Novel clopidogrel mother liquor recovery device

Abstract

The utility model discloses a novel clopidogrel mother liquor recovery device which comprises a neutralization tank, an outlet of the neutralization tank is connected with a raw material preheater through a guide pipe, an outlet of the raw material preheater is connected with a rectifying tower through a guide pipe, and a top outlet of the rectifying tower is connected with a fractional condenser through a guide pipe; after being neutralized, raw materials are pumped into the raw material preheater through the raw material pump to be preheated, the preheated raw materials enter the rectifying tower to be rectified, distillates at the top in the rectifying tower are segregated through the segregation device, distillates at the top enter the superheater through the tower top distillates outlet, and the distillates are filtered by the membrane assembly, and then are separated by the membrane assembly. The filtered waste liquid enters a condenser to be condensed, and the material to be recycled enters a raw material preheater, then enters a finished product cooler to be cooled, then enters a dehydrated product storage tank and is pumped out by a finished product pump; the mother liquor permeated by the condenser enters the neutralization tank again; and recovery of mother liquor and harmless treatment of waste liquor are realized.

Description

Technical Field

[0001] The utility model relates to the technical field of clopidogrel mother liquor recovery, in particular to a novel clopidogrel mother liquor recovery device. Background Art

[0002] Clopidogrel Bisulfate is a new type of thienopyridine derivative, which can irreversibly inhibit platelet aggregation by selectively binding to the ADP receptor coupled to the platelet surface adenylate enzyme, and can reduce the formation of thrombus in blood vessels. At present, there are two main methods for synthesizing clopidogrel: synthesis first and then splitting, and splitting first and then synthesizing. Among them, the splitting first and then synthesizing method is more common in industrial production, that is, first splitting to obtain (S)-o-chlorophenylglycine methyl ester (tartrate or hydrochloride) (compound 1), and then synthesizing the key intermediate (S)-2-(2-thienylethylamino)-(2-chlorophenyl)-acetic acid methyl ester (compound 4) and its salt (compound 5), and then using formaldehyde and acid catalytic cyclization to generate clopidogrel. The general synthesis method of the key intermediate compound 4 and its salt is as follows: first, the raw material (S)-o-chlorophenylglycine methyl ester (tartrate or hydrochloride) (compound 1) is deacidified to obtain (S)-o-chlorophenylglycine methyl ester (compound 2), and then a nucleophilic substitution reaction is carried out with the liquid raw material 2-thiopheneethyl p-toluenesulfonate (compound 3) to obtain compound 4, and then a salt is formed with hydrochloric acid to obtain compound 5. In the process of synthesizing the key intermediate compound 4, after many experiments and literature reports, when (S)-o-chlorophenylglycine methyl ester (compound 2) and 2-thiopheneethyl p-toluenesulfonate (compound 3) undergo nucleophilic substitution reaction, an excess of compound 3 needs to be added so that compound 2 will react completely to obtain compound 4 with a higher yield. For example, in the literature "Hu Jiapeng, et al. Study on the Synthesis Process of Clopidogrel Hydrogen Sulfate [J]. Zhejiang Chemical Industry, 2012, 432: 9-11.", when synthesizing (S)-2-(2-thienylethylamino)-(2-chlorophenyl)acetic acid methyl ester hydrochloride, the amount of compound 2 was 28g (0.14mol), and the amount of compound 3 was 48g (0.17mol), wherein the molar amount of compound 3 was 1.2 times that of compound 2, which was obviously excessive. The excess 2-thienylethyl p-toluenesulfonate (compound 3) will be removed after post-treatment and directly enter the condensation mother liquor. However, in the industrial production process, the production and preparation cost of 2-thienylethyl p-toluenesulfonate is high, and the amount of mother liquor in this step is large. If the mother liquor is treated as production waste liquid, it will not only waste resources and increase the cost of raw materials, but also have a certain impact on the environment. Therefore, there is an urgent need for a device that can recover 2-thienylethyl p-toluenesulfonate in the clopidogrel condensation mother liquor. Utility Model Content

[0003] The utility model aims to provide a novel clopidogrel mother liquor recovery device, which solves the problems that the production and preparation cost of 2-thienylethyl p-toluenesulfonate is high and the amount of mother liquor in this step is large. If the mother liquor is treated as production waste liquid, it will not only waste resources and increase the cost of raw materials, but also cause certain impacts on the environment.

[0004] In order to solve the above technical problems, according to one aspect of the present invention, the present invention provides the following technical solutions:

[0005] A novel clopidogrel mother liquor recovery device comprises a neutralization tank, wherein the outlet of the neutralization tank is connected to a raw material preheater through a conduit, the outlet of the raw material preheater is connected to a distillation tower through a conduit, the top outlet of the distillation tower is connected to a partial condenser through a conduit, the outlet of the partial condenser is connected to a tower top distillate outlet through a conduit, the outlet of the tower top distillate outlet is connected to a superheater through a conduit, the superheater is connected to a membrane module through a conduit, the membrane module is connected to a condenser through a conduit, the outlet of the condenser is connected to a permeate storage tank through a conduit, the outlet of the permeate storage tank is connected to an input end of a permeate pump through a conduit, the output end of the permeate pump is connected to an inlet of a neutralization tank through a conduit, the outlet of the raw material preheater is connected to a finished product cooler through a conduit, and the outlet of the finished product cooler is connected to a dehydrated product storage tank through a conduit.

[0006] Preferably, one of the feed ports of the neutralization tank is connected to a neutralization agent inlet via a conduit, and the other feed port of the neutralization tank is connected to a raw material inlet via a conduit.

[0007] Preferably, the outlet of the condenser is connected to a vacuum unit via a conduit, and the outlet of the vacuum unit is connected to a recycling material outlet via a conduit.

[0008] Preferably, the outlet of the distillation tower is connected to a wastewater cooler via a conduit, and the outlet of the dehydrated product storage tank is connected to a finished product pump via a conduit.

[0009] Preferably, a raw material pump is installed on the conduit connecting the neutralization tank and the raw material preheater.

[0010] Preferably, a reboiler is installed on the conduit connecting the distillation tower and the wastewater cooler.

[0011] Preferably, a supplementary heat device is installed on the conduit connecting each filter membrane in the membrane assembly.

[0012] Compared with the prior art, the beneficial effects of the utility model are:

[0013] After being neutralized, the raw materials of the utility model are pumped into a raw material preheater through a raw material pump for preheating, the preheated raw materials enter a distillation tower for distillation, the distillate at the top of the distillation tower is condensed through a condenser, the top distillate enters a superheater through a tower top distillate outlet, the distillate is filtered by a membrane component, the filtered waste liquid enters a condenser for condensation, the material to be recovered enters the raw material preheater again, then enters a finished product cooler for cooling, then enters a dehydrated product storage tank, and then is pumped out by a finished product pump; the mother liquid permeated by the condenser enters the neutralization tank again, and the recovery of the mother liquid and the harmless treatment of the waste liquid are realized. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 A schematic diagram of the structure provided for Example 1 of the utility model;

[0015] Figure 2 A schematic diagram of the structure provided for Embodiment 2 of the present utility model;

[0016] Figure 3 A schematic diagram of the structure provided for Embodiment 3 of the present utility model;

[0017] Figure 4 This is a structural schematic diagram provided for Example 4 of the utility model.

[0018] In the figure: raw material inlet 1, neutralization tank 2, neutralization agent inlet 3, raw material pump 4, raw material preheater 5, distillation tower 6, partial condenser 7, top distillate outlet 8, superheater 9, membrane module 10, vacuum unit 11, recycled material outlet 12, condenser 13, permeate storage tank 14, permeate pump 15, wastewater cooler 16, finished product cooler 17, dehydrated product storage tank 18, finished product pump 19, reboiler 20, supplementary heat device 21. DETAILED DESCRIPTION

[0019] The preferred embodiments of the present invention are described below in conjunction with the accompanying drawings. It should be understood that the preferred embodiments described herein are only used to illustrate and explain the present invention, and are not used to limit the present invention.

[0020] Example 1, a novel clopidogrel mother liquor recovery device provided by the present invention, please refer to Figure 1, including a neutralization tank 2, the outlet of the neutralization tank 2 is connected to a raw material preheater 5 through a conduit, a raw material pump 4 is installed on the conduit connecting the neutralization tank 2 and the raw material preheater 5, the outlet of the raw material preheater 5 is connected to a distillation tower 6 through a conduit, the top outlet of the distillation tower 6 is connected to a condenser 7 through a conduit, the outlet of the condenser 7 is connected to a tower top distillate outlet 8 through a conduit, the outlet of the tower top distillate outlet 8 is connected to a superheater 9 through a conduit, the superheater 9 is connected to a membrane module 10 through a conduit, the membrane module 10 is connected to a condenser 13 through a conduit, the outlet of the condenser 13 is connected to a permeate storage tank 14 through a conduit, the outlet of the permeate storage tank 14 is connected to an input end of a permeate pump 15 through a conduit, the output end of the permeate pump 15 is connected to the inlet of the neutralization tank 2 through a conduit, the outlet of the raw material preheater 5 is connected to a finished product cooler 17 through a conduit, and the outlet of the finished product cooler 17 is connected to a dehydrated product storage tank 18 through a conduit.

[0021] One of the feed ports of the neutralization tank 2 is connected to the neutralization agent inlet 3 via a conduit, and the other feed port of the neutralization tank 2 is connected to the raw material inlet 1 via a conduit.

[0022] The outlet of the condenser 13 is connected to the vacuum unit 11 through a conduit, and the outlet of the vacuum unit 11 is connected to the recycling material outlet 12 through a conduit.

[0023] The outlet of the distillation tower 6 is connected to a wastewater cooler 16 via a conduit, and the outlet of the dehydrated product storage tank 18 is connected to a finished product pump 19 via a conduit.

[0024] During specific use, the mother liquor is injected into the neutralization tank 2 through the raw material inlet 1, and the neutralizing liquid is injected into the neutralization tank 2 from the neutralizing agent inlet 3; after the raw material is neutralized, it is pumped into the raw material preheater 5 through the raw material pump 4 for preheating, and the preheated raw material enters the distillation tower 6 for distillation, and the distillate at the top of the distillation tower 6 is condensed by the condenser 7, and the top distillate enters the superheater 9 through the top distillate outlet 8, and the distillate is filtered by the membrane component 10, and the filtered waste liquid enters the condenser 13 for condensation, and the material to be recovered enters the raw material preheater 5 again, and then enters the finished product cooler 17 for cooling, and then enters the dehydrated product storage tank 18, and then is pumped out by the finished product pump 19; the mother liquor permeated by the condenser 13 enters the neutralization tank 2 again.

[0025] Example 2, refer to the attached Figure 2 , which is different from Example 1, is that a reboiler 20 is installed on the conduit connecting the distillation tower 6 and the wastewater cooler 16; and reboiler 20 is used for reboiling.

[0026] During specific use, the mother liquor is injected into the neutralization tank 2 through the raw material inlet 1, and the neutralizing liquid is injected into the neutralization tank 2 from the neutralizing agent inlet 3; after the raw material is neutralized, it is pumped into the raw material preheater 5 through the raw material pump 4 for preheating, and the preheated raw material enters the distillation tower 6 for distillation, and the distillate at the top of the distillation tower 6 is condensed by the condenser 7, and the top distillate enters the superheater 9 through the top distillate outlet 8, and the distillate is filtered by the membrane component 10, and the filtered waste liquid enters the condenser 13 for condensation, and the material to be recovered enters the raw material preheater 5 again, and then enters the finished product cooler 17 for cooling, and then enters the dehydrated product storage tank 18, and then is pumped out by the finished product pump 19; the mother liquor permeated by the condenser 13 enters the neutralization tank 2 again.

[0027] Example 3, refer to the attached Figure 3 , which is different from Example 1, is that a supplementary heat device 21 is installed on the conduit connecting each filter membrane in the membrane assembly 10; the supplementary heat device 21 heats the raw materials during filtration to avoid crystallization in the waste liquid and inconvenience in the separation of the waste liquid.

[0028] During specific use, the mother liquor is injected into the neutralization tank 2 through the raw material inlet 1, and the neutralizing liquid is injected into the neutralization tank 2 from the neutralizing agent inlet 3; after the raw material is neutralized, it is pumped into the raw material preheater 5 through the raw material pump 4 for preheating, and the preheated raw material enters the distillation tower 6 for distillation, and the distillate at the top of the distillation tower 6 is condensed by the condenser 7, and the top distillate enters the superheater 9 through the top distillate outlet 8, and the distillate is filtered by the membrane component 10, and the filtered waste liquid enters the condenser 13 for condensation, and the material to be recovered enters the raw material preheater 5 again, and then enters the finished product cooler 17 for cooling, and then enters the dehydrated product storage tank 18, and then is pumped out by the finished product pump 19; the mother liquor permeated by the condenser 13 enters the neutralization tank 2 again.

[0029] Example 4, see attached Figure 4 , which is different from Example 1, is that a reboiler 20 is installed on the conduit connecting the distillation tower 6 and the wastewater cooler 16; and a supplementary heat device 21 is installed on the conduit connecting each filter membrane in the membrane assembly 10.

[0030] During specific use, the mother liquor is injected into the neutralization tank 2 through the raw material inlet 1, and the neutralizing liquid is injected into the neutralization tank 2 from the neutralizing agent inlet 3; after the raw material is neutralized, it is pumped into the raw material preheater 5 through the raw material pump 4 for preheating, and the preheated raw material enters the distillation tower 6 for distillation, and the distillate at the top of the distillation tower 6 is condensed by the condenser 7, and the top distillate enters the superheater 9 through the top distillate outlet 8, and the distillate is filtered by the membrane component 10, and the filtered waste liquid enters the condenser 13 for condensation, and the material to be recovered enters the raw material preheater 5 again, and then enters the finished product cooler 17 for cooling, and then enters the dehydrated product storage tank 18, and then is pumped out by the finished product pump 19; the mother liquor permeated by the condenser 13 enters the neutralization tank 2 again.

[0031] The above is only a preferred embodiment of the utility model. Any person skilled in the art may modify the utility model by using the above technical solution or modify it into an equivalent technical solution. Therefore, any simple modification or equivalent transformation based on the technical solution of the utility model shall fall within the scope of protection claimed by the utility model.

Claims

1. A novel clopidogrel mother liquor recovery device, comprising a neutralization tank (2), characterized in that: The outlet of the neutralization tank (2) is connected to the raw material preheater (5) through a conduit, the outlet of the raw material preheater (5) is connected to the distillation tower (6) through a conduit, the top outlet of the distillation tower (6) is connected to the partial condenser (7) through a conduit, the outlet of the partial condenser (7) is connected to the tower top distillate outlet (8) through a conduit, the outlet of the tower top distillate outlet (8) is connected to the superheater (9) through a conduit, the superheater (9) is connected to the membrane module (10) through a conduit, the membrane module (10) is connected to the condenser (13) through a conduit, the outlet of the condenser (13) is connected to the permeate storage tank (14) through a conduit, the outlet of the permeate storage tank (14) is connected to the input end of the permeate pump (15) through a conduit, the output end of the permeate pump (15) is connected to the inlet of the neutralization tank (2) through a conduit, the outlet of the raw material preheater (5) is connected to the finished product cooler (17) through a conduit, and the outlet of the finished product cooler (17) is connected to the dehydrated product storage tank (18) through a conduit.

2. The novel clopidogrel mother liquor recovery device according to claim 1, characterized in that: One of the feed ports of the neutralization tank (2) is connected to the neutralization agent inlet (3) via a conduit, and the other feed port of the neutralization tank (2) is connected to the raw material inlet (1) via a conduit.

3. The novel clopidogrel mother liquor recovery device according to claim 1, characterized in that: The outlet of the condenser (13) is connected to the vacuum unit (11) via a conduit, and the outlet of the vacuum unit (11) is connected to the recycling material outlet (12) via a conduit.

4. The novel clopidogrel mother liquor recovery device according to claim 2 or 3, characterized in that: The outlet of the distillation tower (6) is connected to a wastewater cooler (16) via a conduit, and the outlet of the dehydrated product storage tank (18) is connected to a finished product pump (19) via a conduit.

5. The novel clopidogrel mother liquor recovery device according to claim 4, characterized in that: A raw material pump (4) is installed on the conduit connecting the neutralization tank (2) and the raw material preheater (5).

6. The novel clopidogrel mother liquor recovery device according to claim 5, characterized in that: A reboiler (20) is installed on the conduit connecting the distillation tower (6) and the wastewater cooler (16).

7. The novel clopidogrel mother liquor recovery device according to claim 5 or 6, characterized in that: A supplementary heat device (21) is installed on the conduit connecting each filter membrane in the membrane assembly (10).

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