Device for preparing 4, 6-dichloropyrimidine by using slicing machine instead of crystallization centrifugation

Abstract

The utility model provides a device for preparing 4, 6-dichloropyrimidine by using a slicing machine instead of crystallization and centrifugation. A gas phase pipe at the top of a distillation kettle in the device is communicated with a condenser, a condensate outlet pipe and a condensate inlet pipe are mounted on the condenser, the condenser is communicated with a heat preservation kettle, a thermometer, a pressure gauge, a steam inlet pipe and a steam outlet pipe are mounted on the heat preservation kettle, a stirring mechanism and a tail gas outlet pipe are mounted at the top of the heat preservation kettle, and a mixed liquid outlet pipe is mounted at the bottom of the heat preservation kettle. The mixed liquid outlet pipe is communicated with the roller slicing machine, a stock bin is installed on the roller slicing machine, the stock bin is communicated with the drying system through the product outlet pipe, and all the electromagnetic valves are installed at inlets and outlets of all the pipelines. According to the device, a crystallization kettle is replaced by a heat preservation kettle, a crystallization and centrifugation operation mode is replaced by a roller slicing machine, and distilled and heat-preserved materials are directly crystallized and sliced by the roller slicing machine. The device is reasonable in structural design, simple in technological process and simple in technological parameter control, material loss is reduced, and working procedure time is saved.

Description

Technical Field

[0001] The utility model relates to the field of chemical equipment, and particularly relates to a device for preparing 4,6-dichloropyrimidine by replacing crystallization and centrifugation with a slicing machine. Background Art

[0002] 4,6-Dichloropyrimidine is one of the important raw materials for the production of synthetic pharmaceutical intermediates. The production process of 4,6-dichloropyrimidine includes processes such as chlorination → hydrolysis → water washing → distillation → crystallization → centrifugation → drying, etc. Among them, from distillation → crystallization → centrifugation → drying are important steps in the production of 4,6-dichloropyrimidine products. Refer to the appendix Figure 2 , the material is input into the distillation kettle 2 for distillation treatment. The liquid phase generated during distillation is transported to the residual liquid storage tank through the liquid phase pipe 19. The formed gas phase is transported to the crystallization kettle 20 through the gas phase pipe 7 and the condenser 11, and crystallization is carried out by controlling the pressure and temperature. The crystallized mixed liquid is transported to the centrifuge 23 through the mixed liquid outlet pipe 15 for centrifugation operation. During centrifugation operation, nitrogen needs to be input through the nitrogen inlet pipe 22 for protection. The centrifuged product is directly sent for drying treatment. The centrifuged mother liquor is transported to the mother liquor pool 25 through the mother liquor input pipe 24 for concentration, and then pumped into the mother liquor storage tank through the acid-base pump 26 and the mother liquor output pipe 27 for storage. This production method takes a relatively long time from the crystallization process to the centrifugation process, generally taking about 8 hours to complete. Moreover, the material loss is relatively large during crystallization and centrifugation, and the material loss is generally about 5%. At the same time, the energy consumption during the production process is high, the process route is complex, and the process parameter control is difficult. Therefore, the technical personnel of this application provide a device for preparing 4,6-dichloropyrimidine by replacing crystallization and centrifugation with a slicing machine. Summary of the Invention

[0003] The purpose of the utility model is to provide a device for preparing 4,6-dichloropyrimidine by replacing crystallization and centrifugation with a slicing machine. The technical problem to be solved by the utility model is: replacing the crystallization kettle with a heat preservation kettle, replacing the operation modes of crystallization and centrifugation with a drum slicing machine, and the drum slicing machine directly crystallizes and slices the material after distillation and heat preservation; simplifying the process flow, reducing the process time of crystallization and centrifugation in the original process from 8 hours to 1 hour, reducing the control difficulty of process parameters and energy consumption, and reducing the material loss from the original 5% to 0.1%.

[0004] To achieve the above purpose, the technical solution of the utility model is as follows:

[0005] An apparatus for preparing 4,6-dichloropyrimidine by replacing crystallization and centrifugation with a slicing machine, comprising: a thermometer, a distillation kettle, a pressure gauge, a stirring mechanism, a gas-phase pipe, a steam inlet pipe, a condensate outlet pipe, a condensate inlet pipe, a condenser, a tail gas outlet pipe, a heat preservation kettle, a steam outlet pipe, a mixed liquid outlet pipe, a drum slicing machine, a feed bin, a product outlet pipe, a solenoid valve, and a control console. The distillation kettle is equipped with a thermometer, a pressure gauge, a steam inlet pipe, and a steam outlet pipe. A stirring mechanism, a material inlet pipe, and a solvent outlet pipe are installed at the top of the distillation kettle. The solvent outlet pipe is connected to a solvent storage tank. A liquid-phase pipe is installed at the bottom, and the liquid-phase pipe is connected to a residual liquid recovery system. In the apparatus, the gas-phase pipe at the top of the distillation kettle is connected to the inlet of the condenser. The condenser is equipped with a condensate outlet pipe and a condensate inlet pipe. The outlet of the condenser is connected to the heat preservation kettle. The heat preservation kettle is equipped with a thermometer, a pressure gauge, a steam inlet pipe, and a steam outlet pipe. The steam inlet pipe and the steam outlet pipe are connected to a steam supply system. A stirring mechanism and a tail gas outlet pipe are installed at the top of the heat preservation kettle. The tail gas outlet pipe is connected to a tail gas treatment system. A mixed liquid outlet pipe is installed at the bottom of the heat preservation kettle, and the other end of the mixed liquid outlet pipe is connected to the drum slicing machine. A feed bin is installed on the drum slicing machine, and the feed bin is connected to a drying system through the product outlet pipe.

[0006] In the described apparatus, each solenoid valve is installed at the inlet and outlet of each pipeline.

[0007] The thermometer, pressure gauge, stirring mechanism, drum slicing machine, and each solenoid valve in the apparatus are respectively connected to the electronic control unit in the control console by wires.

[0008] Compared with the prior art, the positive effects of the present utility model are as follows:

[0009] 1. The apparatus replaces the crystallization kettle with a heat preservation kettle and replaces the operation modes of crystallization and centrifugation with a drum slicing machine. The drum slicing machine directly crystallizes and slices the materials after distillation and heat preservation, and then stores and outputs them through the feed bin.

[0010] 2. The apparatus uses a drum slicing machine for crystallization and centrifugation, eliminating equipment such as centrifuges, mother liquor tanks, acid-base pumps, and nitrogen input, simplifying the process flow, and solving the problem of mother liquor treatment after centrifugation in the original process.

[0011] 3. The apparatus directly crystallizes and slices through the drum slicing machine, reducing the total process time of crystallization and centrifugation in the original process from 8 hours to 1 hour, and at the same time reducing the control difficulty of process parameters during production.

[0012] 4. The process parameters during the production of the apparatus are easy to control, while reducing energy consumption and labor intensity, reducing material loss, and reducing the material loss from 5% in the original to 0.1%.

[0013] 5. The apparatus reduces the number of operators, improves work efficiency, ensures the quality of the produced products, and at the same time improves the working environment of the workshop.

[0014] 6. The device has a reasonable structural design, a simple process flow, simple parameter control, and a wide range of applications. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] The drawings required for the implementation of the technology of the present utility model are briefly introduced. The drawings in the following description are only exemplary. For those of ordinary skill in the art, other implementation drawings can be obtained by extension based on the provided drawings without creative efforts.

[0016] The structures, proportions, sizes, etc. of the drawings illustrated in this specification are only used to cooperate with the content disclosed in the specification for those skilled in the art to understand and read, and are not used to limit the implementation conditions of the present utility model. Any modification of the structure, change of the proportional relationship, or adjustment of the size should still fall within the scope covered by the technical content disclosed in the present utility model without affecting the effects that the technology of the present utility model can produce and the purposes that can be achieved.

[0017] Figure 1 Front view structural schematic diagram of the present utility model;

[0018] Figure 2 Structural schematic diagram of the original process equipment;

[0019] Figure 3 Connection block diagram of each mechanism, each solenoid valve and the console in the device.

[0020] In the figure: 1. Thermometer, 2. Distillation kettle, 3. Pressure gauge, 4. Stirring mechanism, 5. Solvent outlet pipe, 6. Material inlet pipe, 7. Gas phase pipe, 8. Steam inlet pipe, 9. Condensate outlet pipe, 10. Condensate inlet pipe, 11. Condenser, 12. Tail gas outlet pipe, 13. Heat preservation kettle, 14. Steam outlet pipe, 15. Mixed liquid outlet pipe, 16. Drum slicer, 17. Bunker, 18. Product outlet pipe, 19. Liquid phase pipe, 20. Solenoid valve, 21. Crystallization kettle, 22. Nitrogen inlet pipe, 23. Centrifuge, 24. Mother liquor input pipe, 25. Mother liquor tank, 26. Acid-base pump, 27. Mother liquor output pipe, 28. Console. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0021] The technical solutions of the present utility model are further clearly and completely described below in conjunction with the drawings. The following specific embodiments are only used for further illustration of the present application and should not be construed as limiting the protection scope of the present application. Those skilled in the art can make some non-essential improvements and adjustments to the present application based on the above application content.

[0022] See the appendix Figures 1-3, Connection and installation of the device. Connect the gas-phase pipe 7 at the top of the distillation kettle 2 to the inlet of the condenser 11. Install the condensate outlet pipe 9 and the condensate inlet pipe 10 on the condenser 11. Connect the outlet of the condenser 11 to the heat preservation kettle 13. Install the thermometer 1, pressure gauge 3, steam inlet pipe 8 and steam outlet pipe 14 on the heat preservation kettle 13. Connect the steam inlet pipe 8 and the steam outlet pipe 14 to the steam supply system. Install the stirring mechanism 4 and the tail gas outlet pipe 12 on the top of the heat preservation kettle 13. Connect the tail gas outlet pipe 12 to the tail gas treatment system. Install the mixed liquid outlet pipe 15 at the bottom of the heat preservation kettle 13. Connect the other end of the mixed liquid outlet pipe 15 to the drum slicer 16. Install the feed bin 17 on the drum slicer 16. Connect the feed bin 17 to the drying system through the product outlet pipe 18.

[0023] Install each solenoid valve 20 at the inlet and outlet of each pipeline. Connect the thermometer 1, pressure gauge 3, stirring mechanism 4, drum slicer 16, and each solenoid valve 20 in the device to the electronic control unit in the console 28 with wires respectively.

[0024] Preparatory work before use. Input the process parameters of the thermometer 1, pressure gauge 3, stirring mechanism 4, drum slicer 16, and each solenoid valve 20 into the electronic control unit in the console 28 respectively. The operator opens the solenoid valves 20 on each pipeline through the console 28, and sends high-temperature steam into the heat preservation kettle 13 through the steam inlet pipe 8 to make the temperature in the heat preservation kettle 13 reach the process-set value. The low-temperature steam returns to the steam supply system through the steam outlet pipe 14.

[0025] When the temperature in the heat preservation kettle 13 reaches the process-set value, the 4,6-dichloropyrimidine gas phase distilled from the distillation kettle 2 enters the condenser 11 through the gas-phase pipe 7. The condensate enters the condenser 11 through the condensate inlet pipe 10 to cool down the 4,6-dichloropyrimidine gas phase. The condensate with increased temperature is discharged through the condensate outlet pipe 9 for recycling. The 4,6-dichloropyrimidine gas phase in the condenser 11 becomes a liquid phase after cooling and enters the heat preservation kettle 13 along the pipeline for heat preservation. A small amount of tail gas generated during the heat preservation process is transported to the tail gas treatment system through the tail gas outlet pipe 12 for treatment. Keep the materials in the heat preservation kettle 13 in a certain fluidity through the stirring mechanism 4. Then, through the mixed liquid outlet pipe 15 at the bottom of the heat preservation kettle 13, transport the mixed liquid in the heat preservation kettle 13 to the trough of the drum slicer 16. Use the rotation of the drum slicer 16 to crystallize the mixed liquid in the drum slicer 16 and slice the crystallized materials. Finally, transport the sliced materials in the feed bin 17 to the drying process through the product outlet pipe 18 to prepare the product. Monitor the temperature in the heat preservation kettle 13 through the thermometer 1 and monitor the pressure in the heat preservation kettle 13 using the pressure gauge 3.

[0026] The above embodiments are only for illustrating the technical concept and features of the present utility model, and the purpose thereof is to enable those skilled in the art to understand the content of the present utility model and implement it accordingly, and shall not be used to limit the protection scope of the present utility model. Any equivalent changes or modifications made according to the technical essence of the present utility model shall be covered within the protection scope of the present utility model.

Claims

1. An apparatus for preparing 4,6-dichloropyrimidine by replacing crystallization centrifugation with a slicing machine, comprising: Thermometer (1), distillation kettle (2), pressure gauge (3), stirring mechanism (4), gas phase pipe (7), steam inlet pipe (8), condensate outlet pipe (9), condensate inlet pipe (10), condenser (11), tail gas outlet pipe (12), heat preservation kettle (13), steam outlet pipe (14), mixed liquid outlet pipe (15), drum slicer (16), storage bin (17), product outlet pipe (18), solenoid valve (20), control console (28). A thermometer (1), a pressure gauge (3), a steam inlet pipe (8) and a steam outlet pipe (14) are installed on the distillation kettle (2). A stirring mechanism (4), a material inlet pipe (6) and a solvent outlet pipe (5) are installed on its top. The solvent outlet pipe (5) is connected to a solvent storage tank. A liquid phase pipe (19) is installed at the bottom, and the liquid phase pipe (19) is connected to a residual liquid recovery system. It is characterized in that: in the said device, the gas phase pipe (7) at the top of the distillation kettle (2) is connected to the inlet of the condenser (11). A condensate outlet pipe (9) and a condensate inlet pipe (10) are installed on the condenser (11). The outlet of the condenser (11) is connected to the heat preservation kettle (13). A thermometer (1), a pressure gauge (3), a steam inlet pipe (8) and a steam outlet pipe (14) are installed on the heat preservation kettle (13). The steam inlet pipe (8) and the steam outlet pipe (14) are connected to a steam supply system. A stirring mechanism (4) and a tail gas outlet pipe (12) are installed on its top. The tail gas outlet pipe (12) is connected to a tail gas treatment system. A mixed liquid outlet pipe (15) is installed at the bottom, and the other end of the mixed liquid outlet pipe (15) is connected to the drum slicer (16). A storage bin (17) is installed on the drum slicer (16). The storage bin (17) is connected to a drying system through the product outlet pipe (18).

2. The device for preparing 4,6-dichloropyrimidine by replacing the crystallization centrifuge with a slicing machine according to claim 1, wherein: In the said device, each solenoid valve (20) is installed at the inlet and outlet of each pipeline.

3. The device for preparing 4,6-dichloropyrimidine by replacing crystallization centrifugation with a slicing machine according to claim 1, characterized in that: The thermometer (1), the pressure gauge (3), the stirring mechanism (4), the drum slicer (16) and each solenoid valve (20) in the said device are respectively connected to the electronic control unit in the control console (28) by wires.

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