Continuous crystallization device for glyphosate production

Abstract

The utility model relates to a continuous crystallization device for glyphosate production, which is characterized in that a cooling kettle, a neutralization kettle and a cooling kettle have the same structure and respectively comprise a kettle body, a kettle cover, a stirring motor and a stirring paddle, a feeding pipeline and an emptying pipeline a are arranged on the left side of the upper end of the cooling kettle, a discharging pipeline is arranged in the middle of the lower end of the cooling kettle, and a cooling coil pipe is arranged in the cooling kettle; wherein the discharge pipeline is connected with a feed port of the neutralization kettle through a transfer pump; the left side of the upper end of the neutralization kettle is provided with a liquid alkali inlet and an emptying pipeline b, the right side of the upper end of the neutralization kettle is provided with an online PH meter, the middle part of the lower end of the neutralization kettle is provided with a transfer port, the liquid alkali inlet is externally connected with a liquid alkali feeding pipeline, and the transfer port is communicated with the injection port of the cooling kettle through a transfer channel; a flushing opening and an emptying pipeline c are arranged on the left side of the upper end of the cooling kettle, a discharging opening is formed in the middle of the lower end of the cooling kettle, the flushing opening is externally connected with a flushing water pipeline, and the discharging opening is externally connected with a suction filtration tank group through a discharging pipeline; the utility model has the advantages of time saving, convenience and high production efficiency.

Description

Technical Field

[0001] The utility model belongs to the field of chemical equipment, and particularly relates to a continuous crystallization device for glyphosate production. Background Art

[0002] Glyphosate has the characteristics of high efficiency, low toxicity, broad spectrum and non-selective herbicide, and has excellent performance. It is the most produced and popular herbicide in the world. With the rapid increase of the global population and the development of transgenic technology, broad opportunities are provided for glyphosate. At present, the main methods for producing glyphosate are IDA method and alkyl ester method. The main method for producing glyphosate in China is alkyl ester method. The specific process is to use glycine, dimethyl phosphite and paraformaldehyde as raw materials for addition and condensation to prepare a synthesis solution, which is then pumped into a hydrolysis kettle, and then hydrolyzed, desolvated and crystallized by adding alkali after adding hydrochloric acid. In the process of glyphosate production in China, in the crystallization section, the method often adopted is to add the desolvation solution into a neutralization kettle, and then add liquid caustic soda for neutralization. After stirring and cooling, filtration and washing are carried out. The crystallization section is particularly important, and its success or failure is related to the yield of the whole glyphosate synthesis.

[0003] In the crystallization section, the optimal crystallization temperature of glyphosate is 0-40°C. At present, in this process, the pH value during alkali addition and neutralization is mostly measured by a pH test paper after manual sampling, which has certain errors. At the same time, during the neutralization process, due to the high initial temperature of the desolvation solution, about 110°C, directly adding liquid caustic soda for neutralization will continue to generate heat, resulting in a continuous increase in the solution temperature, which has certain risks. In addition, during the neutralization process, the cooling, neutralization and crystallization cooling of the material are all carried out in the same neutralization kettle. Discharging and feeding can only be carried out after the cooling and crystallization time is reached. The continuity of the whole process is not strong, which has a greater impact on the production efficiency of glyphosate. Therefore, in order to improve the production efficiency of the glyphosate crystallization section, stably control the crystallization temperature and crystallization time, reduce manual sampling and analysis, and enhance the continuity of the glyphosate crystallization section, it is necessary to develop a time-saving, convenient and highly efficient continuous crystallization device for glyphosate production. Summary of the Utility Model

[0004] The purpose of the utility model is to overcome the deficiencies of the prior art and provide a time-saving, convenient and highly efficient continuous crystallization device for glyphosate production.

[0005] The object of the present utility model is achieved as follows: A continuous crystallization device for glyphosate production, comprising a cooling kettle, a neutralization kettle and a cooling kettle. The structures of the cooling kettle, the neutralization kettle and the cooling kettle are the same, and they are arranged continuously in sequence. Each of them consists of a kettle body, a kettle cover, a stirring motor fixedly installed above the kettle cover, and a stirring paddle concentrically connected to the stirring motor. Among them, on the left side of the upper end of the cooling kettle, there are a feed pipeline and an exhaust pipeline a. In the middle of the lower end, there is a discharge pipeline. Inside, there is a cooling coil. Liquid flow meters and solenoid valves are installed on both the feed pipeline and the discharge pipeline. And the discharge pipeline is connected to the feed port of the neutralization kettle through a transfer pump. The exhaust pipeline a is externally connected to a gas purification treatment device; on the left side of the upper end of the neutralization kettle, there is a liquid caustic soda inlet and an exhaust pipeline b. On the right side of the upper end, an on-line pH meter is installed. In the middle of the lower end, there is a transfer port. Among them, the liquid caustic soda inlet is externally connected to a liquid caustic soda feed pipeline, and a control valve and a liquid caustic soda content measuring device are installed on the liquid caustic soda feed pipeline. The exhaust pipeline b is externally connected to a gas purification treatment device. The transfer port is communicated with the injection port of the cooling kettle through a transfer channel; on the left side of the upper end of the cooling kettle, there is a flushing port and an exhaust pipeline c. In the middle of the lower end, there is a discharging port. Among them, the flushing port is externally connected to a flushing water pipeline, the exhaust pipeline c is externally connected to a gas purification treatment device, and the discharging port is externally connected to a suction filtration trough group through a discharging pipeline.

[0006] Further, the kettle bodies of the cooling kettle, the neutralization kettle and the cooling kettle are all provided with a sandwich layer, and cooling circulating water is introduced into the sandwich layer.

[0007] Further, the stirring motors in the cooling kettle, the neutralization kettle and the cooling kettle are all variable-frequency motors, and a wire mesh is arranged outside the stirring motors.

[0008] Further, between the kettle body and the kettle cover of the cooling kettle, the neutralization kettle and the cooling kettle, they are all connected by bolt limit, and gaskets are additionally installed between the kettle body and the kettle cover.

[0009] Further, on-line thermometers and radar level gauges are installed on the kettle covers of the cooling kettle, the neutralization kettle and the cooling kettle. And the on-line thermometer, the radar level gauge, the on-line pH meter and the liquid flow meter are all connected to the background control system through a data transmission module.

[0010] Further, the suction filtration trough group is formed by connecting multiple suction filtration troughs in sequence.

[0011] Further, the cooling kettle, the neutralization kettle and the cooling kettle are all made of glass-lined material.

[0012] Advantages of the present utility model: By sequentially subjecting the desolvated material to three-stage gradual cooling crystallization in a cooling kettle, a neutralization kettle, and a cooling kettle, the temperature control in the whole process is more stable, the crystallization effect is better, and the risk of multiple operations in a single kettle is avoided. Meanwhile, continuous feeding and discharging are realized, achieving the continuous operation of the glyphosate crystallization section, breaking the existing glyphosate crystallization mode, and improving the production efficiency of glyphosate. By providing a cooling coil and a cooling kettle with a sandwich on the inner wall of the kettle body, using a dual cooling mode, the cooling speed and cooling effect during the use of the cooling kettle are improved. Moreover, in the present utility model, the on-line thermometer, radar level gauge, on-line pH meter, and liquid flowmeter are all connected to the background control system through a data transmission module. With this structure, during the production and processing process, the measurement results can be transmitted to the control system in real time, facilitating calculation and analysis based on the remote transmission results, and then realizing remote control and adjustment. This reduces on-site manual sampling and measurement analysis, making the operation safer and more convenient while the overall automation level of the equipment is high. By providing a flushing port, the flushing port can be connected to a flushing water pipeline to solve the problem of blockage of the discharging pipeline. Generally, the present utility model has the advantages of time-saving, convenient operation, and high production efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] Figure 1 is a schematic structural diagram of the present utility model.

[0014] In the figure: 1. Cooling kettle; 11. Feed pipeline; 12. Vent pipeline a; 13. Discharge pipeline; 14. Cooling coil; 15. Transfer pump; 2. Neutralization kettle; 21. Liquid caustic soda inlet; 22. Vent pipeline b; 23. On-line pH meter; 24. Transfer port; 25. Liquid caustic soda content measuring device; 3. Cooling kettle; 31. Flushing port; 32. Vent pipeline c; 33. Discharge port; 4. Stirring motor; 5. Stirring paddle; 6. Vacuum filtration trough group. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0015] The present utility model will be further described below with reference to the accompanying drawings.

[0016] Embodiment: As Figure 1As shown in the figure, a continuous crystallization device for glyphosate production includes a cooling kettle 1, a neutralization kettle 2, and a cooling kettle 3. The cooling kettle 1, the neutralization kettle 2, and the cooling kettle 3 have the same structure, are arranged continuously in sequence, and are each composed of a kettle body, a kettle cover, a stirring motor 4 fixedly installed above the kettle cover, and a stirring paddle 5 concentrically connected to the stirring motor 4. Among them, on the left side of the upper end of the cooling kettle 1, there are a feed pipeline 11 and an exhaust pipeline a12, in the middle of the lower end, there is a discharge pipeline 13, and inside, there is a cooling coil 14. Liquid flow meters and solenoid valves are installed on both the feed pipeline 11 and the discharge pipeline 13, and the discharge pipeline 13 is connected to the feed port of the neutralization kettle 2 through a transfer pump 15. The exhaust pipeline a12 is externally connected to a gas purification treatment device; on the left side of the upper end of the neutralization kettle 2, there is a liquid caustic soda inlet 21 and an exhaust pipeline b22, on the right side of the upper end, there is an on-line pH meter 23, and in the middle of the lower end, there is a transfer port 24. Among them, the liquid caustic soda inlet 21 is externally connected to a liquid caustic soda feed pipeline, and a control valve and a liquid caustic soda content measuring device 25 are installed on the liquid caustic soda feed pipeline. The exhaust pipeline b22 is externally connected to a gas purification treatment device, and the transfer port 24 is communicated with the injection port of the cooling kettle 3 through a transfer channel; on the left side of the upper end of the cooling kettle 3, there is a flushing port 31 and an exhaust pipeline c32, in the middle of the lower end, there is a discharging port 33. Among them, the flushing port 31 is externally connected to a flushing water pipeline, the exhaust pipeline c32 is externally connected to a gas purification treatment device, and the discharging port 33 is externally connected to a suction filtration tank group 6 through a discharging pipeline.

[0017] The kettle bodies of the cooling kettle 1, the neutralization kettle 2, and the cooling kettle 3 are all provided with a sandwich layer, and cooling circulating water is introduced into the sandwich layer. Cold water cooling operations can be carried out using the sandwich layer; the stirring motors 4 in the cooling kettle 1, the neutralization kettle 2, and the cooling kettle 3 are all variable-frequency motors, and a wire mesh is arranged outside the stirring motor 4; between the kettle body and the kettle cover of the cooling kettle 1, the neutralization kettle 2, and the cooling kettle 3, they are all connected by bolts for positioning, and gaskets are additionally installed between the kettle body and the kettle cover; on the kettle covers of the cooling kettle 1, the neutralization kettle 2, and the cooling kettle 3, on-line thermometers and radar level gauges are installed, and the on-line thermometer, the radar level gauge, the on-line pH meter 23, and the liquid flow meter are all connected to the background control system through a data transmission module. With this structure, during the production and processing process, the measurement results can be transmitted to the control system in real time, so as to facilitate calculation and analysis according to the remote transmission results, and then remote control and adjustment can be carried out, reducing on-site manual sampling and measurement analysis. While the operation is safer and more convenient, the overall automation degree of the equipment is high; the suction filtration tank group 6 is composed of multiple suction filtration tanks connected in sequence. With this structure, the suction filtration tanks can work independently or simultaneously, reducing material backlog and improving production efficiency; the cooling kettle 1, the neutralization kettle 2, and the cooling kettle 3 are all made of glass-lined material.

[0018] When the utility model is in use, first, the high-temperature material after desolvation of the glyphosate hydrolysis solution is added into the internal part of the cooling kettle 1 through the feed pipeline 11. At this time, by using the cooling circulating water in the cooling coil 14 and the interlayer between the inner wall of the kettle body of the cooling kettle 1, and cooperating with the stirring motor 4 to drive the stirring paddle 5 to uniformly stir the materials inside the cooling kettle 1, the materials inside the cooling kettle 1 can be uniformly cooled. During this process, by using a dual cooling mode, the cooling speed and cooling effect during the use of the cooling kettle 1 are improved. Then, the materials after being cooled once by the cooling kettle 1 are added into the neutralization kettle 2 through the discharge pipeline 13 and under the action of the transfer pump 15 through the feed port. At this time, by using the cooling circulating water in the interlayer between the inner wall of the kettle body of the neutralization kettle 2, and cooperating with the stirring motor 4 to drive the stirring paddle 5 to uniformly stir the materials inside the neutralization kettle 2, the materials added into the neutralization kettle 2 can be cooled for the second time. During this process, the pH value of the materials inside the neutralization kettle 2 is measured by using the on-line pH meter 23. According to the measurement result, liquid caustic soda is added into the neutralization kettle 2 through the liquid caustic soda inlet 21, and through the acid-base neutralization reaction, the pH value of the materials is neutralized and controlled. Finally, the materials after being neutralized and cooled for the second time are injected into the cooling kettle 3 through the transfer port 24, the transfer channel and the injection port. At this time, by using the cooling circulating water in the interlayer between the inner wall of the cooling kettle 3, and cooperating with the stirring motor 4 above the cooling kettle 3 to drive the stirring paddle 5 to uniformly stir the materials inside it, the materials added into the cooling kettle 3 can be cooled for the third time, so as to control the temperature of the materials to the optimal temperature required by the crystallization section. During this process, by using the flushing water pipeline externally connected to the flushing port 31, the problem of material blockage can be avoided;

[0019] The utility model gradually cools and crystallizes the desolvated materials in three stages through the cooling kettle 1, the neutralization kettle 2 and the cooling kettle 3 in sequence, so that the temperature control of the whole process is more stable, the crystallization effect is better, and the danger of multiple operations in a single kettle is avoided. At the same time, continuous feeding and discharging are realized, and the continuous production of the glyphosate crystallization section is achieved, breaking the existing glyphosate crystallization mode and improving the production efficiency of glyphosate. And, the utility model is provided with an on-line thermometer, a radar level gauge, an on-line pH meter 23, and a liquid flowmeter, and these measuring instruments are all connected to the background control system through a data transmission module. By adopting this structure, it is convenient to transmit the measurement results to the control system in real time during the production and processing process, so as to perform calculation and analysis according to the remote transmission results, and then perform remote control and adjustment, reducing on-site manual sampling and measurement analysis. While the operation is safer and more convenient, the overall automation degree of the equipment is high. Generally, the utility model has the advantages of time-saving, convenient and high production efficiency.

[0020] The above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit it. Although the present invention has been described in detail with reference to the above embodiments, those of ordinary skill in the art should understand that it is still possible to modify the specific implementation manners of the present invention or make equivalent replacements. Any modification or equivalent replacement that does not depart from the spirit and scope of the present invention shall be covered by the scope of the claims of the present invention.

Claims

1. A continuous crystallization device for glyphosate production, comprising a cooling kettle (1), a neutralization kettle (2) and a cooling kettle (3), characterized in that: The cooling kettle (1), the neutralization kettle (2) and the cooling kettle (3) have the same structure and are arranged in sequence. They are all composed of a kettle body, a kettle cover, a stirring motor (4) fixedly installed above the kettle cover and a stirring paddle (5) coaxially connected to the stirring motor (4). A feed pipe (11) and an exhaust pipe a (12) are arranged on the left side of the upper end of the cooling kettle (1), and a discharge pipe (13) is arranged in the middle of the lower end. A cooling coil (14) is arranged inside. A liquid flow meter and a solenoid valve are installed on the feed pipe (11) and the discharge pipe (13). The discharge pipe (13) is connected to the feed port of the neutralization kettle (2) through a transfer pump (15). The exhaust pipe a (12) is externally connected to a gas purification treatment device. The neutralization kettle (2) is provided with a liquid alkali inlet (21) and an emptying pipe b (22) on the left side of the upper end, an online pH meter (23) is installed on the right side of the upper end, and a material transfer port (24) is provided in the middle of the lower end, wherein the liquid alkali inlet (21) is externally connected to a liquid alkali feeding pipe, and a control valve and a liquid alkali content measuring device (25) are installed on the liquid alkali feeding pipe, the emptying pipe b (22) is externally connected to a gas purification treatment device, and the material transfer port (24) is connected to the injection port of the cooling kettle (3) through a material transfer channel; The left side of the upper end of the cooling kettle (3) is provided with a flushing port (31) and an emptying pipe c (32), and the middle part of the lower end is provided with a discharge port (33), wherein the flushing port (31) is externally connected to a flushing water pipe, the emptying pipe c (32) is externally connected to a gas purification treatment device, and the discharge port (33) is externally connected to a suction filtration tank group (6) through the discharge pipe.

2. A continuous crystallization device for glyphosate production as claimed in claim 1, characterized in that: The kettle bodies of the temperature-reducing kettle (1), the neutralizing kettle (2) and the cooling kettle (3) are all provided with interlayers, and cooling circulating water is introduced into the interlayers.

3. A continuous crystallization device for glyphosate production as claimed in claim 1, characterized in that: The stirring motors (4) in the cooling kettle (1), the neutralization kettle (2) and the cooling kettle (3) are all variable frequency motors, and a wire mesh is arranged outside the stirring motor (4).

4. A continuous crystallization device for glyphosate production as claimed in claim 1, characterized in that: The kettle bodies and kettle covers in the cooling kettle (1), the neutralization kettle (2) and the cooling kettle (3) are all connected in a limited position by bolts, and a gasket is installed between the kettle body and the kettle cover.

5. A continuous crystallization device for glyphosate production as claimed in claim 1, characterized in that: The kettle covers of the cooling kettle (1), the neutralization kettle (2) and the cooling kettle (3) are all equipped with online thermometers and radar level gauges, and the online thermometers, radar level gauges, online pH meters (23) and liquid flow meters are all connected to the background control system via a data transmission module.

6. A continuous crystallization device for glyphosate production as claimed in claim 1, characterized in that: The suction filtration tank group (6) is composed of a plurality of suction filtration tanks connected in sequence.

7. A continuous crystallization device for glyphosate production as claimed in claim 1, characterized in that: The temperature reduction kettle (1), the neutralization kettle (2) and the cooling kettle (3) are all made of glass-lined material.

Images