Method and device for separating and purifying oxymatrine from oxymatrine eluate

Through the use of the electrodialysis device system, combined with the ultrafiltration membrane and the ion exchange membrane, the problems of many impurities and high energy consumption in the preparation process of oxidized malphurica are solved, and the separation of high-purity oxidized malphurica and the recovery of sodium chloride and hydrochloric acid are achieved, which improves the economic benefits and environmental protection of the process.

CN117000051BActive Publication Date: 2025-04-18ANHUI UNIVERSITY OF TRADITIONAL CHINESE MEDICINE
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Patent Information

Application Number
CN202311009126.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-08-08
Publication Date
2025-04-18
Estimated Expiration
2043-08-08

AI Technical Summary

Technical Problem

The existing preparation process of oxidized malphuridium has problems such as many impurities, high energy consumption, complex process and low separation efficiency, making it difficult to achieve green manufacturing of traditional Chinese medicine.

Method used

The electrodialysis device system, including the first and second stage electrodialysis devices, uses the combination of ultrafiltration membrane and ion exchange membrane to achieve efficient separation and purification of oxidized malpine through electric field action.

Benefits of technology

The high-purity (greater than 98%) oxidized matrine was achieved from the oxidized matrine eluent, and sodium chloride and hydrochloric acid were recovered, improving the economic benefits and environmental protection of the process.

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Abstract

The present invention discloses a method and device for separating and purifying oxymatrine from an oxymatrine eluate. The device comprises a first-stage electrodialysis device and a second-stage electrodialysis device which are sequentially arranged, and the method for separating and purifying oxymatrine comprises: firstly separating the oxymatrine eluate by the first-stage electrodialysis device to obtain a solution rich in oxymatrine, and then purifying the oxymatrine-rich solution by the second-stage electrodialysis device to obtain high-purity oxymatrine. The method is an ion-level membrane separation method with high efficiency, low energy consumption and environmental friendliness, and can obtain high-purity oxymatrine from the oxymatrine eluate.
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Description

Technical Field

[0001] The invention belongs to the technical field of traditional Chinese medicine extraction, and particularly relates to a method and a device for separating and purifying oxymatrine from oxymatrine eluate. Background Art

[0002] Sophora flavescens is the dried root of Sophora flavescens, a plant of the genus Sophora flavescens in the Leguminosae family. It has the effects of clearing away heat and dampness, killing insects, and acting as a diuretic. It is widely used in clinical practice for diseases caused by dampness and heat. It has high medicinal value and significant therapeutic effects. The main components of Sophora flavescens include alkaloids, flavonoids, triterpenoid saponins, amino acids, etc. Among them, matrine and flavonoid glycosides are the main active ingredients, which have multiple pharmacological activities such as anti-inflammatory, anti-tumor, antibacterial, antiarrhythmic, diuretic, immune regulation, analgesia, etc., and have very wide medicinal value. Oxymatrine is the alkaloid with the highest content in Sophora flavescens, with a molecular formula of C 15 H 24 N202 belongs to the quinolizidine alkaloids. Liver disease is a common and extremely harmful disease, and oxymatrine has good pharmacological activity in antiviral hepatitis and has been approved by the Ministry of Health as a new drug of Class V for the treatment of chronic hepatitis B.

[0003] The existing preparation process of oxymatrine is generally divided into two steps: extraction and separation and purification. Generally, traditional acid water extraction is used, and then cation exchange resin and organic solvent extraction are used to separate and purify it. The eluate obtained by cation exchange resin often contains many impurities, such as amino acids (proline), sodium chloride, etc. Moreover, the above process has problems such as large consumption of organic reagents, high energy consumption, complex process, low separation efficiency, etc., which makes it difficult to achieve green manufacturing of traditional Chinese medicine. Summary of the invention

[0004] In view of the above problems, the present invention provides a method and device for separating and purifying oxymatrine from oxymatrine eluate. The method is an ion-grade membrane separation method with high efficiency, low energy consumption and environmental friendliness, and can separate and obtain high-purity oxymatrine from oxymatrine eluate.

[0005] In one aspect of the present invention, there is provided an electrodialysis device system for separating and purifying oxymatrine from an oxymatrine eluate, comprising a first-stage electrodialysis device and a second-stage electrodialysis device arranged in sequence;

[0006] The first-stage electrodialysis device includes an anode plate, a cathode plate and a membrane stack arranged between the anode plate and the cathode plate, and an anode chamber and a cathode chamber are formed between the two sides of the membrane stack and the anode plate and the cathode plate, respectively; the membrane stack includes at least one group of electrodialysis units, and each group of electrodialysis units is sequentially arranged from the anode plate to the cathode plate in the order of a cation exchange membrane, an anion exchange membrane, an ultrafiltration membrane, and a cation exchange membrane to form three compartments, the compartment between the cation exchange membrane and the anion exchange membrane is recorded as a recovery chamber, the compartment between the anion exchange membrane and the ultrafiltration membrane is recorded as a raw material chamber, and the compartment between the ultrafiltration membrane and the cation exchange membrane is recorded as a product chamber; it also includes a plurality of liquid storage tanks and a circulation pump corresponding to the anode chamber, the cathode chamber, the recovery chamber, the raw material chamber, and the product chamber, respectively;

[0007] The second-stage electrodialysis device includes an anode plate, a cathode plate and a membrane stack arranged between the anode plate and the cathode plate, and the two sides of the membrane stack and the anode plate and the cathode plate form an anode chamber and a cathode chamber respectively; the membrane stack includes at least one group of electrodialysis units, and each group of electrodialysis units is arranged in sequence from the anode plate to the cathode plate in the order of a cation exchange membrane, an anion exchange membrane, and a cation exchange membrane to form two compartments, and the side close to the anode plate in the two compartments is recorded as a concentration chamber, and the side close to the cathode plate is recorded as a desalination chamber; it also includes a plurality of liquid storage tanks and a circulation pump corresponding to the anode chamber, the cathode chamber, the concentration chamber and the desalination chamber respectively;

[0008] The anode chamber, cathode chamber, recovery chamber, raw material chamber, product chamber, concentration chamber and desalination chamber are all provided with feed inlets and discharge ports. Each chamber is connected with the corresponding liquid storage tank through a pipeline, and is powered by its own circulation pump to form a self-circulating loop.

[0009] As a specific embodiment of the present invention, the ultrafiltration membrane is a PES ultrafiltration membrane; preferably, the ultrafiltration membrane has a molecular weight cutoff range of 1000 to 50000 Da.

[0010] As a specific embodiment of the present invention, the anion exchange membrane is an AIS anion exchange membrane, and the cation exchange membrane is a CIS cation exchange membrane.

[0011] As a specific embodiment of the present invention, the anode plate and the cathode plate are both titanium-coated ruthenium electrodes.

[0012] As a specific embodiment of the present invention, the membrane stack is formed by n groups of electrodialysis units connected in series, and the value of n is 1-1000.

[0013] Another aspect of the present invention provides a method for separating and purifying oxymatrine from an oxymatrine eluate using the aforementioned electrodialysis device system, comprising: firstly separating the oxymatrine eluate through a first-stage electrodialysis device to obtain an oxymatrine-rich solution, and then purifying the oxymatrine-rich solution through a second-stage electrodialysis device to obtain high-purity oxymatrine;

[0014] The method for separating the oxidized matrine eluate by a first-stage electrodialysis device comprises: S11, adding sodium chloride solution to the storage tanks corresponding to the recovery chamber and the product chamber, adding sodium sulfate solution to the storage tanks corresponding to the anode chamber and the cathode chamber, and adding the oxidized matrine solution adjusted to acidity to the storage tank corresponding to the raw material chamber; specifically, hydrochloric acid can be added to adjust to acidity, the purpose is to make the oxidized matrine positively charged, so that it can migrate under the action of the electric field; S12, starting the self-circulation of each chamber; S13, applying direct current between the anode plate and the cathode plate, and obtaining a salt-containing oxidized matrine solution in the product chamber, and sodium chloride and hydrochloric acid in the recovery chamber;

[0015] The method for purifying a solution rich in oxidized matrine by a second-stage electrodialysis device comprises: S21, adding a sodium chloride solution to a liquid storage tank corresponding to a concentration chamber, adding a sodium sulfate solution to a liquid storage tank corresponding to an anode chamber and a cathode chamber, and adding a solution rich in oxidized matrine to a liquid storage tank corresponding to a desalination chamber; S22, starting self-circulation in each chamber; S23, applying direct current between the anode plate and the cathode plate, so that high-purity oxidized matrine can be obtained in the desalination chamber.

[0016] As a specific embodiment of the present invention, the concentration of the sodium chloride solution is 0.05-1.0 mol / L.

[0017] As a specific embodiment of the present invention, the concentration of the sodium sulfate solution is 0.1 to 0.6 mol / L.

[0018] As a specific embodiment of the present invention, the concentration of oxymatrine in the oxymatrine eluate is 0.04 to 0.64 mol / L.

[0019] As a specific embodiment of the present invention, the first-stage electrodialysis device is operated in a constant current operation mode with a current density of 5 to 30 mA / cm 2 The second-stage electrodialysis device was operated in constant voltage mode, and the experiment ended when the conductivity of the desalination chamber solution dropped to 0.025 mS / cm.

[0020] The beneficial effects of the present invention are:

[0021] The electrodialysis device system provided by the present invention is a combined device system of a first-stage electrodialysis device and a second-stage electrodialysis device, wherein an ultrafiltration membrane is introduced into the membrane stack of the first-stage electrodialysis device. Compared with the ion exchange membrane used in conventional electrodialysis devices, the ultrafiltration membrane has the advantage of a large pore size, and can achieve transmembrane transmission and efficient screening of charged alkaloids. On this basis, in combination with the selective permeability of each ion exchange membrane in the second-stage electrodialysis device to ions, the purpose of further purifying oxymatrine can be achieved.

[0022] The separation and purification method provided by the present invention can separate oxymatrine with a purity greater than 98% from an oxymatrine eluate, while recovering sodium chloride and hydrochloric acid, thereby improving the economic benefits of the process. The method is an economical, green, environmentally friendly and efficient production method with important industrial application value. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 This is a schematic diagram of the principle of ultrafiltration membrane-assisted electrodialysis separation of oxymatrine in the present invention;

[0024] Figure 2 The schematic diagram is a principle diagram of electrodialysis purification of oxymatrine in the present invention. DETAILED DESCRIPTION

[0025] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are 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.

[0026] Example 1

[0027] This embodiment adopts Figure 1 The ultrafiltration membrane assisted electrodialysis device shown in the figure has a membrane stack arrangement of anode-anode chamber-cation exchange membrane-[recovery chamber-anion exchange membrane-raw material chamber-ultrafiltration membrane-product chamber-cation exchange membrane] n - cathode chamber - cathode, the number of repeating units is 2, and the anode and cathode materials are corrosion-resistant titanium coated with ruthenium. The ion exchange membranes used in the membrane stack are CIS cation exchange membranes and AIS anion exchange membranes produced by Shandong Tianwei Membrane Technology Co., Ltd., and the effective area of ​​a single membrane is 20cm 2 The ultrafiltration membrane is a PES ultrafiltration membrane produced by Zhongke Ruiyang Membrane (Beijing) Technology Co., Ltd., with an effective area of ​​20cm per membrane. 2 The anode chamber, cathode chamber, recovery chamber, raw material chamber, and product chamber are all provided with feed ports and discharge ports. Each chamber is connected to the corresponding liquid storage tank through a pipeline, and each circulation pump is used as the power to form a self-circulating loop.

[0028] The anode plate and cathode plate form an anode chamber and a cathode chamber between the adjacent membranes. The anode chamber and the cathode chamber are connected in series, and 200mL of 0.4mol / L sodium sulfate is introduced as the electrode liquid. 200mL of 0.05mol / L sodium chloride solution is introduced into the salt recovery chamber, 200mL of 0.04mol / L oxymatrine, 0.01mol / L proline, and 0.05mol / L sodium chloride mixed solution with a pH of 4 is introduced into the raw material chamber, and 200mL of 0.2mol / L sodium chloride solution is introduced into the product chamber. During the experiment, the linear velocity of the solution flow in each compartment was 3cm / s. The experiment adopted a constant current operation mode and set the current density to 10mA / cm 2 The molecular weight cut-off of the ultrafiltration membrane is 20,000 Da.

[0029] During the separation process, the ultrafiltration membrane-assisted electrodialysis device ended when the operation time was 180 min, and the membrane voltage was 3.4-8.5 V. Finally, the yield of oxymatrine in the product chamber was 40.52%, the purity of oxymatrine in the product chamber was 77.46%, and the energy consumption was 3.68 kWh / kg.

[0030] Example 2

[0031] The ultrafiltration membrane assisted electrodialysis device used in this embodiment is the same as that in embodiment 1.

[0032] The anode plate and cathode plate form an anode chamber and a cathode chamber between the adjacent membranes. The anode chamber and the cathode chamber are connected in series, and 200mL of 0.4mol / L sodium sulfate is introduced as the electrode liquid. 200mL of 0.05mol / L sodium chloride solution is introduced into the salt recovery chamber, 200mL of 0.04mol / L oxymatrine, 0.01mol / L proline, and 0.05mol / L sodium chloride mixed solution with a pH of 4 is introduced into the raw material chamber, and 200mL of 0.2mol / L sodium chloride solution is introduced into the product chamber. During the experiment, the linear velocity of the solution flow in each compartment was 3cm / s. The experiment adopted a constant current operation mode and set the current density to 10mA / cm 2 The molecular weight cut-off of the ultrafiltration membrane is 5000Da.

[0033] During the separation process, the ultrafiltration membrane-assisted electrodialysis device ended when the operation time was 180 min, and the membrane voltage was 3.5-8 V. Finally, the yield of oxymatrine in the product chamber was 50.03%, the purity of oxymatrine in the product chamber was 77.81%, and the energy consumption was 3.76 kWh / kg.

[0034] Example 3

[0035] The ultrafiltration membrane assisted electrodialysis device used in this embodiment is the same as that in embodiment 1.

[0036] The anode plate and cathode plate form an anode chamber and a cathode chamber between the adjacent membranes. The anode chamber and the cathode chamber are connected in series, and 200mL of 0.4mol / L sodium sulfate is introduced as the electrode liquid. 200mL of 0.05mol / L sodium chloride solution is introduced into the salt recovery chamber, 200mL of 0.04mol / L oxymatrine, 0.01mol / L proline, and 0.05mol / L sodium chloride mixed solution with a pH of 4 is introduced into the raw material chamber, and 200mL of 0.2mol / L sodium chloride solution is introduced into the product chamber. During the experiment, the linear velocity of the solution flow in each compartment was 3cm / s. The experiment adopted a constant current operation mode and set the current density to 10mA / cm 2 The molecular weight cut-off of the ultrafiltration membrane is 1000Da.

[0037] During the separation process, the ultrafiltration membrane-assisted electrodialysis device ended when the operation time was 180 min, and the membrane voltage was 4.1-13.4 V. Finally, the yield of oxymatrine in the product chamber was 49.47%, the purity of oxymatrine in the product chamber was 69.08%, and the energy consumption was 3.92 kWh / kg.

[0038] Example 4

[0039] The ultrafiltration membrane assisted electrodialysis device used in this embodiment is the same as that in embodiment 1.

[0040] The anode plate and cathode plate form an anode chamber and a cathode chamber between the adjacent membranes. The anode chamber and the cathode chamber are connected in series, and 200mL of 0.4mol / L sodium sulfate is introduced as the electrode liquid. 200mL of 0.05mol / L sodium chloride solution is introduced into the salt recovery chamber, 200mL of 0.16mol / L oxymatrine, 0.04mol / L proline, and 0.05mol / L sodium chloride mixed solution with a pH of 4 is introduced into the raw material chamber, and 200mL of 0.2mol / L sodium chloride solution is introduced into the product chamber. During the experiment, the linear velocity of the solution flow in each compartment was 3cm / s. The experiment adopted a constant current operation mode and set the current density to 10mA / cm 2 The molecular weight cut-off of the ultrafiltration membrane is 1000Da.

[0041] During the separation process, the ultrafiltration membrane-assisted electrodialysis device ended when the operation time was 180 min, and the membrane voltage was 2.6-10.2 V. Finally, the yield of oxymatrine in the product chamber was 13.77%, the purity of oxymatrine in the product chamber was 64.22%, and the energy consumption was 2.17 kWh / kg.

[0042] Example 5

[0043] The ultrafiltration membrane assisted electrodialysis device used in this embodiment is the same as that in embodiment 1.

[0044] The anode plate and cathode plate form an anode chamber and a cathode chamber between the adjacent membranes. The anode chamber and the cathode chamber are connected in series, and 200mL of 0.4mol / L sodium sulfate is introduced as the electrode liquid. 200mL of 0.05mol / L sodium chloride solution is introduced into the salt recovery chamber, 200mL of 0.08mol / L oxymatrine, 0.02mol / L proline, and 0.05mol / L sodium chloride mixed solution with a pH of 4 is introduced into the raw material chamber, and 200mL of 0.2mol / L sodium chloride solution is introduced into the product chamber. During the experiment, the linear velocity of the solution flow in each compartment was 3cm / s. The experiment adopted a constant current operation mode and set the current density to 10mA / cm 2 The molecular weight cut-off of the ultrafiltration membrane is 1000Da.

[0045] During the separation process, the ultrafiltration membrane-assisted electrodialysis device ended when the operation time was 180 min, and the membrane voltage was 3.2-6.9 V. Finally, the yield of oxymatrine in the product chamber was 23.50%, the purity of oxymatrine in the product chamber was 63.31%, and the energy consumption was 2.70 kWh / kg.

[0046] Example 6

[0047] The ultrafiltration membrane assisted electrodialysis device used in this embodiment is the same as that in embodiment 1.

[0048] The anode plate and cathode plate form an anode chamber and a cathode chamber between the adjacent membranes. The anode chamber and the cathode chamber are connected in series, and 200mL of 0.4mol / L sodium sulfate is introduced as the electrode liquid. 200mL of 0.05mol / L sodium chloride solution is introduced into the salt recovery chamber, 200mL of 0.04mol / L oxymatrine, 0.01mol / L proline, and 0.05mol / L sodium chloride mixed solution with a pH of 4 is introduced into the raw material chamber, and 200mL of 0.2mol / L sodium chloride solution is introduced into the product chamber. During the experiment, the linear velocity of the solution flow in each compartment was 3cm / s. The experiment adopted a constant current operation mode and set the current density to 25mA / cm 2 The molecular weight cut-off of the ultrafiltration membrane is 1000Da.

[0049] During the separation process, the operation was terminated when the conductivity of the feed chamber solution dropped to 3.00 mS / cm, the operation time was 45 min, and the membrane voltage was 9.5-12.8 V. Finally, the yield of oxymatrine in the product chamber was 30.31%, the purity of oxymatrine in the product chamber was 70.44%, and the energy consumption was 6.78 kWh / kg.

[0050] Example 7

[0051] The ultrafiltration membrane assisted electrodialysis device used in this embodiment is the same as that in embodiment 1.

[0052] The anode plate and cathode plate form an anode chamber and a cathode chamber between the adjacent membranes. The anode chamber and the cathode chamber are connected in series, and 200mL of 0.4mol / L sodium sulfate is introduced as the electrode liquid. 200mL of 0.05mol / L sodium chloride solution is introduced into the salt recovery chamber, 200mL of 0.04mol / L oxymatrine, 0.01mol / L proline, and 0.05mol / L sodium chloride mixed solution with a pH of 4 is introduced into the raw material chamber, and 200mL of 0.2mol / L sodium chloride solution is introduced into the product chamber. During the experiment, the linear velocity of the solution flow in each compartment was 3cm / s. The experiment adopted a constant current operation mode and set the current density to 15mA / cm 2 The molecular weight cut-off of the ultrafiltration membrane is 1000Da.

[0053] During the separation process, the operation was terminated when the conductivity of the feed chamber solution dropped to 1.75 mS / cm, the operation time was 105 min, and the membrane voltage was 6.3-13.3 V. Finally, the yield of oxymatrine in the product chamber was 41.61%, the purity of oxymatrine in the product chamber was 68.72%, and the energy consumption was 5.27 kWh / kg.

[0054] Example 8

[0055] The ultrafiltration membrane assisted electrodialysis device used in this embodiment is the same as that in embodiment 1.

[0056] The anode plate and cathode plate form an anode chamber and a cathode chamber between the adjacent membranes. The anode chamber and the cathode chamber are connected in series, and 200mL of 0.4mol / L sodium sulfate is introduced as the electrode liquid, 200mL of 0.05mol / L sodium chloride solution is introduced into the salt recovery chamber, 200mL of 0.04mol / L oxymatrine and 0.01mol / L proline mixed solution with a pH of 4 is introduced into the raw material chamber, and 200mL of 0.2mol / L sodium chloride solution is introduced into the product chamber. During the experiment, the linear velocity of the solution flow in each compartment was 3cm / s. The experiment adopted a constant current operation mode and set the current density to 10mA / cm 2 The molecular weight cut-off of the ultrafiltration membrane is 1000Da.

[0057] During the separation process, the operation was terminated when the conductivity of the feed chamber solution dropped to 0.75 mS / cm, the operation time was 115 min, and the membrane voltage was 5.6-13.5 V. Finally, the yield of oxymatrine in the product chamber was 62.79%, the purity of oxymatrine in the product chamber was 53.75%, and the energy consumption was 2.52 kWh / kg.

[0058] Example 9

[0059] The ultrafiltration membrane assisted electrodialysis device used in this embodiment is the same as that in embodiment 1.

[0060] The anode plate and cathode plate form an anode chamber and a cathode chamber between the adjacent membranes. The anode chamber and the cathode chamber are connected in series, and 200mL of 0.4mol / L sodium sulfate is introduced as the electrode liquid, 200mL of 0.05mol / L sodium chloride solution is introduced into the recovery chamber, 200mL of 0.04mol / L oxymatrine, 0.01mol / L proline, and 0.05mol / L sodium chloride mixed solution with a pH of 4 is introduced into the raw material chamber, and 200mL of 0.2mol / L sodium chloride solution is introduced into the product chamber. During the experiment, the linear velocity of the solution flow in each compartment was 3cm / s, and the conductivity was adjusted by adding sodium chloride to the raw material chamber, and the pH was adjusted by adding hydrochloric acid to make the experiment run continuously. The experiment adopted a constant current operation mode, and the current density was set to 10mA / cm 2 The molecular weight cut-off of the ultrafiltration membrane is 1000Da.

[0061] During the separation process, the ultrafiltration membrane-assisted electrodialysis device ended when the operation time was 380 min, and the membrane voltage was 3.4-13.5 V. Finally, the yield of oxymatrine in the product chamber was 96.99%, the purity of oxymatrine in the product chamber was 93.67%, and the energy consumption was 4.74 kWh / kg.

[0062] Example 10

[0063] This embodiment adopts Figure 2 In the electrodialysis device shown, the membrane stack is arranged in the following manner: anode-anode chamber-[cation exchange membrane-concentration chamber-anion exchange membrane-desalination chamber-cation exchange membrane] n - cathode chamber - cathode, the number of repeating units is 2, the anode and cathode materials in the membrane stack are corrosion-resistant titanium coated with ruthenium. The ion exchange membranes used in the membrane stack are CIS cation exchange membranes and AIS anion exchange membranes produced by Shandong Tianwei Membrane Technology Co., Ltd., and the effective area of ​​a single membrane is 20cm 2 The anode chamber, cathode chamber, concentration chamber and desalination chamber are all provided with feed inlets and discharge ports, and each chamber is connected with the corresponding liquid storage tank through a pipeline, and is powered by its own circulation pump to form a self-circulating loop.

[0064] The anode plate and the cathode plate form an anode chamber and a cathode chamber between the adjacent membranes. The anode chamber and the cathode chamber are connected in series, and 200 mL of 0.4 mol / L sodium sulfate is introduced as the electrode liquid, and a 0.05 mol / L sodium chloride solution is introduced into the concentration chamber, and the feed liquid obtained from the product chamber of Example 9 is introduced into the desalination chamber. During the experiment, the linear velocity of the solution flow in each compartment was 3 cm / s, and the experiment adopted a constant voltage operation mode, and the voltage was set to 30V.

[0065] During the desalination process, the experiment ended when the conductivity of the solution in the desalination chamber dropped to 0.025 mS / cm, and the running time was 65 min. Finally, the purity of oxymatrine increased from 93.67% to 98.66%.

[0066] The embodiments described above are only some embodiments of the present invention, but not all of them. Based on the embodiments of the present invention, other embodiments obtained by ordinary technicians in this field without making creative work belong to the protection scope of the present invention.

Claims

1. An electrodialysis device system for separating and purifying oxymatrine from an oxymatrine eluate, characterized in that: The electrodialysis device system is composed of a first-stage electrodialysis device and a second-stage electrodialysis device arranged in sequence; The first-stage electrodialysis device includes an anode plate, a cathode plate and a membrane stack arranged between the anode plate and the cathode plate, and an anode chamber and a cathode chamber are formed between the two sides of the membrane stack and the anode plate and the cathode plate, respectively; the membrane stack includes at least one group of electrodialysis units, and each group of electrodialysis units is sequentially arranged from the anode plate to the cathode plate in the order of a cation exchange membrane, an anion exchange membrane, an ultrafiltration membrane, and a cation exchange membrane to form three compartments, the compartment between the cation exchange membrane and the anion exchange membrane is recorded as a recovery chamber, the compartment between the anion exchange membrane and the ultrafiltration membrane is recorded as a raw material chamber, and the compartment between the ultrafiltration membrane and the cation exchange membrane is recorded as a product chamber; it also includes a plurality of liquid storage tanks and a circulation pump corresponding to the anode chamber, the cathode chamber, the recovery chamber, the raw material chamber, and the product chamber, respectively; The second-stage electrodialysis device comprises an anode plate, a cathode plate and a membrane stack arranged between the anode plate and the cathode plate, wherein an anode chamber and a cathode chamber are formed between the two sides of the membrane stack and the anode plate and the cathode plate, respectively; the membrane stack comprises at least one group of electrodialysis units, wherein each group of electrodialysis units is sequentially arranged from the anode plate to the cathode plate in the order of a cation exchange membrane, an anion exchange membrane and a cation exchange membrane to form two compartments, wherein the side close to the anode plate of the two compartments is recorded as a concentration chamber, and the side close to the cathode plate is recorded as a desalination chamber; and further comprises a plurality of liquid storage tanks and a circulation pump corresponding to the anode chamber, the cathode chamber, the concentration chamber and the desalination chamber, respectively; The anode chamber, cathode chamber, recovery chamber, raw material chamber, product chamber, concentration chamber and desalination chamber are all provided with a feed inlet and a discharge inlet, and each chamber is connected to a corresponding liquid storage tank through a pipeline, and each circulation pump is used as a power source to form a self-circulating loop; The ultrafiltration membrane is a PES ultrafiltration membrane, and the ultrafiltration membrane has a molecular weight cutoff range of 1000 to 50000 Da.

2. The electrodialysis device system according to claim 1, characterized in that: The anion exchange membrane is an AIS anion exchange membrane, and the cation exchange membrane is a CIS cation exchange membrane.

3. The electrodialysis device system according to claim 1, characterized in that: The anode plate and the cathode plate are both titanium-coated ruthenium electrodes.

4. The electrodialysis device system according to claim 1, characterized in that: The membrane stack is formed by n groups of electrodialysis units connected in series, and the value of n is 1-1000.

5. A method for separating and purifying oxymatrine from an oxymatrine eluate using the electrodialysis device system according to any one of claims 1 to 4, characterized in that: The method comprises: firstly separating the oxymatrine eluate through a first-stage electrodialysis device to obtain an oxymatrine-rich solution, and then purifying the oxymatrine-rich solution through a second-stage electrodialysis device to obtain high-purity oxymatrine; The method for separating the oxidized matrine eluate by the first-stage electrodialysis device comprises: S11, adding sodium chloride solution to the storage tanks corresponding to the recovery chamber and the product chamber, adding sodium sulfate solution to the storage tanks corresponding to the anode chamber and the cathode chamber, and adding the oxidized matrine solution adjusted to acidity to the storage tank corresponding to the raw material chamber; S12, starting the self-circulation of each chamber; S13, applying direct current between the anode plate and the cathode plate; The method for purifying a solution rich in oxymatrine by a second-stage electrodialysis device comprises: S21, adding a sodium chloride solution to a liquid storage tank corresponding to a concentration chamber, adding a sodium sulfate solution to a liquid storage tank corresponding to an anode chamber and a cathode chamber, and adding a feed solution obtained from a product chamber in step S13 to a liquid storage tank corresponding to a desalination chamber; S22, starting self-circulation in each chamber; S23, applying direct current between the anode plate and the cathode plate.

6. The method according to claim 5, characterized in that The concentration of the sodium chloride solution is 0.05-1.0 mol / L.

7. The method according to claim 5, characterized in that The concentration of the sodium sulfate solution is 0.1-0.6 mol / L.

8. The method according to claim 5, characterized in that The concentration of oxymatrine in the oxymatrine eluate is 0.04-0.64 mol / L.

9. The method according to claim 5, characterized in that The first-stage electrodialysis device is operated in a constant current mode with a current density of 5 to 30 mA / cm 2 The second-stage electrodialysis device was operated in constant voltage mode, and the experiment ended when the conductivity of the desalination chamber solution dropped to 0.025 mS / cm.

Citation Information

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