A crystallization system for glufosinate

Abstract

This utility model discloses a crystallization system for glufosinate, relating to the technical field of glufosinate production equipment. It includes a first reactor, a second reactor, and a separator. The first reactor is connected to an alcohol reagent supply line, a gas feed line, and a raw material line. The raw material line is used to supply glufosinate hydrolysate, alkali solution, or concentrated glufosinate to the first reactor. The first reactor is connected to a vacuum pump via pipeline I, and then to a water storage tank via a pipeline connecting a heat exchanger. The bottom of the first reactor is connected to the inlet of the second reactor via pipeline II. The bottom of the second reactor is connected to the raw material line via a circulation line, and the bottom outlet of the second reactor is connected to the inlet of the separator via pipeline III. The second reactor is also connected to a second feed pipe. This system solves the problems of high investment costs and complex operation in existing glufosinate crystallization processes.

Description

Technical Field

[0001] This utility model relates to the technical field of glufosinate production equipment, specifically to a glufosinate crystallization system. Background Technology

[0002] Currently, there is no complete and efficient method for glufosinate crystallization in existing glufosinate preparation processes. Traditional glufosinate crystallization processes generally achieve crystallization rates below 80%, leaving a large amount of glufosinate residue in the mother liquor. Multiple recrystallizations or other purification steps are required to improve the crystallization rate to some extent, significantly increasing energy consumption and material losses in the glufosinate preparation process. Furthermore, traditional glufosinate crystallization processes require multiple steps, resulting in high equipment investment, low operational error tolerance, insufficient mother liquor recycling, high solvent recovery costs, and difficulty in achieving an overall yield exceeding 90%.

[0003] Given this situation, technical personnel in the industry are still conducting research and considering ways to optimize processes and / or production equipment in order to improve production efficiency, reduce production costs, reduce emissions, and reduce the workload of workers. Utility Model Content

[0004] This invention aims to solve the problems of high investment costs and complex operation of existing glufosinate crystallization equipment, and proposes a new glufosinate crystallization system.

[0005] To achieve the above-mentioned objectives, the technical solution of this utility model is as follows:

[0006] A glufosinate crystallization system includes a first reactor, a second reactor, and a separator. The first reactor is connected to an alcohol reagent supply line, a gas feed line, and a raw material line. The raw material line is used to supply glufosinate hydrolysate, alkaline solution, or concentrated glufosinate solution to the first reactor. The first reactor is connected to a vacuum pump via pipeline I, and to a water storage tank via a pipeline connecting a heat exchanger and a water storage tank. The bottom of the first reactor is connected to the inlet of the second reactor via pipeline II. The bottom of the second reactor is connected to the raw material line via a circulation line, and the bottom outlet of the second reactor is connected to the inlet of the separator via pipeline III. The second reactor is also connected to a second feed pipe.

[0007] Furthermore, the first reactor is equipped with a stirring mechanism I, as well as a temperature sensor I and a pressure sensor I for detecting the temperature and pressure in the first reactor, and a jacket I is provided on the outside of the first reactor.

[0008] Furthermore, the jacket I is a jacket that is circulated with water at 40~60℃.

[0009] Furthermore, the second reactor is equipped with a stirring mechanism II, as well as a temperature sensor II and a pressure sensor II for detecting the temperature and pressure in the second reactor, and a jacket II is provided on the outside of the second reactor.

[0010] Furthermore, the jacket II is a jacket that is circulated with water at 25~35℃.

[0011] Furthermore, it also includes a dryer, with the solid discharge port of the separator connected to the feed port of the dryer via pipeline IV.

[0012] Furthermore, the heat exchanger connected to the first reactor is also connected to tail gas pipeline I, the second reactor is connected to tail gas pipeline II, and tail gas pipeline I and tail gas pipeline II are connected to the tail gas treatment system.

[0013] Furthermore, it also includes a controller. Valve I, valve II, and valve III are respectively installed on the alcohol reagent supply line, gas feed line, and raw material line. The controller is connected to valve I, valve II, and valve III respectively.

[0014] Furthermore, the liquid phase outlet of the separator is connected to the raw material pipeline via a recovery pipeline.

[0015] Furthermore, a transfer pump is installed on pipeline II.

[0016] The beneficial effects of this utility model are:

[0017] I. This utility model proposes a new glufosinate crystallization system. By designing two reactors, the glufosinate hydrolysate obtained from the production of glufosinate is processed, and finally pure glufosinate crystals are obtained through a separator. The whole system involves fewer equipment and simpler pipelines, resulting in lower equipment investment costs. In addition, the whole system has fewer control points and the equipment is easy to operate. Furthermore, the whole system generates less waste gas, wastewater, and waste residue, making it economical and environmentally friendly.

[0018] II. In this utility model, a stirring mechanism I is provided on the first reactor. The stirring mechanism I can stir the materials in the first reactor to achieve thorough mixing. The first reactor is equipped with a temperature sensor I and a pressure sensor I. The temperature sensor I is used to detect the temperature in the first reactor, and the pressure sensor I is used to monitor the pressure in the first reactor to ensure that the temperature of the materials in the first reactor and the pressure in the reactor meet the process conditions for glufosinate crystallization. A jacket I is provided on the outside of the first reactor. Preferably, water at 40~60℃ is circulated in the jacket I to keep the temperature of the materials in the first reactor at 40~50℃.

[0019] III. In this utility model, a stirring mechanism II is provided on the second reactor. The stirring mechanism II can stir the materials in the second reactor to achieve thorough mixing. A temperature sensor II and a pressure sensor II are provided on the second reactor. The temperature sensor II is used to detect the temperature in the second reactor, and the pressure sensor II is used to monitor the pressure in the second reactor to ensure that the temperature of the materials in the second reactor and the pressure in the reactor meet the process conditions for glufosinate crystallization. A jacket II is provided on the outside of the second reactor. Preferably, water at 25~35℃ is circulated in the jacket I to maintain the temperature of the materials in the second reactor at 25~30℃.

[0020] Fourth, this utility model also includes a dryer for drying glufosinate crystals output from the solid discharge port of the separator.

[0021] V. In this utility model, the heat exchanger connected to the first reactor is also connected to tail gas pipeline I, and the second reactor is connected to tail gas pipeline II. Tail gas pipeline I and tail gas pipeline II are connected to the tail gas treatment system. The waste gas generated from the first reactor, the second reactor and other equipment is uniformly discharged to the tail gas treatment system for unified treatment, thereby reducing the environmental pollution caused by the glufosinate crystallization system's external emissions.

[0022] VI. This utility model also includes a controller. Valve I, Valve II, and Valve III are respectively installed on the alcohol reagent supply line, gas feed line, and raw material line. The controller is connected to Valve I, Valve II, and Valve III respectively, facilitating automated system control. Furthermore, the controller can be connected to temperature sensors, pressure sensors, and other instruments on the first and second reactors. These sensors provide feedback to the controller regarding the temperature of the materials in the reactors and the internal pressure of the reactors, facilitating automated production and reducing the workload of workers.

[0023] VII. In this utility model, the liquid phase outlet of the separator is connected to the raw material pipeline through a recovery pipeline. The clear liquid obtained after the separator treatment (containing a very small amount of glufosinate mother liquor) is sent back to the first reactor as the raw material for the next round of crystallization treatment, reducing external emissions and recovering and utilizing water, solvents and other resources in the system as much as possible. Attached Figure Description

[0024] Figure 1 This is a schematic diagram of the structure of this utility model.

[0025] Figure 2 This is a schematic diagram of another implementation of the glufosinate crystallization system.

[0026] Figure 3 This is a schematic diagram of another implementation of the glufosinate crystallization system.

[0027] Figure 4 This is a schematic diagram of another preferred embodiment of the glufosinate crystallization system.

[0028] Figure 5 This is a schematic diagram of another preferred embodiment of the glufosinate crystallization system.

[0029] The components are as follows: 1. First reactor; 2. Second reactor; 3. Separator; 4. Dryer; 5. Controller; 6. Alcohol reagent supply line; 7. Gas feed line; 8. Raw material line; 9. Line I; 10. Vacuum pump; 11. Heat exchanger; 12. Water storage tank; 13. Line II; 14. Circulation line; 15. Line III; 16. Stirring mechanism I; 17. Temperature sensor I; 18. Pressure sensor I; 19. Jacket I; 20. Stirring mechanism II; 21. Temperature sensor II; 22. Temperature sensor II; 23. Jacket II; 24. Line IV; 25. Second feed pipe; 26. Tail gas line I; 27. Tail gas line II; 28. Tail gas treatment system; 29. ​​Valve I; 30. Valve II; 31. Valve III; 32. Transfer pump; 33. Recovery line; 3.1. Solid discharge port; 3.2. Liquid phase outlet. Detailed Implementation

[0030] The present invention will be further described in detail below with reference to the embodiments, but the implementation of the present invention is not limited thereto.

[0031] Example 1

[0032] A crystallization system for glufosinate, relating to the technical field of glufosinate production equipment, includes a first reactor 1, a second reactor 2, and a separator 3. (Reference) Figure 1 The first reactor 1 is connected to an alcohol reagent supply line 6, a gas feed line 7, and a raw material line 8. The raw material line 8 is used to supply the first reactor 1 with glufosinate hydrolysate, alkaline solution, or concentrated glufosinate. The first reactor 1 is connected to a vacuum pump 10 via line I9, and then to a heat exchanger 11 via a pipeline, followed by a water storage tank 12. The water storage tank 12 is used to store the water and solvent evaporated during concentration.

[0033] The bottom of the first reactor 1 is connected to the inlet of the second reactor 2 via pipeline II 13. The bottom of the first reactor 1 is connected to the raw material pipeline 8 via circulation pipeline 14. The bottom outlet of the second reactor 2 is connected to the inlet of the separator 3 via pipeline III 15. The second reactor 2 is connected to a second feed pipe 25, which is used to replenish reagents such as alkali solution or to introduce ammonia gas.

[0034] Preferably, a transfer pump 32 is installed on pipeline II13.

[0035] In use, firstly: the glufosinate hydrolysate obtained from the production of glufosinate (the mass concentration of glufosinate is 5~60%) is sent into the first reactor 1 from the raw material pipeline 8. The material can be heated to the preset temperature by introducing jacket water at the preset temperature outside the first reactor 1, or the material can be heated by the heat exchanger 11. The pressure in the first reactor 1 is controlled to the preset pressure by the vacuum pump 10, so that the hydrolysate in the first reactor 1 is concentrated for the first time to obtain material a.

[0036] Step 2: Transfer material a into the second reactor 2, add alkaline solution through the second feed pipe 25, adjust the pH value, and control the material temperature in the second reactor 2. After reacting for a period of time, material b is obtained.

[0037] Step 3: Transfer material b to the first reactor 1 through circulation pipeline 14, control the temperature and pressure in the first reactor 1, concentrate the material for the second time, and then add an appropriate proportion of alcohol reagent through alcohol reagent supply pipeline 6. After mixing and reacting for a period of time, material c is obtained.

[0038] Step 4: The material is then transported to the second reactor 2. The temperature inside the second reactor 2 is controlled, and an appropriate proportion of ammonia or alkaline reagent is introduced into the second reactor 2 through the second feed pipe 25 to adjust the pH. The mixture is stirred until crystals precipitate to obtain material d.

[0039] Step 5: The material d is transported to separator 3 for separation. The obtained glufosinate crystals are sent to the next stage (drying) for further processing. The remaining clear liquid is discharged from the liquid phase outlet 3.2 of separator 3.

[0040] Example 2

[0041] Compared with Embodiment 1, this embodiment differs in that the first reactor 1 is equipped with a stirring mechanism I16, a temperature sensor I17 and a pressure sensor I18 for detecting the temperature and pressure in the first reactor 1, and a jacket I19 is provided on the outside of the first reactor 1. Figure 2 .

[0042] Example 3

[0043] This embodiment is a further optimization of embodiment 2, the difference being that the jacket I19 is a jacket through which water at 40~60℃ is circulated.

[0044] Example 4

[0045] Compared with embodiments 1-3, this embodiment differs in that the second reactor 2 is equipped with a stirring mechanism II 20, a temperature sensor II 21 and a pressure sensor II for detecting the temperature and pressure in the second reactor 2, and a jacket II 23 is provided on the outside of the second reactor 2. (Refer to...) Figure 2 .

[0046] Example 5

[0047] This embodiment is a further optimization of embodiment 4, the difference being that the jacket II23 is a jacket through which water at 25~35℃ is supplied.

[0048] Example 6

[0049] Compared with embodiments 1-5, this embodiment also includes a dryer 4, and the solid discharge port 3.1 of the separator 3 is connected to the feed port of the dryer 4 through pipeline IV24. (Refer to...) Figure 3 .

[0050] Example 7

[0051] Compared with Examples 1-6, the difference in this embodiment is that the heat exchanger 11 connected to the first reactor 1 is also connected to the tail gas pipeline I 26, and the second reactor 2 is connected to the tail gas pipeline II 27. (Refer to...) Figure 3 Exhaust gas pipeline I 26 and exhaust gas pipeline II 27 are connected to exhaust gas treatment system 28.

[0052] Example 8

[0053] Compared with Examples 1-7, this embodiment differs in that it also includes a controller 5, and valves I 29, II 30, and III 31 are respectively installed on the alcohol reagent supply line 6, the gas feed line 7, and the raw material line 8. (See reference...) Figure 4 The controller 5 is connected to valve I 29, valve II 30, and valve III 31 respectively.

[0054] Example 9

[0055] The difference between this embodiment and embodiments 1-8 is that the liquid phase outlet 3.2 of separator 3 is connected to the raw material pipeline 8 through the recovery pipeline 33. (Refer to...) Figure 5 After the material is centrifuged by separator 3, the supernatant (containing a very small amount of glufosinate mother liquor) is transported from recovery pipeline 33 to the first reactor 1 as the reaction raw material for the next round of crystallization treatment, reducing external emissions.

[0056] Example 10

[0057] To facilitate public understanding of this solution, this embodiment uses a preferred glufosinate crystallization system as an example to further illustrate the solution.

[0058] refer to Figure 5The system includes a first reactor 1, a second reactor 2, a separator 3, a dryer 4, and a controller 5. The first reactor 1 is connected to an alcohol reagent supply line 6, a gas feed line 7, and a raw material line 8. The raw material line 8 is used to supply the first reactor 1 with glufosinate hydrolysate, alkaline solution, or concentrated glufosinate. The first reactor 1 is connected to a vacuum pump 10 via line I 9, and to a water storage tank 12 via a line connecting a heat exchanger 11. The bottom of the first reactor 1 is connected to the inlet of the second reactor 2 via line II 13. The bottom of the first reactor 1 is connected to the raw material line 8 via a circulation line 14, and the bottom outlet of the second reactor 2 is connected to the inlet of the separator 3 via line III 15. The solid outlet 3.1 of the separator 3 is connected to the inlet of the dryer 4 via line IV 24. A transfer pump 32 is installed on line II 13.

[0059] In this embodiment, the first reactor 1 is provided with a stirring mechanism I16, as well as a temperature sensor I17 and a pressure sensor I18 for detecting the temperature and pressure in the first reactor 1. The first reactor 1 is provided with a jacket I19 on the outside, and the jacket I19 is a jacket through which water at 40~60℃ is passed.

[0060] In this embodiment, the second reactor 2 is provided with a stirring mechanism II 20, as well as a temperature sensor II 21 and a pressure sensor II for detecting the temperature and pressure in the second reactor 2. The second reactor 2 is provided with a jacket II 23 on the outside, and the jacket II 23 is a jacket through which water at 25~35℃ is passed.

[0061] In this embodiment, the second reactor 2 is also connected to a second feed pipe 25, which is used to add alkaline reagents or introduce ammonia gas.

[0062] In this embodiment, the heat exchanger 11 connected to the first reactor 1 is also connected to the tail gas pipeline I 26, the second reactor 2 is connected to the tail gas pipeline II 27, and the tail gas pipeline I 26 and the tail gas pipeline II 27 are connected to the tail gas treatment system 28.

[0063] In this embodiment, valves I29, II30, and III31 are respectively installed on the alcohol reagent supply line 6, the gas feed line 7, and the raw material line 8, and the controller 5 is connected to valves I29, II30, and III31 for control.

[0064] In this embodiment, the liquid phase outlet 3.2 of the separator 3 is connected to the raw material pipeline 8 through the recovery pipeline 33.

[0065] The method of using this glufosinate crystallization system is as follows:

[0066] Step 1: The glufosinate hydrolysate (glufosinate mass concentration of 5-60%) obtained from the production of glufosinate is fed into the first reactor 1. Water at 40-60℃ is circulated into the jacket I19 to control the material temperature in the first reactor 1 to 40-50℃. The pressure in the first reactor 1 is controlled to -0.08--0.09MPa by the vacuum pump 10, so that the hydrolysate in the first reactor 1 is concentrated to a glufosinate concentration of 22-24%, and material a is obtained.

[0067] Step 2: Transfer material a into the second reactor 2 through the transfer pump 32, add alkaline solution through the second feed pipe 25, adjust the pH to 7~8, and cool the material in the second reactor 2 to 25~30℃ by passing water at 25~35℃ through the jacket II 23 to obtain material b;

[0068] Step 3: Material b is then transferred to the first reactor 1 through the circulation pipeline 14. The temperature in the first reactor 1 is controlled at 40~50℃ and the pressure is -0.08~-0.09MPa. The material is further concentrated to a glufosinate concentration of 36~37%. Then, an appropriate proportion of alcohol reagent is added through the alcohol reagent supply pipeline 6. The material in the first reactor 1 is stirred by the stirring mechanism I16 to fully disperse the material and obtain material c.

[0069] Step 4: The material is then transported to the second reactor 2, where it is further cooled to 25-30°C. An appropriate proportion of ammonia gas is introduced into the second reactor 2 through the second feed pipe 25 to adjust the pH to 7-8. The mixture is stirred for 6-8 hours until crystals precipitate, yielding material d.

[0070] Step 5: Material d is conveyed to separator 3 for separation. The obtained glufosinate crystals are conveyed to dryer for drying to obtain glufosinate technical powder. The obtained mother liquor is returned to the first reactor 1 through recovery pipeline 33 as raw material for the next round of crystallization.

Claims

1. A crystallization system for glufosinate, characterized in that, The reactor includes a first reactor (1), a second reactor (2), and a separator (3). The first reactor (1) is connected to an alcohol reagent supply line (6), a gas feed line (7), and a raw material line (8). The raw material line (8) is used to supply the first reactor (1) with glufosinate hydrolysate, alkaline solution, or concentrated glufosinate solution. The first reactor (1) is connected to a vacuum pump (10) via line I (9). The first reactor (1) is connected to a heat exchanger (11) via a line and then to a water storage tank (12). The bottom of the first reactor (1) is connected to the inlet of the second reactor (2) via line II (13). The bottom of the second reactor (2) is connected to the raw material line (8) via a circulation line (14). The bottom outlet of the second reactor (2) is connected to the inlet of the separator (3) via line III (15). The second reactor (2) is connected to a second feed pipe (25).

2. The crystallization system for glufosinate according to claim 1, characterized in that: The first reactor (1) is provided with a stirring mechanism I (16), a temperature sensor I (17) and a pressure sensor I (18) for detecting the temperature and pressure in the first reactor (1), and a jacket I (19) is provided on the outside of the first reactor (1).

3. The glufosinate crystallization system according to claim 2, characterized in that: The jacket I (19) is a jacket through which water at 40~60℃ is supplied.

4. The glufosinate crystallization system according to claim 1, characterized in that: The second reactor (2) is equipped with a stirring mechanism II (20), a temperature sensor II (21) and a pressure sensor II for detecting the temperature and pressure in the second reactor (2), and a jacket II (23) is provided on the outside of the second reactor (2).

5. The glufosinate crystallization system according to claim 4, characterized in that: The jacket II (23) is a jacket through which water at 25~35℃ is supplied.

6. The crystallization system for glufosinate according to claim 1, characterized in that: It also includes a dryer (4), and the solid discharge port (3.1) of the separator (3) is connected to the feed port of the dryer (4) via pipeline IV (24).

7. The crystallization system for glufosinate according to claim 1, characterized in that: The heat exchanger (11) connected to the first reactor (1) is also connected to the tail gas pipeline I (26), the second reactor (2) is connected to the tail gas pipeline II (27), and the tail gas pipeline I (26) and the tail gas pipeline II (27) are connected to the tail gas treatment system (28).

8. The crystallization system for glufosinate according to claim 1, characterized in that: It also includes a controller (5), and valves I (29), II (30) and III (31) are respectively installed on the alcohol reagent supply line (6), gas feed line (7) and raw material line (8). The controller (5) is connected to valves I (29), II (30) and III (31) respectively.

9. The crystallization system for glufosinate according to claim 1, characterized in that: The liquid phase outlet (3.2) of the separator (3) is connected to the raw material pipeline (8) through the recovery pipeline (33).

10. The crystallization system for glufosinate according to claim 1, characterized in that: The pipeline II (13) is equipped with a transfer pump (32).

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