A system for preparing glufosinate
By simplifying the structure and process of the glufosinate preparation system and adopting nitrogen protection and vacuum deammoniation treatment, the problem of high equipment investment in the existing technology has been solved, achieving cost reduction and efficiency improvement.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- FUHUA TONGDA CHEM CO LTD
- Filing Date
- 2025-06-13
- Publication Date
- 2026-07-31
AI Technical Summary
Existing glufosinate preparation systems are complex in structure and have long process flows, resulting in high equipment investment costs.
A glufosinate preparation system was designed, comprising a phosphonation reactor, a cyanamide reactor, a hydrolysis reactor, a mixing tank, a transfer pump, a vacuum pump, and a condenser. By using nitrogen protection and vacuum deammoniation treatment, the process flow is simplified and energy consumption is reduced.
It reduced equipment investment costs, reduced energy consumption, increased the yield of glufosinate, and reduced impurity generation and waste treatment.
Smart Images
Figure CN224573742U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to a glufosinate preparation system. Background Technology
[0002] Currently, glufosinate is a phosphonic acid herbicide that inhibits glutamine synthase in the plant nitrogen metabolism pathway, thereby interfering with plant metabolism and ultimately causing plant death. There are many chemical synthesis routes for glufosinate, and regardless of the route used, a glufosinate preparation system is required. For example, Chinese patent application CN202110729193.4 discloses a glufosinate preparation system; however, this system has a complex structure and a long process flow, resulting in high equipment costs. 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 glufosinate preparation system with a simpler structure and shorter process flow, thereby reducing equipment investment costs.
[0004] To solve the above-mentioned technical problems, the technical solution of this utility model is: a glufosinate preparation system, including a phosphine reaction vessel, a cyanamide reaction vessel, a hydrolysis reaction vessel, a mixing tank, a first delivery pump, a second delivery pump, a third delivery pump, a first vacuum pump, a first condenser, and a receiving tank;
[0005] The phosphating reactor is equipped with a diethyl ester inlet and a first nitrogen inlet.
[0006] The cyanammoniation reactor is equipped with an ammonia inlet and a second nitrogen inlet.
[0007] The hydrolysis reactor is equipped with a hydrochloric acid inlet.
[0008] The mixing tank is used to store a mixture of acrolein and acetic acid. The inlet of the first delivery pump is connected to the outlet of the mixing tank, and the outlet of the first delivery pump is connected to the phosphating reactor.
[0009] The inlet of the second delivery pump is connected to the outlet of the phosphating reactor, and the outlet of the second delivery pump is connected to the cyanamide reactor.
[0010] The inlet of the third pump is connected to the outlet of the cyanamide reactor, and the outlet of the third pump is connected to the hydrolysis reactor.
[0011] The first vacuum pump is connected to the cyanamide reaction vessel and is used to evacuate the cyanamide reaction vessel. A first valve is connected between the first vacuum pump and the cyanamide reaction vessel.
[0012] The inlet of the first condenser is connected to the gas phase outlet of the hydrolysis reactor, and the reflux port of the first condenser is connected to the receiving tank.
[0013] Furthermore, the glufosinate preparation system also includes a second vacuum pump, which is connected to the phosphating reactor and used to evacuate the phosphating reactor. A second valve is connected between the second vacuum pump and the phosphating reactor.
[0014] Furthermore, the glufosinate preparation system also includes a second condenser and a third condenser;
[0015] The inlet and reflux port of the second condenser are both connected to the gas phase outlet of the phosphating reactor;
[0016] The inlet and reflux port of the third condenser are both connected to the gas phase outlet of the cyanamide reactor.
[0017] Furthermore, control valves are connected to the gas phase outlets of the phosphating reactor, the cyanamide reactor, and the hydrolysis reactor, respectively.
[0018] Furthermore, the diethyl ester inlet, the first nitrogen inlet, the ammonia inlet, the second nitrogen inlet, and the hydrochloric acid inlet are each connected to a feed valve.
[0019] Furthermore, conveying valves are respectively connected between the inlet of the first conveying pump and the outlet of the mixing tank, between the outlet of the first conveying pump and the phosphating reactor, between the inlet of the second conveying pump and the outlet of the phosphating reactor, between the outlet of the second conveying pump and the cyanamide reactor, between the inlet of the third conveying pump and the outlet of the cyanamide reactor, and between the outlet of the third conveying pump and the hydrolysis reactor.
[0020] Furthermore, the glufosinate preparation system also includes a first discharge pump connected to the discharge port of the hydrolysis reactor and a second discharge pump connected to the discharge port of the receiving tank.
[0021] Furthermore, discharge valves are respectively connected between the first discharge pump and the discharge port of the hydrolysis reactor, and between the second discharge pump and the discharge port of the receiving tank.
[0022] Furthermore, the phosphating reactor is connected to a first jacket, the first jacket is provided with a first inner cavity, the first jacket is provided with a first inlet medium port communicating with the first inner cavity and a first outlet medium port communicating with the first inner cavity.
[0023] The cyanamide reaction vessel is connected to a second jacket, which has a second inner cavity. The second jacket has a second inlet medium port communicating with the second inner cavity and a second outlet medium port communicating with the second inner cavity.
[0024] The hydrolysis reactor is connected to a third jacket, which has a third inner cavity. The third jacket has a third inlet medium port communicating with the third inner cavity and a third outlet medium port communicating with the third inner cavity.
[0025] Furthermore, temperature sensors and pressure sensors are respectively connected to the phosphating reactor, the cyanamide reactor, and the hydrolysis reactor;
[0026] The phosphating reactor, the cyanamide reactor, and the hydrolysis reactor are each equipped with a stirring device.
[0027] After adopting the above technical solution, nitrogen gas can be injected into the phosphating reactor through the first nitrogen inlet to replace the air in the phosphating reactor and fill it with nitrogen. Diethyl methylphosphite is added to the nitrogen-purged phosphating reactor through the diethyl ester inlet. The mixture of acrolein and acetic acid in the mixing tank is pumped to the phosphating reactor through the first transfer pump, allowing the diethyl methylphosphite, acrolein, and acetic acid in the phosphating reactor to react under nitrogen protection. Nitrogen gas can be injected into the cyanamation reactor through the second nitrogen inlet to replace the air in the cyanamation reactor and fill it with nitrogen. An ammonia solution containing sodium cyanide and ammonium chloride is injected into the nitrogen-purged cyanamation reactor through the ammonia inlet. The reacted material in the phosphating reactor is pumped to the cyanamation reactor by the second transfer pump for further reaction. After the material in the cyanamation reactor has reacted under nitrogen protection, the cyanamation reactor is evacuated by the first vacuum pump to remove ammonia. Then, nitrogen gas is injected into the cyanamation reactor through the second nitrogen inlet to break the vacuum. Then, the third pump pumps the reacted material from the cyanamide reactor to the hydrolysis reactor. Hydrochloric acid is injected into the hydrolysis reactor through the hydrochloric acid inlet to heat the material in the hydrolysis reactor to remove low-boiling-point substances. The low-boiling-point substances in the material in the hydrolysis reactor will vaporize after heating. The vaporized low-boiling-point substances will enter the first condenser from the gas phase outlet of the hydrolysis reactor and, after condensation and liquefaction, will enter the receiving tank for storage. After removing the low-boiling-point substances, the material in the hydrolysis reactor yields glufosinate hydrolysate. The glufosinate preparation system of this embodiment has a simpler structure and shorter process flow, thus reducing equipment investment costs and overall system energy consumption. Furthermore, using the glufosinate preparation system of this embodiment can reduce preparation costs, increase yield, and reduce impurity generation and waste treatment. Attached Figure Description
[0028] Figure 1 This is a process flow diagram of the glufosinate preparation system of this utility model;
[0029] In the diagram: 1. Phosphating reactor; 2. Cyanamide reactor; 3. Hydrolysis reactor; 4. Mixing tank; 5. First transfer pump; 6. Second transfer pump; 7. Third transfer pump; 8. First vacuum pump; 9. First condenser; 10. Receiving tank; 11. Diethyl ester inlet; 12. First nitrogen inlet; 13. Ammonia inlet; 14. Second nitrogen inlet; 15. Hydrochloric acid inlet; 16. First valve; 17. Second vacuum pump; 18. Second valve; 19. Second condenser; 20. Third condenser; 21. Control valve; 22. First discharge pump; 23. Second discharge pump; 24. First jacket; 25. Second jacket; 26. Third jacket. Detailed Implementation
[0030] 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.
[0031] like Figure 1 As shown, a glufosinate preparation system includes a phosphonation reactor 1, a cyanamide reactor 2, a hydrolysis reactor 3, a mixing tank 4, a first transfer pump 5, a second transfer pump 6, a third transfer pump 7, a first vacuum pump 8, a first condenser 9, and a receiving tank 10.
[0032] The phosphating reactor 1 is equipped with a diethyl ester inlet 11 and a first nitrogen inlet 12.
[0033] The cyanammoniation reactor 2 is equipped with an ammonia inlet 13 and a second nitrogen inlet 14.
[0034] The hydrolysis reactor 3 is equipped with a hydrochloric acid inlet 15;
[0035] The mixing tank 4 is used to store a mixture of acrolein and acetic acid. The inlet of the first delivery pump 5 is connected to the outlet of the mixing tank 4, and the outlet of the first delivery pump 5 is connected to the phosphating reactor 1.
[0036] The inlet of the second delivery pump 6 is connected to the outlet of the phosphating reactor 1, and the outlet of the second delivery pump 6 is connected to the cyanamide reactor 2.
[0037] The inlet of the third delivery pump 7 is connected to the outlet of the cyanamide reaction vessel 2, and the outlet of the third delivery pump 7 is connected to the hydrolysis reaction vessel 3.
[0038] The first vacuum pump 8 is connected to the cyanamide reaction vessel 2 and is used to evacuate the cyanamide reaction vessel 2. A first valve 16 is connected between the first vacuum pump 8 and the cyanamide reaction vessel 2.
[0039] The inlet of the first condenser 9 is connected to the gas phase outlet of the hydrolysis reactor 3, and the reflux port of the first condenser 9 is connected to the receiving tank 10.
[0040] Specifically, nitrogen gas can be injected into the phosphating reactor 1 through the first nitrogen inlet 12 to displace the air in the phosphating reactor 1 and fill it with nitrogen. Diethyl methylphosphite is added to the nitrogen-displaced phosphating reactor 1 through the diethyl ester inlet 11. The mixture of acrolein and acetic acid in the mixing tank 4 is pumped to the phosphating reactor 1 by the first transfer pump 5, so that the diethyl methylphosphite, acrolein, and acetic acid in the phosphating reactor 1 react under nitrogen protection. Nitrogen gas can be injected into the cyanamation reactor 2 through the second nitrogen inlet 14 to replace the air in the cyanamation reactor 2 and fill the cyanamation reactor 2 with nitrogen gas. An ammonia solution containing sodium cyanide and ammonium chloride is injected into the nitrogen-purged cyanamation reactor 2 through the ammonia inlet 13. The reacted material in the phosphine reaction reactor 1 is pumped to the cyanamation reactor 2 for reaction by the second transfer pump 6. After the material in the cyanamation reactor 2 has reacted under nitrogen protection, the cyanamation reactor 2 is evacuated by the first vacuum pump 8 to perform vacuum deammoniation. Then, nitrogen gas is injected into the cyanamation reactor 2 through the second nitrogen inlet 14 to break the vacuum. Then, the third transfer pump 7 pumps the reacted material from the cyanamide reaction vessel 2 to the hydrolysis reaction vessel 3. Hydrochloric acid is injected into the hydrolysis reaction vessel 3 through the hydrochloric acid inlet 15 to heat the material in the hydrolysis reaction vessel 3 to remove low-boiling-point substances. The low-boiling-point substances in the material in the hydrolysis reaction vessel 3 will vaporize after heating. The vaporized low-boiling-point substances will enter the first condenser 9 from the gas phase outlet of the hydrolysis reaction vessel 3 and be condensed and liquefied before entering the receiving tank 10 for storage. After the low-boiling-point substances are removed from the material in the hydrolysis reaction vessel 3, glufosinate hydrolysate is obtained. The glufosinate preparation system of this application embodiment has a simpler structure and a shorter process flow, thus reducing the cost of equipment investment and the energy consumption of the entire system. In addition, using the glufosinate preparation system of this application embodiment to prepare glufosinate can also reduce the preparation cost, increase the yield, and reduce the generation of impurities and the treatment of waste.
[0041] like Figure 1As shown, the glufosinate preparation system may further include a second vacuum pump 17, which is connected to the phosphine reaction vessel 1 and used to evacuate the phosphine reaction vessel 1. A second valve 18 is connected between the second vacuum pump 17 and the phosphine reaction vessel 1. Specifically, while injecting nitrogen into the cyanamation reaction vessel 2 through the second nitrogen inlet 14, the first valve 16 can be opened and the original air in the cyanamation reaction vessel 2 can be extracted by the first vacuum pump 8, thereby allowing the air in the cyanamation reaction vessel 2 to be replaced more quickly by nitrogen. Similarly, while injecting nitrogen into the phosphine reaction vessel 1 through the first nitrogen inlet 12, the second valve 18 can be opened and the original air in the phosphine reaction vessel 1 can be extracted by the second vacuum pump 17, thereby allowing the air in the phosphine reaction vessel 1 to be replaced more quickly by nitrogen.
[0042] like Figure 1 As shown, the glufosinate preparation system may further include a second condenser 19 and a third condenser 20;
[0043] The inlet and the return port of the second condenser 19 are both connected to the gas phase outlet of the phosphating reactor 1, so that the gas phase in the phosphating reactor 1 flows into the second condenser 19, is condensed and liquefied, and then flows back to the phosphating reactor 1.
[0044] The inlet and reflux port of the third condenser 20 are both connected to the gas phase outlet of the cyanamide reaction vessel 2, so that the gas phase in the cyanamide reaction vessel 2 flows into the third condenser 20, is condensed and liquefied, and then flows back to the cyanamide reaction vessel 2.
[0045] like Figure 1 As shown, the gas phase outlets of the phosphating reactor 1, the cyanamide reactor 2, and the hydrolysis reactor 3 can each be connected to a control valve 21.
[0046] like Figure 1 As shown, the diethyl ester inlet 11, the first nitrogen inlet 12, the ammonia inlet 13, the second nitrogen inlet 14, and the hydrochloric acid inlet 15 can each be connected to a feed valve.
[0047] like Figure 1As shown, conveying valves can be connected between the inlet of the first conveying pump 5 and the outlet of the mixing tank 4, between the outlet of the first conveying pump 5 and the phosphating reactor 1, between the inlet of the second conveying pump 6 and the outlet of the phosphating reactor 1, between the outlet of the second conveying pump 6 and the cyanamide reactor 2, between the inlet of the third conveying pump 7 and the outlet of the cyanamide reactor 2, and between the outlet of the third conveying pump 7 and the hydrolysis reactor 3.
[0048] like Figure 1 As shown, the glufosinate preparation system may further include a first discharge pump 22 connected to the discharge port of the hydrolysis reactor 3 and a second discharge pump 23 connected to the discharge port of the receiving tank 10; wherein, discharge valves are respectively connected between the first discharge pump 22 and the discharge port of the hydrolysis reactor 3 and between the second discharge pump 23 and the discharge port of the receiving tank 10.
[0049] like Figure 1 As shown, the phosphating reactor 1 is connected to a first jacket 24, the first jacket 24 is provided with a first inner cavity, the first jacket 24 is provided with a first inlet medium port communicating with the first inner cavity and a first outlet medium port communicating with the first inner cavity; specifically, the heat-conducting medium can flow into the first inner cavity from the first inlet medium port and then flow out from the first outlet medium port in order to heat the material in the phosphating reactor 1.
[0050] The cyanamide reaction vessel 2 is connected to a second jacket 25, which has a second inner cavity. The second jacket 25 has a second inlet medium port communicating with the second inner cavity and a second outlet medium port communicating with the second inner cavity. Specifically, the heat-conducting medium can flow into the second inner cavity from the second inlet medium port and then flow out from the second outlet medium port in order to heat the material in the cyanamide reaction vessel 2.
[0051] The hydrolysis reactor 3 is connected to a third jacket 26, which has a third inner cavity. The third jacket 26 has a third inlet and a third outlet that communicate with the third inner cavity. Specifically, the heat-conducting medium can flow into the third inner cavity from the third inlet and then flow out from the third outlet to heat the material in the hydrolysis reactor 3.
[0052] like Figure 1 As shown, temperature sensors and pressure sensors are respectively connected to the phosphating reactor 1, the cyanamide reactor 2, and the hydrolysis reactor 3;
[0053] The phosphating reactor 1, the cyanamide reactor 2, and the hydrolysis reactor 3 are each equipped with a stirring device; wherein, the specific structure of the stirring device is prior art well known to those skilled in the art, and will not be described in detail in this embodiment.
[0054] In summary, nitrogen gas can be injected into the phosphating reactor 1 through the first nitrogen inlet 12 to displace the air in the phosphating reactor 1, thereby filling the phosphating reactor 1 with nitrogen. Diethyl methylphosphite is added to the nitrogen-displaced phosphating reactor 1 through the diethyl ester inlet 11. The mixture of acrolein and acetic acid in the mixing tank 4 is pumped to the phosphating reactor 1 by the first transfer pump 5, so that the diethyl methylphosphite, acrolein, and acetic acid in the phosphating reactor 1 react under nitrogen protection. Nitrogen gas can be injected into the cyanamation reactor 2 through the second nitrogen inlet 14 to replace the air in the cyanamation reactor 2 and fill the cyanamation reactor 2 with nitrogen gas. An ammonia solution containing sodium cyanide and ammonium chloride is injected into the nitrogen-purged cyanamation reactor 2 through the ammonia inlet 13. The reacted material in the phosphine reaction reactor 1 is pumped to the cyanamation reactor 2 for reaction by the second transfer pump 6. After the material in the cyanamation reactor 2 has reacted under nitrogen protection, the cyanamation reactor 2 is evacuated by the first vacuum pump 8 to perform vacuum deammoniation. Then, nitrogen gas is injected into the cyanamation reactor 2 through the second nitrogen inlet 14 to break the vacuum. Then, the third transfer pump 7 pumps the reacted material from the cyanamide reaction vessel 2 to the hydrolysis reaction vessel 3. Hydrochloric acid is injected into the hydrolysis reaction vessel 3 through the hydrochloric acid inlet 15 to heat the material in the hydrolysis reaction vessel 3 to remove low-boiling-point substances. The low-boiling-point substances in the material in the hydrolysis reaction vessel 3 will vaporize after heating. The vaporized low-boiling-point substances will enter the first condenser 9 from the gas phase outlet of the hydrolysis reaction vessel 3 and be condensed and liquefied before entering the receiving tank 10 for storage. After the low-boiling-point substances are removed from the material in the hydrolysis reaction vessel 3, glufosinate hydrolysate is obtained. The glufosinate preparation system of this application embodiment has a simpler structure and a shorter process flow, thus reducing the cost of equipment investment and the energy consumption of the entire system. In addition, using the glufosinate preparation system of this application embodiment to prepare glufosinate can also reduce the preparation cost, increase the yield, and reduce the generation of impurities and the treatment of waste.
[0055] 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 system for preparing glufosinate-ammonium, characterized by It includes a phosphating reactor (1), a cyanamide reactor (2), a hydrolysis reactor (3), a mixing tank (4), a first transfer pump (5), a second transfer pump (6), a third transfer pump (7), a first vacuum pump (8), a first condenser (9), and a receiving tank (10); The phosphating reactor (1) is provided with a diethyl ester inlet (11) and a first nitrogen inlet (12); The cyanamide reaction vessel (2) is equipped with an ammonia water inlet (13) and a second nitrogen gas inlet (14); The hydrolysis reactor (3) is equipped with a hydrochloric acid inlet (15); The mixing tank (4) is used to store a mixture of acrolein and acetic acid. The inlet of the first delivery pump (5) is connected to the outlet of the mixing tank (4), and the outlet of the first delivery pump (5) is connected to the phosphating reactor (1). The inlet of the second delivery pump (6) is connected to the outlet of the phosphating reactor (1), and the outlet of the second delivery pump (6) is connected to the cyanamide reactor (2). The inlet of the third pump (7) is connected to the outlet of the cyanamide reaction vessel (2), and the outlet of the third pump (7) is connected to the hydrolysis reaction vessel (3). The first vacuum pump (8) is connected to the cyanamide reaction vessel (2) and is used to evacuate the cyanamide reaction vessel (2). A first valve (16) is connected between the first vacuum pump (8) and the cyanamide reaction vessel (2). The inlet of the first condenser (9) is connected to the gas phase outlet of the hydrolysis reactor (3), and the reflux port of the first condenser (9) is connected to the receiving tank (10).
2. The glufosinate preparation system according to claim 1, characterized by It also includes a second vacuum pump (17), which is connected to the phosphating reactor (1) and used to evacuate the phosphating reactor (1). A second valve (18) is connected between the second vacuum pump (17) and the phosphating reactor (1).
3. The glufosinate production system according to claim 1, characterized by It also includes a second condenser (19) and a third condenser (20); The inlet of the second condenser (19) and the reflux port of the second condenser (19) are both connected to the gas phase outlet of the phosphating reactor (1); The inlet of the third condenser (20) and the reflux port of the third condenser (20) are both connected to the gas phase outlet of the cyanamide reaction vessel (2).
4. The glufosinate production system according to claim 3, characterized in that The gas phase outlets of the phosphating reactor (1), the cyanamide reactor (2), and the hydrolysis reactor (3) are respectively connected to control valves (21).
5. The glufosinate preparation system according to claim 1, characterized by The diethyl ester inlet (11), the first nitrogen inlet (12), the ammonia inlet (13), the second nitrogen inlet (14), and the hydrochloric acid inlet (15) are each connected to a feed valve.
6. The glufosinate preparation system according to claim 1, characterized by A conveying valve is connected between the inlet of the first conveying pump (5) and the outlet of the mixing tank (4), between the outlet of the first conveying pump (5) and the phosphating reactor (1), between the inlet of the second conveying pump (6) and the outlet of the phosphating reactor (1), between the outlet of the second conveying pump (6) and the cyanamide reactor (2), between the inlet of the third conveying pump (7) and the outlet of the cyanamide reactor (2), and between the outlet of the third conveying pump (7) and the hydrolysis reactor (3).
7. The glufosinate preparation system according to claim 1, characterized by It also includes a first discharge pump (22) connected to the discharge port of the hydrolysis reactor (3) and a second discharge pump (23) connected to the discharge port of the receiving tank (10).
8. The glufosinate production system according to claim 7, characterized by Discharge valves are connected between the first discharge pump (22) and the discharge port of the hydrolysis reactor (3) and between the second discharge pump (23) and the discharge port of the receiving tank (10).
9. The glufosinate preparation system according to claim 1, characterized in that, The phosphating reactor (1) is connected to a first jacket (24), the first jacket (24) is provided with a first inner cavity, the first jacket (24) is provided with a first inlet medium port communicating with the first inner cavity and a first outlet medium port communicating with the first inner cavity; The cyanamide reaction vessel (2) is connected to a second jacket (25), the second jacket (25) is provided with a second inner cavity, the second jacket (25) is provided with a second inlet medium port communicating with the second inner cavity and a second outlet medium port communicating with the second inner cavity; The hydrolysis reactor (3) is connected to a third jacket (26), which has a third inner cavity. The third jacket (26) is provided with a third inlet medium port communicating with the third inner cavity and a third outlet medium port communicating with the third inner cavity.
10. The glufosinate preparation system according to claim 1, characterized in that, Temperature sensors and pressure sensors are respectively connected to the phosphating reactor (1), the cyanamide reactor (2), and the hydrolysis reactor (3); The phosphating reactor (1), the cyanamide reactor (2), and the hydrolysis reactor (3) are each equipped with a stirring device.