Crystallization device for phenylephrine hydrochloride

Abstract

The utility model discloses a phenylephrine hydrochloride crystallizing device which comprises a dissolving tank and a crystallizing tank which are communicated with each other, the dissolving tank is communicated with a methanol storage tank, the crystallizing tank is communicated with an ethyl acetate storage tank, the upper part of the crystallizing tank is provided with a material distribution disc, and the material distribution disc is communicated with the ethyl acetate storage tank through a first liquid conveying pipeline; a plurality of material spraying heads are arranged on the material distribution disc; the dissolving tank is communicated with the crystallizing tank through a second liquid conveying pipeline, a spiral material distributing pipe is arranged at the lower part of the crystallizing tank, and a plurality of material outlets are formed in the spiral material distributing pipe; a first stirring device is arranged in the dissolving tank, a second stirring device is arranged in the crystallizing tank, a reflux inlet is formed in the crystallizing tank, the reflux inlet is communicated to the material distribution disc through a reflux pipeline, and a reflux pump and a cooler are arranged on the reflux pipeline. The device is high in heat exchange efficiency, easy to control the crystallization process and good in crystallization effect.

Description

TECHNICAL FIELD

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

[0002] The hydrochloric acid phenylephrine is white or white crystalline powder, has no smell, is easily soluble in water, methanol, ethylene glycol etc., can be soluble in ethanol, is difficultly soluble in acetone, ethyl acetate etc. The hydrochloric acid phenylephrine can be used to relieve the symptoms such as headache, fever, all-over aches and pains caused by influenza or common cold, can also be used to treat symptoms such as nasal mucosa hyperemia, acute hypotension, and is used as the effective component of cold medicine. The synthesis method of the hydrochloric acid phenylephrine at present mainly has the following several kinds: one is to use m-hydroxyacetophenone as raw material, after acylation, bromination, amination, hydrogenation, resolution, salt formation process, the hydrochloric acid phenylephrine is obtained. Two is to use 3-methoxybenzaldehyde as raw material, and the hydrochloric acid phenylephrine is obtained by asymmetric synthesis. Three is to use α-benzylmethylamino-3-hydroxyacetophenone hydrochloride as starting material, and the debenzyl reaction is carried out under palladium carbon catalytic hydrogenation, and the intermediate debenzyl is obtained, and the debenzyl is subjected to reduction and free after being obtained, and the intermediate racemic phenylephrine is obtained. Use water as solvent, use dextro-tartaric acid as resolving agent and resolve, and after free refining, the phenylephrine left-handed body is obtained, and the salt formation reaction with hydrochloric acid is carried out, and the final product hydrochloric acid phenylephrine is obtained. The above preparation process all involves the crystallization process. The existing crystallization device is single in structure, and the crystallization process is not easy to control, thereby affecting the product performance. CONTENT OF UTILITY MODEL

[0003] The utility model solves the technical problem that: in view of the deficiency of prior art, provide a kind of crystallization device for hydrochloric acid phenylephrine, the device heat exchange efficiency is high, crystallization process is easy to control, and crystallization effect is good.

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

[0005] A kind of crystallization device for hydrochloric acid phenylephrine, including the communication of dissolving tank and crystallization tank, the dissolving tank is connected with methanol storage tank, the crystallization tank is connected with ethyl acetate storage tank, the upper portion of the crystallization tank is equipped with cloth distribution disc, the cloth distribution disc is connected with ethyl acetate storage tank by first liquid conveying pipeline;Multiple material spraying heads are arranged on the cloth distribution disc;The dissolving tank is connected with the crystallization tank by second liquid conveying pipeline, the lower portion of the crystallization tank is equipped with spiral cloth distribution pipe, multiple discharge ports are arranged on the spiral cloth distribution pipe;First stirring device is arranged in the dissolving tank, second stirring device is arranged in the crystallization tank, reflux port is arranged on the crystallization tank, the reflux port is connected to cloth distribution disc by reflux pipeline, reflux pump and cooler are arranged on the reflux pipeline.

[0006] Preferably, the first stirring device comprises a first stirring shaft arranged in the dissolving tank and a first stirring motor arranged at the top of the dissolving tank and driving the first stirring shaft to rotate, and a plurality of first stirring rods are arranged on the first stirring shaft, and a plurality of first stirring blades are arranged on the first stirring rods.

[0007] Preferably, the plurality of first stirring blades are arranged non-parallelly.

[0008] Preferably, a jacket is arranged on the outer side of the dissolving tank and the crystallizing tank, and a plurality of baffle plates are arranged in the jacket.

[0009] Preferably, the second stirring device comprises a second stirring shaft arranged in the crystallizing tank and a second stirring motor arranged at the top of the crystallizing tank and driving the second stirring shaft to rotate, and a second stirring rod is arranged on the second stirring shaft, and a second stirring blade is arranged on the second stirring rod.

[0010] Preferably, the distribution disc is sleeved on the outer side of the second stirring shaft.

[0011] Preferably, a scraper abutting against the inner wall of the crystallizing tank is arranged on the second stirring shaft through a supporting rod.

[0012] Preferably, the shell side of the cooler is in communication with the outlet of the heat exchange medium on the jacket of the crystallizing tank.

[0013] Preferably, a liquid distribution plate is arranged in the cooler, and a liquid distribution hole is arranged on the liquid distribution plate.

[0014] Preferably, a plurality of flow guide grooves are circumferentially arranged in the liquid distribution hole.

[0015] Thanks to the above technical scheme, the present application has the following advantages:

[0016] The utility model provides a kind of crystallization device for phenylephrine hydrochloride, including the dissolving tank and the crystallizing tank, the dissolving tank is connected with methanol storage tank, the crystallizing tank is connected with ethyl acetate storage tank, the upper portion of crystallizing tank is equipped with distribution disc, distribution disc is connected with ethyl acetate storage tank by first liquid conveying pipeline;Multiple spray heads are arranged on the distribution disc;The dissolving tank is connected with the crystallizing tank by second liquid conveying pipeline, and the lower portion of the crystallizing tank is equipped with spiral distribution pipe, and multiple discharge ports are arranged on the spiral distribution pipe;First stirring device is arranged in the dissolving tank, and second stirring device is arranged in the crystallizing tank, and reflux port is arranged on the crystallizing tank, and the reflux port is connected to distribution disc by reflux pipeline, and reflux pump and cooler are arranged on the reflux pipeline.The device uses methanol as solvent, uses ethyl acetate as solvent, and the target product is crystallized and purified, and the dissolving efficiency and the crystallization efficiency are high, and the crystallization material liquid is discharged through reflux port in the crystallization process, enters cooler again, and then reenters the crystallizing tank to be crystallized, to further improve the crystallization efficiency.

[0017] The jacket is internally provided with a plurality of baffle plates, thereby strengthening the heat transfer of the crystallization tank and the dissolving tank, and better ensuring the dissolving temperature and the crystallization temperature.

[0018] The second stirring shaft is provided with a scraper abutting against the inner wall of the crystallization tank through a supporting rod, so that the crystals adhered to the wall can be scraped in real time.

[0019] The shell side of the cooler is communicated with the outlet of the heat exchange medium on the jacket of the crystallization tank, the heat exchange medium of the crystallization tank is reused, and energy consumption is reduced.

[0020] The cooler is internally provided with a liquid distribution plate, the liquid distribution plate is provided with liquid distribution holes, and a plurality of flow guide grooves are circumferentially arranged in the liquid distribution holes, so that the crystallization liquid can be uniformly entered into the cooler through the liquid distribution plate, and the cooling efficiency is improved. BRIEF DESCRIPTION OF DRAWINGS

[0021] In order to more clearly illustrate the technical scheme in the embodiments of the present application or the prior art, the drawings needed to be used in the embodiments or the prior art description will be briefly introduced as follows. 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 creative labor.

[0022] Figure 1 is a structural schematic view of the embodiment 1 of the present application;

[0023] Figure 2 is Figure 1 is an enlarged structural schematic view of A in the embodiment 1 of the present application;

[0024] Figure 3 is a structural schematic view of the liquid distribution plate;

[0025] In the drawings, 1 is a dissolving tank, 2 is a crystallization tank, 3 is a methanol storage tank, 4 is an ethyl acetate storage tank, 5 is a material distribution disc, 6 is a first liquid conveying pipeline, 7 is a material spraying head, 8 is a second liquid conveying pipeline, 9 is a spiral material conveying pipe, 10 is a discharge port, 11 is a reflux port, 12 is a reflux pipeline, 13 is a reflux pump, 14 is a cooler, 15 is a first stirring shaft, 16 is a first stirring motor, 17 is a first stirring rod, 18 is a first stirring blade, 19 is a jacket, 20 is a baffle plate, 21 is a second stirring shaft, 22 is a second stirring motor, 23 is a second stirring rod, 24 is a second stirring blade, 25 is a supporting rod, 26 is a scraper, 27 is a liquid distribution plate, 28 is a liquid distribution hole, and 29 is a flow guide groove. DETAILED DESCRIPTION

[0026] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present utility model.

[0027] Example 1

[0028] like Figures 1 to 3 As shown, a crystallization apparatus for desoxyrepinephrine hydrochloride includes a dissolving tank 1 and a crystallizing tank 2 connected together. The dissolving tank 1 is connected to a methanol storage tank 3, and the crystallizing tank 2 is connected to an ethyl acetate storage tank 4. A feeding disc 5 is provided at the upper part of the crystallizing tank 2, and the feeding disc 5 is connected to the ethyl acetate storage tank 4 through a first liquid delivery pipe 6. The feeding disc 5 is provided with multiple spray nozzles 7. The dissolving tank 1 is connected to the crystallizing tank 2 through a second liquid delivery pipe 8. A spiral feeding pipe 9 is provided at the lower part of the crystallizing tank 2, and the spiral feeding pipe 9 is provided with multiple discharge ports 10. A first stirring device is provided in the dissolving tank 1, and a second stirring device is provided in the crystallizing tank 2. A reflux port 11 is provided on the crystallizing tank 2, and the reflux port 11 is connected to the feeding disc 5 through a reflux pipe 12. A reflux pump 13 and a cooler 14 are provided on the reflux pipe 12.

[0029] This device uses methanol as the solvent and ethyl acetate as the precipitant. The arrangement of the feeding disc 5 and the spray head 7, as well as the spiral feeding pipe 9 and the outlet 10, ensures that the crude desoxyrepinephrine hydrochloride solution and the precipitant are in full contact, greatly improving the crystallization efficiency. The reflux pipe 12 and the cooler 14 allow the primary crystallization solution to be pre-cooled by the cooler 14 before re-entering the crystallization tank 2 for crystallization, further improving the crystallization efficiency.

[0030] In this embodiment, the first stirring device includes a first stirring shaft 15 disposed inside the dissolving tank 1 and a first stirring motor 16 that drives the first stirring shaft 15 to rotate and is disposed on the top of the dissolving tank 1. The first stirring shaft 15 is provided with a plurality of first stirring rods 17, and the first stirring rods 17 are provided with a plurality of first stirring blades 18; the plurality of first stirring blades 18 are not arranged in parallel. The first stirring device can effectively improve the dissolution efficiency of desoxyrepinephrine hydrochloride.

[0031] In the embodiment, the jacket 19 is arranged outside the dissolving tank 1 and the crystallization tank 2, and a plurality of baffle plates 20 are arranged in the jacket 19. The baffle plates 20 can increase the flow rate of the heat exchange medium in the jacket 19, so that the flow form of the heat exchange medium is turbulent flow, and the fluid in the jacket 19 can pass through all the heat transfer areas. When the heat exchange medium passes between the baffle plates 20, the flow direction and flow rate of the heat exchange medium are constantly changing, the disturbance is increased, the heat transfer is strengthened, and the dissolving temperature and the crystallization temperature can be better ensured.

[0032] In the embodiment, the second stirring device comprises a second stirring shaft 21 arranged in the crystallization tank 2, and a second stirring motor 22 arranged at the top of the crystallization tank 2 and configured to drive the second stirring shaft 21 to rotate. The second stirring shaft 21 is provided with a second stirring rod 23, and the second stirring rod 23 is provided with a second stirring blade 24. The above arrangement can improve the heat exchange efficiency in the crystallization tank 2, and further improve the crystallization efficiency.

[0033] In the embodiment, the cloth disc 5 is sleeved outside the second stirring shaft 21.

[0034] In the embodiment, the second stirring shaft 21 is provided with a scraper 26 abutting against the inner wall of the crystallization tank 2 through a support rod 25.

[0035] In the embodiment, the shell side of the cooler 14 is communicated with the outlet of the heat exchange medium on the jacket 19 of the crystallization tank 2. The heat exchange medium in the crystallization tank 2 enters the shell side of the cooler 14 and is reused as the heat exchange medium of the cooler 14, thereby reducing the preparation cost of the product.

[0036] In the embodiment, the cooler 14 is provided with a liquid distribution plate 27, and the liquid distribution plate 27 is provided with a plurality of liquid distribution holes 28. A plurality of flow guide grooves 29 are circumferentially arranged in the liquid distribution hole 28. The combined arrangement of the plurality of liquid distribution holes 28 and the flow guide grooves 29 can make the material liquid uniformly enter the cooler and be better cooled.

[0037] The above description of the disclosed embodiments enables a person skilled in the art to implement 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 crystallization apparatus for phenylephrine hydrochloride, characterized by: The device comprises a communication dissolving tank and a crystallization tank, the dissolving tank is communicated with a methanol storage tank, the crystallization tank is communicated with an ethyl acetate storage tank, an upper part of the crystallization tank is provided with a distributing disc, the distributing disc is communicated with the ethyl acetate storage tank through a first liquid conveying pipeline; a plurality of material spraying heads are arranged on the distributing disc; the dissolving tank is communicated with the crystallization tank through a second liquid conveying pipeline, a spiral distributing pipe is arranged on a lower part of the crystallization tank, and a plurality of discharge ports are arranged on the spiral distributing pipe; a first stirring device is arranged in the dissolving tank, a second stirring device is arranged in the crystallization tank, a reflux port is arranged on the crystallization tank, the reflux port is communicated with the distributing disc through a reflux pipeline, and a reflux pump and a cooler are arranged on the reflux pipeline.

2. A crystallization apparatus for phenylephrine hydrochloride as claimed in claim 1, wherein: The first stirring device comprises a first stirring shaft arranged in the dissolving tank and a first stirring motor arranged on a top of the dissolving tank and driving the first stirring shaft to rotate, a plurality of first stirring rods are arranged on the first stirring shaft, and a plurality of first stirring blades are arranged on the first stirring rods.

3. A crystallization apparatus for phenylephrine hydrochloride as claimed in claim 2, wherein: The plurality of first stirring blades are arranged in a non-parallel mode.

4. The crystallization apparatus for phenylephrine hydrochloride according to claim 1, wherein: A jacket is arranged on an outer side of the dissolving tank and the crystallization tank, and a plurality of baffle plates are arranged in the jacket.

5. The crystallization apparatus for phenylephrine hydrochloride according to claim 1, wherein: The second stirring device comprises a second stirring shaft arranged in the crystallization tank and a second stirring motor arranged on a top of the crystallization tank and driving the second stirring shaft to rotate, a second stirring rod is arranged on the second stirring shaft, and a second stirring blade is arranged on the second stirring rod.

6. A crystallization apparatus for phenylephrine hydrochloride as claimed in claim 5, wherein: The distributing disc is sleeved on an outer side of the second stirring shaft.

7. A crystallization apparatus for phenylephrine hydrochloride as claimed in claim 6, wherein: A scraper is arranged on the second stirring shaft through a support rod and abuts against an inner wall of the crystallization tank.

8. The crystallization apparatus for phenylephrine hydrochloride according to claim 1, wherein: A shell side of the cooler is communicated with an outlet of a heat exchange medium on the jacket of the crystallization tank.

9. The crystallization apparatus for phenylephrine hydrochloride according to claim 1, wherein A liquid distributing plate is arranged in the cooler, and a liquid distributing hole is arranged on the liquid distributing plate.

10. The crystallization apparatus for phenylephrine hydrochloride according to claim 9, wherein: A plurality of guide grooves are circumferentially arranged in the liquid distributing hole.

Images