Reaction device for producing chlorinated homoserine hydrochloride

Abstract

The utility model relates to a reaction device for producing chlorinated homoserine hydrochloride, which comprises a reaction kettle and a stirring assembly, the stirring assembly is arranged in the reaction kettle along the longitudinal direction, the reaction device also comprises at least two gas conveying pipes, and the at least two gas conveying pipes are arranged in the reaction kettle along the vertical direction. The gas inlet end of each gas conveying pipe is communicated with the hydrogen chloride gas conveying pipe, and the gas outlet end of each gas conveying pipe is sealed; a plurality of ring-shaped ventilation pipes are arranged in the reaction kettle from top to bottom along the horizontal direction and are arranged outside the stirring assembly in a sleeving manner, each horizontally arranged ring-shaped ventilation pipe is communicated with each gas conveying pipe, and a plurality of gas outlets are formed in each ring-shaped ventilation pipe; the anti-blocking cover is arranged on the circular-ring-shaped ventilation pipe outside each air outlet hole, and the opening direction of the anti-blocking cover is consistent with the stirring direction of the stirring assembly. The reaction kettle can avoid or reduce the blockage of the air outlet holes, so that the normal reaction is not influenced.

Description

Technical Field

[0001] The utility model relates to the field of chemical technology and engineering technology, in particular to a reaction device for producing chlorohomoserine hydrochloride. Background Art

[0002] Glufosinate is a mixture of L-glufosinate and D-glufosinate racemates, and is a highly effective, low-toxic, broad-spectrum contact-type organophosphorus herbicide, with increasing usage year by year and huge market potential. Therefore, the preparation of intermediates (i.e., (S)-4-chloro-2-aminobutyrate and (S)-4-chloro-2-aminobutyric acid) for the synthesis of L-glufosinate has attracted widespread attention.

[0003] Among them, U.S. Patent Application US20060135602A1 provides a method for preparing (S)-4-chloro-2-aminobutyrate by reacting L-homoserine (i.e., L-2-amino-4-hydroxybutyric acid) with thionyl chloride and ethanol. However, this method requires a large amount of thionyl chloride, which not only increases the reaction cost, but also produces a large amount of waste acid and wastewater to pollute the environment, so it is necessary to improve this process.

[0004] In order to overcome the above problems, our company has developed a process in which hydrogen chloride gas is used as a chlorination agent to react with L-homoserine to prepare chlorohomoserine hydrochloride, and further esterification is performed to prepare (S)-4-chloro-2-aminobutyrate. Figure 1 As shown, a certain volume of L-homoserine solution is fed into the reactor, and hydrogen chloride gas is fed into the reactor through an air inlet pipe to react chemically with the L-homoserine solution under the stirring of a stirring device. However, since there is only one air outlet on the air inlet pipe, and hydrogen chloride gas and L-homoserine are heterogeneous reactants, this will cause the hydrogen chloride to be unevenly dispersed in the reaction system, so that the raw materials cannot react completely, thereby generating a large amount of solid impurities that accumulate at the air outlet of the delivery pipe, which is easy to cause the air outlet to be blocked, thereby affecting the normal progress of the reaction, resulting in reaction failure and wasting a lot of manpower and material resources. Utility Model Content

[0005] The purpose of the utility model is to overcome the above problems existing in the prior art and provide a reaction device for producing chlorohomoserine hydrochloride, which can avoid or reduce the blockage of the vent holes and thus will not affect the normal progress of the reaction.

[0006] The utility model provides a reaction device for producing chlorohomoserine hydrochloride, comprising a reaction kettle and a stirring component, wherein the stirring component is arranged in the reaction kettle along the longitudinal direction, and further comprises:

[0007] There are at least two gas pipes, and at least two gas pipes are arranged in the reactor along the vertical direction, the gas inlet end of each gas pipe is connected to the hydrogen chloride gas delivery pipe, and the gas outlet end of each gas pipe is sealed;

[0008] A plurality of annular ventilation pipes are provided, each of which is arranged in the reactor from top to bottom along the horizontal direction and sleeved on the outside of the stirring assembly. Each horizontally arranged annular ventilation pipe is connected to each air delivery pipe, and each annular ventilation pipe is provided with a plurality of air outlets, so that the air flow sent into each annular ventilation pipe by the air delivery pipe is discharged into the reactor through the plurality of air outlets;

[0009] The anti-blocking cover is arranged on the annular vent pipe outside each air outlet. The opening direction of the anti-blocking cover is consistent with the stirring direction of the stirring assembly, so that the liquid in the reactor is disturbed and drives the solid impurities formed at the anti-blocking cover to collide with the anti-blocking cover.

[0010] Preferably, the plurality of air outlet holes are evenly distributed at equal intervals on each annular ventilation pipe.

[0011] Preferably, the anti-blocking cover includes a top plate and two vertical plates, the top plate is tilted on the circular ventilation pipe, and there is an angle between the bottom end of the top plate and the center line of each circular ventilation pipe, the two vertical plates are symmetrically arranged on both sides of the top plate along the center line of the top plate, the top end of each vertical plate is sealed with the top plate, and the bottom end of each vertical plate is connected to the wall of the circular ventilation pipe.

[0012] Preferably, the angle is 30-45°.

[0013] Preferably, the air outlet is in a rectangular shape, and the area at the outlet of the anti-blocking cover is larger than the area of ​​the air outlet.

[0014] Preferably, there are four air outlet holes, and the four air outlet holes are symmetrically arranged on each circular ventilation pipe.

[0015] Preferably, the stirring assembly is arranged at the inner center of the annular ventilation pipe, and there are two gas pipes, and the two gas pipes are symmetrically arranged on both sides of the reactor along the axis of the reactor, and the gas inlet end of each gas pipe is connected to the hydrogen chloride gas delivery pipe.

[0016] Preferably, there are at least two annular ventilation pipes.

[0017] Preferably, the gas delivery pipe and the annular ventilation pipe are both stainless steel pipes or pipes with the inner wall sprayed with anti-corrosion materials.

[0018] Preferably, anti-corrosion material is sprayed on the inner wall of the reactor.

[0019] Compared with the prior art, the beneficial effects of the utility model are:

[0020] The utility model provides a reaction device for producing chlorohomoserine hydrochloride, which can avoid or reduce the problem of affecting the normal operation of the reaction due to blockage of the air outlet. In addition, the device can uniformly and stably introduce hydrogen chloride during the reaction process, reducing the probability of solids in the system blocking the vents. In the utility model, the hydrogen chloride gas delivery pipe delivers gas into at least two gas delivery pipes connected thereto, and each horizontally arranged circular vent pipe is connected to at least two gas delivery pipes, so that the hydrogen chloride gas in the gas delivery pipe enters the circular vent pipe, and each circular vent pipe is provided with a plurality of gas outlets, and the hydrogen chloride gas is discharged from the plurality of gas outlets, thereby increasing the contact area between the hydrogen chloride gas and the liquid, and the reaction is more complete. In addition, since the flow direction of the liquid surface disturbed by the stirring component is consistent with the opening direction of the anti-blocking cover arranged on the annular vent pipe outside each gas outlet, not only can it be ensured that when the liquid flows, the solid particles formed by the reaction collide with the cover plate of the anti-blocking cover to be broken under the drive of the disturbed liquid, but also the vortex formed by the liquid flow at the cover plate of the anti-blocking cover will prevent the horizontal solid particles from entering the pores, thereby preventing the problem that the generated solid particles will not enter the pores and block the pores. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 This is a schematic diagram of a reaction device for producing chlorohomoserine hydrochloride before the technical transformation of the prior art;

[0022] Figure 2 This is a schematic diagram of a reaction device for producing chlorohomoserine hydrochloride according to the utility model;

[0023] Figure 3 It is a top view of the circular annular vent pipe of the utility model;

[0024] Figure 4 It is a structural schematic diagram of the anti-blocking cover of the utility model.

[0025] Description of reference numerals:

[0026] 1. Reactor, 2-1. Air delivery pipe, 2-2. Circular ventilation pipe, 2-3. Air outlet, 2-4. Anti-blocking cover, 2-41. Top plate, 2-42. Vertical plate, 3. Stirring assembly, 4. Air inlet pipe. DETAILED DESCRIPTION

[0027] The specific implementation of the utility model is described in detail below in conjunction with the accompanying drawings, but it should be understood that the protection scope of the utility model is not limited by the specific implementation. Based on the embodiments of the utility model, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the utility model.

[0028] The inventors found that since there is only one outlet on the air inlet pipe, and hydrogen chloride gas and L-homoserine are heterogeneous reactants, this will cause the hydrogen chloride to be unevenly dispersed in the reaction system, so that the raw materials cannot react completely, thereby generating a large amount of solid impurities that accumulate at the outlet of the delivery pipe, which can easily cause the outlet to be blocked.

[0029] In order to solve the problems existing in the above-mentioned prior art, the utility model provides a reaction device for producing chlorohomoserine hydrochloride, which can avoid or reduce the blockage of the vent holes and thus will not affect the normal progress of the reaction.

[0030] Refer to the attached Figure 2-4 As shown, in the embodiment, a reaction device for producing chlorohomoserine hydrochloride includes a reactor 1 and a stirring assembly 3, wherein the stirring assembly 3 is arranged in the reactor 1 along the longitudinal direction, and further includes:

[0031] There are at least two gas pipes 2-1, and at least two gas pipes 2-1 are arranged in the reactor 1 along the vertical direction, the gas inlet end of each gas pipe 2-1 is connected to the hydrogen chloride gas delivery pipe, and the gas outlet end of each gas pipe 2-1 is sealed;

[0032] There are multiple annular ventilation pipes 2-2, and each annular ventilation pipe 2-2 is horizontally arranged from top to bottom in the reactor 1, and is sleeved on the outside of the stirring assembly 3. Each horizontally arranged annular ventilation pipe 2-2 is connected to each air supply pipe 2-1, and each annular ventilation pipe 2-2 is provided with a plurality of air outlet holes 2-3, so that the air flow sent into each annular ventilation pipe 2-2 by the air supply pipe 2-1 is discharged into the reactor 1 through the plurality of air outlet holes 2-3. An anti-blocking cover 2-4 is provided on the annular ventilation pipe 2-2 located outside each air outlet hole 2-3, and the opening direction of the anti-blocking cover 2-4 is consistent with the stirring direction of the stirring assembly 2, so that the disturbed liquid drives the solid impurities formed at the anti-blocking cover 2-4 to collide with the anti-blocking cover 2-4, so that the solid impurities will not accumulate on each air outlet hole 2-3.

[0033] Working principle: The hydrogen chloride gas delivery pipe delivers the gas into at least two gas pipes 2-1 connected thereto, and each circular ventilation pipe 2-2 is connected to at least two gas pipes 2-1 located at the same height, so that the hydrogen chloride gas in the gas pipe 2-1 enters the circular ventilation pipe 2-2, and each circular ventilation pipe 2-2 is provided with a plurality of gas outlet holes 2-3, and the hydrogen chloride gas is discharged from the plurality of gas outlet holes 2-3, thereby increasing the contact area between the hydrogen chloride gas and the liquid, and making the reaction more complete. In addition, since the flow direction of the liquid surface disturbed by the stirring component 3 is consistent with the opening direction of the anti-blocking cover 2-4 arranged on the outside of each gas outlet hole 2-3 on the annular ventilation pipe 2-2, it can not only ensure that when the liquid flows, the solid particles formed by the reaction collide with the cover plate of the anti-blocking cover 2-4 under the drive of the disturbed liquid to be broken, but also the vortex formed by the liquid flow at the cover plate of the anti-blocking cover 2-4 will prevent the horizontal solid particles from entering the pores, thereby preventing the problem that the generated solid particles will not enter the pores and block the pores. In addition, the hydrogen chloride gas enters the kettle through the annular vent pipe, and the evenly arranged vent holes can ensure that the gas is fully dispersed into the system. The opening of the anti-blocking cover 2-4 is consistent with the rotation direction of the disturbed liquid surface, which reduces the probability of solid materials directly colliding with the vent holes 2-4, and at the same time reduces the probability of solid materials entering the vent holes 2-4 and blocking the vent holes.

[0034] Specifically, the multiple gas outlet holes 2-3 evenly arranged can ensure that the gas is fully dispersed into the system, increasing the probability of complete reaction of the raw materials, so the multiple gas outlet holes 2-3 are evenly distributed on each circular ventilation pipe 2-2 at equal intervals.

[0035] Specifically, the anti-blocking cover 2-4 includes a top plate 2-41 and two vertical plates 2-42. The top plate 2-41 is tilted on the circular ventilation pipe 2-2, and there is an angle between the bottom end of the top plate 2-41 and the center line of each circular ventilation pipe 2-2. The two vertical plates 2-42 are symmetrically arranged on both sides of the top plate 2-41 along the center line of the top plate 2-41. The top end of each vertical plate 2-42 is sealed and connected to the top plate 2-41, and the bottom end of each vertical plate 2-42 is connected to the wall of the circular ventilation pipe 2-2.

[0036] The setting of an angle between the bottom end of the top plate 2-41 in the anti-blocking cover and the center line of each annular ventilation pipe 2-2 can ensure that ventilation is completed, and after the liquid surface is still, the solid materials generated will not fall into the air outlet 2-3 to a certain extent. At the same time, by controlling the opening direction to be consistent with the stirring, it can be ensured that when the liquid flows, the solid particles hit the top plate instead of directly entering the air outlet 2-3. The flowing liquid here will form a vortex at the bottom end of the top plate 2-41, thereby further preventing the solid particles from entering the air outlet 2-3.

[0037] Specifically, when the angle between the bottom end of the top plate 2-41 in the anti-blocking cover and the center line of each annular ventilation pipe 2-2 is 30-45°, the probability of solid particles hitting the top plate is the highest.

[0038] Specifically, the shape of the air outlet 2-3 is rectangular, and the area at the outlet of the anti-blocking cover 2-4 is larger than the area of ​​the air outlet 2-3. The enlarged ventilation area can ensure the ventilation efficiency and ensure that the gas is fully dispersed in the system.

[0039] Specifically, there are four air outlet holes 2-3, and the four air outlet holes 2-3 are symmetrically arranged on each circular ventilation pipe 2-2, so as to ensure that there are enough ventilation points and ensure that the gas can be evenly and fully dispersed in the system.

[0040] Specifically, the stirring component 3 is located at the inner center of the annular vent pipe 2-2. At this time, the amplitude of the liquid disturbance by the stirring component 3 is the largest, so that the disturbed liquid is at the same distance from the air outlet 2-3 opened in each annular vent pipe 2-2, and the degree of disturbance is consistent. In addition, there are two gas pipes 2-1, and the two gas pipes 2-1 are symmetrically arranged on both sides of the reactor 1 along the axial direction of the reactor, and the gas inlet end of each gas pipe 2-1 is connected to the hydrogen chloride gas delivery pipe.

[0041] Specifically, there are at least two annular ventilation pipes 2-2.

[0042] Specifically, the gas delivery pipe 2-1 and the annular ventilation pipe 2-2 are both stainless steel pipes, and the stainless steel is 316L stainless steel. The gas delivery pipe 2-1 and the annular ventilation pipe 2-2 can also be pipes with anti-corrosion materials sprayed on the inner wall.

[0043] Specifically, an anti-corrosion material is sprayed on the inner wall of the reactor 1 , and the anti-corrosion material is a halar material, or an outer lining plastic is fixed on the inner wall of the reactor 1 .

[0044] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A reaction device for producing chlorohomoserine hydrochloride, comprising a reaction kettle (1) and a stirring assembly (3), wherein the stirring assembly (3) is arranged in the reaction kettle (1) along the longitudinal direction, and is characterized in that: Also includes: The gas delivery pipes (2-1) are provided in at least two pieces, and the at least two gas delivery pipes (2-1) are both arranged in the reaction kettle (1) along the vertical direction, the gas inlet end of each gas delivery pipe (2-1) is connected to the hydrogen chloride gas delivery pipe, and the gas outlet end of each gas delivery pipe (2-1) is sealed; A plurality of annular ventilation pipes (2-2) are provided, each annular ventilation pipe (2-2) is arranged in the reactor (1) from top to bottom along the horizontal direction, and is sleeved on the outside of the stirring assembly (3), each horizontally arranged annular ventilation pipe (2-2) is connected to each gas delivery pipe (2-1), and each annular ventilation pipe (2-2) is provided with a plurality of air outlet holes (2-3), so that the airflow sent into each annular ventilation pipe (2-2) by the gas delivery pipe (2-1) is discharged into the reactor (1) through the plurality of air outlet holes (2-3); The anti-blocking cover (2-4) is arranged on the annular vent pipe (2-2) outside each gas outlet (2-3), and the opening direction of the anti-blocking cover (2-4) is consistent with the stirring direction of the stirring assembly (3), so that the liquid in the reaction kettle (1) is disturbed and drives the solid impurities formed at the anti-blocking cover (2-4) to collide with the anti-blocking cover (2-4).

2. A reaction device for producing chlorohomoserine hydrochloride according to claim 1, characterized in that: The plurality of air outlet holes (2-3) are evenly distributed at equal intervals on each annular ventilation pipe (2-2).

3. A reaction device for producing chlorohomoserine hydrochloride according to claim 1, characterized in that: The anti-blocking cover (2-4) comprises a top plate (2-41) and two vertical plates (2-42); the top plate (2-41) is arranged obliquely on the annular ventilation pipe (2-2), and an angle is formed between the bottom end of the top plate (2-41) and the center line of each annular ventilation pipe (2-2); the two vertical plates (2-42) are symmetrically arranged on both sides of the top plate (2-41) along the center line of the top plate (2-41); the top end of each vertical plate (2-42) is sealed and connected to the top plate (2-41), and the bottom end of each vertical plate (2-42) is connected to the wall of the annular ventilation pipe (2-2).

4. A reaction device for producing chlorohomoserine hydrochloride according to claim 3, characterized in that: The angle is 30-45°.

5. A reaction device for producing chlorohomoserine hydrochloride according to claim 1, characterized in that: The shape of the air outlet hole (2-3) is rectangular, and the area at the outlet of the anti-blocking cover (2-4) is larger than the area of ​​the air outlet hole (2-3).

6. A reaction device for producing chlorohomoserine hydrochloride according to claim 1, characterized in that: There are four air outlet holes (2-3), and the four air outlet holes (2-3) are symmetrically arranged on each annular vent pipe (2-2).

7. A reaction device for producing chlorohomoserine hydrochloride according to claim 1, characterized in that: The stirring assembly (3) is arranged at the inner center of the annular ventilation pipe (2-2), and there are two gas pipes (2-1), and the two gas pipes (2-1) are symmetrically arranged on both sides of the reactor (1) along the axial direction of the reactor, and the gas inlet end of each gas pipe (2-1) is connected to the hydrogen chloride gas delivery pipe.

8. The reaction device for producing chlorohomoserine hydrochloride according to claim 1, characterized in that: There are at least two annular ventilation pipes (2-2).

9. The reaction device for producing chlorohomoserine hydrochloride according to claim 1, characterized in that: The gas delivery pipe (2-1) and the annular ventilation pipe (2-2) are both stainless steel pipes or pipes with the inner walls sprayed with anti-corrosion materials.

10. The reaction device for producing chlorohomoserine hydrochloride according to claim 1, characterized in that: The inner wall of the reaction kettle (1) is sprayed with anti-corrosion material.

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