Device for extracting and preparing D-calcium pantothenate from fermentation liquor

Abstract

The utility model discloses a device for extracting and preparing D-calcium pantothenate from fermentation liquor, and relates to the technical field of D-calcium pantothenate production, an inlet of a flocculation tank is communicated with a fermentation liquor tank, a chitosan tank and a calcium oxide tank, an outlet of the flocculation tank is communicated with a plate-and-frame filter press, a liquid phase outlet of the plate-and-frame filter press is communicated with a cation exchange resin column, and a liquid phase outlet of the cation exchange resin column is communicated with a liquid phase outlet of the chitosan tank. An outlet of the cation exchange resin column is communicated with a desalted liquid tank; an outlet of the desalted liquid tank is communicated with a neutralization tank; an inlet of the neutralization tank is communicated with a calcium hydroxide tank; an outlet of the neutralization tank is communicated with a concentration tank; an outlet of the centrifuge is communicated to the finished product tank through the dryer. And the crystallization yield and the purity of the product are improved.

Description

Technical Field

[0001] This utility model relates to the field of D-calcium pantothenate production technology, specifically to an apparatus for extracting and preparing D-calcium pantothenate from fermentation broth. Background Technology

[0002] D-Calcium pantothenate is one of the 13 essential vitamins for the human body and a member of the B vitamins. It is also a water-soluble vitamin and a component of coenzyme A. Specifically, D-Calcium pantothenate participates in the metabolism of carbohydrates, fats, and proteins, becoming an indispensable trace element for maintaining normal physiological functions in humans and animals.

[0003] Chinese patent CN119371329A discloses a method for preparing D-calcium pantothenate from fermentation broth, relating to the field of D-calcium pantothenate production technology. The fermentation broth for D-calcium pantothenate is flocculated, pressure filtered, and then filtered through an ultrafiltration membrane. The resulting ultrafiltration membrane supernatant is extracted, and the lower layer is concentrated through a nanofiltration membrane. The concentrated solution is then eluted using a chromatography column to collect the target component containing D-pantothenic acid. A calcium chloride solution is then added to initiate the reaction. The reaction solution is collected, cooled, and crystallized, followed by suction filtration, washing, and repeated suction filtration and drying to obtain the final product, D-calcium pantothenate. This invention not only simplifies the production process and shortens the production cycle, effectively improving production efficiency, but also increases product purity and yield, achieving a purity of over 99.5% and a yield of over 95%. However, chromatography processes typically require a long time, especially for high-resolution separation. To obtain better separation results, lower flow rates are often necessary, making the entire separation process time-consuming. Furthermore, the high maintenance costs of the chromatography column increase production costs. Summary of the Invention

[0004] The technical problem to be solved by this utility model is to provide an apparatus for extracting and preparing D-calcium pantothenate from fermentation broth, which has low production cost and short production cycle, in order to address the shortcomings of the existing technology.

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

[0006] An apparatus for extracting and preparing D-calcium pantothenate from fermentation broth includes a flocculation tank. The inlet of the flocculation tank is connected to a fermentation broth tank, a chitosan tank, and a calcium oxide tank via pipelines. The outlet of the flocculation tank is connected to a plate and frame filter press via a pipeline. The liquid phase outlet of the plate and frame filter press is connected to a cation exchange resin column via a pipeline. The outlet of the cation exchange resin column is connected to a desalination tank via a pipeline. The outlet of the desalination tank is connected to a neutralization tank via a pipeline. The inlet of the neutralization tank is connected to a calcium hydroxide tank via a pipeline. The outlet of the neutralization tank is connected to a concentration tank via a pipeline. The outlet of the concentration tank is connected to a crystallization tank via a pipeline. The inlet of the crystallization tank is connected to an ethanol tank via a pipeline. The outlet of the crystallization tank is connected to a centrifuge via a pipeline. The solid phase outlet of the centrifuge is connected to a finished product tank via a dryer.

[0007] As an improved technical solution, the inlet of the flocculation tank is connected to a diatomaceous earth tank via a pipeline.

[0008] As an improved technical solution, the liquid phase outlet of the plate and frame filter press is connected to an ultrafiltration membrane device via a pipeline, and the clear liquid outlet of the ultrafiltration membrane device is connected to the cation exchange resin column via a pipeline.

[0009] As an improved technical solution, the clear liquid outlet of the ultrafiltration membrane device is connected to a nanofiltration membrane device via a pipeline, and the clear liquid outlet of the nanofiltration membrane device is connected to the cation exchange resin column via a pipeline.

[0010] As an improved technical solution, the inlet of the nanofiltration membrane device is connected to a purified water tank via a pipeline.

[0011] As an improved technical solution, the outlet of the concentration tank is connected to a decolorization tank via a pipeline, the inlet of the decolorization tank is connected to an activated carbon tank via a pipeline, and the outlet of the decolorization tank is connected to the crystallization tank via a pipeline.

[0012] As a preferred technical solution, the liquid phase outlet of the centrifuge is connected to a mother liquor tank via a pipeline, and the outlet of the mother liquor tank is connected to the concentration tank via a pipeline.

[0013] As a preferred technical solution, the inlet of the cation exchange resin column is connected to a dilute hydrochloric acid solution tank and a deionized water tank via pipelines.

[0014] As a preferred technical solution, the flocculation tank is equipped with a first online pH sensor, and the outlet pipe of the calcium oxide tank is equipped with a first shut-off valve. The first online pH sensor and the first shut-off valve are interlocked to the control system.

[0015] As a preferred technical solution, the neutralization tank is equipped with a second online pH sensor, and the outlet pipe of the calcium hydroxide tank is equipped with a second shut-off valve. The second online pH sensor and the second shut-off valve are interlocked to the control system.

[0016] Due to the adoption of the above technical solution, the beneficial effects of this utility model are:

[0017] This invention discloses an apparatus for extracting and preparing D-calcium pantothenate from fermentation broth, comprising a flocculation tank. The inlet of the flocculation tank is connected to a fermentation broth tank, a chitosan tank, and a calcium oxide tank via pipelines. The outlet of the flocculation tank is connected to a plate and frame filter press via a pipeline. The liquid phase outlet of the plate and frame filter press is connected to a cation exchange resin column via a pipeline. The outlet of the cation exchange resin column is connected to a desalination tank via a pipeline. The outlet of the desalination tank is connected to a neutralization tank via a pipeline. The inlet of the neutralization tank is connected to a calcium hydroxide tank via a pipeline. The outlet of the neutralization tank is connected to a concentration tank via a pipeline. The outlet of the concentration tank is connected to a crystallization tank via a pipeline. The inlet of the crystallization tank is connected to an ethanol tank via a pipeline. The outlet of the crystallization tank is connected to a centrifuge via a pipeline. The solid phase outlet of the centrifuge is connected to a finished product tank via a dryer. Adding chitosan to the fermentation broth allows it to act as a flocculant, removing microbial cells. Calcium oxide adjusts the pH to 8-9, removing organic and inorganic acids that affect the purity of D-calcium pantothenate. The synergistic effect of both effectively removes macromolecular impurities and suspended solids, improving subsequent separation efficiency and ensuring product purity. A cation exchange resin column selectively adsorbs cationic impurities from the fermentation broth, removing interfering components such as metal ions, further purifying the D-calcium pantothenate solution and improving product quality. Adding calcium hydroxide to the desalination solution for neutralization adjusts the pH, allowing D-pantothenate ions to combine with calcium ions to form D-calcium pantothenate, creating conditions for subsequent concentration and crystallization, ensuring product formation. A concentration tank concentrates the neutralized solution, reducing volume, increasing D-calcium pantothenate concentration, lowering energy consumption in subsequent crystallization, and improving production efficiency. Adding ethanol to the concentrate reduces the solubility of D-calcium pantothenate, promoting crystallization and improving crystallization yield and product purity.

[0018] The inlet of the flocculation tank of this invention is connected to a diatomaceous earth tank via a pipe. Diatomaceous earth is added to the flocculation tank as a filter aid, which can improve the structure of the flocs, enhance the filtration performance of the plate and frame filter press, reduce filtration resistance, accelerate filtration speed, improve production efficiency, and further improve the clarity of the filtrate.

[0019] The liquid outlet of the plate and frame filter press is connected to an ultrafiltration membrane device via a pipeline, and the clarified liquid outlet of the ultrafiltration membrane device is connected to the cation exchange resin column via a pipeline. The ultrafiltration membrane device can remove proteins and large organic molecules from the feed liquid, further remove impurities, and purify the target product.

[0020] The superfiltration membrane device's clarified liquid outlet is connected to a nanofiltration membrane device via a pipeline, and the nanofiltration membrane device's clarified liquid outlet is connected to the cation exchange resin column via a pipeline. The nanofiltration membrane device can selectively retain divalent and higher valent ions, further removing salts and small molecule impurities from the solution, improving the purity of the D-calcium pantothenate solution, providing higher-quality raw materials for subsequent processes, and enhancing product quality.

[0021] The inlet of the nanofiltration membrane device is connected to a purified water tank via a pipeline. By adding purified water and dialyzing 2-3 times to control the conductivity of the concentrate to <10000 μS / cm, other cations in the feed solution are removed, further improving the purity of the product.

[0022] The outlet of the concentration tank is connected to a decolorization tank via a pipeline, the inlet of the decolorization tank is connected to an activated carbon tank via a pipeline, and the outlet of the decolorization tank is connected to the crystallization tank via a pipeline. Decolorization further improves the color and purity of the product.

[0023] The liquid outlet of the centrifuge is connected to a mother liquor tank via a pipeline, and the outlet of the mother liquor tank is connected to the concentration tank via a pipeline. By recycling the centrifuged mother liquor, the product yield is improved.

[0024] The inlet of the cation exchange resin column is connected to a dilute hydrochloric acid solution tank and a deionized water tank via pipelines. Before use, the cation exchange resin is regenerated with a 4-5% wt dilute hydrochloric acid solution, and then washed with deionized water until the pH is >6 and the conductivity is <300 μS / cm, in order to improve the treatment capacity of the cation exchange resin and better remove impurities from the feed solution.

[0025] The flocculation tank is equipped with a first online pH sensor, and the outlet pipe of the calcium oxide tank is equipped with a first shut-off valve. The first online pH sensor and the first shut-off valve are interlocked to the control system. The control system controls the opening and closing of the first shut-off valve based on the value of the first online pH sensor, so that the pH value of the flocculation tank is maintained at 8-9, which improves the removal effect of organic acids and other inorganic acids, and enhances product quality and the automation level of the production process.

[0026] The neutralization tank is equipped with a second online pH sensor, and the outlet pipe of the calcium hydroxide tank is equipped with a second shut-off valve. The second online pH sensor and the second shut-off valve are interlocked to the control system. Based on the value of the second online pH sensor, the control system controls the opening and closing of the second shut-off valve to maintain the pH value of the neutralization tank at 6-7, precisely controlling the pH value of the neutralization reaction to ensure the complete and stable formation of D-calcium pantothenate, improving product yield and quality, and achieving automated and precise control of the production process. Attached Figure Description

[0027] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0028] Figure 1 This is a structural schematic diagram of an embodiment of the present utility model;

[0029] The components include: 1. Flocculation tank; 2. Fermentation broth tank; 3. Chitosan tank; 4. Calcium oxide tank; 5. Plate and frame filter press; 6. Cation exchange resin column; 7. Desalination tank; 8. Neutralization tank; 9. Calcium hydroxide tank; 10. Concentration tank; 11. Crystallization tank; 12. Ethanol tank; 13. Centrifuge; 14. Dryer; 15. Finished product tank; 16. Diatomaceous earth tank; 17. Ultrafiltration membrane device; 18. Nanofiltration membrane device; 19. Purified water tank; 20. Decolorization tank; 21. Activated carbon tank; 22. Mother liquor tank; 23. Dilute hydrochloric acid solution tank; 24. Deionized water tank; 25. First online pH sensor; 26. First shut-off valve; 27. Second online pH sensor; 28. Second shut-off valve. Detailed Implementation

[0030] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0031] like Figure 1As shown, an apparatus for extracting and preparing D-calcium pantothenate from fermentation broth includes a flocculation tank 1. The inlet of the flocculation tank 1 is connected to a fermentation broth tank 2, a chitosan tank 3, and a calcium oxide tank 4 via pipelines. The outlet of the flocculation tank 1 is connected to a plate and frame filter press 5 via a pipeline. The liquid phase outlet of the plate and frame filter press 5 is connected to a cation exchange resin column 6 via a pipeline. The outlet of the cation exchange resin column 6 is connected to a desalination liquid tank 7 via a pipeline. The outlet of the desalination liquid tank 7 is connected to a neutralization tank 8 via a pipeline. The inlet of the neutralization tank 8 is connected to a calcium hydroxide tank 9 via a pipeline. The outlet of the neutralization tank 8 is connected to a concentration tank 10 via a pipeline. The outlet of the concentration tank 10 is connected to a crystallization tank 11 via a pipeline. The inlet of the crystallization tank 11 is connected to an ethanol tank 12 via a pipeline. The outlet of the crystallization tank 11 is connected to a centrifuge 13 via a pipeline. The solid phase outlet of the centrifuge 13 is connected to a finished product tank 15 via a dryer 14. Adding chitosan to the fermentation broth allows it to act as a flocculant, removing microbial cells. Calcium oxide adjusts the pH to 8-9, removing organic and inorganic acids that affect the purity of D-calcium pantothenate. The synergistic effect of both effectively removes macromolecular impurities and suspended solids from the fermentation broth, improving subsequent separation efficiency and ensuring product purity. The cation exchange resin column 6 selectively adsorbs cationic impurities from the fermentation broth, removing interfering components such as metal ions, further purifying the D-calcium pantothenate solution and improving product quality. Adding calcium hydroxide to the desalination solution for neutralization adjusts the pH, allowing D-pantothenate ions to combine with calcium ions to form D-calcium pantothenate, creating conditions for subsequent concentration and crystallization, ensuring product formation. The concentration tank 10 concentrates the neutralized solution, reducing solution volume, increasing the concentration of D-calcium pantothenate, lowering energy consumption in subsequent crystallization processes, and improving production efficiency. Adding ethanol to the concentrate reduces the solubility of D-calcium pantothenate, promoting crystallization and improving crystallization yield and product purity.

[0032] The inlet of the flocculation tank 1 is connected to a diatomaceous earth tank 16 via a pipe. Diatomaceous earth is added to the flocculation tank 1 as a filter aid, which can improve the structure of the flocs, enhance the filtration performance of the plate and frame filter press 5, reduce filtration resistance, accelerate filtration speed, improve production efficiency, and further improve the clarity of the filtrate.

[0033] The liquid outlet of the plate and frame filter press 5 is connected to an ultrafiltration membrane device 17 via a pipeline, and the clear liquid outlet of the ultrafiltration membrane device 17 is connected to the cation exchange resin column 6 via a pipeline. The ultrafiltration membrane device 17 can remove proteins and large molecular organic matter from the feed liquid, further remove impurities, and purify the target product.

[0034] The supernatant outlet of the ultrafiltration membrane device 17 is connected to a nanofiltration membrane device 18 via a pipeline, and the supernatant outlet of the nanofiltration membrane device 18 is connected to the cation exchange resin column 6 via a pipeline. The nanofiltration membrane device 18 can selectively retain divalent and higher ions, further removing salts and small molecule impurities from the solution, improving the purity of the D-calcium pantothenate solution, providing higher-quality raw materials for subsequent processes, and improving product quality.

[0035] The inlet of the nanofiltration membrane device 18 is connected to a purified water tank 19 via a pipeline. By adding purified water and dialyzing 2-3 times, the conductivity of the concentrate is controlled to be <10000 μS / cm, other cations in the feed solution are removed, further improving the purity of the product.

[0036] The outlet of the concentration tank 10 is connected to the decolorization tank 20 via a pipeline, the inlet of the decolorization tank 20 is connected to the activated carbon tank 21 via a pipeline, and the outlet of the decolorization tank 20 is connected to the crystallization tank 11 via a pipeline. Decolorization further improves the color and purity of the product.

[0037] The liquid outlet of the centrifuge 13 is connected to a mother liquor tank 22 via a pipeline, and the outlet of the mother liquor tank 22 is connected to the concentration tank 10 via a pipeline. By recycling the centrifuged mother liquor, the product yield is improved.

[0038] The inlet of the cation exchange resin column 6 is connected to a dilute hydrochloric acid solution tank 23 and a deionized water tank 24 via pipes. Before use, the cation exchange resin is regenerated with a 4-5% wt dilute hydrochloric acid solution, and then washed with deionized water until the pH is >6 and the conductivity is <300 μS / cm, in order to improve the processing capacity of the cation exchange resin and better remove impurities from the feed solution.

[0039] The flocculation tank 1 is equipped with a first online pH sensor 25, and the outlet pipe of the calcium oxide tank 4 is equipped with a first shut-off valve 26. The first online pH sensor 25 and the first shut-off valve 26 are interlocked to the control system. The control system controls the opening and closing of the first shut-off valve 26 based on the value of the first online pH sensor 25, so that the pH value of the flocculation tank 1 is maintained at 8-9, which improves the removal effect of organic acids and other inorganic acids, and enhances product quality and the automation level of the production process.

[0040] The neutralization tank 8 is equipped with a second online pH sensor 27, and the outlet pipe of the calcium hydroxide tank 94 is equipped with a second shut-off valve 28. The second online pH sensor 27 and the second shut-off valve 28 are interlocked to the control system. Based on the value of the second online pH sensor 27, the control system controls the opening and closing of the second shut-off valve 28 to maintain the pH value of the neutralization tank 8 at 6-7, precisely controlling the pH value of the neutralization reaction to ensure the full and stable formation of D-calcium pantothenate, improving product yield and quality, and achieving automated and precise control of the production process.

[0041] It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that after reading the teachings of this invention, those skilled in the art can make various alterations or modifications to the invention, and these equivalent forms also fall within the scope defined by the appended claims.

Claims

1. An apparatus for extracting and preparing D-calcium pantothenate from fermentation broth, characterized in that: The system includes a flocculation tank, the inlet of which is connected via pipes to a fermentation broth tank, a chitosan tank, and a calcium oxide tank. The outlet of the flocculation tank is connected via pipes to a plate and frame filter press. The liquid phase outlet of the plate and frame filter press is connected via pipes to a cation exchange resin column. The outlet of the cation exchange resin column is connected via pipes to a desalination tank. The outlet of the desalination tank is connected via pipes to a neutralization tank. The inlet of the neutralization tank is connected via pipes to a calcium hydroxide tank. The outlet of the neutralization tank is connected via pipes to a concentration tank. The outlet of the concentration tank is connected via pipes to a crystallization tank. The inlet of the crystallization tank is connected via pipes to an ethanol tank. The outlet of the crystallization tank is connected via pipes to a centrifuge. The solid phase outlet of the centrifuge is connected via a dryer to a finished product tank.

2. The apparatus for extracting and preparing D-calcium pantothenate from fermentation broth as described in claim 1, characterized in that: The inlet of the flocculation tank is connected to a diatomaceous earth tank via a pipe.

3. The apparatus for extracting and preparing D-calcium pantothenate from fermentation broth as described in claim 1, characterized in that: The liquid outlet of the plate and frame filter press is connected to an ultrafiltration membrane device via a pipeline, and the clear liquid outlet of the ultrafiltration membrane device is connected to the cation exchange resin column via a pipeline.

4. The apparatus for extracting and preparing D-calcium pantothenate from fermentation broth as described in claim 3, characterized in that: The clear liquid outlet of the ultrafiltration membrane device is connected to a nanofiltration membrane device via a pipeline, and the clear liquid outlet of the nanofiltration membrane device is connected to the cation exchange resin column via a pipeline.

5. The apparatus for extracting and preparing D-calcium pantothenate from fermentation broth as described in claim 4, characterized in that: The inlet of the nanofiltration membrane device is connected to a purified water tank via a pipe.

6. The apparatus for extracting and preparing D-calcium pantothenate from fermentation broth as described in claim 1, characterized in that: The outlet of the concentration tank is connected to a decolorization tank via a pipeline, the inlet of the decolorization tank is connected to an activated carbon tank via a pipeline, and the outlet of the decolorization tank is connected to the crystallization tank via a pipeline.

7. The apparatus for extracting and preparing D-calcium pantothenate from fermentation broth as described in claim 1, characterized in that: The liquid outlet of the centrifuge is connected to a mother liquor tank via a pipeline, and the outlet of the mother liquor tank is connected to the concentration tank via a pipeline.

8. The apparatus for extracting and preparing D-calcium pantothenate from fermentation broth as described in claim 1, characterized in that: The inlet of the cation exchange resin column is connected to a dilute hydrochloric acid solution tank and a deionized water tank via pipes.

9. The apparatus for extracting and preparing D-calcium pantothenate from fermentation broth as described in claim 1, characterized in that: The flocculation tank is equipped with a first online pH sensor, and the outlet pipe of the calcium oxide tank is equipped with a first shut-off valve. The first online pH sensor and the first shut-off valve are interlocked to the control system.

10. The apparatus for extracting and preparing D-calcium pantothenate from fermentation broth as described in claim 1, characterized in that: The neutralization tank is equipped with a second online pH sensor, and the outlet pipe of the calcium hydroxide tank is equipped with a second shut-off valve. The second online pH sensor and the second shut-off valve are interlocked to the control system.

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