Ethanol purification and recycling device in carbamazepine ammonification process

Abstract

The utility model discloses an ethanol purifying and recycling device in a carbamazepine ammonification process, and belongs to the technical field of chemical production equipment. The device comprises a rectification and purification device, a reflux control device connected with the rectification and purification device, and a molecular sieve dryer used for ethanol recycling, and the rectification and purification device comprises a supergravity bed used for rectification and purification, a reboiler and a condenser. The backflow control device comprises a main conveying pipe connected to the condenser, a first branch conveying pipe and a second branch conveying pipe, wherein the first branch conveying pipe and the second branch conveying pipe are arranged at the end of the main conveying pipe. According to the utility model, the rectification recovery of ethanol is realized through the supergravity bed, the reboiler and the condenser, and the reflux ratio is controlled through the reflux control device, so that the purity and the recovery efficiency of the recovered ethanol are improved; ethanol in the collecting tank after rectification is dried through the molecular sieve dryer, absolute ethanol is obtained, and the crude carbamazepine product is subjected to secondary refining, so that the ethanol in the carbamazepine ammoniation process is recycled with the advantages of industrial production, simple process and low energy consumption.

Description

Technical Field

[0001] This utility model belongs to the field of chemical production equipment technology, specifically relating to an ethanol purification and reuse device in the carbamazepine ammoniation process. Background Technology

[0002] Currently, the main route for preparing carbamazepine both domestically and internationally is the bromocarbamazepine synthesis route, which uses iminodibenzyl as the starting material and proceeds through acyl chloride, bromination dehydrogenation, and ammoniation reactions. In the carbamazepine ammoniation process, ethanol primarily acts as a solvent: 1) Dissolution and reaction: During the ammoniation reaction, ethanol acts as a solvent, helping to dissolve carbamazepine and other reactants, ensuring uniform distribution of the reactants and improving reaction efficiency; 2) Crystallization and purification: After the reaction, ethanol is also used in the crystallization process. Recrystallization with ethanol effectively purifies the product, removes impurities, and improves the purity of the product.

[0003] Therefore, a large amount of ethanol is required in the production process of carbamazepine. If the mother liquor generated from the carbamazepine amination process is not recycled and treated, it will cause environmental pollution. The mother liquor has a complex composition, and conventional treatment methods are difficult to meet the recycling standards.

[0004] Currently, there are many methods for recovering used ethanol, including membrane separation, extraction, adsorption, and distillation. Distillation is the most widely used method. Traditional distillation columns, such as plate columns or packed columns, are bulky and energy-intensive for ethanol recovery. Therefore, there is a need for a device that can purify and reuse the solvent ethanol from the carbamazepine amination process, reducing ethanol solvent emissions, saving costs on purchasing ethanol solvent and treating waste liquid, and bringing considerable economic value to enterprises. Utility Model Content

[0005] The technical problem solved by this utility model is to provide an ethanol purification and reuse device in the carbamazepine ammoniation process, which can simultaneously realize the purification, recovery and reuse of ethanol in the carbamazepine ammoniation process, and reduce the amount of ethanol solvent used.

[0006] To solve the above-mentioned technical problems, the technical solution adopted by this utility model is as follows:

[0007] An ethanol purification and reuse device in a carbamazepine amination process includes a distillation purification unit, a reflux control device connected to the distillation purification unit, and a molecular sieve dryer for ethanol reuse. The distillation purification unit includes a high-gravity bed, a reboiler, and a condenser for distillation purification. The reflux control device includes a main delivery pipe connected to the condenser and a first and a second branch delivery pipe located at the end of the main delivery pipe.

[0008] Preferably, the system also includes a concentration tank connected to the feed pipe, a first collection tank, a transfer pump, a second collection tank, and a coarse product collection trough connected to the bottom of the concentration tank.

[0009] Preferably, the concentrate outlet pipe of the concentration tank is connected to the first collection tank, and the first collection tank is connected to the liquid phase inlet of the supergravity bed via a transfer pump.

[0010] Preferably, the liquid phase outlet of the supergravity bed is connected to the gas phase inlet of the supergravity bed via a reboiler, and the gas phase outlet of the supergravity bed is connected to the second collection tank via a condenser.

[0011] Preferably, the first branch delivery pipe is connected to the reflux liquid inlet of the high gravity bed, and the second branch delivery pipe is connected to the second collection tank.

[0012] Preferably, both the first and second branch conveying pipes are equipped with rotor flow meters and reflux valves.

[0013] Preferably, a second outlet pipe is connected to the bottom of the second collection tank.

[0014] Preferably, a first outlet pipe connected to the molecular sieve dryer is also provided below the second collection tank.

[0015] Preferably, the molecular sieve dryer is provided with a third liquid outlet pipe.

[0016] Beneficial effects: Compared with the prior art, the present invention has the following advantages:

[0017] 1) This utility model achieves ethanol distillation recovery from the collected concentrate through a supergravity bed, reboiler and condenser, and controls the reflux ratio through a reflux control device, which can greatly improve the purity and recovery efficiency of the recovered ethanol, save the floor space of the separation equipment, and realize industrial production, simple process and low energy consumption for the recovery of ethanol in the carbamazepine ammoniation process.

[0018] 2) This invention dries the ethanol in the collection tank after distillation using a molecular sieve dryer to obtain anhydrous ethanol, which can realize the secondary purification of crude carbamazepine.

[0019] 3) The device of this utility model first collects the ethanol solution obtained after distillation and purification. The collected aqueous ethanol is then used to purify the crude carbamazepine product for the first time. The aqueous ethanol is then passed through a molecular sieve dryer to remove water, resulting in anhydrous ethanol. This achieves secondary purification of the crude carbamazepine product, greatly reducing the amount of ethanol used. It also recovers, purifies, and reuses the ethanol in the carbamazepine ammoniation process, making reasonable use of resources, avoiding waste, and reducing costs. Attached Figure Description

[0020] Figure 1 This is a schematic diagram of the overall structure of this utility model;

[0021] The components are as follows: 1. Concentrator; 2. First collection tank; 3. Transfer pump; 4. High gravity bed; 5. Reboiler; 6. Condenser; 7. Second collection tank; 8. Molecular sieve dryer; 9. Crude product collection tank; 10. Feed inlet; 11. Concentrate outlet pipe; 12. Liquid phase feed inlet; 13. Gas phase feed inlet; 14. Gas phase outlet; 15. Liquid phase outlet; 16. Reflux inlet; 17. Main conveying pipe; 18. First branch conveying pipe; 19. Second branch conveying pipe; 20. Rotor flow meter; 21. Reflux valve; 22. First outlet pipe; 23. Second outlet pipe; 24. Third outlet pipe. Detailed Implementation

[0022] The present invention will be further illustrated below with reference to specific embodiments. The embodiments are implemented based on the technical solution of the present invention. It should be understood that these embodiments are only used to illustrate the present invention and are not intended to limit the scope of the present invention.

[0023] like Figure 1 As shown, this utility model discloses an ethanol purification and reuse device in a carbamazepine amination process, comprising a concentration tank 1 connected to a feed pipe 10. The concentrate outlet pipe 11 of the concentration tank 1 is connected to the inlet of a first collection tank 2. The outlet of the first collection tank 2 is connected to the liquid phase inlet 12 of a supergravity bed 4 via a transfer pump 3. The liquid phase outlet 15 of the supergravity bed 4 is connected to the gas phase inlet 13 of the supergravity bed 4 via a reboiler 5. The gas phase outlet 14 of the supergravity bed 4 is connected to a second collection tank 7 via a condenser 6. The bottom of the concentration tank 1 is connected to a crude product collection tank 9.

[0024] The condenser 6 is connected to a main delivery pipe 17. The end of the main delivery pipe 17 is provided with a first branch delivery pipe 18 for connecting to the reflux liquid inlet 16 and a second branch delivery pipe 19 for connecting to the second collection tank 7. Both the first branch delivery pipe 18 and the second branch delivery pipe 19 are provided with a rotor flow meter 20 and a reflux valve 21.

[0025] The bottom of the second collection tank 7 is connected to a second outlet pipe 23. A portion of the aqueous ethanol in the second collection tank 7 is discharged through the second outlet pipe 23, performing the first purification of the crude carbamazepine in the crude product collection tank 9. The bottom of the second collection tank 7 is also connected to a molecular sieve dryer 8 through a first outlet pipe 22. Another portion of the aqueous ethanol in the second collection tank 7 is dried in the molecular sieve dryer 8, and the resulting anhydrous ethanol is discharged through a third outlet pipe 24, performing the second purification of the crude carbamazepine to obtain the finished carbamazepine product.

[0026] The supergravity bed 4 is a baffle-type supergravity bed.

[0027] In operation, the material after the carbamazepine ammoniation reaction is conveyed through feed pipe 10 to concentration tank 1 for concentration, yielding crude carbamazepine and concentrated liquid. The crude carbamazepine enters crude product collection tank 9 for later use, while the concentrated liquid is collected through concentrated liquid outlet pipe 11 into first collection tank 2, obtaining primary collected liquid. The primary collected liquid is conveyed to centrifugal bed 4 by transfer pump 3 and enters reboiler 5 through liquid phase outlet 15 for heating and evaporation. The gas phase enters centrifugal bed 4 through gas phase inlet 13 for separation. The temperature and pressure within centrifugal bed 4 are controlled, and the ethanol vapor purified by centrifugal bed 4 enters condenser 6 through gas phase outlet 14 for condensation into ethanol solution.

[0028] When the concentration of the ethanol solution condensed from condenser 6 is insufficient, the condensate is completely refluxed back to the high-gravity bed 4 via the first distribution pipe 18 for further distillation, and the second distribution pipe 19 is closed. When the desired ethanol concentration is reached, the opening of the first distribution pipe 18 is appropriately reduced, and the second distribution pipe 19 is opened to collect the distillate into the second collection tank 7. The feed, reflux, and discharge rates are adjusted to stabilize the system and obtain a distillate with a stable content. The distillate is collected in the second collection tank 7, achieving ethanol purification and recovery.

[0029] A portion of the aqueous ethanol collected in the second collection tank 7 is discharged through the second outlet pipe 23, performing the first purification of the crude carbamazepine in the crude product collection tank 9. The remaining aqueous ethanol in the second collection tank 7 is dried in the molecular sieve dryer 8 through the first outlet pipe 22, and the resulting anhydrous ethanol is discharged through the third outlet pipe 24, performing the second purification of the crude carbamazepine to obtain the finished carbamazepine product, thus achieving the reuse of ethanol.

[0030] The above description is only a preferred embodiment of the present utility model. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present utility model, and these improvements and modifications should also be considered within the protection scope of the present utility model.

Claims

1. An ethanol purification and reuse device in a carbamazepine ammoniation process, characterized in that, It includes a distillation purification device, a reflux control device connected to the distillation purification device, and a molecular sieve dryer (8) for ethanol reuse. The distillation purification device includes a supergravity bed (4), a reboiler (5), and a condenser (6) for distillation purification. The reflux control device includes a main delivery pipe (17) connected to the condenser (6) and a first branch delivery pipe (18) and a second branch delivery pipe (19) located at the end of the main delivery pipe (17).

2. The ethanol purification and reuse apparatus in the carbamazepine ammoniation process according to claim 1, characterized in that, It also includes a concentration tank (1) connected to the feed pipe (10), a first collection tank (2), a transfer pump (3), a second collection tank (7), and a crude product collection trough (9) connected to the bottom of the concentration tank (1).

3. The ethanol purification and reuse apparatus in the carbamazepine ammoniation process according to claim 2, characterized in that, The concentrated liquid outlet pipe (11) of the concentration tank (1) is connected to the first collection tank (2), and the first collection tank (2) is connected to the liquid phase inlet (12) of the supergravity bed (4) through the transfer pump (3).

4. The ethanol purification and reuse apparatus in the carbamazepine ammoniation process according to claim 1, characterized in that, The liquid phase outlet (15) of the supergravity bed (4) is connected to the gas phase inlet (13) of the supergravity bed (4) through the reboiler (5), and the gas phase outlet (14) of the supergravity bed (4) is connected to the second collection tank (7) through the condenser (6).

5. The ethanol purification and reuse apparatus in the carbamazepine ammoniation process according to claim 1, characterized in that, The first sub-transfer pipe (18) is connected to the reflux liquid inlet (16) on the supergravity bed (4), and the second sub-transfer pipe (19) is connected to the second collection tank (7).

6. The ethanol purification and reuse apparatus in the carbamazepine ammoniation process according to claim 1, characterized in that, Both the first sub-conveying pipe (18) and the second sub-conveying pipe (19) are equipped with a rotor flow meter (20) and a return valve (21).

7. The ethanol purification and reuse apparatus in the carbamazepine ammoniation process according to claim 2, characterized in that, The bottom of the second collection tank (7) is connected to a second outlet pipe (23).

8. The ethanol purification and reuse apparatus in the carbamazepine ammoniation process according to claim 7, characterized in that, Below the second collection tank (7) is a first liquid outlet pipe (22) that is connected to the molecular sieve dryer (8).

9. The ethanol purification and reuse apparatus in the carbamazepine ammoniation process according to claim 1, characterized in that, The molecular sieve dryer (8) is equipped with a third liquid outlet pipe (24).

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