An esterification separation column

Abstract

The utility model relates to an esterification separation tower including the upper tower body of lower tower body connection, through the coaxial setting inside, middle, outer three layer coil pipe components in the lower tower body, the lower tower body bottom end is equipped with the heat medium inlet pipe, and the inlet of inside coil pipe, middle coil pipe and outer coil pipe is linked with the heat medium inlet pipe, and the lower tower body top end side is equipped with the heat medium outlet pipe, and the outlet of inside coil pipe, middle coil pipe and outer coil pipe is linked with the heat medium outlet pipe, has built three -dimensional heating system, and three layer coil pipe passes through covering the center of lower tower body, the intermediate of lower tower body and inner wall and the edge area of inner wall, has formed the uniform stable temperature field, has eliminated the problem that the material coking phenomenon and the reaction of low temperature area are not sufficient caused by local overheating significantly, has promoted the heat transfer efficiency and energy utilization ratio, has guaranteed the stability and fullness of esterification reaction and separation process simultaneously, has improved the efficiency of separation.

Description

Technical Field

[0001] This utility model relates to the field of esterification technology, and in particular to an esterification separation tower. Background Technology

[0002] In the esterification reaction process in the chemical industry, the esterification separation tower is a key piece of equipment used to achieve product separation and purification. Traditional heating methods often use single-layer coils for heating. Due to the large internal space of the tower and the non-uniformity of material flow, a single heat source is difficult to form a uniform temperature field, which can easily lead to local overheating causing material coking or local insufficient temperature causing incomplete reaction.

[0003] It should be noted that the information disclosed in the background section above is only used to enhance the understanding of the background of this disclosure, and therefore may include information that does not constitute prior art known to those skilled in the art. Utility Model Content

[0004] To address the shortcomings of existing technologies, this utility model discloses an esterification separation tower to solve the problems of large internal space and uneven material flow, making it difficult for a single heat source to form a uniform temperature field, which can easily lead to local overheating causing material coking or local insufficient temperature causing incomplete reaction.

[0005] The technical solution adopted in this utility model is as follows: An esterification separation column includes a lower column body connected to an upper column body; The bottom of the lower tower body is connected to a BDO outlet pipe. A multi-layer coil assembly is coaxially arranged inside the lower tower body. The multi-layer coil assembly includes an inner coil, a middle coil, and an outer coil. The inner coil is coiled in the central region of the lower tower body; the outer coil is coiled in the region near the inner wall of the lower tower body; the middle coil is coiled in the region between the inner and outer coils. A heat medium inlet pipe is provided at the bottom of the lower tower body, and the inlets of the inner, middle, and outer coils are connected to the heat medium inlet pipe. A heat medium outlet pipe is provided on the side of the top of the lower tower body, and the outlets of the inner, middle, and outer coils are connected to the heat medium outlet pipe. The top of the upper column is connected to an esterification vapor outlet pipe, the bottom side of the upper column is connected to an esterification vapor inlet pipe, the side of the upper column is connected to several BDO inlet pipes, and a separation packing assembly is installed inside the upper column.

[0006] A further technical solution is that the inlets of the inner coil, the middle coil, and the outer coil are respectively connected in parallel to the heat medium inlet pipe, and the outlets of the inner coil, the middle coil, and the outer coil are respectively connected in parallel to the heat medium outlet pipe.

[0007] A further technical solution is that a hollow frustum-shaped liquid-blocking cone and a hollow cylindrical annular plate are coaxially arranged at one end of the upper column body near the esterification vapor inlet pipe. The end of the liquid-blocking cone with a larger inner diameter is arranged upwards. The outer side of the upper end of the liquid-blocking cone is fixed to the inner wall of the upper column body. The top end of the annular plate is fixed and connected to the bottom end of the liquid-blocking cone. The liquid outlet end of one of the BDO inlet pipes faces the top end of the liquid-blocking cone.

[0008] A further technical solution is that the separation packing assembly includes one Pall ring packing and two structured packings. The Pall ring packing is spaced apart at the upper end of the liquid-retaining cone, and the two structured packings are spaced apart at the upper end of the Pall ring packing. The two structured packings are spaced apart from each other. The liquid outlet of one BDO inlet pipe is located at the upper end of the Pall ring packing, and the liquid outlets of the two BDO inlet pipes are respectively located at the upper ends of the two structured packings.

[0009] A further technical solution is that the separation packing assembly further includes three liquid distributors, one of which is located between the Pall ring packing and its corresponding BDO inlet pipe, and the other two are located between the two structured packings and their corresponding BDO inlet pipes.

[0010] A further technical solution is that both the lower ends of the Pall ring packing and the structured packing are provided with packing support plates, and both the upper ends of the Pall ring packing and the structured packing are provided with packing pressure plates.

[0011] A further technical solution is that two hand holes are opened on the side of the upper tower body, and the positions of the two hand holes correspond to the upper and lower ends of the Pall ring packing.

[0012] A further technical solution is that a skirt is provided at the bottom end of the lower tower body.

[0013] A further technical solution is that the upper and lower tower bodies are provided with a number of remote thermometer ports, a number of remote liquid level ports, and a number of nitrogen inlets.

[0014] The beneficial effects of this utility model embodiment are as follows: (i) An esterification separation tower includes an upper tower body connected to a lower tower body. Three layers of coils (inner, middle, and outer) are coaxially arranged within the lower tower body. A heat medium inlet pipe is located at the bottom of the lower tower body, and the inlets of the inner, middle, and outer coils are connected to the heat medium inlet pipe. A heat medium outlet pipe is located on the side of the top of the lower tower body, and the outlets of the inner, middle, and outer coils are connected to the heat medium outlet pipe. This constructs a three-dimensional heating system. The three layers of coils cover the center of the lower tower body, the area between the lower tower body and the inner wall, and the edge area of ​​the inner wall, forming a uniform and stable temperature field. This significantly eliminates the material coking phenomenon caused by local overheating and the problem of insufficient reaction in the low-temperature zone, improving heat transfer efficiency and energy utilization. Simultaneously, it ensures the stability and sufficiency of the esterification reaction and separation process, thereby improving separation efficiency.

[0015] (ii) Furthermore, a hollow frustum-shaped liquid-retaining cone and a hollow cylindrical annular plate are coaxially arranged at one end of the upper column body near the esterification vapor inlet pipe. The end of the liquid-retaining cone with a larger inner diameter faces upward, and the outer side of the upper end of the liquid-retaining cone is fixed to the inner wall of the upper column body. The top of the annular plate is fixed and connected to the bottom end of the liquid-retaining cone, and the outlet end of a circulating BDO inlet pipe faces the top of the liquid-retaining cone. Esterification vapor enters from the esterification vapor inlet pipe, impacts the annular plate, moves downward, and enters the annular plate through the opening at the bottom end of the annular plate, rising upward. The matching arrangement of the liquid-retaining cone and the annular plate prevents the esterification vapor entering the upper column body from carrying liquid droplets and rising directly, while guiding the downward flowing BDO liquid to the center of the upper column body. At the same time, the connection between the annular plate and the liquid-retaining cone forms a channel, allowing the BDO liquid to be sprayed onto the top of the liquid-retaining cone and evenly dispersed along the inner wall of the liquid-retaining cone into the annular plate, so that the gas phase and liquid phase are in full contact, enhancing the mass transfer effect of the gas and liquid phases.

[0016] (III) Further, the separation packing assembly includes one Pall ring packing and two structured packings. The Pall ring packing is spaced apart at the upper end of the liquid-retaining cone, and the two structured packings are spaced apart at the upper end of the Pall ring packing. The outlet end of a circulating BDO inlet pipe is located at the upper end of the Pall ring packing, and the outlet ends of a low-temperature BDO inlet pipe and a reflux pipe are respectively located at the upper ends of the two structured packings. The reflux pipe is located at the upper end of the uppermost structured packing. For example, both the lower end of the Pall ring packing and the structured packing are provided with packing support plates, and both the upper end of the Pall ring packing and the structured packing are provided with packing pressure plates. The lower Pall ring packing, with its good anti-fouling performance and large porosity, performs preliminary washing and distribution of the rising steam, while preventing material blockage; while the upper two-stage structured packing, with its extremely high mass transfer efficiency, performs deep and fine separation of gas and liquid phase components. Different types of BDOs are distributed above different packing sections, enabling the cascade utilization of heat and materials, and improving the separation accuracy and operational stability of the entire tower. Attached Figure Description

[0017] Figure 1This is a front view of the internal structure of an esterification separation tower according to the present invention.

[0018] In the picture: 100. Lower tower body; 101. Heat medium inlet pipe; 102. Heat medium outlet pipe; 110. Multi-layer coil assembly; 111. Inner coil; 112. Middle coil; 113. Outer coil; 200. Upper tower body; 201. Esterification vapor outlet pipe; 202. Esterification vapor inlet pipe; 203. Circulating BDO inlet pipe; 204. Low-temperature BDO inlet pipe; 205. Reflux pipe; 206. Liquid-retaining cone; 207. Ring plate; 208. Manhole; 209. BDO outlet pipe; 300. Skirt; 400. Separation packing assembly; 410. Pall ring packing; 420. Structured packing; 430. Packing support plate; 440. Packing pressure plate. Detailed Implementation

[0019] To further illustrate the technical means and effects adopted by this utility model in order to achieve the intended utility model purpose, the following detailed description of the specific implementation methods, structure, features and effects of this utility model is provided in conjunction with the accompanying drawings and preferred embodiments.

[0020] First embodiment: An esterification separation column includes a lower column body 100 and an upper column body 200 connected to the lower column body 100. Exemplarily, a skirt 300 is provided at the bottom end of the lower column body 100. A BDO outlet pipe 209 (BDO is 1,4-butanediol) is connected to the bottom end of the lower column body 100. A multi-layer coil assembly 110 is coaxially arranged inside the lower column body 100. The multi-layer coil assembly 110 includes an inner coil 111, a middle coil 112, and an outer coil 113. The inner coil 111 is coiled in the central region inside the lower column body 100. The outer coil 113 is coiled in the region inside the lower column body 100 near the inner wall. The middle coil 112 is coiled in the region between the inner coil 111 and the outer coil 113. The lower tower body 100 has a heat medium inlet pipe 101 at its bottom end. The inlets of the inner coil 111, the middle coil 112, and the outer coil 113 are connected to the heat medium inlet pipe 101. The lower tower body 100 has a heat medium outlet pipe 102 on its top side. The outlets of the inner coil 111, the middle coil 112, and the outer coil 113 are connected to the heat medium outlet pipe 102. For example, the inlets of the inner coil 111, the middle coil 112, and the outer coil 113 are connected in parallel to the heat medium inlet pipe 101, and the outlets of the inner coil 111, the middle coil 112, and the outer coil 113 are connected in parallel to the heat medium outlet pipe 102.

[0021] The top of the upper column 200 is connected to an esterification vapor outlet pipe 201, and the bottom side of the upper column 200 is connected to an esterification vapor inlet pipe 202. Several BDO inlet pipes are also connected to the side of the upper column 200. For example, the BDO inlet pipes include two circulating BDO inlet pipes 203, one low-temperature BDO inlet pipe 204, and one reflux pipe 205. A separation packing assembly 400 is installed inside the upper column 200.

[0022] Furthermore, a hollow frustum-shaped liquid-retaining cone 206 and a hollow cylindrical ring plate 207 are coaxially arranged at one end of the upper column body 200 near the esterification vapor inlet pipe 202. The end of the liquid-retaining cone 206 with a larger inner diameter is arranged upwards. The outer side of the upper end of the liquid-retaining cone 206 is fixed to the inner wall of the upper column body 200. The top end of the ring plate 207 is fixed and connected to the bottom end of the liquid-retaining cone 206. The liquid outlet end of a circulating BDO inlet pipe 203 faces the top end of the liquid-retaining cone 206. Esterification vapor enters from the esterification vapor inlet pipe 202, impacts the annular plate 207, moves downwards, and enters the annular plate 207 through the opening at the bottom end of the annular plate 207, rising upwards. The fitting arrangement of the liquid-retaining cone 206 and the annular plate 207 prevents the esterification vapor, upon entering the upper column body 200, from carrying liquid droplets and rising directly, while simultaneously guiding the downward-flowing BDO liquid to the center of the upper column body 200. At the same time, the connection between the annular plate 207 and the liquid-retaining cone 206 forms a channel, allowing the BDO liquid to be sprayed onto the top of the liquid-retaining cone 206 and evenly dispersed along the inner wall of the liquid-retaining cone 206 into the annular plate 207, ensuring sufficient contact between the gas and liquid phases and enhancing the mass transfer effect between the gas and liquid phases.

[0023] Furthermore, the separation packing assembly 400 includes one Pall ring packing 410 and two structured packings 420. The Pall ring packing 410 is spaced apart at the upper end of the liquid-retaining cone 206, and the two structured packings 420 are spaced apart at the upper end of the Pall ring packing 410. The two structured packings 420 are spaced apart from each other. The outlet end of a circulating BDO inlet pipe 203 is located at the upper end of the Pall ring packing 410, and the outlet ends of a low-temperature BDO inlet pipe 204 and a return pipe 205 are respectively located at the upper ends of the two structured packings 420. The return pipe 205 is located at the upper end of the uppermost structured packing 420. For example, both the lower ends of the Pall ring packing 410 and the structured packing 420 are provided with packing support plates 430, and the upper ends of both the Pall ring packing 410 and the structured packing 420 are provided with packing pressure plates 440. The lower layer of Pall ring packing 410, with its excellent anti-fouling properties and large porosity, performs preliminary washing and distribution of rising steam while preventing material blockage. Meanwhile, the upper two-stage structured packing 420, with its extremely high mass transfer efficiency, performs deep and fine separation of gas and liquid phase components. Different functional BDO feeds (circulation, cryogenic, reflux) are distributed above different packing sections, achieving cascaded utilization of heat and materials, and improving the overall separation accuracy and operational stability of the tower.

[0024] Furthermore, the separation packing assembly 400 also includes three liquid distributors. One liquid distributor is located between the Pall ring packing 410 and its corresponding BDO inlet pipe, and the other two liquid distributors are located between the two structured packings 420 and their corresponding BDO inlet pipes, respectively. The liquid distributor located above the Pall ring packing 410 ensures that the circulating BDO feed can uniformly cover the entire cross-section of the lower packing layer, giving full play to its initial washing and distribution functions. The liquid distributors located above the two structured packings 420 respectively refine the distribution of low-temperature BDO and reflux liquid, so that the liquid forms a uniform liquid film in the channels of the structured packing 420, which greatly enhances the gas-liquid contact area and mass transfer efficiency. The resulting staged distribution system eliminates the uneven distribution phenomena such as wall flow and channel flow common in packed towers, enabling each section of packing to achieve optimal separation performance and improving the separation accuracy and operational stability of the entire tower.

[0025] Furthermore, two handholes 208 are provided on the side of the upper tower body 200, corresponding to the upper and lower ends of the Pall ring packing 410. The upper handhole 208 allows for direct observation of the packing surface condition, while the lower handhole 208 allows for inspection of the bottom layer of the packing and the support plate. During maintenance, these two handholes 208 allow for quick cleaning or partial replacement of the Pall ring packing 410 layer without the need for large-scale disassembly of the tower structure, reducing maintenance difficulty and time costs, and ensuring long-term stable operation of the equipment.

[0026] Furthermore, the upper column 200 and the lower column 100 are equipped with several remote thermometer ports, several remote level gauge ports, and several nitrogen inlets. One remote thermometer port is located at the bottom end of the lower column 100, and one remote level gauge port and one nitrogen inlet are located on the side of the bottom end of the lower column 100. One remote level gauge port and one nitrogen inlet are located on the side of the bottom end of the upper column 200, positioned relative to the esterification vapor inlet pipe 202. The remaining remote thermometer ports are positioned relative to the BDO inlet pipe. The remote thermometer port located at the bottom of the lower column 100 monitors the product outlet temperature in real time. The remote liquid level port and nitrogen inlet on the side of the lower column 100 are used to monitor the liquid level and inject protective gas, respectively. The remote thermometer port on the upper column 200, corresponding to the esterification vapor inlet, can detect the feed status and introduce nitrogen in time to prevent oxidation. The remote thermometer ports specifically set at each BDO inlet position can obtain the temperature distribution data of each packing section in real time, thereby adjusting the heat medium supply of the three-layer coil to form a closed-loop temperature control system, ensuring that the entire column is always in the optimal reaction temperature range, improving the safety of the process and the stability of the product.

[0027] In operation, this embodiment is as follows: Esterification vapor enters the lower part of the upper column 200 through esterification vapor inlet pipe 202 and flows upward. BDO materials at different temperatures are fed into the column through their respective BDO inlet pipes. The rising vapor and the falling liquid come into countercurrent contact in the Pall ring packing 410 and structured packing 420 layers, carrying out mass transfer and esterification reactions. The vapor generated by the reaction continues to rise and is discharged through esterification vapor outlet pipe 201, while the liquid phase material gathers downward. During this process, the inner, middle and outer three-layer coil assembly in the lower column 100 is heated by the heat medium introduced through the heat medium inlet pipe 101, providing uniform and stable heat to the entire column. The BDO product after participating in the reaction is finally output through the BDO outlet pipe 209 at the bottom of the lower column 100, thus completing a highly efficient continuous esterification and separation process.

[0028] In this embodiment, the three-layer coil forms a uniform and stable temperature field by covering the center of the lower tower body 100, the middle area between the lower tower body 100 and the inner wall, and the edge area of ​​the inner wall. This significantly eliminates the material coking phenomenon caused by local overheating and the problem of insufficient reaction in the low-temperature zone, improves heat transfer efficiency and energy utilization, and at the same time ensures the stability and sufficiency of the esterification reaction and separation process, thereby improving the separation efficiency.

[0029] The above description is merely a preferred embodiment of the present utility model and is not intended to limit the present utility model in any way. Although the present utility model has been disclosed above with reference to a preferred embodiment, it is not intended to limit the present utility model. Any person skilled in the art can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the present utility model. Any simple modifications, equivalent changes and alterations made to the above embodiments based on the technical essence of the present utility model without departing from the scope of the present utility model shall still fall within the scope of the present utility model.

Claims

1. An esterification separation tower, characterized in that, include: The lower tower body is connected to the upper tower body; The bottom of the lower tower body is connected to a BDO outlet pipe. A multi-layer coil assembly is coaxially arranged inside the lower tower body. A heat medium inlet pipe is located at the bottom of the lower tower body, and a heat medium outlet pipe is located on the side of the top of the lower tower body. The inlet and outlet of the multi-layer coil assembly are respectively connected to the heat medium inlet pipe and the heat medium outlet pipe. The multi-layer coil assembly includes an inner coil, a middle coil, and an outer coil. The inner coil is coiled in the central region of the lower tower body; the outer coil is coiled in the region near the inner wall of the lower tower body; and the middle coil is coiled in the region between the inner and outer coils. The top of the upper column is connected to an esterification vapor outlet pipe, the bottom side of the upper column is connected to an esterification vapor inlet pipe, the side of the upper column is connected to several BDO inlet pipes, and a separation packing assembly is installed inside the upper column.

2. The esterification separation tower according to claim 1, characterized in that: The inlets of the inner coil, the middle coil, and the outer coil are connected in parallel to the heat medium inlet pipe, and the outlets of the inner coil, the middle coil, and the outer coil are connected in parallel to the heat medium outlet pipe.

3. The esterification separation tower according to claim 1, characterized in that: A hollow frustum-shaped liquid-retaining cone and a hollow cylindrical annular plate are coaxially arranged at one end of the upper column body near the esterification vapor inlet pipe. The end of the liquid-retaining cone with the larger inner diameter faces upward. The outer side of the upper end of the liquid-retaining cone is fixed to the inner wall of the upper column body. The top end of the annular plate is fixed and connected to the bottom end of the liquid-retaining cone. The liquid outlet end of one of the BDO inlet pipes faces the top end of the liquid-retaining cone.

4. The esterification separation tower according to claim 3, characterized in that: The separation packing assembly includes one Pall ring packing and two structured packings. The Pall ring packing is spaced apart at the upper end of the liquid-retaining cone, and the two structured packings are spaced apart at the upper end of the Pall ring packing. The two structured packings are spaced apart from each other. The liquid outlet of one BDO inlet pipe is located at the upper end of the Pall ring packing, and the liquid outlets of the two BDO inlet pipes are respectively located at the upper ends of the two structured packings.

5. The esterification separation tower according to claim 4, characterized in that: The separation packing assembly also includes three liquid distributors. One liquid distributor is located between the Pall ring packing and its corresponding BDO inlet pipe, and the other two liquid distributors are respectively located between the two structured packings and their corresponding BDO inlet pipes.

6. The esterification separation tower according to claim 4, characterized in that: Both the Pall ring packing and the structured packing have packing support plates at their lower ends, and both have packing pressure plates at their upper ends.

7. The esterification separation tower according to claim 4, characterized in that: Two hand holes are provided on the side of the upper tower body, and the positions of the two hand holes correspond to the upper and lower ends of the Pall ring packing.

8. The esterification separation tower according to claim 1, characterized in that: The bottom of the lower tower body is provided with a skirt.

9. The esterification separation tower according to claim 1, characterized in that: The upper and lower tower bodies are equipped with several remote thermometer ports, several remote liquid level ports, and several nitrogen inlets.

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