A continuous hydrolysis and separation system for glufosinate

Abstract

This invention discloses a continuous hydrolysis and separation system for glufosinate, comprising a mixing and preheating device, a first feed pump, a second feed pump, a tubular reactor, a flash tank, a low-boiling-point collection device, a neutralization reactor, a crystallization reactor, separation equipment, a first storage tank for storing aminonitrile, and a second storage tank for storing hydrochloric acid. The inlet of the first feed pump is connected to the first storage tank, the inlet of the second feed pump is connected to the second storage tank, the outlets of the first and second feed pumps are respectively connected to the inlet of the mixing and preheating device, the outlet of the mixing and preheating device is connected to the inlet of the tubular reactor, the outlet of the tubular reactor is connected to the inlet of the flash tank, and the outlet at the bottom of the flash tank is connected to the inlet of the neutralization reactor. This invention enables continuous synthesis of glufosinate, improving the efficiency and yield of glufosinate synthesis.

Description

Technical Field

[0001] This utility model relates to a continuous hydrolysis and separation system for glufosinate. Background Technology

[0002] Currently, glufosinate is a broad-spectrum contact herbicide. There are several methods for preparing glufosinate, including the Strecker process and the Bayer monoester process. A method for preparing glufosinate is also disclosed in Chinese patent CN111018906B. In both the Strecker and Bayer monoester methods, the glufosinate precursor aminonitrile is first obtained, then hydrolyzed to obtain glufosinate hydrochloride, and finally neutralized with ammonia and separated to obtain glufosinate acid or glufosinate ammonium salt. Currently, many manufacturers commonly use batch operations in the synthesis of glufosinate, that is, adding hydrochloric acid to the reactor, waiting for the reaction to complete, then evaporating the hydrochloric acid, and then separating the products. Multiple steps cannot be performed simultaneously, resulting in low efficiency in the synthesis of glufosinate and consequently low yield. Utility Model Content

[0003] The technical problem to be solved by this utility model is to overcome the defects of the prior art and provide a continuous hydrolysis and separation system for glufosinate, which can continuously synthesize glufosinate and improve the efficiency and yield of glufosinate synthesis.

[0004] To solve the above-mentioned technical problems, the technical solution of this utility model is: a continuous hydrolysis and separation system for glufosinate, including a mixing and preheating device, a first raw material pump, a second raw material pump, a tubular reactor, a flash tank, a low-boiling-point collection device, a neutralization reaction vessel, a crystallization vessel, a separation device, a first storage tank for storing aminonitrile, and a second storage tank for storing hydrochloric acid.

[0005] The inlet of the first raw material pump is connected to the first storage tank;

[0006] The inlet of the second raw material pump is connected to the second storage tank;

[0007] The outlets of the first raw material pump and the second raw material pump are respectively connected to the inlet of the mixing preheating device;

[0008] The outlet of the mixing preheating device is connected to the inlet of the tubular reactor;

[0009] The outlet of the tubular reactor is connected to the inlet of the flash tank;

[0010] The outlet at the bottom of the flash tank is connected to the inlet of the neutralization reactor;

[0011] The vapor phase outlet of the flash tank is connected to the low-boiling-point substance collection device;

[0012] The outlet of the neutralization reactor is connected to the inlet of the crystallization reactor;

[0013] The outlet of the crystallization vessel is connected to the separation equipment.

[0014] Further, a specific structure of the mixing preheating device is provided, the mixing preheating device including a static mixer and a preheater; wherein, the outlet of the first raw material pump and the outlet of the second raw material pump are respectively connected to the inlet of the static mixer, the outlet of the static mixer is connected to the inlet of the preheater, and the outlet of the preheater is connected to the inlet of the tubular reactor.

[0015] Furthermore, a first flow meter is connected between the outlet of the first raw material pump and the inlet of the static mixer, and a second flow meter is connected between the outlet of the second raw material pump and the inlet of the static mixer.

[0016] Further, a specific structure of the low-boiling-point substance collection device is provided, the low-boiling-point substance collection device including a condenser and a low-boiling-point substance storage tank;

[0017] The vapor phase outlet of the flash tank is connected to the inlet of the condenser;

[0018] The outlet of the condenser is connected to the low-boiling-point storage tank.

[0019] Furthermore, a first material conveying pump is provided between the outlet of the flash tank and the inlet of the neutralization reactor, a second material conveying pump is provided between the outlet of the neutralization reactor and the inlet of the crystallization reactor, and a third material conveying pump is provided between the outlet of the crystallization reactor and the separation equipment.

[0020] Furthermore, the separation device is a centrifuge.

[0021] Furthermore, the neutralization reactor is provided with a first raw material inlet for introducing methanol and a second raw material inlet for introducing ammonia.

[0022] Furthermore, both the neutralization reactor and the crystallization reactor are equipped with exhaust gas outlets.

[0023] Furthermore, both the neutralization reactor and the crystallization reactor are equipped with stirring devices.

[0024] Furthermore, a first jacket is provided on the outer wall of the neutralization reactor, and a first heating chamber is provided between the first jacket and the outer wall of the neutralization reactor. The first jacket is provided with a first inlet medium port communicating with the first heating chamber and a first outlet medium port communicating with the first heating chamber.

[0025] The outer wall of the crystallization vessel is provided with a second jacket, and a second heating chamber is provided between the second jacket and the outer wall of the crystallization vessel. The second jacket is provided with a second inlet medium port communicating with the second heating chamber and a second outlet medium port communicating with the second heating chamber.

[0026] After adopting the above technical solution, under the suction action of the first raw material pump and the second raw material pump, the aminonitrile in the first storage tank and the hydrochloric acid in the second storage tank are continuously fed into the mixing and preheating device in a certain molar ratio for thorough mixing and preheating. Then, they are continuously pumped to the tubular reactor for hydrolysis. The material after hydrolysis directly enters the flash tank from the outlet of the tubular reactor for flash evaporation to remove low-boiling materials such as hydrogen chloride and water. After the low-boiling materials are vaporized, they flow from the gas phase outlet above the flash tank to the low-boiling material collection device for collection and storage. The remaining material after the low-boiling materials are removed in the flash tank is continuously discharged from the outlet at the bottom of the flash tank and continuously enters the neutralization reactor. At the same time, methanol and ammonia are continuously introduced into the neutralization reactor. The material injected into the neutralization reactor mixes with the methanol and ammonia and reacts, then directly enters the crystallization reactor for glufosinate-ammonium salt crystallization. Then, the material in the crystallization reactor enters the separation equipment from the outlet of the crystallization reactor for separation to obtain solid products and mother liquor. The glufosinate continuous hydrolysis and separation system described in this application enables continuous hydrolysis and continuous ammonium salting. Combined with continuous distillation in a tubular reactor and flash tank, continuous synthesis of glufosinate is achieved, improving the efficiency and yield of glufosinate synthesis. Furthermore, it increases reaction conversion rate, improves hydrogen chloride separation, shortens the process flow, significantly reduces the reaction cycle, lowers energy consumption, enhances process automation, and reduces labor load. Attached Figure Description

[0027] Figure 1 This is a process flow diagram of the glufosinate continuous hydrolysis and separation system of this utility model;

[0028] In the diagram: 1. First feed pump; 2. Tubular reactor; 3. Flash tank; 4. Neutralization reactor; 5. Crystallization reactor; 6. First storage tank; 7. Second storage tank; 8. Static mixer; 9. Preheater; 10. First flow meter; 11. Second flow meter; 12. Condenser; 13. Low-boiling-point substance storage tank; 15. First feed inlet; 16. Second feed inlet; 17. Tail gas outlet; 18. Stirring device; 19. First jacket; 20. Second jacket; 21. Second feed pump. Detailed Implementation

[0029] To make the contents of this utility model easier to understand, the present utility model will be further described in detail below with reference to specific embodiments and accompanying drawings.

[0030] like Figure 1 As shown, a continuous hydrolysis and separation system for glufosinate includes a mixing and preheating device, a first raw material pump 1, a second raw material pump 21, a tubular reactor 2, a flash tank 3, a low-boiling-point collection device, a neutralization reactor 4, a crystallization reactor 5, separation equipment, a first storage tank 6 for storing aminonitrile, and a second storage tank 7 for storing hydrochloric acid.

[0031] The inlet of the first raw material pump 1 is connected to the first storage tank 6;

[0032] The inlet of the second raw material pump 21 is connected to the second storage tank 7;

[0033] The outlet of the first raw material pump 1 and the outlet of the second raw material pump 21 are respectively connected to the inlet of the mixing preheating device;

[0034] The outlet of the mixing preheating device is connected to the inlet of the tubular reactor 2;

[0035] The outlet of the tubular reactor 2 is connected to the inlet of the flash tank 3;

[0036] The discharge port at the bottom of the flash tank 3 is connected to the inlet of the neutralization reactor 4;

[0037] The vapor phase outlet of the flash tank 3 is connected to the low-boiling-point substance collection device;

[0038] The outlet of the neutralization reactor 4 is connected to the inlet of the crystallization reactor 5;

[0039] The outlet of the crystallization vessel 5 is connected to the separation equipment.

[0040] Specifically, under the suction action of the first raw material pump 1 and the second raw material pump 21, the aminonitrile in the first storage tank 6 and the hydrochloric acid in the second storage tank 7 are continuously fed into the mixing and preheating device in a certain molar ratio for thorough mixing and preheating. Then, they are continuously pumped to the tubular reactor 2 for hydrolysis. The material after hydrolysis directly enters the flash tank 3 from the outlet of the tubular reactor 2 for flash evaporation to remove low-boiling materials such as hydrogen chloride and water. After the low-boiling materials are vaporized, they flow from the gas phase outlet above the flash tank 3 to the low-boiling material collection device for collection and storage. The remaining material after the low-boiling materials are removed in the flash tank 3 is continuously discharged from the outlet at the bottom of the flash tank 3 and continuously enters the neutralization reactor 4. At the same time, methanol and ammonia are continuously introduced into the neutralization reactor 4. The material injected into the neutralization reactor 4 mixes with the methanol and ammonia and reacts, then directly enters the crystallization reactor 5 for glufosinate-ammonium salt crystallization. Then, the material in the crystallization reactor 5 enters the separation equipment from the outlet of the crystallization reactor 5 for separation to obtain solid products and mother liquor. The continuous hydrolysis and separation system for glufosinate, as described in this application, enables continuous hydrolysis and ammonium salting. Combined with continuous distillation in tubular reactor 2 and flash tank 3, continuous synthesis of glufosinate is achieved, improving the efficiency and yield of glufosinate synthesis. Furthermore, it increases reaction conversion rate, improves hydrogen chloride separation, shortens the process flow, significantly reduces the reaction cycle, lowers energy consumption, enhances process automation, and reduces labor load.

[0041] like Figure 1 As shown, the mixing and preheating device may include a static mixer 8 and a preheater 9; wherein, the outlet of the first raw material pump 1 and the outlet of the second raw material pump 21 are respectively connected to the inlet of the static mixer 8, the outlet of the static mixer 8 is connected to the inlet of the preheater 9, and the outlet of the preheater 9 is connected to the inlet of the tubular reactor 2. Specifically, under the suction action of the first raw material pump 1 and the second raw material pump 21, the aminonitrile in the first storage tank 6 and the hydrochloric acid in the second storage tank 7 are continuously fed into the static mixer 8 in a certain molar ratio for thorough mixing, and then into the preheater 9 for preheating, and then continuously pumped to the tubular reactor 2 for hydrolysis reaction.

[0042] like Figure 1 As shown, a first flow meter 10 is connected between the outlet of the first raw material pump 1 and the inlet of the static mixer 8, and a second flow meter 11 is connected between the outlet of the second raw material pump 21 and the inlet of the static mixer 8.

[0043] like Figure 1 As shown, the low-boiling-point substance collection device may include a condenser 12 and a low-boiling-point substance storage tank 13;

[0044] The gas phase outlet of the flash tank 3 is connected to the inlet of the condenser 12;

[0045] The outlet of the condenser 12 is connected to the low-boiling-point material storage tank 13. Specifically, when the low-boiling-point materials such as hydrogen chloride and water are flashed and removed from the material in the flash tank 3, the vaporized low-boiling-point materials will flow from the gas phase outlet above the flash tank 3 to the condenser 12 for condensation and liquefaction to form a liquid, and then enter the low-boiling-point material storage tank 13 for storage.

[0046] Specifically, a first material transfer pump can be installed between the outlet of the flash tank 3 and the inlet of the neutralization reactor 4; a second material transfer pump can be installed between the outlet of the neutralization reactor 4 and the inlet of the crystallization vessel 5; and a third material transfer pump can be installed between the outlet of the crystallization vessel 5 and the separation device. Specifically, the first material transfer pump is used to pump the material remaining in the flash tank 3 after the removal of low-boiling substances to the neutralization reactor 4; the second material transfer pump is used to pump the material in the neutralization reactor 4 to the crystallization vessel 5; and the third material transfer pump is used to pump the material in the crystallization vessel 5 to the separation device.

[0047] In this embodiment, the separation device can be a centrifuge.

[0048] like Figure 1 As shown, the neutralization reactor 4 is provided with a first raw material inlet 15 for introducing methanol and a second raw material inlet 16 for introducing ammonia. The neutralization reactor 4 and the crystallization reactor 5 are respectively provided with tail gas outlets 17. The neutralization reactor 4 and the crystallization reactor 5 are respectively provided with stirring devices 18. The specific structure of the stirring device 18 is prior art well known to those skilled in the art, and will not be described in detail in this embodiment.

[0049] like Figure 1 As shown, a first jacket 19 is provided on the outer wall of the neutralization reactor 4, and a first heating chamber is provided between the first jacket 19 and the outer wall of the neutralization reactor 4. The first jacket 19 is provided with a first inlet medium port communicating with the first heating chamber and a first outlet medium port communicating with the first heating chamber. Specifically, injecting heating medium into the first heating chamber through the first inlet medium port can ensure the reaction temperature in the neutralization reactor 4.

[0050] The outer wall of the crystallization vessel 5 is provided with a second jacket 20, and a second heating chamber is provided between the second jacket 20 and the outer wall of the crystallization vessel 5. The second jacket 20 is provided with a second inlet medium port communicating with the second heating chamber and a second outlet medium port communicating with the second heating chamber. Specifically, injecting heating medium into the second heating chamber through the second inlet medium port can ensure the reaction temperature in the crystallization vessel 5.

[0051] In summary, under the suction action of the first raw material pump 1 and the second raw material pump 21, the aminonitrile in the first storage tank 6 and the hydrochloric acid in the second storage tank 7 are continuously fed into the mixing and preheating device in a certain molar ratio for thorough mixing and preheating. Then, they are continuously pumped to the tubular reactor 2 for hydrolysis. The material after hydrolysis directly enters the flash tank 3 from the outlet of the tubular reactor 2 for flash evaporation to remove low-boiling materials such as hydrogen chloride and water. After vaporization, the low-boiling materials flow from the gas phase outlet above the flash tank 3 to the low-boiling matter collection device for collection and storage. The remaining material after removing low-boiling materials in the flash tank 3 is continuously discharged from the outlet at the bottom of the flash tank 3 and continuously enters the neutralization reactor 4. Simultaneously, methanol and ammonia are continuously introduced into the neutralization reactor 4. The material injected into the neutralization reactor 4 mixes with the methanol and ammonia and reacts before directly entering the crystallization reactor 5 for glufosinate-ammonium salt crystallization. The material in the crystallization reactor 5 then enters the separation equipment from the outlet of the crystallization reactor 5 for separation to obtain solid products and mother liquor. The continuous hydrolysis and separation system for glufosinate, as described in this application, enables continuous hydrolysis and ammonium salting. Combined with continuous distillation in tubular reactor 2 and flash tank 3, continuous synthesis of glufosinate is achieved, improving the efficiency and yield of glufosinate synthesis. Furthermore, it increases reaction conversion rate, improves hydrogen chloride separation, shortens the process flow, significantly reduces the reaction cycle, lowers energy consumption, enhances process automation, and reduces labor load.

[0052] The specific embodiments described above further illustrate the technical problems, technical solutions, and beneficial effects of this utility model. It should be understood that the above descriptions are merely specific embodiments of this utility model and are not intended to limit this utility model. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this utility model should be included within the protection scope of this utility model.

Claims

1. A continuous hydrolysis and separation system for glufosinate, characterized in that, It includes a mixing and preheating device, a first raw material pump (1), a second raw material pump (21), a tubular reactor (2), a flash tank (3), a low-boiling-point collection device, a neutralization reactor (4), a crystallization reactor (5), a separation device, a first storage tank (6) for storing aminonitrile and a second storage tank (7) for storing hydrochloric acid; The inlet of the first raw material pump (1) is connected to the first storage tank (6); The inlet of the second raw material pump (21) is connected to the second storage tank (7); The outlet of the first raw material pump (1) and the outlet of the second raw material pump (21) are respectively connected to the inlet of the mixing preheating device; The outlet of the mixing preheating device is connected to the inlet of the tubular reactor (2); The outlet of the tubular reactor (2) is connected to the inlet of the flash tank (3); The outlet at the bottom of the flash tank (3) is connected to the inlet of the neutralization reactor (4); The gas phase outlet of the flash tank (3) is connected to the low-boiling-point collection device; The outlet of the neutralization reactor (4) is connected to the inlet of the crystallization reactor (5); The outlet of the crystallization vessel (5) is connected to the separation equipment.

2. The glufosinate-ammonium continuous hydrolysis and separation system according to claim 1, characterized in that, The mixing and preheating device includes a static mixer (8) and a preheater (9); wherein the outlet of the first raw material pump (1) and the outlet of the second raw material pump (21) are respectively connected to the inlet of the static mixer (8), the outlet of the static mixer (8) is connected to the inlet of the preheater (9), and the outlet of the preheater (9) is connected to the inlet of the tubular reactor (2).

3. The continuous hydrolysis and separation system for glufosinate according to claim 2, characterized in that, A first flow meter (10) is connected between the outlet of the first raw material pump (1) and the inlet of the static mixer (8); A second flow meter (11) is connected between the outlet of the second raw material pump (21) and the inlet of the static mixer (8).

4. The continuous hydrolysis and separation system for glufosinate according to claim 1, characterized in that, The low-boiling-point collection device includes a condenser (12) and a low-boiling-point storage tank (13); The gas phase outlet of the flash tank (3) is connected to the inlet of the condenser (12); The outlet of the condenser (12) is connected to the low-boiling-point storage tank (13).

5. The continuous hydrolysis and separation system for glufosinate according to claim 1, characterized in that, A first material conveying pump is provided between the outlet of the flash tank (3) and the inlet of the neutralization reactor (4), a second material conveying pump is provided between the outlet of the neutralization reactor (4) and the inlet of the crystallization reactor (5), and a third material conveying pump is provided between the outlet of the crystallization reactor (5) and the separation equipment.

6. The continuous hydrolysis and separation system for glufosinate according to claim 1, characterized in that, The separation device is a centrifuge.

7. The continuous hydrolysis and separation system for glufosinate according to claim 1, characterized in that, The neutralization reactor (4) is provided with a first raw material inlet (15) for introducing methanol and a second raw material inlet (16) for introducing ammonia.

8. The continuous hydrolysis and separation system for glufosinate according to claim 1, characterized in that, The neutralization reactor (4) and the crystallization reactor (5) are respectively provided with exhaust gas outlets (17).

9. The continuous hydrolysis and separation system for glufosinate according to claim 1, characterized in that, The neutralization reactor (4) and the crystallization reactor (5) are respectively equipped with stirring devices (18).

10. The continuous hydrolysis and separation system for glufosinate according to claim 1, characterized in that, The neutralization reactor (4) is provided with a first jacket (19) on its outer wall. A first heating chamber is provided between the first jacket (19) and the outer wall of the neutralization reactor (4). The first jacket (19) is provided with a first inlet medium port communicating with the first heating chamber and a first outlet medium port communicating with the first heating chamber. The crystallization vessel (5) is provided with a second jacket (20) on its outer wall. A second heating chamber is provided between the second jacket (20) and the outer wall of the crystallization vessel (5). The second jacket (20) is provided with a second inlet medium port communicating with the second heating chamber and a second outlet medium port communicating with the second heating chamber.

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