Apparatus for the preparation and isolation of acethydrazides

Abstract

This application relates to an apparatus for the preparation and separation of acetylhydrazine, belonging to the technical field of acetylhydrazine production. It includes a methyl acetate transfer tank, a hydrazine hydrate transfer tank, an acetylhydrazine synthesis reactor, a rising film preheater, a rising film evaporator, a rising film gas-liquid separator, a rising film condenser, a methyl acetate receiving tank, a rising film receiving tank, a falling film preheater, a falling film evaporator, a falling film condenser, a falling film water receiving tank, and an acetylhydrazine receiving tank. By incorporating a rising film preheater and a rising film evaporator, this application can perform preliminary preheating and evaporation treatment on the reaction materials in the acetylhydrazine synthesis reactor. Utilizing the efficient heat transfer characteristics of rising film evaporation, the residence time of materials in a high-temperature environment can be shortened, reducing the possibility of acetylhydrazine decomposition due to prolonged heating. The entire apparatus, through the combined application of rising and falling film evaporation, forms an efficient and continuous preparation and separation process, effectively solving the problems of excessively long distillation times, high energy consumption, and impurity generation in traditional distillation systems, significantly improving production efficiency and product quality.

Description

Technical Field

[0001] This application relates to the production of acetylhydrazine, and more particularly to an apparatus for the preparation and separation of acetylhydrazine. Background Technology

[0002] Acetylhydrazine is an important chemical raw material used in the synthesis of analgesics, anticancer drugs, dental erosion inhibitors, flake activity index inhibitors, antifogging agents and stabilizers for color fixing solutions, and metal pickling preservatives. Acetylhydrazine is a white crystalline substance and an important organic synthesis intermediate. In pesticides, it is an intermediate for the insecticide pyrazinone and the herbicide benzoyl sulfadiazine. In pharmaceuticals, it is mainly used in the synthesis of nifuran.

[0003] The current preparation process of acetylhydrazine is complex, often requiring catalysts that are difficult to recover. In existing technologies, methyl acetate and hydrazine hydrate are fed into the acetylhydrazine synthesis reactor via flow meters for methyl acetate and hydrazine hydrate, respectively, and then transferred to an acetylhydrazine distillation reactor for continuous high-temperature distillation. The distillate is then transferred to an acetylhydrazine transfer tank. The disadvantages of this method are excessively long distillation time, low production efficiency, and high energy consumption. During distillation, acetylhydrazine is exposed to a high-temperature environment for an extended period, leading to thermal decomposition and the generation of thermal decomposition impurities. These impurities may cause pipeline blockages and substandard acetylhydrazine quality. To address these issues, a preparation and separation device for acetylhydrazine is proposed. Utility Model Content

[0004] The purpose of this application is to provide a device for the preparation and separation of acetylases, which has the advantages of improving production efficiency, reducing energy consumption, and reducing the generation of impurities from the thermal decomposition of acetylases. It solves the problems of low production efficiency and high energy consumption caused by excessively long distillation time in the existing acetylases preparation process, as well as the problem that acetylases are prone to thermal decomposition at high temperatures, which generates impurities and leads to pipeline blockage and substandard product quality.

[0005] The acetylhydrazine preparation and separation apparatus provided in this application adopts the following technical solution: it includes a methyl acetate transfer tank, a hydrazine hydrate transfer tank, an acetylhydrazine synthesis reactor, a rising film preheater, a rising film evaporator, a rising film gas-liquid separator, a rising film condenser, a methyl acetate receiving tank, a rising film receiving tank, a falling film preheater, a falling film evaporator, a falling film condenser, a falling film water receiving tank, an acetylhydrazine receiving tank, a rising film feed pump, a receiving tank transfer pump, a methyl acetate transfer pump, and an acetylhydrazine transfer pump. The bottom of the methyl acetate transfer tank and the bottom of the hydrazine hydrate transfer tank are both connected to the top of the acetylhydrazine synthesis reactor through pipelines. The bottom of the acetylation hydrazine synthesis reactor is connected to the input end of the rising film feed pump via a pipe. The output end of the rising film feed pump is connected to the inlet of the rising film preheater. The bottom of the rising film evaporator is connected to the outlet of the rising film preheater via a pipe. The top of the rising film evaporator is connected to the inside of the rising film gas-liquid separator via a pipe. The bottom of the rising film gas-liquid separator is connected to the top of the rising film receiving tank via a pipe. The bottom of the rising film receiving tank is connected to the input end of the receiving tank transfer pump via a pipe. The output end of the receiving tank transfer pump is connected to the inlet of the rising film preheater and the inlet of the falling film preheater. The inlet of the falling film evaporator is connected to the outlet of the falling film preheater via a pipe, the top of the falling film evaporator is connected to the top of the falling film condenser via a pipe, the bottom of the falling film condenser is connected to the top of the falling film water receiving tank via a pipe, and the bottom of the falling film evaporator is connected to the top of the acetylhydrazine receiving tank via a pipe. By adopting the above technical solution and setting up a rising film preheater and a rising film evaporator, the reactants in the acetylass synthesis reactor can be preheated and evaporated. Utilizing the efficient heat transfer characteristics of rising film evaporation, the residence time of the materials in the high-temperature environment can be shortened, reducing the possibility of acetylass decomposition due to prolonged heating. The entire device, through the combined application of rising film and falling film evaporation, forms an efficient and continuous preparation and separation process, effectively solving the problems of excessively long distillation time, high energy consumption, and impurity generation in traditional distillation systems, and significantly improving production efficiency and product quality.

[0006] Preferably, a methyl acetate flow meter is installed on the bottom pipe of the methyl acetate transfer tank, a hydrazine hydrate flow meter is installed on the bottom pipe of the hydrazine hydrate transfer tank, a rising film flow meter is installed on the bottom pipe of the rising film evaporator, and a falling film flow meter is installed on the inlet pipe of the falling film evaporator. By adopting the above technical solution and setting multiple flow meters, the flow rates of methyl acetate, hydrazine hydrate, and materials entering the rising film evaporator and falling film evaporator can be monitored and precisely controlled in real time. This allows operators to adjust the feed rate of materials according to process requirements by observing the readings of each flow meter, ensuring that methyl acetate and hydrazine hydrate enter the reaction system in the set ratio, and avoiding the impact on reaction efficiency and product purity due to material imbalance.

[0007] Preferably, the top of the rising film gas-liquid separator is connected to the top of the rising film condenser via a pipe, the bottom of the rising film condenser is connected to the top of the methyl acetate receiving tank via a pipe, the bottom of the methyl acetate receiving tank is connected to the input end of the methyl acetate transfer pump via a pipe, and the output end of the methyl acetate transfer pump is located inside the methyl acetate transfer tank. By adopting the above technical solution, and by setting up a circulation system consisting of a rising film gas-liquid separator, a rising film condenser, a methyl acetate receiving tank, and a methyl acetate transfer pump, the methyl acetate vapor generated during the rising film evaporation process can be effectively recovered. When the material in the rising film evaporator is heated and evaporated, the vapor enters the rising film gas-liquid separator to achieve gas-liquid separation. The separated methyl acetate vapor enters the rising film condenser to condense into liquid, and then flows into the methyl acetate receiving tank for temporary storage. The recovered methyl acetate is then transported back to the methyl acetate transfer tank by the methyl acetate transfer pump, so that the unreacted methyl acetate can be recycled. This not only reduces raw material consumption and production costs, but also reduces waste emissions and improves resource utilization.

[0008] Preferably, the bottom of the acetylass receiving tank is connected to the input end of the acetylass transfer pump via a pipe, and the output end of the acetylass transfer pump is connected to the inlet of the falling film preheater; By adopting the above technical solution, and by setting up a material conveying path consisting of an acetylated hydrazine receiving tank, an acetylated hydrazine transfer pump, and a falling film preheater, problems such as excessive moisture content and substandard quality of acetylated hydrazine encountered during production can be effectively addressed. Substandard acetylated hydrazine is further processed through the falling film stage via the acetylated hydrazine transfer pump. The falling film preheater preheats the acetylated hydrazine material, raising its temperature to a suitable level for subsequent falling film evaporation operations. This effectively improves the efficiency and effect of falling film evaporation and reduces heat consumption during subsequent evaporation processes.

[0009] Preferably, the top and bottom of the acetylass synthesis reactor are respectively provided with a feed pipe and a discharge pipe, the bottom of the methyl acetate transfer tank and the bottom of the hydrazine hydrate transfer tank are connected to the input end of the feed pipe, and the output end of the discharge pipe is connected to the input end of the rising film feed pump; By adopting the above technical solution and setting up the feed pipe and discharge pipe of the acetylhydrazine synthesis reactor, an efficient channel for raw material input and product output is constructed.

[0010] Preferably, a heating plate is provided on the surface of the acetylhydrazine synthesis reactor, a heating tube is provided inside the heating plate, and a heat-retaining pad and a heat-insulating pad are respectively provided inside and outside the heating plate; By adopting the above technical solution, and by setting up a heating plate and its internal heating tubes, a stable heat source can be provided for the reaction in the acetylhydrazine synthesis reactor, ensuring that the reaction is carried out under suitable temperature conditions. The heat-concentrating pads and insulation pads inside and outside the heating plate can effectively reduce heat loss. The heat-concentrating pads can concentrate the heat generated by the heating tubes and guide it into the reactor, improving heat utilization efficiency. The insulation pads can prevent heat from diffusing to the external environment and maintain the stability of the temperature inside the reactor, thereby promoting the full reaction of raw materials and improving the synthesis rate and yield of acetylhydrazine.

[0011] Preferably, the top of the acetylhydrazine synthesis reactor is provided with a fixed shell, and a rotating rod is tightly nested on the top of the acetylhydrazine synthesis reactor via a bearing. A wire is provided inside the rotating rod, and multiple heating blocks are provided on the surface of the rotating rod. Heating wires are provided inside the heating blocks. A temperature sensor is provided on the surface of the acetylhydrazine synthesis reactor, and multiple temperature sensors are provided on the inner wall of the acetylhydrazine synthesis reactor. By adopting the above technical solution and setting multiple heating blocks distributed on the surface of the rotating rod, the raw materials in different areas of the reactor can be uniformly heated during the rotation process. Combined with the heat output of the heating wire, the uniformity of the temperature inside the reactor is further improved. The thermometer can display the temperature inside the reactor in real time, which is convenient for operators to monitor the reaction environment. The multiple temperature sensors set on the inner wall can collect temperature data at multiple points, which can ensure accurate control of the temperature status inside the reactor.

[0012] Preferably, a first gear is fixedly connected to the surface of the rotating rod, a rotary motor is fixedly connected to the top of the fixed shell through multiple support frames, the output end of the rotary motor rotates through the top of the fixed shell and is fixedly connected to a second gear, the second gear meshes with the first gear, and an agitator is fixedly connected to the surface of the rotating rod. By adopting the above technical solution, and by setting up a rotary motor, the rotary motor can drive the rotating rod to rotate stably through the meshing transmission of the second gear and the first gear, thereby enabling the stirring blade to fully stir the raw materials in the reactor, promoting uniform mixing and reaction contact between the raw materials.

[0013] In summary, this application includes at least one of the following beneficial technical effects: This apparatus for the preparation and separation of acetylhydrazine utilizes a rising film preheater and a rising film evaporator to preheat and evaporate the reactants in the acetylhydrazine synthesis reactor. Leveraging the high-efficiency heat transfer characteristics of rising film evaporation, the residence time of materials in the high-temperature environment is shortened, reducing the possibility of decomposition of acetylhydrazine due to prolonged heating. The rising film gas-liquid separator effectively separates the gas and liquid phases generated during evaporation. After the liquid phase enters the rising film receiving tank, a portion of the material is returned to the outlet of the rising film preheater for secondary evaporation via a transfer pump, improving material processing efficiency. Then, another portion of the material is conveyed to the falling film preheater to prepare for the subsequent falling film evaporation process. The falling film evaporator further performs deep evaporation and separation of the material. The falling film condenser connected to the top can condense the vapor generated by evaporation into liquid and collect it in the falling film water receiving tank. The acetylhydrazine receiving tank at the bottom is used to collect the acetylhydrazine product obtained by the final separation. The entire device forms an efficient and continuous preparation and separation process through the combined application of rising film and falling film evaporation. It effectively solves the problems of excessive time, high energy consumption and impurity generation in traditional distillation stations, and significantly improves production efficiency and product quality. Attached Figure Description

[0014] Figure 1 This is a schematic diagram of the structure of an embodiment of the present utility model; Figure 2 This is a schematic diagram of the falling film preheater in this application; Figure 3 This is a schematic diagram of the acetylhydrazine synthesis reactor in this application; Figure 4 for Figure 3 Enlarged structural diagram at point A; Figure 5 for Figure 3 Enlarged structural diagram at point B.

[0015] In the diagram: 1. Methyl acetate transfer tank; 2. Hydrazine hydrate transfer tank; 3. Methyl acetate flow meter; 4. Hydrazine hydrate flow meter; 5. Acetylhydrazine synthesis reactor; 6. Rising film preheater; 7. Rising film flow meter; 8. Rising film evaporator; 9. Rising film gas-liquid separator; 10. Rising film condenser; 11. Methyl acetate receiving tank; 12. Rising film receiving tank; 13. Falling film preheater; 14. Falling film flow meter; 15. Falling film evaporator; 16. Falling film condenser; 17. Falling film water receiving tank; 18. Acetylhydrazine receiving tank; 19. Rising film feed pump; 20. Receiving tank transfer pump; 21. Methyl acetate transfer pump; 22. Acetylhydrazine transfer pump; 501. Feed pipe; 502. Discharge pipe; 503. Heating plate; 504. Heating tube; 505. Heat-concentrating pad; 506. Insulation pad; 507. Fixed shell; 508. Rotating rod; 509. First gear; 5010. Support frame; 5011. Rotary motor; 5012. Second gear; 5013. Wire; 5014. Heating block; 5015. Heating wire; 5016. Stirring blade; 5017. Temperature sensor; 5018. Temperature sensor. Detailed Implementation

[0016] The following is in conjunction with the appendix Figure 1 - Appendix Figure 5 This application will be described in further detail below.

[0017] Example 1: An apparatus for the preparation and separation of acetylhydrazine, referring to... Figure 1 and Figure 2The reactor includes a methyl acetate transfer tank 1, a hydrazine hydrate transfer tank 2, an acetylhydrazine synthesis reactor 5, a rising film preheater 6, a rising film evaporator 8, a rising film gas-liquid separator 9, a rising film condenser 10, a methyl acetate receiving tank 11, a rising film receiving tank 12, a falling film preheater 13, a falling film evaporator 15, a falling film condenser 16, a falling film water receiving tank 17, an acetylhydrazine receiving tank 18, a rising film feed pump 19, a receiving tank transfer pump 20, a methyl acetate transfer pump 21, and an acetylhydrazine transfer pump 22. The bottoms of the methyl acetate transfer tank 1 and the hydrazine hydrate transfer tank 2 are both connected to the top of the acetylhydrazine synthesis reactor 5 via pipes. The bottom of the acetylation hydrazine synthesis reactor 5 is connected to the input end of the rising film feed pump 19 via a pipe. The output end of the rising film feed pump 19 is connected to the inlet of the rising film preheater 6. The bottom of the rising film evaporator 8 is connected to the outlet of the rising film preheater 6 via a pipe. The top of the rising film evaporator 8 is connected to the inside of the rising film gas-liquid separator 9 via a pipe. The bottom of the rising film gas-liquid separator 9 is connected to the top of the rising film receiving tank 12 via a pipe. The bottom of the rising film receiving tank 12 is connected to the input end of the receiving tank transfer pump 20 via a pipe. The output end of the receiving tank transfer pump 20 is connected to the outlet of the rising film preheater 6 and the inlet of the falling film preheater 13. The inlet of the falling film evaporator 15 is connected to the outlet of the falling film preheater 13 via a pipe. The top of the falling film evaporator 15 is connected to the top of the falling film condenser 16 via a pipe. The bottom of the falling film condenser 16 is connected to the top of the falling film water receiving tank 17 via a pipe. The bottom of the falling film evaporator 15 is connected to the top of the acetylhydrazine receiving tank 18 via a pipe. By setting up the rising film preheater 6 and the rising film evaporator 8, the reaction materials in the acetylhydrazine synthesis kettle 5 can be preheated and evaporated. Utilizing the efficient heat transfer characteristics of rising film evaporation, the residence time of the materials in the high-temperature environment can be shortened, reducing the possibility of acetylhydrazine decomposition due to prolonged heating. Among them, the rising film gas-liquid separator 9 can effectively separate the gas phase and liquid phase generated during the evaporation process. After the liquid phase material enters the rising film receiving tank 12... The receiving tank transfer pump 20 allows some material to be returned to the outlet of the rising film preheater 6 for secondary evaporation, improving material processing efficiency. Then, another part of the material is transported to the falling film preheater 13 to prepare for the subsequent falling film evaporation process. The falling film evaporator 15 further performs deep evaporation and separation of the material. The falling film condenser 16 connected to its top can condense the vapor generated by evaporation into liquid and collect it in the falling film water receiving tank 17. The acetylhydrazine receiving tank 18 at the bottom is used to collect the acetylhydrazine product obtained by the final separation. The entire device forms an efficient and continuous preparation and separation process through the combined application of rising film and falling film evaporation, effectively solving the problems of excessive time, high energy consumption and impurity generation in traditional distillation stations, and significantly improving production efficiency and product quality.

[0018] Please see Figure 1 and Figure 2A methyl acetate flow meter 3 is installed on the bottom pipe of the methyl acetate transfer tank 1, a hydrazine hydrate flow meter 4 is installed on the bottom pipe of the hydrazine hydrate transfer tank 2, a rising film flow meter 7 is installed on the bottom pipe of the rising film evaporator 8, and a falling film flow meter 14 is installed on the inlet pipe of the falling film evaporator 15. By installing multiple flow meters, the flow rates of methyl acetate, hydrazine hydrate, and materials entering the rising film evaporator 8 and the falling film evaporator 15 can be monitored and precisely controlled in real time. This allows operators to adjust the material flow rate according to process requirements by observing the readings of each flow meter. The feed rate is set to ensure that methyl acetate and hydrazine hydrate enter the reaction system in the set ratio, avoiding the impact of material imbalance on reaction efficiency and product purity. The top of the rising film gas-liquid separator 9 is connected to the top of the rising film condenser 10 via a pipe, and the bottom of the rising film condenser 10 is connected to the top of the methyl acetate receiving tank 11 via a pipe. The bottom of the methyl acetate receiving tank 11 is connected to the input end of the methyl acetate transfer pump 21 via a pipe. The output end of the methyl acetate transfer pump 21 is located in the methyl acetate transfer tank 1. By setting up the rising film gas-liquid separator 9, the rising film condenser 10, and the methyl acetate transfer pump 21, the reaction system can be effectively controlled. The circulating system formed by the methyl acetate receiving tank 11 and the methyl acetate transfer pump 21 can effectively recover the methyl acetate vapor generated during the rising film evaporation process. After the material in the rising film evaporator 8 is heated and evaporated, the vapor enters the rising film gas-liquid separator 9 to achieve gas-liquid separation. The separated methyl acetate vapor enters the rising film condenser 10 to condense into liquid, and then flows into the methyl acetate receiving tank 11 for temporary storage. The recovered methyl acetate is then transported back to the methyl acetate transfer tank 1 by the methyl acetate transfer pump 21, so that the unreacted methyl acetate can be recycled. This reduces raw material consumption and production costs, decreases waste emissions, and improves resource utilization. The bottom of the acetylass receiving tank 18 is connected to the input of the acetylass transfer pump 22 via a pipe, and the output of the acetylass transfer pump 22 is connected to the inlet of the falling film preheater 13. By setting up the material conveying path formed by the acetylass receiving tank 18, the acetylass transfer pump 22, and the falling film preheater 13, problems such as excessive moisture content and substandard quality of acetylas encountered during production can be effectively addressed. Substandard acetylas is then reprocessed in the falling film stage via the acetylass transfer pump 22. The falling film preheater 13 preheats the acetylas material, raising its temperature to a suitable level for subsequent falling film evaporation operations. This effectively improves the efficiency and effect of falling film evaporation and reduces heat consumption during subsequent evaporation processes.

[0019] Please see Figure 3 , Figure 4 and Figure 5The acetylhydrazine synthesis reactor 5 is equipped with a feed pipe 501 at the top and a discharge pipe 502 at the bottom. The bottom of the methyl acetate transfer tank 1 and the bottom of the hydrazine hydrate transfer tank 2 are connected to the input end of the feed pipe 501, and the output end of the discharge pipe 502 is connected to the input end of the rising film feed pump 19. By setting the feed pipe 501 and discharge pipe 502 of the acetylhydrazine synthesis reactor 5, an efficient channel for raw material input and product output is constructed. A heating plate 503 is set on the surface of the acetylhydrazine synthesis reactor 5, and a heating pipe 504 is set inside the heating plate 503. A heat-retaining pad 505 and a heat-insulating pad 506 are set inside and outside the heating plate 503, respectively. By setting the heating plate 503 and the heating pipe 504 inside it, the reaction inside the acetylhydrazine synthesis reactor 5 can be energized. A stable heat source is provided to ensure the reaction proceeds under suitable temperature conditions. The heat-concentrating pads 505 and insulation pads 506 inside and outside the heating plate 503 effectively reduce heat loss. The heat-concentrating pad 505 concentrates the heat generated by the heating tube 504 and directs it into the reactor, improving heat utilization efficiency. The insulation pad 506 prevents heat from diffusing to the external environment, maintaining the stability of the reactor temperature. This promotes the full reaction of the raw materials and increases the synthesis rate and yield of acetylass. A fixed shell 507 is provided at the top of the acetylass synthesis reactor 5. A rotating rod 508 is tightly nested at the top of the acetylass synthesis reactor 5 via bearings. A wire 5013 is installed inside the rotating rod 508, and multiple heating blocks are installed on the surface of the rotating rod 508. 5014, a heating block 5014 is internally equipped with a heating wire 5015, a thermometer 5017 is installed on the surface of the acetylhydrazine synthesis reactor 5, and multiple temperature sensors 5018 are installed on the inner wall of the acetylhydrazine synthesis reactor 5. By distributing multiple heating blocks 5014 on the surface of the rotating rod 508, the raw materials in different areas of the reactor can be uniformly heated during rotation. Combined with the heat output of the heating wire 5015, the uniformity of the temperature inside the reactor is further improved. The thermometer 5017 can display the temperature inside the reactor in real time, which is convenient for operators to monitor the reaction environment, while the multiple temperature sensors 5018 on the inner wall can collect temperature data at multiple points, which can ensure accurate control of the temperature status inside the reactor. The rotating rod 5018... A first gear 509 is fixedly connected to the surface of the rotating rod 508. A rotary motor 5011 is fixedly connected to the top of the fixed shell 507 via multiple support frames 5010. The output end of the rotary motor 5011 rotates through the top of the fixed shell 507 and is fixedly connected to a second gear 5012. The second gear 5012 meshes with the first gear 509. An agitator 5016 is fixedly connected to the surface of the rotating rod 508. By setting the rotary motor 5011, the operation of the rotary motor 5011, through the meshing transmission of the second gear 5012 and the first gear 509, can drive the rotating rod 508 to rotate stably, thereby enabling the agitator 5016 to fully stir the raw materials in the reactor, promoting uniform mixing and reaction contact between the raw materials.

[0020] The implementation principle of this application embodiment is as follows: First, methyl acetate in methyl acetate transfer tank 1 and hydrazine hydrate in hydrazine hydrate transfer tank 2 are transported to acetylhydrazine synthesis reactor 5 through bottom pipe and feed pipe 501 according to the set ratio. At this time, heating tube 504 in heating plate 503 starts to work, and together with heat-insulating pad 505 and heat-preserving pad 506, it provides stable heat for the reaction. At the same time, rotary motor 5011 starts, and drives rotary rod 508 and stirring blade 5016 to rotate through gear transmission to stir and mix the raw materials. Heating block 5014 and heating wire 5015 on the surface of rotary rod 508 assist in heating to ensure that the temperature in the reactor is uniform and meets the reaction requirements. Temperature sensor 5018 monitors the temperature in real time and displays it through temperature display 5017. After the reaction is completed, the material at the bottom of the acetylhydrazine synthesis reactor 5 enters the rising film feed pump 19 through the discharge pipe 502, and is then transported to the rising film preheater 6 for preheating. The preheated material enters the rising film evaporator 8, where it is heated and evaporated. The resulting gas-liquid mixture enters the rising film gas-liquid separator 9 for separation. The liquid phase material flows into the rising film receiving tank 12. Part of the material is returned to the outlet of the rising film preheater 6 for secondary evaporation via the receiving tank transfer pump 20, while the other part is transported to the falling film preheater 13. The gas phase separated by the rising film gas-liquid separator 9 enters the rising film condenser 10 and is condensed into liquid, which flows into the methyl acetate receiving tank 11 and is then sent back to the methyl acetate transfer tank 1 for recycling via the methyl acetate transfer pump 21. After the material enters the falling film preheater 13, it enters the falling film evaporator 15. The vapor generated by evaporation enters the falling film condenser 16 for condensation, and the liquid is collected in the falling film water receiving tank 17. The acetylhydrazine material at the bottom of the falling film evaporator 15 enters the acetylhydrazine receiving tank 18. Throughout the process, various flow meters can monitor and control the material flow in real time to ensure the continuous and efficient operation of the device.

Claims

1. An apparatus for the preparation and separation of acetylhydrazine, comprising a methyl acetate transfer tank (1), a hydrazine hydrate transfer tank (2), an acetylhydrazine synthesis vessel (5), a rising film preheater (6), a rising film evaporator (8), a rising film gas-liquid separator (9), a rising film condenser (10), a methyl acetate receiving tank (11), a rising film receiving tank (12), a falling film preheater (13), a falling film evaporator (15), a falling film condenser (16), a falling film water receiving tank (17), an acetylhydrazine receiving tank (18), a rising film feed pump (19), a receiving tank transfer pump (20), a methyl acetate transfer pump (21), and an acetylhydrazine transfer pump (22), characterized in that: The bottom of the methyl acetate transfer tank (1) and the bottom of the hydrazine hydrate transfer tank (2) are both connected to the top of the acetylhydrazine synthesis reactor (5) via pipes; The bottom of the acetylhydrazine synthesis reactor (5) is connected to the input end of the rising film feed pump (19) via a pipe. The output end of the rising film feed pump (19) is connected to the inlet of the rising film preheater (6). The bottom of the rising film evaporator (8) is connected to the outlet of the rising film preheater (6) via a pipe. The top of the rising film evaporator (8) is connected to the inside of the rising film gas-liquid separator (9) via a pipe. The bottom of the rising film gas-liquid separator (9) is connected to the top of the rising film receiving tank (12) via a pipe. The bottom of the rising film receiving tank (12) is connected to the input end of the receiving tank transfer pump (20) via a pipe. The output end of the receiving tank transfer pump (20) is connected to the inlet of the rising film preheater (6) and the inlet of the falling film preheater (13). The inlet of the falling film evaporator (15) is connected to the outlet of the falling film preheater (13) via a pipe. The top of the falling film evaporator (15) is connected to the top of the falling film condenser (16) via a pipe. The bottom of the falling film condenser (16) is connected to the top of the falling film water receiving tank (17) via a pipe. The bottom of the falling film evaporator (15) is connected to the top of the acetylhydrazine receiving tank (18) via a pipe.

2. The apparatus for preparing and separating acetylhydrazine according to claim 1, characterized in that: A methyl acetate flow meter (3) is installed on the bottom pipe of the methyl acetate transfer tank (1), a hydrazine hydrate flow meter (4) is installed on the bottom pipe of the hydrazine hydrate transfer tank (2), a rising film flow meter (7) is installed on the bottom pipe of the rising film evaporator (8), and a falling film flow meter (14) is installed on the inlet pipe of the falling film evaporator (15).

3. The apparatus for preparing and separating acetylhydrazine according to claim 1, characterized in that: The top of the rising film gas-liquid separator (9) is connected to the top of the rising film condenser (10) via a pipe. The bottom of the rising film condenser (10) is connected to the top of the methyl acetate receiving tank (11) via a pipe. The bottom of the methyl acetate receiving tank (11) is connected to the input end of the methyl acetate transfer pump (21) via a pipe. The output end of the methyl acetate transfer pump (21) is located in the methyl acetate transfer tank (1).

4. The apparatus for preparing and separating acetylhydrazine according to claim 1, characterized in that: The bottom of the acetylhydrazine receiving tank (18) is connected to the input end of the acetylhydrazine transfer pump (22) via a pipe, and the output end of the acetylhydrazine transfer pump (22) is connected to the inlet of the falling film preheater (13).

5. The apparatus for preparing and separating acetylhydrazine according to claim 1, characterized in that: The top and bottom of the acetylhydrazine synthesis reactor (5) are respectively provided with a feed pipe (501) and a discharge pipe (502). The bottom of the methyl acetate transfer tank (1) and the bottom of the hydrazine hydrate transfer tank (2) are connected to the input end of the feed pipe (501), and the output end of the discharge pipe (502) is connected to the input end of the rising film feed pump (19).

6. The apparatus for preparing and separating acetylhydrazine according to claim 1, characterized in that: The surface of the acetylhydrazine synthesis reactor (5) is provided with a heating plate (503), the heating plate (503) is provided with a heating tube (504), and the heating plate (503) is provided with a heat-retaining pad (505) and a heat-insulating pad (506) on the inside and outside of the heating plate (503).

7. The apparatus for preparing and separating acetylhydrazine according to claim 6, characterized in that: The top of the acetylhydrazine synthesis reactor (5) is provided with a fixed shell (507). A rotating rod (508) is tightly nested on the top of the acetylhydrazine synthesis reactor (5) through a bearing. A wire (5013) is provided inside the rotating rod (508). Multiple heating blocks (5014) are provided on the surface of the rotating rod (508). A heating wire (5015) is provided inside the heating block (5014). A thermometer (5017) is provided on the surface of the acetylhydrazine synthesis reactor (5). Multiple temperature sensors (5018) are provided on the inner wall of the acetylhydrazine synthesis reactor (5).

8. The apparatus for preparing and separating acetylhydrazine according to claim 7, characterized in that: A first gear (509) is fixedly connected to the surface of the rotating rod (508). A rotary motor (5011) is fixedly connected to the top of the fixed shell (507) through multiple support frames (5010). The output end of the rotary motor (5011) rotates through the top of the fixed shell (507) and is fixedly connected to a second gear (5012). The second gear (5012) meshes with the first gear (509). An agitator (5016) is fixedly connected to the surface of the rotating rod (508).

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