Purification production system for pyrroloquinoline quinone disodium salt

By designing a purification and production system for pyrroloquinoline quinone disodium salt, and utilizing multi-reactor interconnection and stirring, crystallization, washing, and drying steps, the problems of low purity, small processing capacity, and high cost in existing technologies have been solved, achieving efficient industrial production.

CN223454044UActive Publication Date: 2025-10-21ZHUCHENG HAOTIAN PHARMA CO LTD
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Patent Information

Application Number
CN202422593936.1
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-10-25
Publication Date
2025-10-21
Estimated Expiration
2034-10-25

AI Technical Summary

Technical Problem

The existing purification methods for pyrroloquinoline quinone disodium salt have low purity, small processing capacity, and high cost, making them unsuitable for industrial production.

Method used

A purification production system for disodium pyrroloquinoline quinone was designed, comprising multiple interconnected vessels and filtration devices. The system utilizes stirring, crystallization, washing, and drying steps, employing a jacket for temperature control and stirring plates or impellers for dissolution, crystallization, and washing. Combined with a vacuum filter and dryer, efficient purification is achieved.

Benefits of technology

It improves the purity of pyrroloquinoline quinone disodium salt, increases the throughput, and reduces production costs, making it suitable for industrial production.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model relates to the technical field of pyrroloquinoline quinone disodium salt production, in particular to a purification production system for pyrroloquinoline quinone disodium salt, which comprises a first dissolving kettle, an outlet of the first dissolving kettle is communicated with a first crystallization kettle, and an outlet of the first crystallization kettle is communicated with a first filtering device. A discharge port of the first filtering device is communicated with a first washing kettle, a discharge port of the first washing kettle is communicated with a first drying device, a discharge port of the first drying device is communicated with a second dissolving kettle, an outlet of the second dissolving kettle is communicated with a second crystallization kettle, and a discharge port of the second crystallization kettle is communicated with a second filtering device; a discharge hole of the second filtering device is communicated with a second washing kettle; a discharge hole of the second washing kettle is communicated with a second drying device. The purification production system is reasonable in design, large in treatment capacity and suitable for industrial production, the purity of the pyrroloquinoline quinone disodium salt is greatly improved, and the cost is reduced.
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Description

TECHNICAL FIELD

[0001] The utility model relates to pyrroloquinoline quinone disodium salt production technical field especially relates to a kind of purification production system for pyrroloquinoline quinone disodium salt. BACKGROUND

[0002] Pyrroloquinoline quinone (PQQ) disodium salt (hereinafter simply referred to as: "PQQ"), chemical name: 4,5-dioxo-4,5-dihydro-1H-pyrrolo[2,3-F]quinoline-2,3,9-tricarboxylic acid disodium salt, is a new type of water-soluble vitamin, is a kind of oxidoreductase auxiliary group, has important physiological role to microorganism and animal and plant: can improve the immunity of human body, reduce the harm of free radical to human body, regulate various nervous system diseases, promote the absorption of amino acid, promote the synthesis of growth factor, prevent senile dementia, promote the synthesis of glutathione etc. Chinese invention patent CN201510843823.5 discloses a kind of pyrroloquinoline quinone PQQ disodium salt impurity purification method, with 5 microns's GP C18 filling material, column pressure is about 12MPa, sample purity is greater than 95%, load is less than 0.2%, method purification precision is lower, cost is high, processing capacity is small, not suitable for industrial production. In view of the above problems, it is necessary to provide a kind of purification production system for pyrroloquinoline quinone disodium salt. SUMMARY

[0003] The technical problem to be solved by the utility model is: in view of the deficiencies of prior art, provide a kind of purification production system for pyrroloquinoline quinone disodium salt, utilize the purification system, can improve the purity of pyrroloquinoline quinone disodium salt, processing capacity is large, suitable for industrial production, also reduce cost.

[0004] To solve the above technical problems, the technical scheme of the utility model is:

[0005] A kind of purification production system for pyrroloquinoline quinone disodium salt, including first dissolving kettle, the outlet of the first dissolving kettle is connected with first crystallization kettle, the outlet of the first crystallization kettle is connected with first filter device, the discharge port of the first filter device is connected with first washing kettle, the discharge port of the first washing kettle is connected with first drying device, the discharge port of the first drying device is connected with second dissolving kettle, the outlet of the second dissolving kettle is connected with second crystallization kettle, the discharge port of the second crystallization kettle is connected with second filter device, the discharge port of the second filter device is connected with second washing kettle, the discharge port of the second washing kettle is connected with second drying device, the discharge port of the second drying device is connected with product storage tank.

[0006] As an improved technical scheme, the first dissolving kettle and the second dissolving kettle each comprise a kettle body, an outer wall of the kettle body is provided with a jacket, a top of the kettle body is provided with a feeding port and a solvent inlet, a bottom of the kettle body is provided with a discharging port, an inside of the kettle body is provided with a stirring shaft, one end of the stirring shaft is connected with a motor, and the stirring shaft is provided with a plurality of stirring plates with hollow structures.

[0007] As an improved technical scheme, the first dissolving kettle and the second dissolving kettle each comprise a kettle body, an outer wall of the kettle body is provided with a jacket, a top of the kettle body is provided with a feeding port and a solvent inlet, a bottom of the kettle body is provided with a discharging port, an inside of the kettle body is provided with a stirring shaft, one end of the stirring shaft is connected with a motor, and the stirring shaft is provided with a plurality of stirring plates with hollow structures.

[0008] As an improved technical scheme, the first dissolving kettle and the second dissolving kettle each comprise a kettle body, an outer wall of the kettle body is provided with a jacket, a top of the kettle body is provided with a feeding port and a solvent inlet, a bottom of the kettle body is provided with a discharging port, an inside of the kettle body is provided with a stirring shaft, one end of the stirring shaft is connected with a motor, and the stirring shaft is provided with a plurality of stirring plates with hollow structures.

[0009] As an improved technical scheme, the first dissolving kettle and the second dissolving kettle each comprise a kettle body, an outer wall of the kettle body is provided with a jacket, a top of the kettle body is provided with a feeding port and a solvent inlet, a bottom of the kettle body is provided with a discharging port, an inside of the kettle body is provided with a stirring shaft, one end of the stirring shaft is connected with a motor, and the stirring shaft is provided with a plurality of stirring plates with hollow structures.

[0010] As an improved technical scheme, the first dissolving kettle and the second dissolving kettle each comprise a kettle body, an outer wall of the kettle body is provided with a jacket, a top of the kettle body is provided with a feeding port and a solvent inlet, a bottom of the kettle body is provided with a discharging port, an inside of the kettle body is provided with a stirring shaft, one end of the stirring shaft is connected with a motor, and the stirring shaft is provided with a plurality of stirring plates with hollow structures.

[0011] After the above technical scheme is adopted, the beneficial effects of the present application are as follows:

[0012] The production system for purifying pyrroloquinoline quinone disodium salt comprises a first dissolving kettle, an outlet of the first dissolving kettle being connected with a first crystallizing kettle, an outlet of the first crystallizing kettle being connected with a first filtering device, a discharge port of the first filtering device being connected with a first washing kettle, a discharge port of the first washing kettle being connected with a first drying device, a discharge port of the first drying device being connected with a second dissolving kettle, an outlet of the second dissolving kettle being connected with a second crystallizing kettle, a discharge port of the second crystallizing kettle being connected with a second filtering device, a discharge port of the second filtering device being connected with a second washing kettle, a discharge port of the second washing kettle being connected with a second drying device, and an outlet of the second drying device being connected with a product storage tank. In actual production, pyrroloquinoline quinoline disodium salt is first put into the first dissolving kettle, a solvent is added, and after stirring and dissolving, the pyrroloquinoline quinoline disodium salt is pumped into the first crystallizing kettle. The pyrroloquinoline quinoline disodium salt is cooled by the coolant in the jacket of the first crystallizing kettle, and then the crystallization solvent and the feed liquid are fully contacted by stirring to promote the crystallization of the pyrroloquinoline quinoline disodium salt. After the crystallization is completed, the feed liquid is pumped into the first filtering device, the filtered crystal product is then put into the first washing kettle, and after being fully washed by the washing liquid, the crystal is transported into the first drying device. After drying, the pyrroloquinoline quinoline disodium salt is obtained. Then, the pyrroloquinoline quinoline disodium salt is put into the second dissolving kettle, stirred and dissolved, and then pumped into the second crystallizing kettle. After cooling by the coolant in the jacket and stirring, the crystal product is put into the second filtering device, and then into the second washing kettle. After being fully washed by the washing liquid, the crystal is transported into the second drying device, and then into the product storage tank. The above-mentioned production system is reasonable in design, has a large processing capacity, is suitable for industrial production, greatly improves the purity of pyrroloquinoline quinoline disodium salt, and reduces the cost.

[0013] The first dissolving kettle and the second dissolving kettle each comprise a kettle body, an outer wall of the kettle body being provided with a jacket, a top of the kettle body being provided with a feed inlet and a solvent inlet, a bottom of the kettle body being provided with a discharge port, an inside of the kettle body being provided with a stirring shaft, one end of the stirring shaft being connected with a motor, and the stirring shaft being provided with a plurality of stirring plates with hollow structures. The motor drives the stirring shaft and the stirring plates with hollow structures to rotate after being started, so that the solvent fully contacts and dissolves the pyrroloquinoline quinoline disodium salt or the pyrroloquinoline quinoline disodium salt primary crystal. The heat medium in the jacket provides the temperature required for dissolving, and the dissolved feed liquid is discharged from the discharge port. The first dissolving kettle and the second dissolving kettle with the above-mentioned structure improve the dissolving efficiency and are helpful for subsequent crystallization operations.

[0014] The first crystallization kettle and the second crystallization kettle comprise a kettle body, the top of the kettle body is provided with a feed inlet and a crystallization solvent inlet, the top of the kettle body is provided with a discharge outlet, and the outside of the kettle body is provided with a jacket; the inside of the kettle body is provided with a stirring shaft, one end of the stirring shaft is connected with a motor, and the stirring shaft is provided with multiple layers of stirring plates; the motor drives the stirring shaft and the multiple layers of stirring plates to rotate and fully stir and mix the liquid and the crystallization solvent; and the refrigerant in the jacket provides the temperature required for crystallization, the liquid and the crystallization solvent are fully contacted, and the crystallization efficiency is greatly improved.

[0015] The first washing kettle and the second washing kettle comprise a kettle body, the top of the kettle body is provided with a feed inlet and a washing liquid inlet, the bottom of the kettle body is provided with a discharge outlet, the lower part of the kettle body is provided with a liquid outlet on one side, and the inner wall of the kettle body is provided with a filter screen at a position corresponding to the liquid outlet; the inside of the kettle body is provided with a rotating shaft, one end of the rotating shaft is connected with a motor, the upper part of the rotating shaft is provided with multiple layers of hollow-structured stirring paddles, and the bottom of the rotating shaft is provided with a stirring frame; the motor drives the rotating shaft, the multiple layers of stirring paddles and the stirring frame to rotate, so that the crystals and the washing liquid are fully contacted, the impurities in the crystals are dissolved in the washing liquid, and after the washing is completed, the washing liquid is discharged from the liquid outlet through the filter screen, and the crystals are discharged from the discharge outlet. The first washing kettle and the second washing kettle have the above structure, are reasonable in design, effectively wash the impurities in the crystals, and improve the purity of the crystals.

[0016] The liquid outlet is communicated with the suction filter pump through a pipeline. In actual production, the washing liquid can be pumped out through the suction filter pump, so that the washing liquid and the crystals are effectively separated. BRIEF DESCRIPTION OF DRAWINGS

[0017] Figure 1 It is a structure diagram of a purification production system for pyrroloquinoline quinone disodium salt;

[0018] 1, the first dissolution kettle, 2, the first crystallization kettle, 3, the first filter device, 4, the first washing kettle, 5, the first drying device, 6, the second dissolution kettle, 7, the second crystallization kettle, 8, the second filter device, 9, the second washing kettle, 10, the second drying device, 11, the product storage tank, 12, the filter screen, 13, the suction filter pump. DETAILED DESCRIPTION

[0019] In order to make the purpose, technical scheme and advantages of the utility model more clearly, the following will be further described in detail by combining with the drawings and examples. It should be understood that the specific examples described here are only used to explain the utility model, and are not used to limit the utility model.

[0020] A purification production system for pyrroloquinoline quinone disodium salt, like Figure 1As shown, including the first dissolution kettle 1, the outlet of the first dissolution kettle 1 is communicated with the first crystallization kettle 2, the outlet of the first crystallization kettle 2 is communicated with the first filter device 3 (belt vacuum filter, purchased from the manufacturer), the discharge port of the first filter device 3 is communicated with the first washing kettle 4, the discharge port of the first washing kettle 4 is communicated with the first drying device 5 (oven), the discharge port of the first drying device 5 is communicated with the second dissolution kettle 6, the outlet of the second dissolution kettle 6 is communicated with the second crystallization kettle 7, the discharge port of the second crystallization kettle 7 is communicated with the second filter device 8 (vacuum filter, purchased from the manufacturer), the discharge port of the second filter device 8 is communicated with the second washing kettle 9, the discharge port of the second washing kettle 9 is communicated with the second drying device 10 (double-cone dryer), and the outlet of the second drying device is communicated with the product storage tank 11.

[0021] In actual production, the pyrroloquinoline quinone disodium salt is first put into the inside of the first dissolution kettle, the solvent is added, and after stirring and dissolution, it is pumped into the inside of the first crystallization kettle. The coolant in the jacket outside the first crystallization kettle is used for cooling, then the crystallization solvent is fully contacted with the feed liquid through stirring to promote the crystallization of the pyrroloquinoline quinone disodium salt. After the crystallization is completed, the feed liquid is pumped into the first filter device, and the filtered crystal product is conveyed into the first washing kettle through the conveying belt. After being fully washed by the washing liquid, the crystal is conveyed into the inside of the first drying device through the conveying belt or trolley, etc. After drying, the pyrroloquinoline quinone disodium salt is obtained. Then the pyrroloquinoline quinone disodium salt is put into the inside of the second dissolution kettle through the trolley or conveying belt, etc. After stirring, it is dissolved in the solvent, and then it is pumped into the inside of the second crystallization kettle through the conveying pump. After cooling by the coolant in the jacket and stirring, the obtained crystal product is conveyed into the inside of the second filter device. After filtration, the filtered crystal is conveyed into the inside of the second washing kettle through the conveying belt. After being fully washed by the washing liquid, the crystal is conveyed into the inside of the second drying device through the conveying belt for drying. The above-mentioned purification production system is reasonable in design, large in processing capacity, suitable for industrial production, greatly improves the purity of the pyrroloquinoline quinone disodium salt, and reduces the cost.

[0022] The first dissolution kettle 1 and the second dissolution kettle 6 each include a kettle body, the outer wall of the kettle body is provided with a jacket, the top of the kettle body is provided with a feed inlet and a solvent inlet, and the bottom of the kettle body is provided with a discharge port. The inside of the kettle body is provided with a stirring shaft, one end of the stirring shaft is connected with a motor, and the stirring shaft is provided with a plurality of stirring plates with hollow structures. After the motor is started, the stirring shaft and the plurality of stirring plates with hollow structures are rotated, so that the solvent is fully contacted with the pyrroloquinoline quinone disodium salt or the pyrroloquinoline quinone disodium salt primary crystal for dissolution. The heat medium in the jacket provides the temperature required for dissolution, and the dissolved feed liquid is discharged from the discharge port. The first dissolution kettle and the second dissolution kettle with the above-mentioned structure improve the dissolution efficiency and are helpful for subsequent crystallization operation.

[0023] The first crystallization kettle 2 and the second crystallization kettle 7 comprise a kettle body, the top of the kettle body is provided with a feed inlet and a crystallization solvent inlet, the top of the kettle body is provided with a discharge outlet, and the outside of the kettle body is provided with a jacket; the inside of the kettle body is provided with a stirring shaft, one end of the stirring shaft is connected with a motor, and the stirring shaft is provided with multiple stirring plates.

[0024] The first washing kettle 4 and the second washing kettle 9 each comprise a kettle body, the top of the kettle body is provided with a feed inlet and a washing liquid inlet, the bottom of the kettle body is provided with a discharge outlet, the lower part of the kettle body is provided with a liquid outlet on one side, and the inner wall of the kettle body is provided with a filter screen 12 at a position corresponding to the liquid outlet; the inside of the kettle body is provided with a rotating shaft, one end of the rotating shaft is connected with a motor, the upper part of the rotating shaft is provided with multiple stirring blades with hollow structures, and the bottom of the rotating shaft is provided with a stirring frame. After the motor is started, the rotating shaft, the multiple stirring blades and the stirring frame are driven to rotate, so that the crystals and the washing liquid are fully contacted, the impurities in the crystals are dissolved in the washing liquid, after the washing is completed, the washing liquid is discharged from the liquid outlet through the filter screen, and the crystals are discharged from the discharge outlet. The first washing kettle and the second washing kettle with the above structure are reasonable in design, effectively wash the impurities in the crystals, and improve the purity of the crystals.

[0025] The liquid outlet is communicated with the suction filter pump 13 through a pipeline. In actual production, the washing liquid can be pumped out through the suction filter pump, so that the washing liquid and the crystals are effectively separated.

[0026] The above only describes the preferred embodiments of the present application, and is not intended to limit the present application, and any modification, equivalent replacement and improvement made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A system for the purification production of pyrroloquinoline quinone disodium salt, characterized by, The first dissolution kettle is connected with the first crystallization kettle, the first crystallization kettle is connected with the first filter device, the first filter device is connected with the first washing kettle, the first washing kettle is connected with the first drying device, the first drying device is connected with the second dissolution kettle, the second dissolution kettle is connected with the second crystallization kettle, the second crystallization kettle is connected with the second filter device, the second filter device is connected with the second washing kettle, the second washing kettle is connected with the second drying device, and the second drying device is connected with the product storage tank.

2. The system for purifying production of pyrroloquinoline quinone disodium salt according to claim 1, characterized by, The first dissolution kettle and the second dissolution kettle each comprise a kettle body, an outer wall of the kettle body is provided with a jacket, a top of the kettle body is provided with a feed inlet and a solvent inlet, a bottom of the kettle body is provided with a discharge outlet, an inside of the kettle body is provided with a stirring shaft, one end of the stirring shaft is connected with a motor, and the stirring shaft is provided with a plurality of layers of hollow-structured stirring plates.

3. The system for purifying production of pyrroloquinoline quinone disodium salt according to claim 1, characterized in that, The first filter device and the second filter device are vacuum filters.

4. The system for purifying production of pyrroloquinoline quinone disodium salt according to claim 1, characterized by, The first crystallization kettle and the second crystallization kettle each comprise a kettle body, a top of the kettle body is provided with a feed inlet and a crystallization solvent inlet, a top of the kettle body is provided with a discharge outlet, an outside of the kettle body is provided with a jacket, an inside of the kettle body is provided with a stirring shaft, one end of the stirring shaft is connected with a motor, and the stirring shaft is provided with a plurality of stirring plates.

5. The system for purifying production of pyrroloquinoline quinone disodium salt according to claim 1, characterized in that, The first washing kettle and the second washing kettle each comprise a kettle body, a top of the kettle body is provided with a feed inlet and a washing liquid inlet, a bottom of the kettle body is provided with a discharge outlet, a lower side of the kettle body is provided with a liquid outlet, an inner wall of the kettle body is provided with a filter screen at a position corresponding to the liquid outlet, an inside of the kettle body is provided with a rotating shaft, one end of the rotating shaft is connected with a motor, an upper portion of the rotating shaft is provided with a plurality of layers of hollow-structured stirring paddles, and a bottom of the rotating shaft is provided with a stirring frame.

6. The system for purifying production of pyrroloquinoline quinone disodium salt according to claim 5, wherein The liquid outlet is connected with a suction pump through a pipeline.

Citation Information

Patent Citations

  • Pyrrolo quinoline quinone (PQQ) disodium salt impurity separation and purification method

    CN105334301A