A system for rapid crystallization of glufosinate
By designing a rapid crystallization system for glufosinate, and utilizing internal heat exchange pipes and jacket temperature control, efficient concentration and crystallization of glufosinate are achieved. This solves the problems of low crystallization rate and high equipment investment, improves the crystallization rate and mother liquor recycling rate, and reduces production costs.
Patent Information
- Application Number
- CN202521259105.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-19
- Publication Date
- 2026-07-31
- Estimated Expiration
- 2035-06-19
AI Technical Summary
The existing glufosinate crystallization process has a low crystallization rate, insufficient mother liquor recycling rate, high equipment investment, complex operation, large energy consumption and material loss, and the overall yield is difficult to exceed 90%.
Design a glufosinate rapid crystallization system comprising a first reaction vessel, a second-stage concentration vessel, and a third-stage concentration vessel. Employ an internal heat exchanger structure and jacket temperature control to achieve continuous concentration and crystallization of glufosinate hydrolysate. Combined with a separator and tail gas treatment system, optimize material temperature and pH value to improve crystallization rate and recover solvent.
It significantly improves the crystallization rate of glufosinate to 95%, reduces mother liquor residue, lowers production costs, enables efficient recovery and recycling of mother liquor solvent, simplifies operation procedures, and reduces organic solvent residue in wastewater.
Smart Images
Figure CN224573257U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the technical field of glufosinate production equipment, specifically to a rapid crystallization system for glufosinate. 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 system for rapid crystallization of glufosinate includes a first reaction vessel, a second-stage concentration vessel, and a third-stage concentration vessel connected in sequence. The first reaction vessel is connected to a feed pipe I and an ammonia water feed pipe. The interior of the first reaction vessel, from top to bottom, is provided with a uniformly distributed frame area, a baffle plate area, a heat exchange plate group area, and a liquid collection plate area. The bottom of the first reaction vessel is connected to a discharge pipe. The second-stage and third-stage concentration vessels are each equipped with a stirring mechanism, a pressure sensor, and a temperature sensor. Both the second-stage and third-stage concentration vessels are connected to a vacuum pump and a heat exchanger. The other end of the heat exchanger is connected to a storage tank. The outer sides of the second-stage and third-stage concentration vessels are equipped with jackets. The second-stage concentration vessel is connected to an alcohol reagent supply line, a gas feed line, and a feed pipe II. The third-stage concentration vessel is connected to a feed pipe III.
[0007] Furthermore, the heat exchange plate assembly includes an inner heat exchange pipe for introducing the heat exchange medium.
[0008] Furthermore, separators are connected to the pipeline connected to the rear end of the discharge pipe of the first reactor, as well as to the pipelines connected to the discharge ports of the secondary and tertiary concentration reactors.
[0009] Furthermore, the discharge port at the bottom of the separator is connected to the dryer via a pipeline.
[0010] Furthermore, the liquid phase outlet of the separator connected to the rear end of the three-stage concentration vessel is connected to feed pipe I or feed pipe II via a recovery pipeline.
[0011] Furthermore, the top of the first reactor is provided with a tail gas outlet, which is connected to the tail gas treatment system via a pipeline.
[0012] Furthermore, the heat exchangers connected to the secondary and tertiary concentration vessels are respectively connected to the exhaust gas treatment system via pipelines.
[0013] Furthermore, transfer pumps are installed between the first reaction vessel and the second-stage concentration vessel, and between the second-stage concentration vessel and the third-stage concentration vessel.
[0014] The beneficial effects of this utility model are:
[0015] I. This utility model proposes a new system for rapid crystallization of glufosinate. By designing a first reactor, a second-stage concentration vessel, and a third-stage concentration vessel, it achieves the concentration and crystallization of glufosinate hydrolysate obtained from the production of glufosinate. Finally, pure glufosinate crystals are obtained through a separator. Using this system can significantly improve the crystallization rate of glufosinate, up to 95%, greatly reduce the residue of glufosinate in the mother liquor, and also reduce the difficulty of subsequent mother liquor treatment.
[0016] Second, in this utility model, the glufosinate rapid crystallization system can realize continuous production, and the "concentration" and "crystallization" processes can be carried out in the same equipment, reducing losses caused by material transfer, improving the operational error tolerance rate, and accelerating the production speed.
[0017] Third, in this utility model, the glufosinate rapid crystallization system is a closed-loop circulation system, which realizes efficient recovery of solvent in the mother liquor (recovery rate > 95%). The system can also realize the recycling of mother liquor solvent, reduce solvent consumption, and reduce production costs; at the same time, it reduces the organic solvent residue in wastewater, which is conducive to discharge.
[0018] IV. This utility model proposes a preferred first reactor structure. The first reactor adopts an internal heat exchange pipe structure, and a medium of suitable temperature is introduced into the internal heat exchange pipe to heat the material, which helps to ensure that the temperature of the material is within a preset temperature range. Preferably, the medium in the internal heat exchange pipe can be water or the solvent used in the production of glufosinate, etc.
[0019] V. In this utility model, media of different temperatures can be introduced into jacket I and jacket II to achieve temperature control in the secondary and tertiary concentration vessels.
[0020] VI. In this utility model, the top of the first reaction vessel is provided with a tail gas outlet, which is connected to the tail gas treatment system through a pipeline. The heat exchangers connecting the second-stage and third-stage concentration vessels are connected to the tail gas treatment system through pipelines, which is conducive to collecting the waste gas / non-condensable gas generated by the first reaction vessel and the heat exchanger and discharging it to the tail gas treatment system for centralized treatment. Attached Figure Description
[0021] Figure 1 This is a schematic diagram of the structure of this utility model.
[0022] Figure 2 This is a schematic diagram of another implementation of the glufosinate-ammonium rapid crystallization system.
[0023] Figure 3 This is a schematic diagram of another implementation of the glufosinate-ammonium rapid crystallization system.
[0024] Figure 4 This is a schematic diagram of another preferred embodiment of the glufosinate-ammonium rapid crystallization system.
[0025] Figure 5 This is a schematic diagram of another preferred embodiment of the glufosinate-ammonium rapid crystallization system.
[0026] The components include: 1. First reaction vessel; 2. Secondary concentration vessel; 3. Tertiary concentration vessel; 4. Feed pipe I; 5. Ammonia water feed line; 6. Discharge pipe; 7. Stirring mechanism; 8. Pressure sensor; 9. Temperature sensor; 10. Vacuum pump; 11. Heat exchanger; 12. Storage tank; 13. Alcohol reagent supply line; 14. Gas feed line; 15. Feed pipe II; 16. Feed pipe III; 17. Jacket I; 18. 19. Jacket II; 20. Separator; 21. Dryer; 22. Recovery pipeline; 23. Tail gas outlet; 24. Tail gas treatment system; 25. Transfer pump; 26. Pipeline I; 27. Pipeline II; 1.1. Uniform distribution frame area; 1.2. Baffle plate area; 1.3. Heat exchange plate group area; 1.4. Liquid collection plate area; 19.1. Liquid phase outlet; 1.3.1. Medium inlet pipe; 1.3.2. Medium outlet pipe. Detailed Implementation
[0027] 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.
[0028] Example 1
[0029] A system for rapid crystallization of glufosinate, relating to the technical field of glufosinate production equipment, see reference. Figure 1It includes a first reaction vessel 1, a second-stage concentration vessel 2 and a third-stage concentration vessel 3 connected in sequence. The discharge pipe 6 of the first reaction vessel 1 is connected to the feed pipe Ⅱ15 of the second-stage concentration vessel 2 through pipeline Ⅰ25. The discharge port of the second-stage concentration vessel 2 is connected to the feed pipe Ⅲ16 of the third-stage concentration vessel 3 through pipeline Ⅱ26.
[0030] The first reactor 1 is connected to a feed pipe I 4 and an ammonia water feed pipe 5. The interior of the first reactor 1 is provided with a uniformly distributed frame area 1.1, a baffle plate area 1.2, a heat exchange plate group area 1.3 and a liquid collection plate area 1.4 from top to bottom. The bottom of the first reactor 1 is connected to a discharge pipe 6. The secondary concentration reactor 2 and the tertiary concentration reactor 3 are each equipped with a stirring mechanism 7, a pressure sensor 8 and a temperature sensor 9. The secondary concentration reactor 2 and the tertiary concentration reactor 3 are each connected to a vacuum pump 10 and a heat exchanger 11. The other end of the heat exchanger 11 is connected to a storage tank 12, which is used to store the water and solvent distilled during the concentration process. The outer sides of the secondary concentration reactor 2 and the tertiary concentration reactor 3 are respectively provided with a jacket I 17 and a jacket II 18. The secondary concentration reactor 2 is connected to an alcohol reagent supply pipe 13, a gas feed pipe 14 and a feed pipe II 15. The tertiary concentration reactor 3 is connected to a feed pipe III 16.
[0031] Preferably, a transfer pump 24 is provided between the first reaction vessel 1 and the second-stage concentration vessel 2, and between the second-stage concentration vessel 2 and the third-stage concentration vessel 3.
[0032] In use, firstly, a certain amount of glufosinate hydrolysate and wood powder activated carbon mixture are added to the first reaction vessel 1. The activated carbon powder is filtered out through the uniformly distributed frame area 1.1 to obtain the decolorized hydrolysate. Then, a medium of appropriate temperature is introduced into the internal heat exchange tube of the heat exchange plate group area 1.3 to control the temperature and pressure inside the first reaction vessel 1, and the hydrolysate undergoes the first concentration in the first reaction vessel 1. During the concentration process, when the concentrated liquid is collected in the liquid collection plate area 1.4 and the concentration of glufosinate in the vessel reaches a certain level, ammonia water is added to the liquid collection plate area 1.4 to adjust the pH. Then, a low-temperature medium is introduced into the internal heat exchange tube to cool the material and precipitate crystals. The material is then sent to the separator 19 to separate the glufosinate crystals, and the crystals are then sent to the dryer for drying. The liquid phase obtained after processing by the separator 19 is transferred to the secondary concentration vessel 2 by the transfer pump 24.
[0033] Then, a medium (water) at a suitable temperature is introduced into the jacket I17 of the secondary concentration vessel 2 to control the temperature and pressure inside the secondary concentration vessel 2. When the concentration of glufosinate in the solution reaches a certain concentration, a certain amount of alcohol reagent is added into the secondary concentration vessel 2 through the alcohol reagent supply line 13 to disperse and stir. A medium at a suitable temperature is then introduced into the jacket I17 to cool the material in the secondary concentration vessel 2, causing glufosinate crystals to precipitate. After separation by the separator 19, the resulting liquid phase is transported by the transfer pump 24 to the tertiary concentration vessel 3 for further processing.
[0034] Finally, a medium of suitable temperature is introduced into the jacket I17 of the tertiary concentration vessel 3 to gradually raise the temperature inside the tertiary concentration vessel 3 to 100°C. The pressure inside the vessel is adjusted, and concentration is stopped when the temperature inside the tertiary concentration vessel 3 reaches 100°C. At this time, when the content of glufosinate in the solution in the vessel reaches a certain value, a certain amount of alcohol reagent is slowly added dropwise into the tertiary concentration vessel 3 through the feed pipe III16, and the mixture is stirred continuously until it is completely added. Then, a low-temperature medium is introduced into the jacket I17 of the tertiary concentration vessel 3 to lower the temperature inside the tertiary concentration vessel 3 to a certain temperature. Then, ammonia gas is introduced into the vessel to adjust the pH value. Then, porous material COFs are added and impregnated in the glufosinate crystallization solution. After stirring slowly (with the aid of ultrasound) for a period of time, crystals are precipitated. The crystals are separated and dried by the separator 19 and the dryer to obtain glufosinate technical powder. The remaining clear liquid is sent back to the first reaction vessel 1 or the second-stage concentration vessel 2 for further processing through the recovery pipeline 21.
[0035] This system can significantly increase the crystallization rate of glufosinate in glufosinate hydrolysate, up to 95% or more.
[0036] Example 2
[0037] This embodiment is a further optimization of Embodiment 1, the difference being that the heat exchange plate assembly 1.3 includes an inner heat exchange pipe for introducing the heat exchange medium. (Reference) Figure 1 The heat exchange plate group 1.3 of the first reactor 1 is provided with a medium inlet pipe 1.3.1 and a medium outlet pipe 1.3.2. The medium is introduced through the medium inlet pipe 1.3.1. After the medium exchanges heat with the material in the reactor in the internal heat exchange tube, it is output from the medium outlet pipe 1.3.2.
[0038] Example 3
[0039] The difference between this embodiment and embodiments 1-2 is that, in reference to... Figure 2 Separators 19 are connected to the pipeline connected to the rear end of the discharge pipe 6 of the first reactor 1, as well as to the pipeline connected to the discharge ports of the secondary concentration reactor 2 and the tertiary concentration reactor 3.
[0040] Example 4
[0041] The difference between this embodiment and embodiments 1-3 is that, in reference... Figure 3 The solid phase outlet at the bottom of separator 19 is connected to dryer 20 via pipeline.
[0042] Example 5
[0043] Compared with Examples 1-4, the difference in this embodiment is that the liquid phase outlet 19.1 of the separator 19 connected to the rear end of the three-stage concentration vessel 3 is connected to the feed pipe I 4 or the feed pipe II 15 through the recovery pipeline 21. (Refer to...) Figure 4The material containing glufosinate crystals in the three-stage concentration vessel 3 is processed by the back-end separator 19, and the resulting glufosinate mother liquor containing a very small amount is sent to the first reaction vessel 1 and / or the second-stage concentration vessel 2, and returned to the system for circulation, so as to recover glufosinate as much as possible and reduce external emissions; the obtained glufosinate crystals are sent to the dryer for drying to obtain glufosinate powder.
[0044] Example 6
[0045] The difference between this embodiment and embodiments 1-5 is that, in reference... Figure 5 The top of the first reactor 1 is provided with a tail gas outlet 22, which is connected to the tail gas treatment system 23 via a pipeline.
[0046] Preferably, the heat exchanger 11 connecting the secondary concentration vessel 2 and the tertiary concentration vessel 3 is connected to the exhaust gas treatment system 23 via pipeline.
[0047] Example 7
[0048] To facilitate public understanding of this solution, this embodiment uses a preferred system for rapid crystallization of glufosinate as an example to further illustrate the solution.
[0049] refer to Figure 5 Specifically, it includes a first reaction vessel 1, a second-stage concentration vessel 2, and a third-stage concentration vessel 3. The discharge pipe 6 of the first reaction vessel 1 is connected to the feed pipe II 15 of the second-stage concentration vessel 2 through pipeline I 25, and the discharge port of the second-stage concentration vessel 2 is connected to the feed pipe III 16 of the third-stage concentration vessel 3 through pipeline II 26.
[0050] In this embodiment, the first reactor 1 is connected to a feed pipe I 4 and an ammonia water feed pipe 5. The interior of the first reactor 1 is provided with a uniformly distributed frame area 1.1, a baffle plate area 1.2, a heat exchange plate group area 1.3 and a liquid collection plate area 1.4 from top to bottom. The bottom of the first reactor 1 is connected to a discharge pipe 6. The secondary concentration reactor 2 and the tertiary concentration reactor 3 are each provided with a stirring mechanism 7, a pressure sensor 8 and a temperature sensor 9. The secondary concentration reactor 2 and the tertiary concentration reactor 3 are each connected to a vacuum pump 10 and a heat exchanger 11. The other end of the heat exchanger 11 is connected to a storage tank 12. The outer sides of the secondary concentration reactor 2 and the tertiary concentration reactor 3 are respectively provided with a jacket I 17 and a jacket II 18. The secondary concentration reactor 2 is connected to an alcohol reagent supply pipe 13, a gas feed pipe 14 and a feed pipe II 15. The tertiary concentration reactor 3 is connected to a feed pipe III 16.
[0051] In this embodiment, the heat exchange plate assembly area 1.3 includes an inner heat exchange pipe, which is used to introduce the heat exchange medium.
[0052] In this embodiment, separators 19 are connected to the pipeline connected to the rear end of the discharge pipe 6 of the first reaction vessel 1, as well as to the pipelines connected to the discharge ports of the secondary concentration vessel 2 and the tertiary concentration vessel 3.
[0053] In this embodiment, the discharge port at the bottom of the separator 19 is connected to the dryer 20 via a pipeline.
[0054] In this embodiment, the liquid phase outlet 19.1 of the separator 19 connected to the rear end of the three-stage concentration vessel 3 is connected to the feed pipe I 4 or the feed pipe II 15 through the recovery pipeline 21.
[0055] In this embodiment, the top of the first reactor 1 is provided with a tail gas outlet 22, and the tail gas outlet 22 is connected to the tail gas treatment system 23 through a pipeline.
[0056] In this embodiment, the heat exchanger 11, which is connected to the secondary concentration vessel 2 and the tertiary concentration vessel 3 respectively, is connected to the exhaust gas treatment system 23 via pipeline.
[0057] In this embodiment, a transfer pump 24 is provided between the first reaction vessel 1 and the secondary concentration vessel 2, and between the secondary concentration vessel 2 and the tertiary concentration vessel 3.
[0058] In use, this system can process glufosinate hydrolysate with a mass concentration of 5-60% to obtain glufosinate product. The specific operating steps are as follows:
[0059] (1) A certain amount of glufosinate hydrolysate is added to the first reactor 1. A medium (water) of appropriate temperature is introduced into the heat exchange tube of the heat exchange plate group 1.3 to control the temperature of the first reactor 1 to 40~50℃. The vacuum negative pressure of the first reactor 1 is adjusted to -0.08~-0.09MPa. The hydrolysate is concentrated for the first time in the first reactor 1. During the concentration process, when the concentrated liquid is collected in the collection plate area 1.4 and the concentration of glufosinate in the reactor reaches about 20%, a certain amount of 25% ammonia water is added to the collection plate area 1.4 to adjust the pH to about 7~8. After cooling to 25~30℃, the glufosinate crystals are separated by the separator 19. The obtained liquid phase is transferred to the secondary concentration reactor 2 by the transfer pump 24. The glufosinate crystals are then sent to the dryer for drying.
[0060] (2) Then, a medium (water) of appropriate temperature is introduced into the jacket I17 of the secondary concentration vessel 2 to control the temperature inside the secondary concentration vessel 2 to 40~50℃. The pressure inside the secondary concentration vessel 2 is adjusted by the vacuum pump 10 to adjust the vacuum negative pressure to -0.08~-0.09MPa. When the concentration of glufosinate in the solution reaches 35~36%, 1.5 times the mass of methanol of glufosinate is added to the secondary concentration vessel 2 through the alcohol reagent supply line 13 and then dispersed and stirred. A medium of appropriate temperature is introduced into the jacket I17 to cool the material in the secondary concentration vessel 2 to 25~30℃. After separation by the separator 19, the obtained liquid phase is transported to the tertiary concentration vessel 3 by the transfer pump 24 for further processing.
[0061] (3) Introduce a medium (saturated steam) at a suitable temperature into the jacket I17 of the tertiary concentration vessel 3, gradually raise the temperature inside the tertiary concentration vessel 3 to 100°C, and adjust the vacuum negative pressure to -0.085MPa. When the temperature inside the tertiary concentration vessel 3 reaches 100°C, stop the concentration. At this time, the content of glufosinate in the solution inside the vessel is 55~56%. Then, slowly add a mixture of methanol and ethanol at 3 times the mass of glufosinate to the tertiary concentration vessel 3 through the feed pipe III16, and stir continuously until it is completely added. Then, introduce a low temperature medium into the jacket I17 of the tertiary concentration vessel 3 to lower the temperature inside the tertiary concentration vessel 3 to 40°C. Then, introduce ammonia into the vessel, adjust the pH to 7~8, and stir slowly for 6~8 hours to crystallize. Then, separate the crystals through the separator 19 and dry them through the dryer to obtain glufosinate raw powder. The remaining clear liquid is sent back to the first reaction vessel 1 or the second-stage concentration vessel 2 through the recovery pipeline 21.
Claims
1. A system for rapid crystallization of glufosinate-ammonium, characterized by: It includes a first reaction vessel (1), a second-stage concentration vessel (2), and a third-stage concentration vessel (3) connected in sequence. The first reactor (1) is connected to a feed pipe I (4) and an ammonia water feed line (5). The interior of the first reactor (1) is provided with a uniformly distributed frame area (1.1), a baffle plate area (1.2), a heat exchange plate group area (1.3) and a liquid collection plate area (1.4) from top to bottom. The bottom of the first reactor (1) is connected to a discharge pipe (6). Both the secondary concentration vessel (2) and the tertiary concentration vessel (3) are equipped with a stirring mechanism (7), a pressure sensor (8) and a temperature sensor (9). Both the secondary concentration vessel (2) and the tertiary concentration vessel (3) are connected to a vacuum pump (10) and a heat exchanger (11). The other end of the heat exchanger (11) is connected to a storage tank (12). The outer sides of the secondary concentration vessel (2) and the tertiary concentration vessel (3) are provided with jackets. The secondary concentration vessel (2) is connected to an alcohol reagent supply line (13), a gas feed line (14), and a feed pipe II (15), while the tertiary concentration vessel (3) is connected to a feed pipe III (16).
2. A system for rapid crystallization of glufosinate-ammonium according to claim 1, characterized in that: The heat exchange plate assembly area (1.3) includes an inner heat exchange pipe, which is used to introduce the heat exchange medium.
3. A system for rapid crystallization of glufosinate-ammonium according to claim 2, characterized in that: Separators (19) are connected to the pipeline connected to the rear end of the discharge pipe (6) of the first reactor (1), as well as to the pipeline connected to the discharge port of the secondary concentration reactor (2) and the tertiary concentration reactor (3).
4. A system for rapid crystallization of glufosinate-ammonium according to claim 1, characterized by the fact that: The discharge port at the bottom of the separator (19) is connected to the dryer (20) via a pipeline.
5. The system for rapid crystallization of glufosinate according to claim 1, characterized in that: The liquid phase outlet (19.1) of the separator (19) connected to the rear end of the three-stage concentration vessel (3) is connected to the feed pipe I (4) or the feed pipe II (15) through the recovery pipeline (21).
6. The system for rapid crystallization of glufosinate according to claim 1, characterized in that: The top of the first reactor (1) is provided with a tail gas outlet (22), and the tail gas outlet (22) is connected to the tail gas treatment system (23) through a pipeline.
7. The system for rapid crystallization of glufosinate according to claim 1, characterized in that: The heat exchangers (11) connected to the secondary concentration vessel (2) and the tertiary concentration vessel (3) are respectively connected to the exhaust gas treatment system (23) via pipelines.
8. A system for rapid crystallization of glufosinate-ammonium according to claim 1, characterized by the fact that: A transfer pump (24) is installed between the first reaction vessel (1) and the second-stage concentration vessel (2), and between the second-stage concentration vessel (2) and the third-stage concentration vessel (3).