim 1, characterized in that: The reaction vessel is equipped with pressure and temperature sensors.

7. The apparatus for separating and purifying neochlorogenic acid according to claim 1, characterized in that: pH sensors are installed in the dissolving tank, buffer tank one, buffer tank two, and crystallizing tank two.

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