Treatment device for triazine ring sodium salt cyclization mother liquor

Abstract

The utility model belongs to the technical field of chemical equipment, and particularly relates to a treatment device for triazine ring sodium salt cyclization mother liquor. Comprising a raw material buffer tank, an alcohol separation tower, a rectifying tower raw material tank, a batch rectification system, a DMF tower raw material tank and a falling film evaporator which are sequentially connected through pipelines, a vapor phase outlet of the falling film evaporator is sequentially connected to a gas-liquid separator and a DMF rectifying tower, and a liquid phase outlet of the falling film evaporator is connected to a scraper evaporator; a liquid phase outlet of the scraper evaporator is connected to a residual liquid kettle, a discharge port of the residual liquid kettle is sequentially connected to a centrifugal machine and a double-cone vacuum dryer, and a dichloromethane feeding pipeline is arranged on the residual liquid kettle; the batch rectification system comprises a batch evaporation kettle and a batch rectification tower; a control system is further included. According to the device, efficient recovery of methanol, ethanol and DMF and purification of sodium acetate are achieved, generation of hazardous waste is reduced, the cost is reduced, equipment connection is smooth, regulation and control are accurate, and the device is suitable for industrial efficient treatment requirements.

Description

Technical Field

[0001] This utility model belongs to the field of chemical equipment technology, specifically relating to a treatment device for the mother liquor of triazine sodium cyclization. Background Technology

[0002] In the field of chemical synthesis, triazine rings are a core intermediate in the synthesis of ceftriaxone sodium. The mother liquor generated during its production, which involves the cyclization of sodium triazine rings, has a complex composition, including methanol, ethanol, DMF, diethyl oxalate, and sodium acetate. Currently, the industry's treatment of this type of mother liquor is limited, typically only recovering methanol and ethanol, while the more valuable DMF is not effectively recovered, and the residual liquid is directly disposed of as hazardous waste. This treatment method not only wastes solvent resources such as DMF and increases raw material procurement costs, but also significantly increases environmental protection pressure due to the large amount of hazardous waste generated, resulting in high disposal costs and severely restricting the economic benefits and green sustainable development of enterprises. Furthermore, existing treatment devices often lack systematic integration design, with material conveying and parameter control relying on manual operation, leading to low processing efficiency and unstable product purity, making it difficult to meet the demands of efficient and precise processing in industrial production. Utility Model Content

[0003] In view of the shortcomings of the prior art, the purpose of this utility model is to provide a treatment device for the mother liquor of triazine sodium salt cyclization, which realizes the efficient recovery of methanol, ethanol and DMF and the purification of sodium acetate, reduces the generation of hazardous waste, lowers costs, and the equipment is smoothly connected and precisely controlled, making it suitable for the needs of efficient industrial treatment.

[0004] This utility model is achieved using the following technical solution:

[0005] The device for processing the mother liquor of triazine sodium cyclization includes a raw material buffer tank, an alcohol separation tower, a raw material tank for a distillation tower, a batch distillation system, a raw material tank for a DMF tower, and a falling film evaporator connected in sequence by pipelines. The vapor phase outlet of the falling film evaporator is connected in sequence by pipelines to a gas-liquid separator and a DMF distillation tower. The liquid phase outlet of the falling film evaporator is connected in sequence by pipelines to a scraped evaporator. The vapor phase outlet of the scraped evaporator is connected in sequence by pipelines to a gas-liquid separator. The liquid phase outlet of the scraped evaporator is connected in sequence by pipelines to a residual liquid tank. The outlet of the residual liquid tank is connected in sequence by pipelines to a centrifuge and a double cone vacuum dryer. A dichloromethane feeding pipeline is provided on the residual liquid tank.

[0006] The batch distillation system includes a batch evaporator and a batch distillation column. The top vapor outlet of the batch evaporator is connected to the bottom feed inlet of the batch distillation column via a pipeline, and the bottom outlet of the batch evaporator is connected to the feed inlet of the DMF column feed tank via a pipeline.

[0007] It also includes the control system.

[0008] The alcohol separation tower is equipped with a vapor phase outlet pipeline at the top, and a condenser and a methanol collection tank are sequentially installed on the vapor phase outlet pipeline.

[0009] The batch distillation column is equipped with a vapor phase outlet pipeline at the top, and a condenser and an ethanol collection tank are sequentially installed on the vapor phase outlet pipeline.

[0010] The DMF distillation column is equipped with a vapor phase outlet pipeline at the top, and a condenser and a DMF collection tank are sequentially installed on the vapor phase outlet pipeline.

[0011] The pipelines between the raw material buffer tank and the alcohol separation tower, between the alcohol separation tower and the raw material tank of the distillation tower, and between the raw material tank of the distillation tower and the intermittent evaporator are all equipped with delivery pumps and flow control valves, and each delivery pump and flow control valve is electrically connected to the control system.

[0012] The dichloromethane feeding pipeline is equipped with a metering pump and a valve, and the residual liquid vessel is equipped with a liquid level sensor. The metering pump, valve and liquid level sensor are all electrically connected to the control system.

[0013] The mother liquor of the triazine sodium salt cyclization comprises, by mass fraction: 66% methanol, 7% ethanol, 12% DMF, 5% diethyl oxalate and 10% sodium salt (mainly sodium acetate, containing a small amount of triazine sodium salt).

[0014] The working principle of the device for treating the mother liquor from the sodium triazine cyclization is as follows:

[0015] The mother liquor from the sodium triazine cyclization process is stored in a feed buffer tank to provide a stable supply for subsequent processing. The mother liquor is then pumped to an alcohol separation tower via a transfer pump and flow control valve. Atmospheric distillation separates methanol from other components. Methanol vapor is condensed in a condenser via the top vapor exit line and collected in a methanol collection tank. The remaining material at the bottom of the alcohol separation tower is temporarily stored in the feed tank of the distillation tower via a pipeline. When the material in the feed tank of the distillation tower reaches a set level, it is pumped into the batch evaporator of the batch distillation system via a transfer pump and flow control valve. The material is heated and vaporized in the batch evaporator. The vapor phase components enter the batch distillation tower via a pipeline. After gas-liquid mass transfer separation, ethanol vapor is condensed in a condenser via the top vapor exit line and finally collected in an ethanol collection tank. The remaining material at the bottom of the batch evaporator is temporarily stored in the DMF tower feed tank. Once the material in the DMF tower feed tank reaches the set quantity, it is sent to a falling film evaporator for evaporation. The vapor phase is then piped into a gas-liquid separator for separation and introduced into a DMF distillation tower for vacuum distillation. The purified DMF vapor is condensed in a condenser and collected in a DMF collection tank. The liquid phase concentrated by the falling film evaporator is sent to a scraped evaporator for further concentration. The vapor phase from the scraped evaporator also enters the gas-liquid separator. The concentrated residue is then piped into a residue tank. After the residue in the residue tank is cooled, the liquid level data is monitored in real time by a level sensor and fed back to the control system. A set amount of dichloromethane is added through a metering pump and valve on the dichloromethane feed line to extract diethyl oxalate. The extracted material is then sent to a centrifuge through the residue tank outlet for solid-liquid separation. The separated solid material is then sent to a double cone vacuum dryer for drying, ultimately yielding a relatively pure sodium acetate product. The entire system is electrically connected to various components such as delivery pumps, flow control valves, metering pumps, and level sensors through a control system, enabling automated control of parameters such as material delivery rate and extractant addition amount, ensuring precise and efficient processing.

[0016] Compared with the prior art, the beneficial effects of this utility model are as follows:

[0017] The triazine sodium salt cyclization mother liquor treatment device described in this invention achieves stepwise recovery and efficient treatment of multiple components in the mother liquor, possessing significant technical advantages and practical value. Firstly, the device sequentially separates and recovers methanol, ethanol, and DMF through the synergistic action of an alcohol separation tower, a batch distillation system, and a DMF distillation tower. Dedicated collection tanks are also provided to ensure the purity of each solvent. The recovered solvents can be directly recycled for subsequent production, significantly reducing raw material consumption costs and avoiding resource waste. Secondly, the device utilizes a combination of staged concentration using a falling film evaporator and a scraped plate evaporator, along with dichloromethane extraction, centrifugal separation, and vacuum drying to convert sodium acetate in the mother liquor into a relatively pure solid product, effectively reducing the generation of hazardous waste and lowering environmental disposal costs. Furthermore, the unit integrates temporary storage equipment such as raw material buffer tanks, distillation column raw material tanks, and DMF column raw material tanks. Combined with transfer pumps, flow control valves, and a control system, it achieves automated regulation of material conveying and precise control of various process parameters, improving the stability and continuity of unit operation, ensuring consistent product quality, while reducing manual labor intensity and increasing production efficiency. In addition, the entire unit has a compact structure, with all equipment connected in an orderly manner through pipelines, resulting in a smooth process that is suitable for industrial production scenarios and has broad application prospects. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of the structure of the treatment device for the mother liquor of triazine sodium cyclization according to the present invention;

[0019] In the diagram: 1. Raw material buffer tank; 2. Alcohol separation column; 3. Distillation column raw material tank; 4. Batch evaporator; 5. DMF column raw material tank; 6. Falling film evaporator; 7. Gas-liquid separator; 8. DMF distillation column; 9. Scraped evaporator; 10. Residue tank; 11. Centrifuge; 12. Double cone vacuum dryer; 13. Dichloromethane feed line; 14. Batch distillation column; 15. Condenser; 16. Methanol collection tank; 17. Ethanol collection tank; 18. DMF collection tank; 19. Transfer pump; 20. Flow control valve; 21. Metering pump; 22. Valve; 23. Liquid level sensor. Detailed Implementation

[0020] To make the objectives and technical solutions of this utility model clearer, the present utility model will be further described in detail below with reference to the accompanying drawings.

[0021] Example 1

[0022] like Figure 1As shown, the treatment device for the mother liquor of triazine sodium cyclization includes a raw material buffer tank 1, an alcohol separation tower 2, a distillation tower raw material tank 3, a batch distillation system, a DMF tower raw material tank 5, and a falling film evaporator 6 connected in sequence by pipelines. The vapor phase outlet of the falling film evaporator 6 is connected in sequence by pipelines to a gas-liquid separator 7 and a DMF distillation tower 8. The liquid phase outlet of the falling film evaporator 6 is connected in sequence by pipelines to a scraped evaporator 9. The vapor phase outlet of the scraped evaporator 9 is connected in sequence by pipelines to the gas-liquid separator 7. The liquid phase outlet of the scraped evaporator 9 is connected in sequence by pipelines to a residual liquid tank 10. The outlet of the residual liquid tank 10 is connected in sequence by pipelines to a centrifuge 11 and a double cone vacuum dryer 12. A dichloromethane feeding pipeline 13 is provided on the residual liquid tank 10.

[0023] The batch distillation system includes a batch evaporator 4 and a batch distillation column 14. The top vapor outlet of the batch evaporator 4 is connected to the bottom feed inlet of the batch distillation column 14 via a pipeline, and the bottom outlet of the batch evaporator 4 is connected to the feed inlet of the DMF column feed tank 5 via a pipeline.

[0024] It also includes the control system.

[0025] The top of the alcohol separation tower 2 is equipped with a vapor phase outlet pipeline, and a condenser 15 and a methanol collection tank 16 are sequentially installed on the vapor phase outlet pipeline.

[0026] The batch distillation column 14 is provided with a vapor phase outlet pipeline at the top of the column, and a condenser 15 and an ethanol collection tank 17 are sequentially installed on the vapor phase outlet pipeline.

[0027] The DMF distillation column 8 is equipped with a vapor phase outlet pipeline at the top of the column, and a condenser 15 and a DMF collection tank 18 are sequentially installed on the vapor phase outlet pipeline.

[0028] The pipelines between the raw material buffer tank 1 and the alcohol separation tower 2, the pipelines between the alcohol separation tower 2 and the raw material tank 3 of the distillation tower, and the pipelines between the raw material tank 3 of the distillation tower and the intermittent evaporator 4 are all equipped with a delivery pump 19 and a flow control valve 20. Each delivery pump 19 and flow control valve 20 is electrically connected to the control system.

[0029] The dichloromethane feeding pipeline 13 is equipped with a metering pump 21 and a valve 22, and the residual liquid vessel 10 is equipped with a liquid level sensor 23. The metering pump 21, valve 22 and liquid level sensor 23 are all electrically connected to the control system.

[0030] The mother liquor of the triazine sodium salt cyclization comprises, by mass fraction: 66% methanol, 7% ethanol, 12% DMF, 5% diethyl oxalate and 10% sodium salt (mainly sodium acetate, containing a small amount of triazine sodium salt).

[0031] The specific steps for doing this are as follows:

[0032] First, the control system starts the transfer pump 19 and flow control valve 20 between the raw material buffer tank 1 and the alcohol separation tower 2, and uniformly feeds the triazine sodium salt cyclization mother liquor stored in the raw material buffer tank 1 into the alcohol separation tower 2. The temperature at the bottom of the alcohol separation tower 2 is controlled at 96°C and the temperature at the top of the tower is controlled at 65°C. Distillation is carried out under normal pressure. The methanol vapor distilled at the top of the tower enters the condenser 15 through the vapor phase outlet pipeline and is condensed and collected in the methanol collection tank 16. The remaining material at the bottom of the alcohol separation tower 2 is transported to the raw material tank 3 of the distillation tower for temporary storage through the pipeline. Once the material in the feed tank 3 of the distillation column has accumulated, the control system starts the corresponding pipeline transfer pump 19 and flow control valve 20 to send the material into the batch evaporator 4 of the batch distillation system. The temperature of the batch evaporator 4 is controlled at 120°C. The vapor phase component generated after the material vaporizes enters the batch distillation column 14. The temperature at the top of the batch distillation column 14 is controlled at 79°C. After separation, the ethanol vapor distilled from the top of the column is condensed and collected in the ethanol collection tank 17 by the condenser 15. The remaining material at the bottom of the batch evaporator 4 is transported to the feed tank 5 of the DMF column for temporary storage via pipeline. Subsequently, the material in the DMF column feed tank 5 is fed into the falling film evaporator 6, and the temperature of the falling film evaporator 6 is controlled at 64°C. The vapor phase after distillation is separated by the gas-liquid separator 7 and enters the DMF distillation column 8, and the top temperature of the DMF distillation column 8 is controlled at 53°C and the bottom temperature at 102°C. After vacuum distillation, the DMF vapor is condensed and collected in the DMF collection tank 18 by the condenser 15. The liquid phase after concentration in the falling film evaporator 6 is fed into the scraped evaporator 9, and the temperature of the scraped evaporator 9 is controlled at 79°C. After further concentration, the vapor phase after distillation enters the gas-liquid separator 7, and the residual liquid is sent to the residual liquid tank 10. After the residual liquid in the residual liquid tank 10 cools to 20°C, the control system starts the metering pump 21 and valve 22 on the dichloromethane feeding pipeline 13 according to the signal fed back by the liquid level sensor 23 in the residual liquid tank 10. Three times the mass of dichloromethane relative to the residual liquid is added to extract diethyl oxalate. After extraction, the material is transported from the discharge port of the residual liquid tank 10 to the centrifuge 11 for solid-liquid separation. The separated solid material is sent to the double cone vacuum dryer 12, and the drying temperature is controlled at 33°C and the pressure at -0.08MPa. After vacuum drying, a relatively pure sodium acetate product is obtained, and the entire process is successfully completed.

Claims

1. A device for treating mother liquor from the cyclization of sodium triazine cyclohexane, characterized in that, The system includes a raw material buffer tank (1), an alcohol separation tower (2), a distillation tower raw material tank (3), a batch distillation system, a DMF tower raw material tank (5), and a falling film evaporator (6) connected in sequence via pipelines. The vapor phase outlet of the falling film evaporator (6) is connected in sequence via pipelines to a gas-liquid separator (7) and a DMF distillation tower (8). The liquid phase outlet of the falling film evaporator (6) is connected in sequence via pipelines to a scraped evaporator (9). The vapor phase outlet of the scraped evaporator (9) is connected in sequence via pipelines to a gas-liquid separator (7). The liquid phase outlet of the scraped evaporator (9) is connected in sequence via pipelines to a residual liquid tank (10). The outlet of the residual liquid tank (10) is connected in sequence via pipelines to a centrifuge (11) and a double cone vacuum dryer (12). A dichloromethane feeding pipeline (13) is provided on the residual liquid tank (10). The batch distillation system includes a batch evaporator (4) and a batch distillation column (14). The top vapor outlet of the batch evaporator (4) is connected to the bottom feed inlet of the batch distillation column (14) via a pipeline. The bottom outlet of the batch evaporator (4) is connected to the feed inlet of the DMF column feed tank (5) via a pipeline. It also includes the control system.

2. The apparatus for treating the mother liquor from the triazine cyclization of sodium salt according to claim 1, characterized in that, The alcohol separation tower (2) is provided with a vapor phase outlet pipeline at the top of the tower, and a condenser (15) and a methanol collection tank (16) are provided in sequence on the vapor phase outlet pipeline.

3. The apparatus for treating the mother liquor from the triazine cyclization of sodium salt according to claim 1, characterized in that, The batch distillation column (14) is provided with a vapor phase outlet pipeline at the top of the column, and a condenser (15) and an ethanol collection tank (17) are provided in sequence on the vapor phase outlet pipeline.

4. The apparatus for treating the mother liquor from the triazine cyclization of sodium salt according to claim 1, characterized in that, The DMF distillation column (8) is provided with a vapor phase outlet pipeline at the top of the column, and a condenser (15) and a DMF collection tank (18) are provided in sequence on the vapor phase outlet pipeline.

5. The apparatus for treating the mother liquor from the triazine cyclization of sodium salt according to claim 1, characterized in that, A delivery pump (19) and a flow control valve (20) are provided on the pipeline between the raw material buffer tank (1) and the alcohol separation tower (2), the pipeline between the alcohol separation tower (2) and the raw material tank (3) of the distillation tower, and the pipeline between the raw material tank (3) of the distillation tower and the intermittent evaporator (4). Each delivery pump (19) and flow control valve (20) is electrically connected to the control system.

6. The apparatus for treating the mother liquor from the triazine cyclization of sodium salt according to claim 1, characterized in that, The dichloromethane feeding pipeline (13) is equipped with a metering pump (21) and a valve (22), and the residual liquid tank (10) is equipped with a liquid level sensor (23). The metering pump (21), valve (22) and liquid level sensor (23) are all electrically connected to the control system.

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