A production device for preparing flumetover crystal form I

Abstract

The utility model relates to a kind of for preparing flumetralin crystal form I production device, including high-pressure transformation crystallizer, and tap water import and feeding port are set on high-pressure transformation crystallizer;High-pressure transformation crystallizer is equipped with transformation crystallizer jacket outside, and is equipped with transformation crystallizer coil pipe inside, high-pressure transformation crystallizer kettle bottom is connected with discharge pipe, discharge pipe is connected with suction filter tank, suction filter tank lower liquid discharge is connected with mother liquor receiving tank, mother liquor receiving tank is connected with vacuum pumping device, and mother liquor receiving tank lower liquid discharge is connected with high-pressure transformation crystallizer by mother liquor circulating pump;Hot water circulating kettle is set with heating jacket outside, and hot water circulating kettle is connected with hot water supply pipe, and hot water supply pipe is connected with coil pipe water inlet pipe and transformation crystallization lower outlet pipe respectively by hot water pump, and cooling hot water return pipe is connected with hot water circulating kettle.The device structure is simple, and water is transformed into crystal by high-pressure transformation crystallizer, avoid traditional solvent transformation crystallization solvent residue, lead to in drying temperature process solvent can dissolve part crystal form 1 and produce steady-state crystal form 2, help to improve the purity and yield of transformation crystallization production, suitable for industrial production use.

Description

Technical Field

[0001] This utility model relates to chemical industrial production equipment, specifically a production equipment for preparing cyazofamid crystal form I. Background Technology

[0002] Cyclocarb, a novel nicotinamide fungicide, exhibits excellent control efficacy against diseases such as black spot, powdery mildew, gray mold, and various rots. As an inhibitor of succinate-coenzyme Q reductase in the mitochondrial respiratory chain, it strongly inhibits spore germination and shows no cross-resistance with other fungicides. Furthermore, this fungicide possesses superior characteristics including rapid diffusion, significant efficacy, fast absorption, crop safety, long-lasting effect, low environmental pollution, and resistance to rain washout.

[0003] Currently, three crystal forms of boscalid have been reported: crystal form I, monohydrate, and crystal form II. Different crystal forms of boscalid can be prepared by different crystal transformation processes.

[0004] Chinese patent CN 100494179C discloses two methods for preparing cyazofamid crystal form II and its application in the pharmaceutical field. Method one involves dissolving cyazofamid in a polar protic solvent or aromatic hydrocarbon, then cooling and crystallizing it out of the solvent. Method two involves heating the dehydrated compound of cyazofamid crystal form I to above 150°C until each component melts, then adding seed crystals of the dehydrated compound of cyazofamid crystal form II, and finally cooling the melt.

[0005] Chinese patent CN 1275943C discloses the transcrystallization hydrates of nicotinamide and benzoylaniline, which include cymoxanil monohydrate. The preparation method of the transcrystallization hydrates of nicotinamide and benzoylaniline in this patent is to dissolve the transcrystallization hydrates of nicotinamide and benzoylaniline in a water-soluble organic solvent and precipitate the hydrate of I by adding water.

[0006] There are few domestic publications on the industrial-scale preparation of boscalid crystal form I, and no related patents were found. This is mainly due to the difficulty in preparing boscalid crystal form I, the unstable process, and the limitation imposed by the crystal form issue. To date, no publicly disclosed industrial-scale boscalid equipment has been developed in China. Therefore, the development of boscalid technical material crystal form I is of positive significance to the development of my country's fungicide industry. Summary of the Invention

[0007] This invention provides a simple production apparatus for preparing cyazofamid crystal form I, which effectively balances production efficiency and crystal conversion purity and efficiency.

[0008] The technical solution adopted in this utility model is: a production device for preparing cyazofamid crystal form I, comprising a high-pressure crystallization reactor, characterized in that: the high-pressure crystallization reactor is provided with a tap water inlet and a feeding port; the high-pressure crystallization reactor is externally equipped with a crystallization reactor jacket and internally equipped with a crystallization reactor coil; an upper crystallization inlet pipe is externally connected to the upper part of one side of the crystallization reactor jacket, which is connected to a steam inlet pipe, a cooling water outlet pipe, and a cooling hot water return pipe; a lower crystallization outlet pipe is externally connected to the lower part or lower end of the other side of the crystallization reactor jacket, which is connected to a steam outlet pipe and a cooling water inlet pipe. The high-pressure crystallizer has a coil with a return water pipe and an inlet water pipe connected to both sides at the top. A discharge pipe is connected to the bottom of the high-pressure crystallizer, which is connected to a filtration tank. The discharge liquid in the filtration tank is connected to a mother liquor receiving tank. A vacuum device is connected to the mother liquor receiving tank. The discharge liquid in the mother liquor receiving tank is returned to the high-pressure crystallizer via a mother liquor circulation pump. The system also includes a hot water circulation tank with a heating jacket. A hot water supply pipe is connected to the bottom of the hot water circulation tank. The hot water supply pipe is connected to the coil inlet water pipe and the crystallizer outlet pipe via a hot water pump. The cooling hot water return pipe is connected back to the hot water circulation tank.

[0009] The high-pressure crystallizer is equipped with a stirrer.

[0010] The high-pressure crystallizer is equipped with a temperature metering port and a pressure gauge interface at its upper end.

[0011] Control valve assemblies are installed on the crystallization inlet pipe, steam inlet pipe, cooling water outlet pipe, cooling hot water return pipe, crystallization outlet pipe, steam outlet pipe, cooling water inlet pipe, coil return water pipe, coil inlet water pipe, discharge pipe, hot water supply pipe, coil inlet water pipe, and crystallization outlet pipe.

[0012] The control valve assembly is a solenoid shut-off valve and / or a check valve.

[0013] The vacuuming device includes a vacuum buffer tank and a vacuum water pump. The vacuum water pump is connected to the vacuum buffer tank, and the vacuum buffer tank is connected to the mother liquor receiving tank.

[0014] Flow meters are installed on the hot water supply pipe and the coil inlet pipe.

[0015] The heating jacket is connected to steam and / or hot water.

[0016] The high-pressure crystallization reactor is a stainless steel reactor, and the filtration tank is a 304 stainless steel filtration tank.

[0017] The hot water circulating kettle is a glass-lined kettle, and the mother liquor receiving tank and the vacuum buffer tank are both vertical glass-lined tanks.

[0018] This invention employs a high-pressure crystallizer with water-inlet crystallization, combined with vacuum filtration. This avoids the solvent residue that occurs in traditional solvent-based crystallization, which causes some crystal form 1 to dissolve during the drying and heating process. As drying progresses, the solvent gradually decreases, and the dissolved cyazofamid precipitates out a stable crystal form 2. This helps improve the purity and yield of the crystallization process and is suitable for industrial production. Attached Figure Description

[0019] Figure 1 This is a schematic diagram of the structure of this utility model.

[0020] In the diagram: 1. High-pressure crystallizer; 2. Filtration mother liquor inlet; 3. Coil return water pipe; 4. Temperature metering port; 5. Pressure gauge interface; 6. Tap water inlet; 7. Feeding port; 8. Safety valve; 9. Coil inlet water pipe; 10. Crystallizer jacket; 11. Crystallizer upper inlet pipe; 12. Steam inlet pipe; 13. Cooling water outlet pipe; 14. Cooling hot water return pipe; 15. Crystallizer lower outlet pipe; 16. Steam outlet pipe; 17. Cooling water inlet pipe; 18. Crystallizer coil; 19. Discharge pipe; 20. Filter tank; 21. Mother liquor receiving tank; 22. Vacuum buffer tank; 23. Vacuum water pump; 24. Hot water circulation tank; 25. Heating jacket; 26. Hot water supply pipe; 27. Hot water pump; 28. Stirrer; 29. ​​Control valve group; 30. Flow meter; 31. Mother liquor circulation pump. Detailed Implementation

[0021] The following explanation, in conjunction with the accompanying drawings, will provide further details.

[0022] Figure 1 As shown: A production apparatus for preparing cyazofamid crystal form I includes a high-pressure crystallization kettle, a vacuum filter tank 20, a mother liquor receiving tank 21, a vacuum buffer tank 22, a vacuum water pump 23, a hot water circulation kettle 24, and a hot water pump 27.

[0023] The high-pressure crystallizer 1 is equipped with a mother liquor inlet 2, a coil return water pipe 3, a temperature metering port 4, a pressure gauge interface 5, a tap water inlet 6, a feeding port 7, a safety valve 8, and a coil inlet water pipe 9. The high-pressure crystallizer 1 is externally equipped with a crystallizer jacket 10 and internally equipped with a crystallizer coil 18. One side of the upper part of the crystallizer jacket 10 is externally connected to an upper crystallizer inlet pipe 11, which is connected to a steam inlet pipe 12, a cooling water outlet pipe 13, and a cooling water return pipe 14. The other side of the lower end of the crystallizer jacket 10 is externally connected to a lower crystallizer outlet pipe 15, which is connected to a steam outlet pipe 16 and a cooling water inlet pipe 17. The crystallizer coil 18 is connected to coil return water pipes on both sides of the upper end of the high-pressure crystallizer 1. Water pipes and coil inlet pipes are connected to the bottom of the high-pressure crystallizer 1, and the discharge pipe 19 is connected to the suction filter tank 20. The discharge liquid of the suction filter tank 20 is connected to the mother liquor receiving tank 21. The mother liquor receiving tank 21 is connected to the vacuum buffer tank 22. The vacuum buffer tank 22 is connected to the vacuum water pump 23. The discharge liquid of the mother liquor receiving tank 21 is connected back to the mother liquor inlet 2 of the high-pressure crystallizer via the mother liquor circulation pump 31. A heating jacket 25 is installed outside the hot water circulation tank 24. The hot water circulation tank 24 is connected to the bottom of the hot water supply pipe 26. The hot water supply pipe 26 is connected to the coil inlet pipe 9 and the crystallizer outlet pipe 15 via the hot water pump 27. The hot water circulation tank 24 is connected to the top of the cooling hot water return pipe 14, tap water, and coil return water pipe 3.

[0024] Based on this embodiment, a stirrer 28 can be installed inside the high-pressure crystallizer 1 and the hot water circulating reactor 24.

[0025] In this implementation, the high-pressure crystallizer 1 is equipped with a temperature metering port 4 and a pressure gauge interface 5 at its upper end for connecting external temperature and pressure metering equipment. A mother liquor inlet 2 is also provided on the hot water circulating reactor.

[0026] In this embodiment, each pipe is equipped with a control valve assembly 29. In industrial chemical production, the use of electromagnetic shut-off valves and / or check valves in pipelines is a conventional technique.

[0027] In this embodiment, a flow meter 30 can be installed on the hot water supply pipe and the coil inlet pipe.

[0028] Based on this embodiment, the heating jacket is externally connected to steam and / or hot water.

[0029] Based on this embodiment, it is preferred that the high-pressure crystallization reactor is a stainless steel reactor, the filtration tank is a 304 stainless steel filtration tank, the hot water circulation reactor is a glass-lined reactor, and the mother liquor receiving tank and the vacuum buffer tank are both vertical glass-lined tanks.

Claims

1. An apparatus for preparing boscalid crystal form I, comprising a high-pressure crystallization reactor, characterized in that: The high-pressure crystallizer is equipped with a tap water inlet and a feeding port. The high-pressure crystallizer is externally fitted with a crystallizer jacket and internally fitted with a crystallizer coil. An upper crystallizer inlet pipe is connected to the upper part of one side of the jacket, which is connected to a steam inlet pipe, a cooling water outlet pipe, and a cooling water return pipe. A lower crystallizer outlet pipe is connected to the lower part or lower end of the other side of the jacket, which is connected to a steam outlet pipe and a cooling water inlet pipe. The crystallizer coil has return water outlets on both sides of the upper end of the high-pressure crystallizer. The system includes a water inlet pipe for the coil, a discharge pipe at the bottom of the high-pressure crystallizer, a filter tank, a mother liquor receiving tank at the bottom of the filter tank, a vacuum pump at the top of the mother liquor receiving tank, and a mother liquor circulation pump at the bottom of the mother liquor receiving tank to return the mother liquor to the high-pressure crystallizer. It also includes a hot water circulation tank with a heating jacket, a hot water supply pipe at the bottom, a hot water pump connecting the coil inlet pipe and the crystallizer outlet pipe, and a cooling hot water return pipe returning to the hot water circulation tank.

2. The apparatus for preparing boscalidamide crystal form I according to claim 1, characterized in that: The high-pressure crystallizer is equipped with a stirrer.

3. The apparatus for preparing boscalidamide crystal form I according to claim 1, characterized in that: The high-pressure crystallizer is equipped with a temperature metering port and a pressure gauge interface at its upper end.

4. The apparatus for preparing boscalidamide crystal form I according to claim 1, characterized in that: Control valve assemblies are installed on the crystallization inlet pipe, steam inlet pipe, cooling water outlet pipe, cooling hot water return pipe, crystallization outlet pipe, steam outlet pipe, cooling water inlet pipe, coil return water pipe, coil inlet water pipe, discharge pipe, hot water supply pipe, coil inlet water pipe, and crystallization outlet pipe.

5. The apparatus for preparing boscalidamide crystal form I according to claim 4, characterized in that: The control valve assembly is a solenoid shut-off valve and / or a check valve.

6. The apparatus for preparing boscalidamide crystal form I according to claim 1, characterized in that: The vacuuming device includes a vacuum buffer tank and a vacuum water pump. The vacuum water pump is connected to the vacuum buffer tank, and the vacuum buffer tank is connected to the mother liquor receiving tank.

7. The apparatus for preparing boscalidamide crystal form I according to claim 1, characterized in that: Flow meters are installed on the hot water supply pipe and the coil inlet pipe.

8. The apparatus for preparing boscalidamide crystal form I according to claim 1, characterized in that: The heating jacket is connected to steam and / or hot water.

9. The apparatus for preparing boscalidamide crystal form I according to claim 1, characterized in that: The high-pressure crystallization reactor is a stainless steel reactor, and the filtration tank is a 304 stainless steel filtration tank.

10. The apparatus for preparing boscalidamide crystal form I according to claim 1, characterized in that: The hot water circulating kettle is a glass-lined kettle, and the mother liquor receiving tank and the vacuum buffer tank are both vertical glass-lined tanks.

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