An esterification column for preparing n-butyl acetate

CN224894143UActive Publication Date: 2026-10-27JINJIANG TAIXING CHEM IND CO LTD
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Patent Information

Application Number
CN202522316652.2
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2025-10-31
Publication Date
2026-10-27
Estimated Expiration
2035-10-31

AI Technical Summary

Technical Problem

[0004]为了解决工作效率较低,对酯水分离的速度较慢的问题,现有技术是采用化学反应釜、冷凝器、第一隔离层、第二隔离层和恒温加热装置搭配使用的方式进行处理,但是还会出现塔内没有配比加热装置、催化剂更换不便的情况,进而导致原料不能很好的反应以及影响加工效率的问题

Benefits of technology

[0014]由于采用了上述技术方案,本实用新型相对现有技术来说,取得的技术进步是:

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Abstract

The utility model discloses an esterification tower for preparing n - butyl acetate relates to esterification tower technical field, including bottom plate, the top surface fixed mounting of bottom plate has esterification tower main part, the one side of esterification tower main part is provided with heating unit, and the top of esterification tower main part is provided with proportioning unit, and the inside of esterification tower main part is provided with catalytic unit, and heating unit includes oil tank and interlayer hopper. The utility model discloses through the cooperation of oil tank, oil pump and interlayer hopper, can more even and efficient preheating to mixed raw material, and first temperature sensor monitors oil temperature, and second temperature sensor monitors raw material temperature, has realized accurate temperature control, has guaranteed material to enter the reaction zone with optimum temperature, through flowmeter and solenoid valve, has realized the accurate proportioning of acetic acid and n - butanol, has guaranteed higher conversion rate when reacting, and the built -in stirring paddle makes two raw materials mix more evenly in the heating process, avoids partial overheating.
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Description

Technical Field

[0001] This utility model relates to the field of esterification tower technology, specifically to an esterification tower for preparing n-butyl acetate. Background Technology

[0002] Butyl acetate is an important industrial solvent, typically produced by the esterification of acetic acid and n-butanol under a catalyst. This reaction is reversible, and traditional production processes generally employ batch reactors, which suffer from low production efficiency, high energy consumption, and difficulty in continuous operation. While subsequent tower-type esterification equipment can achieve continuous production, it still generally suffers from problems such as inconvenient catalyst replacement, long maintenance cycles, and inaccurate control of raw material ratios and preheating, leading to high operating costs and affecting product quality stability. Therefore, developing an esterification tower that is easy to operate, efficient, and maintain is of great significance.

[0003] Patent publication number CN218166992U discloses an esterification tower for the production of n-butyl acetate, comprising an esterification tower body, a chemical reaction vessel, a first condenser, a condenser, a first isolation layer, a second isolation layer, a constant temperature heating device, and a n-butyl acetate tube. The chemical reaction vessel is disposed inside the esterification tower body, and an auxiliary heating device is provided at the bottom of the chemical reaction vessel. A fixing plate is disposed on the outer surface of the esterification tower body, and a condenser is disposed on the top of the fixing plate. The first isolation layer is disposed inside the esterification tower body, a separation reaction vessel is disposed inside the esterification tower body, and the second isolation layer is disposed inside the esterification tower body.

[0004] To address the issues of low efficiency and slow ester-water separation, existing technologies employ a combination of a chemical reactor, condenser, first isolation layer, second isolation layer, and constant temperature heating device. However, this approach still faces challenges such as the lack of a proportioning heating device within the tower and inconvenience in catalyst replacement, leading to inadequate reaction of raw materials and reduced processing efficiency. Utility Model Content

[0005] The purpose of this invention is to provide an esterification tower for preparing n-butyl acetate, so as to solve the problems mentioned in the background art.

[0006] To solve the above-mentioned technical problems, the technical solution adopted by this utility model is as follows: An esterification tower for preparing n-butyl acetate includes a bottom plate, an esterification tower body fixedly mounted on the top surface of the bottom plate, a heating unit provided on one side of the esterification tower body, a proportioning unit provided at the top of the esterification tower body, and a catalytic unit provided inside the esterification tower body.

[0007] The heating unit includes an oil tank and a jacketed funnel. The oil tank is fixedly connected to the top surface of the base plate, and the surface of the jacketed funnel is fixedly connected to the top of the interior of the esterification tower body. The jacketed funnel has a jacketed cavity inside, and an oil pump, a heater, and a first temperature sensor are fixedly installed on the top surface of the oil tank.

[0008] A further improvement of this utility model is that: the input end of the oil pump is connected to the bottom of the oil tank through an oil pipe, the output end of the oil pump is connected to the bottom of the jacket cavity through an oil pipe, the top end of the jacket cavity is connected to the top surface of the oil tank through an oil pipe, a second temperature sensor is fixedly connected inside the jacket funnel, one end of the second temperature sensor extends to the outside of the esterification tower body, and the bottoms of the heater and the first temperature sensor both extend into the inside of the oil tank.

[0009] A further improvement of the present invention is that the proportioning unit includes a motor, a small bracket is fixedly connected to the outside of the motor body, the bottom of the small bracket is fixedly connected to the top surface of the esterification tower body, and a stirring paddle is fixedly connected to the output shaft of the motor, the surface of the stirring paddle is movable inside the jacketed funnel.

[0010] A further improvement of this utility model is that: an acetic acid conveying pipe and a n-butanol conveying pipe are respectively provided on both sides of the top of the jacketed funnel, one end of each of the acetic acid conveying pipe and the n-butanol conveying pipe extends through the outer shell of the esterification tower body to the outside, and a flow meter and a second solenoid valve are sequentially provided in the middle of each of the acetic acid conveying pipe and the n-butanol conveying pipe.

[0011] A further improvement of the present invention is that: the catalytic unit includes a fixed plate, the bottom end of the jacketed funnel is connected to a shower head through a conduit, a first solenoid valve is fixedly installed in the middle of the conduit, the fixed plate is located below the shower head, and sliding grooves are provided on both sides of the interior of the fixed plate. A tray is slidably connected inside the sliding groove, and a wastewater collection box is provided outside the tray. One side of the wastewater collection box is fixedly connected to the middle of the outer wall of the esterification tower body.

[0012] A further improvement of this utility model is that: a control box is fixedly installed on the surface of the oil tank, and the inside of the control box is controlled by a PLC. The first solenoid valve, the first temperature sensor, the second temperature sensor, the flow meter, and the second solenoid valve are all connected to the control box via signal. The motor and the control box are electrically connected.

[0013] A further improvement of this utility model is that: a distillation and dehydration section is provided at the bottom of the inner part of the esterification tower body, and a receiving box is movably provided at the bottom of the outer part of the esterification tower body.

[0014] Due to the adoption of the above technical solution, the technological progress achieved by this utility model compared to the prior art is as follows: This invention provides an esterification tower for preparing n-butyl acetate. Through the cooperation of an oil tank, an oil pump, and a jacketed funnel, the mixed raw materials can be preheated more uniformly and efficiently. A first temperature sensor monitors the oil temperature, and a second temperature sensor monitors the raw material temperature, achieving precise temperature control and ensuring that the materials enter the reaction zone at the optimal temperature. Through a flow meter and a solenoid valve, the precise ratio of acetic acid to n-butanol is achieved, ensuring a higher conversion rate during the reaction. The built-in stirring paddle makes the two raw materials mix more evenly during heating and avoids local overheating.

[0015] This invention provides an esterification tower for the preparation of n-butyl acetate. Through the cooperation of a fixed plate, a tray, and a wastewater collection box, when the catalyst is deactivated, there is no need to enter the tower or disassemble the equipment. The replacement can be completed simply by pulling out the tray from the side of the tower, which shortens the downtime and reduces the maintenance difficulty. The sprinkler above allows the preheated mixture to be evenly distributed on the catalyst bed, making full use of the catalyst activity and improving the reaction efficiency. Key parameters such as raw material ratio, preheating temperature, and feed switch are centrally controlled through a PLC control box. Attached Figure Description

[0016] Figure 1 This is a three-dimensional structural diagram of the present invention; Figure 2 This is a schematic diagram of the structure of this utility model from another perspective; Figure 3 This is a schematic diagram of the proportioning unit and catalytic unit of this utility model; Figure 4 This is a schematic diagram of the heating unit structure of this utility model.

[0017] In the diagram: 1. Base plate; 11. Esterification tower body; 111. First solenoid valve; 112. Shower head; 113. Distillation and dehydration section; 12. Control box; 13. Collection box; 2. Heating unit; 21. Oil tank; 22. Oil pump; 23. Jacketed funnel; 24. Jacket cavity; 25. Heater; 26. First temperature sensor; 27. Second temperature sensor; 3. Proportioning unit; 31. Motor; 32. Small support; 33. Stirring paddle; 34. Acetic acid conveying pipe; 35. n-Butanol conveying pipe; 36. Flow meter; 37. Second solenoid valve; 4. Catalytic unit; 41. Fixing plate; 42. Tray; 43. Wastewater collection box. Detailed Implementation

[0018] The present invention will be further described in detail below with reference to embodiments: Example 1 like Figure 1-4As shown, this utility model provides an esterification tower for preparing n-butyl acetate, including a bottom plate 1, an esterification tower body 11 fixedly mounted on the top surface of the bottom plate 1, a heating unit 2 provided on one side of the esterification tower body 11, a proportioning unit 3 provided at the top of the esterification tower body 11, and a catalytic unit 4 provided inside the esterification tower body 11. The heating unit 2 includes an oil tank 21 and a jacketed funnel 23. The oil tank 21 is fixedly connected to the top surface of the bottom plate 1, and the surface of the jacketed funnel 23 is fixedly connected to the top of the inside of the esterification tower body 11. A jacketed cavity 24 is provided inside the jacketed funnel 23. An oil pump 22, a heater 25, and a first temperature sensor 26 are fixedly installed on the top surface of the oil tank 21. The input end of the oil pump 22 is connected to the bottom of the oil tank 21 through an oil pipe, and the output end of the oil pump 22 is connected to the bottom of the jacket cavity 24 through an oil pipe. The top end of the jacket cavity 24 is connected to the top surface of the oil tank 21 through an oil pipe. A second temperature sensor 27 is fixedly connected inside the jacket funnel 23. One end of the second temperature sensor 27 extends to the outside of the esterification tower body 11. The bottoms of the heater 25 and the first temperature sensor 26 both extend into the inside of the oil tank 21.

[0019] In this embodiment, the target oil temperature and raw material target temperature of the heating unit 2 are adjusted by the control box 12. First, the heater 25 is started to heat the oil in the oil tank. When the oil temperature reaches the target temperature, the oil pump 22 is started to extract the oil and input it into the jacket cavity 24. Then, when the liquid level reaches the top of the jacket cavity 24, it will return to the oil tank 21 from the oil pipe, thus forming a circulating oil heating system that can heat the raw material inside the jacket funnel 23. The first temperature sensor 26 and the second temperature sensor 27 feed back the real-time oil temperature and raw material temperature to the control box 12 for temperature adjustment. All temperature sensors are ultra-high precision PT100 RTD sensors.

[0020] Example 2 like Figure 1-4 As shown, based on Embodiment 1, this utility model provides a technical solution: Preferably, the proportioning unit 3 includes a motor 31, a small bracket 32 ​​is fixedly connected to the outside of the motor 31, the bottom of the small bracket 32 ​​is fixedly connected to the top surface of the esterification tower body 11, the output shaft of the motor 31 is fixedly connected to a stirring paddle 33, the surface of the stirring paddle 33 moves inside the jacketed funnel 23, acetic acid conveying pipe 34 and n-butanol conveying pipe 35 are respectively arranged on the top two sides of the jacketed funnel 23, one end of the acetic acid conveying pipe 34 and the n-butanol conveying pipe 35 both extend through the outer shell of the esterification tower body 11 to the outside, and a flow meter 36 and a second solenoid valve 37 are sequentially arranged in the middle of the acetic acid conveying pipe 34 and the n-butanol conveying pipe 35.

[0021] In this embodiment, raw materials are fed into the jacketed funnel 23 from acetic acid delivery pipe 34 and n-butanol delivery pipe 35, respectively. The flow rate of raw materials passing through n-butanol delivery pipe 35 and acetic acid delivery pipe 34 in real time is fed back to the control box 12 for statistical analysis via flow meter 36. The flow meter 36 can be a Coriolis mass flow meter, which works by causing the measuring tube to vibrate. When the fluid flows through the vibrating tube, the Coriolis effect occurs, causing the tube to twist slightly. This twist is proportional to the mass flow rate of the fluid. The mass flow rate can be directly and accurately measured by detecting the phase difference using a sensor, unaffected by changes in fluid properties. When the acetic acid and n-butanol reach their set target values, the second solenoid valves 37 on the n-butanol delivery pipe 35 and acetic acid delivery pipe 34 sides are closed in time, thereby achieving automatic proportioning. When the heating unit 2 heats the raw materials inside the jacketed funnel 23, the motor 31 is activated to stir, helping the raw materials to mix evenly.

[0022] Example 3 like Figure 1-4 As shown, based on Embodiment 1, this utility model provides a technical solution: Preferably, the catalytic unit 4 includes a fixed plate 41, the bottom end of the jacketed funnel 23 is connected to a shower head 112 through a conduit, a first solenoid valve 111 is fixedly installed in the middle of the conduit, the fixed plate 41 is located below the shower head 112, the fixed plate 41 has grooves on both sides inside, a tray 42 is slidably connected inside the grooves, a wastewater collection box 43 is provided outside the tray 42, one side of the wastewater collection box 43 is fixedly connected to the middle of the outer wall of the esterification tower body 11, a control box 12 is fixedly installed on the surface of the oil tank 21, the control box 12 is controlled by a PLC, the first solenoid valve 111, the first temperature sensor 26, the second temperature sensor 27, the flow meter 36 and the second solenoid valve 37 are all signal connected to the control box 12, the motor 31 is electrically connected to the control box 12, a distillation and dehydration section 113 is provided at the bottom inside the esterification tower body 11, and a receiving box 13 is movably provided at the bottom outside the esterification tower body 11.

[0023] In this embodiment, the second temperature sensor 27 feeds back the raw material temperature inside the jacketed funnel 23 to the control box 12 in real time. When the raw material temperature reaches the set target value, the first solenoid valve 111 is opened, and the raw material is sprinkled onto the catalyst inside the lower tray 42 through the sprinkler 112, so that the raw material is evenly sprinkled and fully contacts the catalyst for reaction. When the catalyst is deactivated after a period of time, the tray 42 can be manually removed for replacement, which improves processing efficiency. In order to prevent the raw material from spilling and affecting the environment during replacement, a wastewater collection box 43 is set to collect waste liquid. When the raw material passes through the catalyst, it forms a liquid mixture, mainly including acetic acid, n-butanol, water and the target product n-butyl acetate, and then enters the interior of the lower distillation and dehydration section 113 for further processing. After processing, it enters the collection box 13 through the bottom of the esterification tower body 11.

[0024] The working principle of the esterification tower used to prepare n-butyl acetate will be explained in detail below.

[0025] like Figure 1-4As shown, the target oil temperature and raw material target temperature of the heating unit 2 are regulated by the control box 12. First, the heater 25 is started to heat the oil in the oil tank. When the oil temperature reaches the target temperature, the oil pump 22 is started to extract the oil and input it into the jacket cavity 24. Then, when the liquid level reaches the top of the jacket cavity 24, it will return to the oil tank 21 from the oil pipe, thus forming a circulating oil heating system that can heat the raw materials inside the jacket funnel 23. The first temperature sensor 26 and the second temperature sensor 27 feed back the real-time oil temperature and raw material temperature to the control box 12 for temperature regulation. The raw materials are input into the jacket funnel 23 from the acetic acid delivery pipe 34 and the n-butanol delivery pipe 35. The flow meter 36 feeds back the amount of raw materials passing through the n-butanol delivery pipe 35 and the acetic acid delivery pipe 34 to the control box 12 for statistics. When the amount of acetic acid and n-butanol passing through reaches the set target values, the second solenoid valves 37 on the n-butanol delivery pipe 35 side and the acetic acid delivery pipe 34 side are closed in time to achieve automatic proportioning. When heating unit 2 heats the raw material inside jacketed funnel 23, motor 31 is activated to stir and help the raw material mix evenly. Second temperature sensor 27 feeds back the temperature of the raw material inside jacketed funnel 23 to control box 12 in real time. When the temperature of the raw material reaches the set target value, the first solenoid valve 111 is opened, and the raw material is sprinkled onto the catalyst inside tray 42 below through sprinkler 112, so that the raw material is evenly sprinkled and fully contacts the catalyst for reaction. When the catalyst is deactivated after a period of time, tray 42 can be manually removed for replacement, improving processing efficiency. To prevent raw material from spilling and affecting the environment during replacement, wastewater collection box 43 is set to collect waste liquid. After the raw material passes through the catalyst, it forms a liquid mixture, mainly including acetic acid, n-butanol, water and the target product n-butyl acetate, and then enters the interior of the lower distillation and dehydration section 113 for further processing. After processing, it enters the collection box 13 through the bottom of the esterification tower body 11.

[0026] The present invention has been described in detail above. However, modifications or improvements can be made to it, which will be obvious to those skilled in the art. Therefore, any modifications or improvements that do not depart from the spirit of the present invention are within the protection scope of the present invention.

Claims

1. An esterification tower for preparing n-butyl acetate, comprising a bottom plate (1), characterized in that: The esterification tower body (11) is fixedly installed on the top surface of the base plate (1). A heating unit (2) is provided on one side of the esterification tower body (11). A proportioning unit (3) is provided at the top of the esterification tower body (11). A catalytic unit (4) is provided inside the esterification tower body (11). The heating unit (2) includes an oil tank (21) and a jacketed funnel (23). The oil tank (21) is fixedly connected to the top surface of the base plate (1). The surface of the jacketed funnel (23) is fixedly connected to the top of the esterification tower body (11). The jacketed funnel (23) has a jacketed cavity (24) inside. The top surface of the oil tank (21) is fixedly installed with an oil pump (22), a heater (25) and a first temperature sensor (26).

2. The esterification tower for preparing n-butyl acetate according to claim 1, characterized in that: The input end of the oil pump (22) is connected to the bottom of the oil tank (21) through an oil pipe. The output end of the oil pump (22) is connected to the bottom of the jacket cavity (24) through an oil pipe. The top end of the jacket cavity (24) is connected to the top surface of the oil tank (21) through an oil pipe. A second temperature sensor (27) is fixedly connected inside the jacket funnel (23). One end of the second temperature sensor (27) extends to the outside of the esterification tower body (11). The bottoms of the heater (25) and the first temperature sensor (26) both extend into the inside of the oil tank (21).

3. The esterification tower for preparing n-butyl acetate according to claim 2, characterized in that: The proportioning unit (3) includes a motor (31), a small bracket (32) is fixedly connected to the outside of the motor (31), the bottom of the small bracket (32) is fixedly connected to the top surface of the esterification tower body (11), and the output shaft of the motor (31) is fixedly connected to a stirring paddle (33), the surface of the stirring paddle (33) moves inside the jacketed funnel (23).

4. The esterification tower for preparing n-butyl acetate according to claim 3, characterized in that: An acetic acid delivery pipe (34) and a n-butanol delivery pipe (35) are respectively provided on the top two sides of the jacketed funnel (23). One end of the acetic acid delivery pipe (34) and the n-butanol delivery pipe (35) extends through the outer shell of the esterification tower body (11) to the outside. A flow meter (36) and a second solenoid valve (37) are respectively provided in the middle of the acetic acid delivery pipe (34) and the n-butanol delivery pipe (35).

5. An esterification tower for preparing n-butyl acetate according to claim 4, characterized in that: The catalytic unit (4) includes a fixed plate (41). The bottom end of the jacketed funnel (23) is connected to a shower head (112) through a conduit. A first solenoid valve (111) is fixedly installed in the middle of the conduit. The fixed plate (41) is located below the shower head (112). Sliding grooves are provided on both sides of the interior of the fixed plate (41). A tray (42) is slidably connected inside the sliding groove. A wastewater collection box (43) is provided outside the tray (42). One side of the wastewater collection box (43) is fixedly connected to the middle of the outer wall of the esterification tower body (11).

6. An esterification tower for preparing n-butyl acetate according to claim 5, characterized in that: A control box (12) is fixedly installed on the surface of the oil tank (21). The inside of the control box (12) is controlled by a PLC. The first solenoid valve (111), the first temperature sensor (26), the second temperature sensor (27), the flow meter (36), and the second solenoid valve (37) are all connected to the control box (12) via signals. The motor (31) is electrically connected to the control box (12).

7. An esterification tower for preparing n-butyl acetate according to claim 1, characterized in that: The esterification tower body (11) is provided with a distillation and dehydration section (113) at the bottom inside, and a receiving box (13) is provided at the bottom outside of the esterification tower body (11).

Citation Information

Patent Citations

  • Esterification tower for producing n-butyl acetate

    CN218166992U