Reaction device for etifolin hydrochloride

Abstract

The reaction device comprises a decoloring tank, a first plate-and-frame filter and a reaction kettle, the decoloring tank is communicated with an ethanol storage tank, a hydrochloric acid solution storage tank and an activated carbon storage tank, the reaction kettle is communicated with a hydrogen storage tank, and the reaction kettle is further sequentially communicated with a second plate-and-frame filter, a concentration tank and a first crystallizing tank. A first centrifugal machine, a buffer tank, a second centrifugal machine, a refining tank, a second crystallizing tank, a third centrifugal machine, a first drying tank and a target product storage tank; the first crystallizing tank and the refining tank are communicated with an isopropanol storage tank, the buffer tank is communicated with an ammonia water solution storage tank, and the refining tank is further communicated with a hydrochloric acid solution storage tank and a methanol storage tank. The device is high in automation degree, simple in structure and high in decoloration process and crystallization process efficiency, the production efficiency of products is improved, the catalyst and activated carbon in the process can be recycled, and energy conservation and consumption reduction are achieved.

Description

TECHNICAL FIELD

[0001] The utility model relates to chemical industry device technical field, concretely relates to a reaction device for hydrochloric acid etilefrine. BACKGROUND

[0002] Hydrochloric acid etilefrine is white to white crystalline powder, easily soluble in water and ethanol, non-toxic, harmless, non-corrosive, odorless, is a kind of commonly used drug for treating hypotension.The preparation process of the current hydrochloric acid etilefrine is mainly as follows: taking etilefrine ketone hydrochloride as reaction raw material, hydrogenation reduction is carried out under the action of hydrogen, and crude product is prepared, then after being isolated by ammonia water, etilefrine base is obtained, methanol is used as solvent, acidification is carried out with hydrochloric acid, after concentration, dilution is carried out with isopropyl alcohol, hydrochloric acid etilefrine wet product is obtained by centrifugation after cooling, and after drying and packaging, hydrochloric acid etilefrine finished product is obtained.The reaction device for producing hydrochloric acid etilefrine in prior art has low degree of automation and production efficiency, and active carbon and catalyst in production process cannot be effectively recycled, greatly increasing the production cost of hydrochloric acid etilefrine. SUMMARY

[0003] The technical problem to be solved by the utility model is: in view of the deficiencies in prior art, provide a reaction device for hydrochloric acid etilefrine, the device has high degree of automation, simple structure, high efficiency in the process of decolorization and crystallization, improve the production efficiency of product, and the catalyst and active carbon in the process can be recycled, energy saving and consumption reduction.

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

[0005] A reaction device for hydrochloric acid etilefrine, including decoloring tank, first plate and frame filter, reaction kettle, the decoloring tank is connected with ethanol storage tank, first hydrochloric acid solution storage tank, active carbon storage tank, the reaction kettle is connected with hydrogen storage tank, the reaction kettle is also connected with second plate and frame filter, concentration tank, first crystallization tank, first centrifuge, buffer tank, second centrifuge, refining tank, second crystallization tank, third centrifuge, first drying tank, target product storage tank in sequence, the first crystallization tank, second crystallization tank are connected with isopropyl alcohol storage tank, the buffer tank is connected with ammonia water solution storage tank, the refining tank is also connected with second hydrochloric acid solution storage tank, methanol storage tank;

[0006] The catalyst adding port is equipped on the reaction kettle, temperature sensor and pH sensor are equipped in the decoloring tank, electric valve is equipped on the connecting pipeline of the decoloring tank and the first hydrochloric acid solution storage tank, the electric valve is interlocked with the pH sensor, adjusting valve is equipped on the connecting pipeline of the reaction kettle and the hydrogen storage tank.

[0007] Preferably, the decoloring tank and the reaction kettle are both provided with a first stirring device, the first stirring device comprises a first stirring shaft and a first stirring motor for driving the first stirring shaft to rotate, a plurality of inclined stirring rods are arranged on the first stirring shaft, and an arc-shaped stirring rod is arranged at the bottom of the first stirring shaft.

[0008] Preferably, the plurality of inclined stirring rods are arranged in a non-parallel manner.

[0009] Preferably, a solid outlet of the first plate-and-frame filter is connected with a second drying tank and an activated carbon recovery tank.

[0010] Preferably, a solid outlet of the second plate-and-frame filter is connected with a third drying tank and a catalyst recovery tank.

[0011] Preferably, the first crystallization tank and the second crystallization tank are both provided with a second stirring device, the second stirring device comprises a second stirring shaft and a second stirring motor for driving the second stirring shaft to rotate, a main stirring blade is arranged on the second stirring shaft, a plurality of auxiliary stirring blades are arranged at the bottom of the second stirring shaft, and a plurality of turbulence teeth are arranged at the end of the auxiliary stirring blades through a support plate.

[0012] Preferably, the plurality of auxiliary stirring blades are arranged in a vertical manner with the main stirring blade.

[0013] Thanks to the above technical scheme, the present application has the following advantages:

[0014] The utility model provides a kind of reaction device for hydrochloric acid etilefrine, including decoloring tank, first plate-and-frame filter, reaction kettle, decoloring tank is connected with ethanol storage tank, first hydrochloric acid solution storage tank, activated carbon storage tank, reaction kettle is connected hydrogen storage tank, reaction kettle is also sequentially connected with second plate-and-frame filter, concentration tank, first crystallization tank, first centrifuge, buffer tank, second centrifuge, refining tank, second crystallization tank, third centrifuge, first drying tank, target product storage tank;First crystallization tank, second crystallization tank are connected with isopropanol storage tank, buffer tank is connected with ammonia solution storage tank, and refining tank is also connected with second hydrochloric acid solution storage tank, methanol storage tank;Catalyst adding port is arranged on reaction kettle, temperature sensor and pH sensor are arranged in decoloring tank, electric valve is arranged on the connecting pipeline of decoloring tank and second hydrochloric acid solution storage tank, and electric valve is interlocked with pH sensor;Adjusting valve is arranged on the connecting pipeline of reaction kettle and hydrogen storage tank.The above device can produce high-purity hydrochloric acid etilefrine, and the degree of automation is high.

[0015] The decoloring tank and the reaction kettle are both provided with a first stirring device, the first stirring device comprises a first stirring shaft and a first stirring motor for driving the first stirring shaft to rotate, a plurality of inclined stirring rods are arranged on the first stirring shaft, and an arc-shaped stirring rod is arranged at the bottom of the first stirring shaft;The plurality of inclined stirring rods are arranged in a non-parallel manner.The above device can greatly improve the decoloring efficiency.

[0016] The solid outlet of the first plate-and-frame filter machine of the device is communicated with a second drying tank and an activated carbon recovery tank, and the solid outlet of the second plate-and-frame filter machine is communicated with a third drying tank and a catalyst recovery tank.

[0017] The first crystallization tank and the second crystallization tank are both provided with a second stirring device, which comprises a second stirring shaft and a second stirring motor for driving the second stirring shaft to rotate, the second stirring shaft is provided with main stirring blades, the bottom of the second stirring shaft is provided with a plurality of auxiliary stirring blades, and the end of the auxiliary stirring blades is provided with a plurality of turbulence teeth. BRIEF DESCRIPTION OF DRAWINGS

[0018] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings needed to be used in the embodiments or the prior art description. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can also be obtained by those skilled in the art without any creative effort on the basis of these drawings.

[0019] Figure 1 is a structural schematic view of the embodiment 1 of the present application;

[0020] Figure 2 is Figure 1 is an enlarged structural schematic view of position A in the figure;

[0021] In the figure, 1 is a decoloring tank, 2 is a first plate-and-frame filter machine, 3 is a reaction kettle, 4 is an ethanol storage tank, 5 is a first hydrochloric acid solution storage tank, 6 is an activated carbon storage tank, 7 is a hydrogen storage tank, 8 is a second plate-and-frame filter machine, 9 is a concentration tank, 10 is a first crystallization tank, 11 is a first centrifuge, 12 is a buffer tank, 13 is a second centrifuge, 14 is a refining tank, 15 is a second crystallization tank, 16 is a third centrifuge, 17 is a first drying tank, 18 is a target product storage tank, 19 is an isopropyl alcohol storage tank, 20 is an ammonia water solution storage tank, 21 is a methanol storage tank, 22 is a catalyst adding port, 23 is a temperature sensor, 24 is a pH sensor, 25 is an electric valve, 26 is an adjusting valve, 27 is a first stirring shaft, 28 is a first stirring motor, 29 is an inclined stirring rod, 30 is an arc-shaped stirring rod, 31 is a second drying tank, 32 is an activated carbon recovery tank, 33 is a third drying tank, 34 is a catalyst recovery tank, 35 is a second stirring shaft, 36 is a second stirring motor, 37 is a main stirring blade, 38 is an auxiliary stirring blade, 39 is a turbulence tooth, 40 is a second hydrochloric acid solution storage tank, and 41 is a support plate. DETAILED DESCRIPTION

[0022] The technical solutions in the embodiments of the utility model will be clearly and completely described below with reference to the drawings in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, rather than all the embodiments. Based on the embodiments in the utility model, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of the utility model

[0023] Embodiment 1

[0024] As shown in Figure 1 and Figure 2 A reaction device for etilefrine hydrochloride, comprising a decoloring tank 1, a first plate and frame filter 2, a reaction kettle 3, the decoloring tank 1 is communicated with an ethanol storage tank 4, a first hydrochloric acid solution storage tank 5, an activated carbon storage tank 6, the reaction kettle 3 is communicated with a hydrogen storage tank 7, the reaction kettle 3 is further communicated with a second plate and frame filter 8, a concentration tank 9, a first crystallization tank 10, a first centrifuge 11, a buffer tank 12, a second centrifuge 13, a refining tank 14, a second crystallization tank 15, a third centrifuge 16, a first drying tank 17, a target product storage tank 18 in sequence, the first crystallization tank 10 and the second crystallization tank 15 are communicated with an isopropyl alcohol storage tank 19, the buffer tank 12 is communicated with an ammonia solution storage tank 20, and the refining tank 14 is further communicated with a second hydrochloric acid solution storage tank 40 and a methanol storage tank 21.

[0025] The reaction kettle 3 is provided with a catalyst adding port 22, the decoloring tank 1 is provided with a temperature sensor 23 and a pH sensor 24, an electric valve 25 is arranged on the connecting pipeline of the decoloring tank 1 and the first hydrochloric acid solution storage tank 5, and the electric valve 25 is interlocked with the pH sensor 24; and an adjusting valve 26 is arranged on the connecting pipeline of the reaction kettle 3 and the hydrogen storage tank 7.

[0026] In the embodiment, the first stirring device is arranged in the decoloring tank 1 and the reaction kettle 3, the first stirring device comprises a first stirring shaft 27 and a first stirring motor 28 for driving the first stirring shaft 27 to rotate, a plurality of inclined stirring rods 29 are arranged on the first stirring shaft 27, and an arc-shaped stirring rod 30 is arranged at the bottom of the first stirring shaft 27. The above arrangement facilitates the mixing of activated carbon and raw material solution and improves the decoloring efficiency.

[0027] In the embodiment, the plurality of inclined stirring rods 29 are arranged in a non-parallel manner, which facilitates the sufficient stirring of the decoloring liquid in the decoloring tank 1.

[0028] In the embodiment, the solid outlet of the first plate-and-frame filter 2 is communicated with the second drying tank 31 and the activated carbon recovery tank 32. The solid outlet of the second plate-and-frame filter 8 is communicated with the third drying tank 33 and the catalyst recovery tank 34. The above arrangement recovers the activated carbon and catalyst in the reaction, which can be reused after subsequent treatment, thereby saving energy and reducing consumption.

[0029] In the embodiment, the first crystallization tank 10 and the second crystallization tank 15 are both provided with a second stirring device, which comprises a second stirring shaft 35 and a second stirring motor 36 for driving the second stirring shaft 35 to rotate. The second stirring shaft 35 is provided with main stirring blades 37, and the bottom of the second stirring shaft 35 is provided with a plurality of auxiliary stirring blades 38. The end of the auxiliary stirring blade 38 is provided with a plurality of turbulence teeth 39 through a support plate 41. Further, the plurality of auxiliary stirring blades 38 are arranged perpendicularly to the main stirring blades 37. The above arrangement can effectively improve the crystallization efficiency and improve the production efficiency of the product.

[0030] The process for producing etilefrine hydrochloride by using the above device is as follows:

[0031] Etilefrine ketone hydrochloride and ethanol are added into the decolorization tank 1. After the pH is adjusted by adding hydrochloric acid solution, activated carbon is added. The temperature is increased for decolorization. After the decolorization is completed, the decolorization liquid is filtered through the first plate-and-frame filter 2. The filter cake is dried through the second drying tank 31 and then enters the activated carbon recovery tank 32. The filtrate enters the reaction kettle 3. Catalyst is added into the reaction kettle 3. Hydrogen is introduced for hydrogenation reduction. After the reaction is completed, the reaction liquid is filtered through the second plate-and-frame filter 8. The filter cake is dried through the third drying tank 33 and then enters the catalyst recovery tank 34. The filtered liquid is concentrated through the concentration tank 9, and then enters the first crystallization tank 10. After dilution by adding isopropyl alcohol, the temperature is reduced for crystallization. Then, centrifugation is performed through the first centrifuge 11. The centrifugal solid enters the buffer tank 12. Ammonia solution is added into the buffer tank 12 for ionization. Then, centrifugation is performed through the second centrifuge 13. The centrifugal solid enters the refining tank 14. Methanol is added into the refining tank 14 as a solvent. Hydrochloric acid is added for acidification. The temperature is increased for concentration. The concentrated liquid enters the second crystallization tank 15. Isopropyl alcohol is added as a crystallization solvent. Then, the temperature is reduced. Finally, centrifugation is performed through the third centrifuge 16. The centrifugal solid is dried and then enters the target product storage tank 18.

[0032] The above description of the disclosed embodiments enables those skilled in the art to carry out or use the present application. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present application. Therefore, the present application will not be limited to the embodiments shown herein, but will conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A reaction apparatus for etilefrine hydrochloride, characterized by: The device comprises a decoloring tank, a first plate-and-frame filter, a reaction kettle, the decoloring tank is connected with an ethanol storage tank, a first hydrochloric acid solution storage tank and an activated carbon storage tank, the reaction kettle is connected with a hydrogen storage tank, the reaction kettle is further connected with a second plate-and-frame filter, a concentration tank, a first crystallization tank, a first centrifuge, a buffer tank, a second centrifuge, a refining tank, a second crystallization tank, a third centrifuge, a first drying tank and a target product storage tank in sequence, the first crystallization tank and the second crystallization tank are connected with an isopropyl alcohol storage tank, the buffer tank is connected with an ammonia water solution storage tank, and the refining tank is further connected with a second hydrochloric acid solution storage tank and a methanol storage tank. A catalyst adding port is arranged on the reaction kettle, temperature sensors and pH sensors are arranged in the decoloring tank, an electric valve is arranged on the connecting pipeline of the decoloring tank and the first hydrochloric acid solution storage tank, and the electric valve is interlocked with the pH sensors, and an adjusting valve is arranged on the connecting pipeline of the reaction kettle and the hydrogen storage tank.

2. A reaction apparatus for etilefrine hydrochloride according to claim 1, characterized in that: First stirring devices are arranged in the decoloring tank and the reaction kettle, the first stirring device comprises a first stirring shaft and a first stirring motor for driving the first stirring shaft to rotate, a plurality of inclined stirring rods are arranged on the first stirring shaft, and an arc-shaped stirring rod is arranged at the bottom of the first stirring shaft.

3. A reaction apparatus for etilefrine hydrochloride according to claim 2, characterized in that: The plurality of inclined stirring rods are arranged in a non-parallel manner.

4. The reaction apparatus for etilefrine hydrochloride according to claim 1, characterized by: The solid outlet of the first plate-and-frame filter is connected with a second drying tank and an activated carbon recovery tank.

5. A reaction apparatus for etilefrine hydrochloride according to claim 1, characterized in that: The solid outlet of the second plate-and-frame filter is connected with a third drying tank and a catalyst recovery tank.

6. A reaction apparatus for etilefrine hydrochloride according to claim 1, characterized by: Second stirring devices are arranged in the first crystallization tank and the second crystallization tank, the second stirring device comprises a second stirring shaft and a second stirring motor for driving the second stirring shaft to rotate, main stirring blades are arranged on the second stirring shaft, a plurality of auxiliary stirring blades are arranged at the bottom of the second stirring shaft through a support plate, and a plurality of turbulence teeth are arranged at the end of the auxiliary stirring blades.

7. A reaction apparatus for etilefrine hydrochloride according to claim 6, characterized in that: The plurality of auxiliary stirring blades are arranged perpendicularly to the main stirring blades.

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