A purification system for refined glufosinate-ammonium

Abstract

The utility model discloses a purification system for refined glufosinate ammonium, belonging to the technical field of refined glufosinate ammonium production, wherein refined glufosinate ammonium solution flows into a concentration kettle through a refined glufosinate ammonium solution inlet pipe, after the refined glufosinate ammonium solution is concentrated to a certain degree, methanol is added into the concentration kettle through a methanol inlet pipe twice, after the methanol is added dropwise, the mixed solution is transferred into an ultrasonic kettle through a first liquid outlet pipe, and the first crystallization is directly insulated in the concentration kettle, after the first crystallization is completed, the system is cooled, and the system is transferred to a centrifuge through a second material outlet pipe for centrifugal separation to obtain refined glufosinate ammonium hydrate solid, refined glufosinate ammonium hydrate is added into the ultrasonic kettle through a silo and a screw conveyor, and then anhydrous methanol is added through a second methanol inlet pipe, an ultrasonic device is turned on, and after ultrasonic treatment for a period of time, the temperature is lowered and centrifuged, and the mother liquor is partially used in the ultrasonic step, and the filter cake is dried to obtain a refined glufosinate ammonium product. The refined glufosinate ammonium product obtained by the utility model has high purity.

Description

Technical Field

[0001] The utility model belongs to the technical field of refined glufosinate-ammonium production, and in particular relates to a purification system for refined glufosinate-ammonium. Background Art

[0002] In the production process of refined glufosinate ammonium, generally speaking, a refined glufosinate ammonium aqueous solution is obtained, and its concentration ranges from 10% to 20%. The aqueous solution contains not only refined glufosinate ammonium, but also acids or other amino acid compounds and impurities. Usually, most companies adjust the pH of the refined glufosinate ammonium aqueous solution to the required range and increase its concentration to 30% to 50%, and then sell it directly; however, the packaging and transportation costs of selling refined glufosinate ammonium aqueous solution are relatively high, and some downstream customers require refined glufosinate ammonium raw powder.

[0003] Since the components in the refined glufosinate ammonium aqueous solution are relatively complex, the crystallization effect of refined glufosinate ammonium is not ideal and the impurity content in the original powder is relatively high. Moreover, since refined glufosinate ammonium is easy to form crystalline hydrates, the traditional refined glufosinate ammonium crystallization process is prone to high water content in the original powder, reduced crystallization rate, and compaction of the crystallization system. Utility Model Content

[0004] The utility model aims to solve the problems of the prior art and provides a purification system for refined glufosinate ammonium. Refined glufosinate ammonium solution flows into a concentration kettle through a refined glufosinate ammonium solution inlet pipe. After the refined glufosinate ammonium solution is concentrated to a certain degree, methanol is added to the concentration kettle through a methanol inlet pipe twice. After the methanol is added dropwise, the mixed solution is transferred to an ultrasonic kettle through a first liquid outlet pipe, and the first crystallization is directly kept warm in the concentration kettle. After the first crystallization is completed, the mixture is cooled and transferred to a centrifuge through a second discharge pipe for centrifugal separation to obtain refined glufosinate ammonium hydrate solid. Refined glufosinate ammonium hydrate is added to the ultrasonic kettle through a silo and a screw conveyor, and then anhydrous methanol is added through a second methanol inlet pipe, an ultrasonic device is turned on, and the temperature is lowered and centrifuged after ultrasonic treatment for a period of time. The mother liquor is partially used in the ultrasonic step, and the filter cake is dried to obtain a refined glufosinate ammonium product. The refined glufosinate ammonium product obtained by the utility model has high purity.

[0005] The utility model is realized by the following technical solutions:

[0006] A purification system for refined glufosinate ammonium comprises a concentration kettle and an ultrasonic kettle. The concentration kettle is provided with a first methanol inlet pipe, a refined glufosinate ammonium solution inlet pipe, a first liquid outlet pipe and a first gas outlet pipe. The concentration kettle is connected to the ultrasonic kettle via the first liquid outlet pipe. The ultrasonic kettle is provided with a second methanol inlet pipe, an ultrasonic device, a second liquid outlet pipe and a second gas outlet pipe.

[0007] Preferably, the first methanol inlet pipe, the refined glufosinate-ammonium solution inlet pipe and the second methanol inlet pipe are all provided with flow meters and flow regulating valves.

[0008] Preferably, a first material transfer pump is provided on the first liquid outlet pipe.

[0009] Preferably, a heat exchanger is provided on the first air outlet pipe, a liquid outlet end of the heat exchanger is connected to a concentrated water receiving tank, and a second material transfer pump is provided at the lower end of the concentrated water receiving tank.

[0010] Preferably, the concentration kettle is provided with a third gas outlet pipe, the third gas outlet pipe is provided with a vacuum pump, and the first gas outlet pipe is connected to the third gas outlet pipe through a connecting pipe.

[0011] Preferably, the concentration kettle is also provided with an air inlet pipe.

[0012] Preferably, the concentration kettle is provided with a first heat exchange jacket, on which a first heat exchange medium inlet pipe and a first heat exchange medium outlet pipe are provided; the ultrasonic kettle is provided with a second heat exchange jacket, on which a second heat exchange jacket is provided with a second heat exchange medium inlet pipe and a second heat exchange medium outlet pipe.

[0013] Preferably, the concentration kettle is provided with a first pressure gauge and a first temperature sensor.

[0014] Preferably, the ultrasonic reactor is provided with a second pressure gauge and a second temperature sensor.

[0015] Preferably, the ultrasonic kettle is provided with a first feed pipe; the first feed pipe is connected to a silo, and the silo is provided with a screw conveyor and a second feed pipe.

[0016] Compared with the prior art, the utility model has the following advantages and beneficial effects:

[0017] 1. The utility model provides a purification system for refined glufosinate ammonium, wherein the refined glufosinate ammonium solution flows into the concentration kettle through the refined glufosinate ammonium solution inlet pipe, and after the refined glufosinate ammonium solution is concentrated to a certain extent, methanol is added to the concentration kettle through the methanol inlet pipe twice, and after the methanol is added dropwise, the mixed solution is transferred to the ultrasonic kettle through the first liquid outlet pipe, and the first crystallization is directly kept warm in the concentration kettle, and after the first crystallization is completed, it is cooled and transferred to the centrifuge through the second discharge pipe to obtain the refined glufosinate ammonium hydrate solid, and the refined glufosinate ammonium hydrate is added to the ultrasonic kettle through the silo and the screw conveyor, and then anhydrous methanol is added through the second methanol inlet pipe, and the ultrasonic device is turned on. After ultrasonic treatment for a period of time, the temperature is lowered and centrifuged, and the mother liquor is partially used in the ultrasonic step, and the filter cake is dried to obtain the refined glufosinate ammonium product. The refined glufosinate ammonium product obtained by the utility model has high purity.

[0018] 2. The utility model provides a purification system for refined glufosinate ammonium. Flow meters and flow regulating valves arranged on the first methanol inlet pipe, the refined glufosinate ammonium solution inlet pipe and the second methanol inlet pipe ensure that the refined glufosinate ammonium solution is accurately added to the concentration kettle and the methanol is accurately added to the concentration kettle and the ultrasonic kettle.

[0019] 3. The utility model provides a purification system for refined glufosinate ammonium. The heat exchanger is arranged so that the volatilized methanol is cooled by the heat exchanger and then flows into the concentrated water receiving tank, so that the methanol is recovered and utilized.

[0020] 4. The utility model provides a purification system for refined glufosinate ammonium, in which a vacuum pump, an air inlet pipe and a first pressure gauge are arranged to balance the pressure in the concentration kettle.

[0021] 5. The utility model provides a purification system for refined glufosinate ammonium, wherein a heat exchange jacket, a second heat exchange jacket, a first temperature sensor and a second temperature sensor are arranged to facilitate adjusting the temperature in the concentration kettle and the ultrasonic kettle to the desired temperature. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 It is a structural schematic diagram of the utility model;

[0023] Wherein: 1. first methanol inlet pipe; 2. air inlet pipe; 3. refined glufosinate-ammonium solution inlet pipe; 4. first temperature sensor; 5. concentration kettle; 6. first pressure gauge; 7. heat exchanger; 8. first material transfer pump; 9. ultrasonic kettle; 10. ultrasonic device; 11. vacuum pump; 12. screw conveyor; 13. silo; 14. concentrated water receiving tank; 15. second material transfer pump; 16. second temperature sensor; 17. second pressure gauge; 18. first liquid outlet pipe; 19. First air outlet pipe; 20. First heat exchange jacket; 201. First heat exchange medium inlet pipe; 202. First heat exchange medium outlet pipe; 21. Second methanol inlet pipe; 22. Second heat exchange jacket; 221. Second heat exchange medium inlet pipe; 222. Second heat exchange medium outlet pipe; 23. Flow meter; 24. Flow regulating valve; 25. Third air outlet pipe; 26. Second air outlet pipe; 27. Second liquid outlet pipe; 28. First feed pipe; 29. ​​Second feed pipe. DETAILED DESCRIPTION

[0024] The present invention is further described in detail below in conjunction with the embodiments, but the implementation manner of the present invention is not limited thereto.

[0025] Example 1

[0026] like Figure 1 As shown, this embodiment provides a purification system for refined glufosinate ammonium, including a concentration kettle 5 and an ultrasonic kettle 9, wherein the concentration kettle 5 is provided with a first methanol inlet pipe 1, a refined glufosinate ammonium solution inlet pipe 3, a first liquid outlet pipe 18 and a first gas outlet pipe 19, the concentration kettle 5 is connected to the ultrasonic kettle 9 via the first liquid outlet pipe 18, and the ultrasonic kettle 9 is provided with a second methanol inlet pipe 21, an ultrasonic device 10, a second liquid outlet pipe 27 and a second gas outlet pipe 26.

[0027] Example 2

[0028] The difference between this embodiment and embodiment 1 is that the first methanol inlet pipe 1, the refined glufosinate ammonium solution inlet pipe 3 and the second methanol inlet pipe 21 are all provided with a flow meter 23 and a flow regulating valve 24.

[0029] Wherein, the first liquid outlet pipe 18 is provided with a first material transfer pump 8 .

[0030] The first outlet pipe 19 is provided with a heat exchanger 7, the liquid outlet end of the heat exchanger 7 is connected to the concentrated water receiving tank 14, and the lower end of the concentrated water receiving tank 14 is provided with a second transfer pump 15. A third medium feed pipe and a third medium discharge pipe are provided on the heat exchanger 7. The first outlet pipe 19 and the second outlet pipe 26 are connected to the exhaust main pipe.

[0031] The concentration kettle 5 is provided with a third gas outlet pipe 25 , the third gas outlet pipe 25 is provided with a vacuum pump 11 , and the first gas outlet pipe 19 is connected to the third gas outlet pipe 25 via a connecting pipe.

[0032] Wherein, the concentration kettle 5 is also provided with an air inlet pipe 2 .

[0033] Among them, the concentration kettle 5 is provided with a first heat exchange jacket 20, and the first heat exchange jacket 20 is provided with a first heat exchange medium inlet pipe 201 and a first heat exchange medium outlet pipe 202; the ultrasonic kettle 9 is provided with a second heat exchange jacket 22, and the second heat exchange jacket 22 is provided with a second heat exchange medium inlet pipe 221 and a second heat exchange medium outlet pipe 222.

[0034] Wherein, the concentration kettle 5 is provided with a first pressure gauge 6 and a first temperature sensor 4 .

[0035] Wherein, the ultrasonic reactor 9 is provided with a second pressure gauge 17 and a second temperature sensor 16 .

[0036] The ultrasonic kettle 9 is provided with a first feed pipe 28 ; the first feed pipe 28 is connected to the silo 13 , and the silo 13 is provided with a screw conveyor 12 and a second feed pipe 29 .

[0037] Compared with the prior art, the utility model has the following advantages and beneficial effects:

[0038] 1. The utility model provides a purification system for refined glufosinate ammonium, wherein the refined glufosinate ammonium solution flows into the concentration kettle 5 through the refined glufosinate ammonium solution inlet pipe 3, and after the refined glufosinate ammonium solution is concentrated to a certain extent, methanol is added to the concentration kettle 5 through the methanol inlet pipe twice, and after the methanol is added dropwise, the mixed solution is transferred to the ultrasonic kettle 9 through the first liquid outlet pipe 18, and the first crystallization is directly insulated in the concentration kettle 5. After the first crystallization is completed, it is cooled and transferred to the centrifuge through the second discharge pipe for centrifugal separation to obtain refined glufosinate ammonium hydrate solid, and the refined glufosinate ammonium hydrate is added to the ultrasonic kettle 9 through the silo 13 and the screw conveyor 12, and then anhydrous methanol is added through the second methanol inlet pipe 21, and the ultrasonic device 10 is turned on. After ultrasonic treatment for a period of time, the temperature is lowered and centrifuged, and the mother liquor is partially used in the ultrasonic step, and the filter cake is dried to obtain the refined glufosinate ammonium product. The refined glufosinate ammonium product obtained by the utility model has high purity.

[0039] 2. The utility model provides a purification system for refined glufosinate ammonium. The flowmeter 23 and the flow regulating valve 24 arranged on the first methanol inlet pipe 1, the refined glufosinate ammonium solution inlet pipe 3 and the second methanol inlet pipe 21 ensure that the refined glufosinate ammonium solution is accurately added to the concentration kettle 5 and the methanol is accurately added to the concentration kettle 5 and the ultrasonic kettle 9.

[0040] 3. The utility model provides a purification system for refined glufosinate ammonium. The heat exchanger 7 is arranged so that the volatilized methanol is cooled by the heat exchanger 7 and then flows into the concentrated water receiving tank 14, so that the methanol is recovered and utilized.

[0041] 4. The utility model provides a purification system for refined glufosinate-ammonium, in which a vacuum pump 11, an air inlet pipe 2 and a first pressure gauge 6 are arranged to balance the pressure in the concentration kettle 5.

[0042] 5. The utility model provides a purification system for refined glufosinate ammonium, wherein a heat exchange jacket, a second heat exchange jacket 22, a first temperature sensor 4 and a second temperature sensor 16 are arranged to facilitate adjusting the temperature in the concentration kettle 5 and the ultrasonic kettle 9 to the desired temperature.

[0043] Example 3

[0044] This embodiment uses a method for purifying refined glufosinate-ammonium by using a purification system for refined glufosinate-ammonium described in Example 2, comprising the following steps:

[0045] Step 1, adding the synthesized refined glufosinate ammonium aqueous solution into a concentration kettle through a refined glufosinate ammonium solution inlet pipe, and concentrating the refined glufosinate ammonium aqueous solution to a concentration of 60%;

[0046] Step 2: Add methanol to the concentration kettle through the methanol inlet tube at a temperature of 60°C, the amount of methanol added: the amount of glufosinate ammonium solution added = 0.5:1, and after the addition is completed, keep warm and stir for crystallization for 130 minutes;

[0047] Step 3: Then, at a temperature of 35° C., methanol is added to the concentration kettle through the methanol inlet tube, and the amount of methanol added: the amount of glufosinate ammonium solution added = 0.5:1. After the addition is completed, the mixed solution is transferred to an ultrasonic kettle;

[0048] Step 4B, directly heat the first crystallization in the concentration kettle for 260 minutes, cool after the first crystallization is completed, transfer the material to the centrifuge through the discharge valve at the bottom of the kettle for centrifugal separation to obtain a refined glufosinate ammonium hydrate solid, add the refined glufosinate ammonium hydrate to the ultrasonic kettle through the silo and the screw conveyor, and then add anhydrous methanol, the amount of methanol added: the amount of refined glufosinate ammonium solution added = 1:1, turn on the ultrasonic device, ultrasonically treat for 30 minutes, then cool and centrifuge, the mother liquor is partially used for the ultrasonic step, and the filter cake is dried to obtain the refined glufosinate ammonium product.

[0049] Wherein, in the step 1, the concentration environment is a negative pressure of -95KPa to -90KPa and 40°C.

[0050] Wherein, in the step 2, the speed of methanol in the methanol inlet pipe is 10L / min.

[0051] Wherein, in the step three, the speed of methanol in the methanol inlet pipe is 10L / min.

[0052] Wherein, in the step 4B, during the first crystallization, the mixture is cooled to 35°C within 30 minutes; during the cooling, the mixture is cooled to 35°C within 30 minutes; during the drying, the filter cake is dried at -95Kpa~-50Kpa and 50°C for 120 minutes.

[0053] Wherein, in step 4B, the speed of adding anhydrous methanol into the ultrasonic reactor is 50 L / min.

[0054] Wherein, the power of the ultrasonic device is 2000W.

[0055] The refined glufosinate-ammonium product was quantitatively detected by HPLC external standard and the purification yield was calculated based on the content. The purity of the refined glufosinate-ammonium product was 99.2% and the yield was 97.5%.

[0056] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. Any simple modification or equivalent changes made to the above embodiments based on the technical essence of the present invention shall fall within the protection scope of the present invention.

Claims

1. A purification system for refined glufosinate-ammonium, characterized in that: The invention comprises a concentration kettle (5) and an ultrasonic kettle (9); the concentration kettle (5) is provided with a first methanol inlet pipe (1), a refined glufosinate ammonium solution inlet pipe (3), a first liquid outlet pipe (18) and a first gas outlet pipe (19); the concentration kettle (5) is connected to the ultrasonic kettle (9) via the first liquid outlet pipe (18); and the ultrasonic kettle (9) is provided with a second methanol inlet pipe (21), an ultrasonic device (10), a second liquid outlet pipe (27) and a second gas outlet pipe (26).

2. A purification system for refined glufosinate-ammonium according to claim 1, characterized in that: The first methanol inlet pipe (1), the refined glufosinate ammonium solution inlet pipe (3) and the second methanol inlet pipe (21) are all provided with a flow meter (23) and a flow regulating valve (24).

3. A purification system for refined glufosinate-ammonium according to claim 1, characterized in that: The first liquid outlet pipe (18) is provided with a first material transfer pump (8).

4. A purification system for refined glufosinate-ammonium according to claim 1, characterized in that: A heat exchanger (7) is provided on the first air outlet pipe (19); a liquid outlet end of the heat exchanger (7) is connected to a concentrated water receiving tank (14); and a second material transfer pump (15) is provided at the lower end of the concentrated water receiving tank (14).

5. A purification system for refined glufosinate-ammonium according to claim 4, characterized in that: The concentration kettle (5) is provided with a third gas outlet pipe (25), the third gas outlet pipe (25) is provided with a vacuum pump (11), and the first gas outlet pipe (19) is connected to the third gas outlet pipe (25) via a connecting pipe.

6. A purification system for refined glufosinate-ammonium according to claim 1, characterized in that: The concentration kettle (5) is also provided with an air inlet pipe (2).

7. A purification system for refined glufosinate-ammonium according to claim 1, characterized in that: The concentration kettle (5) is provided with a first heat exchange jacket (20), and the first heat exchange jacket (20) is provided with a first heat exchange medium inlet pipe (201) and a first heat exchange medium outlet pipe (202); the ultrasonic kettle (9) is provided with a second heat exchange jacket (22), and the second heat exchange jacket (22) is provided with a second heat exchange medium inlet pipe (221) and a second heat exchange medium outlet pipe (222).

8. A purification system for refined glufosinate-ammonium according to claim 1, characterized in that: The concentration kettle (5) is provided with a first pressure gauge (6) and a first temperature sensor (4).

9. A purification system for refined glufosinate-ammonium according to claim 1, characterized in that: The ultrasonic kettle (9) is provided with a second pressure gauge (17) and a second temperature sensor (16).

10. A purification system for refined glufosinate-ammonium according to claim 1, characterized in that: The ultrasonic kettle (9) is provided with a first feed pipe (28); the first feed pipe (28) is connected to a silo (13); and the silo (13) is provided with a screw conveyor (12) and a second feed pipe (29).

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