Distillation recovery device for preparing ethylene glycol butyl ether

Abstract

The invention relates to a distillation recovery device for ethylene glycol butyl ether preparation, and relates to the technical field of chemical preparation distillation devices. The device comprises a distillation tower, a reaction liquid tank is arranged in the distillation tower, a heating mechanism is arranged below the reaction liquid tank, a partition plate is arranged in the distillation tower, a condensation cavity is formed above the partition plate, a plurality of condensation pipes are arranged in the condensation cavity, a rising hole is formed in the partition plate in a penetrating mode in the thickness direction, and the rising hole is communicated with the heating mechanism. An ascending pipe is arranged in the ascending hole and communicates with the upper end and the lower end of the partition plate, a flow guide cover is arranged on the portion, located below the partition plate, of the ascending pipe, a plurality of outflow holes are formed in the portion, located above the partition plate, of the side wall of the ascending pipe, and a recycling pipe communicates with the side wall of the condensation cavity; and the other end of the recovery pipe is communicated with a distillate separation mechanism. The butanol recovery device has the effects of further separating and purifying the distillate in the distillation process and improving the purity of recovered butanol.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of distillation devices for preparing chemical products, in particular to a distillation recovery device for preparing ethylene glycol butyl ether. BACKGROUND

[0002] Ethylene glycol butyl ether is an important organic compound, has good safety and environmental protection, and has a wide range of industrial applications, including but not limited to the fields of solvents, coating aids, electronic chemicals and the like.

[0003] In the prior art, distillation is one of the indispensable processes in the preparation of ethylene glycol butyl ether. In the raw material preparation stage, butanol and boron trifluoride-ethyl ether complex are mixed as raw materials, and then ethylene oxide is introduced at 25-30 DEG C. Subsequently, the temperature is raised to 80 DEG C to complete the etherification reaction. After the reaction is completed, the reaction liquid is placed in a distillation device, and the low-boiling-point components (such as unreacted butanol and water) are vaporized by heating. After condensation, the distillate is collected, and the remaining reaction liquid in the distillation device is ethylene glycol butyl ether. For the above related technology, the inventors found that in the distillation process, butanol and water in the low-boiling-point components will be separated together and discharged from the distillation device after condensation. However, butanol and water cannot be effectively separated, which may easily affect the purity of butanol, and therefore needs to be improved. SUMMARY

[0004] In order to further separate and purify the distillate in the distillation process and improve the purity of the recovered butanol, the application provides a distillation recovery device for preparing ethylene glycol butyl ether.

[0005] The distillation recovery device for preparing ethylene glycol butyl ether provided by the application adopts the following technical scheme: A distillation recovery device for preparing ethylene glycol butyl ether comprises a distillation tower, a reaction liquid tank is arranged in the distillation tower, a heating mechanism is arranged below the reaction liquid tank, a partition plate is arranged in the distillation tower, a condensation cavity is formed above the partition plate, a plurality of condensation pipes are arranged in the condensation cavity, an ascending hole is formed in the partition plate along the thickness direction, an ascending pipe is arranged in the ascending hole, the ascending pipe is connected between the upper end and the lower end of the partition plate, a flow guide cover is arranged on the ascending pipe below the partition plate, a plurality of outflow holes are formed in the side wall of the ascending pipe above the partition plate, a recovery pipe is connected to the side wall of the condensation cavity, and a distillate separation mechanism is connected to the other end of the recovery pipe.

[0006] By adopting the technical scheme, in the process of distilling the reaction liquid, low-boiling-point components are condensed in the condensing cavity and enter the distillate separation mechanism through the recovery pipe, and the butanol and water in the low-boiling-point components are separated by the distillate separation mechanism, so that the distillate is separated and purified, the purity of the recovered butanol is improved, and the butanol that does not participate in the reaction can be efficiently recovered, thereby improving the economic benefit.

[0007] Preferably, the distillate separation mechanism comprises a static stratification tower, a liquid discharge valve, a water discharge valve, an intermediate tower and a recovery tower, the static stratification tower is connected with the recovery pipe, the static stratification tower is provided with a cooling module, the liquid discharge valve is communicated with the side wall of the static stratification tower, the water discharge valve is communicated with the bottom wall of the static stratification tower, the intermediate tower is communicated with one end of the liquid discharge valve away from the static stratification tower, the intermediate tower is provided with a loading container, the loading container is communicated with the liquid discharge valve, a metering valve is arranged at the communication position of the liquid discharge valve and the loading container, the loading container is provided with a weight sensing module at the bottom, the metering valve is in communication connection with the weight sensing module, the loading container is communicated with a discharge pipe and a reflux pipe, the discharge pipe is communicated with the recovery tower, and the other end of the reflux pipe is communicated with the static stratification tower.

[0008] By adopting the technical scheme, the condensate enters the static stratification tower for long-time standing, because the density of butanol is less than that of water, the solubility of butanol and water is reduced under the action of the cooling module, after long-time standing, the butanol and water are obviously stratified, the butanol can be discharged through the liquid discharge valve, and the water in the lower layer is discharged through the water discharge valve, the butanol entering the intermediate tower through the liquid discharge valve is calculated for the density of butanol at the current temperature under the action of the metering valve and the weight sensing module, and then the purity of butanol in the intermediate tower is judged, if the purity meets the standard, the butanol is discharged into the recovery tower through the discharge pipe, and if the purity does not meet the standard, the butanol is discharged into the static stratification tower again through the reflux pipe for standing and stratification, thereby improving the purity of the recovered butanol.

[0009] Preferably, the intermediate tower is provided with a temperature control module at the top.

[0010] By adopting the technical scheme, the temperature in the intermediate tower can be controlled in a certain range by the temperature control module, so that the stability of the density of butanol is maintained, and the purity of the recovered butanol is effectively ensured.

[0011] Preferably, the side wall of the condensing cavity is communicated with a plurality of recovery pipes, one end of each of the recovery pipes is communicated with a distillate separation mechanism, and an on-off valve is arranged on each of the recovery pipes.

[0012] By adopting the technical scheme, the separation and recovery process of butanol can be continuously carried out by arranging a plurality of recovery pipes and distillate separation mechanisms, so that the work efficiency is maintained.

[0013] Preferably, the top of the ascending pipe is provided with a negative pressure module.

[0014] By adopting the above technical scheme, the negative pressure module can make the gas flow towards the ascending pipe direction, thereby improving the working efficiency of the overall distillation recovery device.

[0015] Preferably, a guide slope is arranged on the inner bottom wall of the condensation cavity, and the guide slope is arranged to be inclined towards the direction of the recovery pipe.

[0016] By adopting the above technical scheme, the guide slope can make the condensate continuously flow towards the recovery pipe, thereby effectively preventing the accumulation of liquid in the condensation cavity, and improving the use safety of the distillation recovery device.

[0017] Preferably, a plurality of support rods are arranged on the inner wall of the flow guide cover, the plurality of support rods are arranged in the horizontal direction, the plurality of support rods are distributed in the circumferential direction of the flow guide cover, one end of the plurality of support rods close to each other is provided with a plurality of rotating members, the output shaft of the rotating member is arranged in the vertical direction, a stirring shaft is arranged on the output shaft of the rotating member, and the stirring shaft is inserted into the reaction liquid tank.

[0018] By adopting the above technical scheme, the stirring shaft can effectively improve the distillation efficiency, thereby accelerating the precipitation efficiency of the low-boiling-point component, thereby improving the preparation rate of ethylene glycol butyl ether and effectively improving the recovery efficiency of butanol.

[0019] Preferably, an isolation cover is arranged on the surface of the support rod, the isolation cover is arranged around the rotating member, and a flow inclined surface is arranged on the side wall of the isolation cover.

[0020] By adopting the above technical scheme, the isolation cover can effectively separate the steam from the rotating member, thereby protecting the use safety of the rotating member.

[0021] Preferably, a barrier cover is arranged around the reaction liquid tank.

[0022] By adopting the above technical scheme, the barrier cover arranged around the reaction liquid tank can effectively reduce the space below the partition plate, so that the gas heated and evaporated can flow more concentratedly towards the ascending pipe direction, thereby improving the distillation recovery efficiency.

[0023] Preferably, a liquid outlet pipe is communicated with the side wall of the reaction liquid tank, the liquid outlet pipe sequentially penetrates through the barrier cover and the distillation tower, a recovery box is communicated with the other end of the liquid outlet pipe, and a molecular sieve is arranged on the liquid outlet pipe.

[0024] By adopting the above technical scheme, the molecular sieve can absorb the trace amount of water in the ethylene glycol butyl ether left after distillation, thereby further improving the purity of the ethylene glycol butyl ether.

[0025] To sum up, the present application includes at least one of the following beneficial technical effects: 1. In the process of distilling the reaction liquid, the low-boiling-point components are condensed in the condensing cavity and enter the distillate separation mechanism through the recovery pipe. The butanol and water in the low-boiling-point components are separated by the distillate separation mechanism, so as to separate and purify the distillate and improve the purity of butanol recovery. In turn, the butanol not involved in the reaction can be efficiently recovered, thereby improving the economic benefits. 2. The condensed liquid enters the static stratification tower for long-time standing. Since the density of butanol is less than that of water, the solubility of the two is reduced under the action of the cooling module. After long-time standing, the butanol and water will be obviously stratified. The butanol can be discharged through the liquid discharge valve, and the water in the lower layer can be discharged through the water discharge valve. The butanol entering the intermediate tower through the liquid discharge valve calculates the density of the butanol at the current temperature under the action of the metering valve and the weight sensing module, and then judges the purity of the butanol in the intermediate tower. If the purity meets the standard, the butanol is discharged into the recovery tower through the discharge pipe. If the purity does not meet the standard, the butanol is discharged into the static stratification tower through the reflux pipe for standing and stratification, thereby improving the purity of butanol recovery. 3. The temperature control module of the present application can control the temperature in the intermediate tower within a certain range, thereby maintaining the stability of the butanol density and effectively ensuring the purity of the recovered butanol. BRIEF DESCRIPTION OF DRAWINGS

[0026] Figure 1 is a structural schematic diagram of a distillation and recovery device for preparing ethylene glycol butyl ether according to an embodiment of the present application.

[0027] Figure 2 is a structural schematic diagram of a distillate separation mechanism according to an embodiment of the present application.

[0028] BRIEF DESCRIPTION OF DRAWINGS 1. Distillation tower; 2. Reaction liquid tank; 3. Heating mechanism; 4. Partition plate; 5. Condensing cavity; 6. Condensing pipe; 7. Upward hole; 8. Upward pipe; 9. Flow guide cover; 10. Flow-out hole; 11. Recovery pipe; 12. Distillate separation mechanism; 1201. Static stratification tower; 1202. Liquid discharge valve; 1203. Water discharge valve; 1204. Intermediate tower; 1205. Recovery tower; 1206. Cooling module; 1207. Loading container; 1208. Metering valve; 1209. Weight sensing module; 1210. Discharge pipe; 1211. Reflux pipe; 1212. Temperature control module; 13. On-off valve; 14. Negative pressure module; 15. Flow guide slope; 16. Support rod; 17. Rotating part; 18. Stirring shaft; 19. Isolation cover; 20. Flow-through slope; 21. Blocking cover; 22. Liquid outlet pipe; 23. Recovery box; 24. Molecular sieve. DETAILED DESCRIPTION

[0029] The following will be described in detail with reference to the accompanying drawings. Figures 1-2This application will be described in further detail.

[0030] This application discloses a distillation recovery apparatus for the preparation of ethylene glycol butyl ether. (Refer to...) Figure 1 and Figure 2 The system includes a distillation column 1, a reaction liquid tank 2 inside the distillation column 1, and a heating mechanism 3 below the reaction liquid tank 2 to heat the reaction liquid inside the reaction liquid tank 2, thereby realizing the distillation process. In this embodiment, the heating mechanism 3 can be an electric heating wire. The distillation column 1 is also equipped with a partition plate 4, which is located above the reaction liquid tank 2. A condensation chamber 5 is formed above the partition plate 4, and a condenser pipe 6 is installed in the condensation chamber 5 to condense the steam entering the condensation chamber 5. The partition plate 4 has a rising hole 7 through it along the thickness direction to connect the upper and lower spaces of the partition plate 4. A barrier cover 21 is provided around the reaction liquid tank 2 to reduce the space below the partition plate 4, so that the steam can enter the condensation chamber 5 more concentratedly.

[0031] Reference Figure 1 and Figure 2 A riser pipe 8 is installed inside the riser hole 7, and the riser pipe 8 passes through the partition plate 4. Several outflow holes 10 are opened on the side wall of the riser pipe 8 above the partition plate 4 to allow steam to enter the condensation chamber 5. A flow guide shroud 9 is installed at the end of the riser pipe 8 below the partition plate 4 to allow steam to flow concentratedly into the riser pipe 8. Several support rods 16 are installed on the inner wall of the flow guide shroud 9, all arranged horizontally and distributed along the circumference of the flow guide shroud 9. The ends of the support rods 16 away from the flow guide shroud 9 are all oriented towards the axis of the flow guide shroud 9. Rotating elements 17 are provided on the surface of the ends of the support rods 16 away from the flow guide shroud 9. In this embodiment... The output shaft of the rotating component 17 is arranged vertically. The rotating component 17 is powered by a motor. A stirring shaft 18 is coaxially arranged on the output shaft of the rotating component 17. The stirring shaft 18 is inserted into the reaction liquid tank 2, thereby effectively improving the distillation speed of the reaction liquid. An isolation cover 19 is provided on the surface of the support rod 16. The isolation cover 19 is fitted around the rotating component 17, thereby isolating the rotating component 17 from the steam and protecting the structural safety of the rotating component 17. A flow slope 20 is provided on the side wall of the isolation cover 19, so that the steam can flow in the direction of the guide shroud 9. In this embodiment, a negative pressure module 14 is provided on the top wall of the riser pipe 8 to allow the steam to flow into the riser pipe 8 in a concentrated manner. The negative pressure module 14 is a negative pressure fan.

[0032] Reference Figure 1 and Figure 2The side wall of the reaction liquid tank 2 is communicated with a liquid outlet pipe 22, the liquid outlet pipe 22 passes through the blocking cover 21 and the distillation tower 1 in sequence, the other end of the liquid outlet pipe 22 is communicated with a recovery tank 23, a molecular sieve 24 is arranged on the liquid outlet pipe 22, the molecular sieve 24 can absorb the trace water in the ethylene glycol butyl ether left after distillation, and the purity of the ethylene glycol butyl ether is further improved.

[0033] With reference to Figure 1 and Figure 2 The bottom wall of the condensation cavity 5 is provided with a flow guide slope 15, one end of the flow guide slope 15 close to the axis of the distillation tower 1 is inclined upward, the outer wall of the condensation cavity 5 is communicated with a plurality of recovery pipes 11, each recovery pipe 11 is provided with an on-off valve 13, and each recovery pipe 11 is communicated with a distillate liquid separation mechanism 12 at the other end, so as to separate butanol and water in the low-boiling-point component.

[0034] With reference to Figure 1 and Figure 2 The distillate liquid separation mechanism 12 comprises a static stratification tower 1201, a liquid discharge valve 1202, a water discharge valve 1203, an intermediate tower 1204 and a recovery tower 1205, the static stratification tower 1201 is connected with the recovery pipe 11, and a cooling module 1206 is arranged in the static stratification tower 1201, in the embodiment, the cooling module 1206 is a cold air machine, so that the condensate is maintained at a low temperature, and the solubility of butanol and water is reduced; the liquid discharge valve 1202 is communicated with the side wall of the static stratification tower 1201, the water discharge valve 1203 is communicated with the bottom wall of the static stratification tower 1201, the intermediate tower 1204 is communicated with one end of the liquid discharge valve 1202 away from the static stratification tower 1201, a loading container 1207 is arranged in the intermediate tower 1204, the loading container 1207 is communicated with the liquid discharge valve 1202, a metering valve 1208 is arranged at the communication position of the liquid discharge valve 1202 and the loading container 1207, a weight sensing module 1209 is arranged at the bottom of the loading container 1207, the weight sensing module 1209 is a weight sensor, the metering valve 1208 and the weight sensing module 1209 are communicatively connected, a temperature control module 1212 is arranged on the inner top wall of the intermediate tower 1204, so as to maintain the temperature in the intermediate tower 1204 and stabilize the density of butanol, the loading container 1207 is communicated with a discharge pipe 1210 and a reflux pipe 1211, the discharge pipe 1210 is communicated with the recovery tower 1205, and the other end of the reflux pipe 1211 is communicated with the static stratification tower 1201.

[0035] The implementation principle of the distillation recovery device for preparing ethylene glycol butyl ether according to the embodiment of the application is as follows: in the process of distilling the reaction liquid, low-boiling-point components are condensed in the condensing cavity 5 and enter the distillate separation mechanism 12 through the recovery pipe 11; the condensed liquid enters the static stratification tower 1201 and is statically stratified for a long time; because the density of butanol is less than that of water, the solubility of butanol and water is reduced under the action of the cooling module 1206; after long-time static stratification, butanol and water are obviously stratified, butanol can be discharged through the liquid discharge valve 1202, and the lower water is discharged through the water discharge valve 1203; the butanol entering the intermediate tower 1204 through the liquid discharge valve 1202 is used to calculate the density of butanol at the current temperature under the action of the metering valve 1208 and the weight sensing module 1209, so as to determine the purity of butanol in the intermediate tower 1204; if the purity meets the standard, butanol is discharged into the recovery tower 1205 through the discharge pipe 1210; if the purity does not meet the standard, butanol is discharged into the static stratification tower 1201 through the reflux pipe 1211 to be statically stratified again, so that the distillate is separated and purified, the purity of butanol is improved, and butanol not participating in the reaction can be efficiently recovered, thereby improving the economic benefit.

[0036] The above are preferred embodiments of the application, and do not limit the protection scope of the application; therefore, equivalent changes made on the basis of the structure, shape, and principle of the application should be covered by the protection scope of the application.

Claims

1. A distillation recovery apparatus for the preparation of ethylene glycol butyl ether, characterized in that: The device includes a distillation column, a reaction liquid tank inside the distillation column, a heating mechanism below the reaction liquid tank, a partition plate inside the distillation column, a condensation chamber above the partition plate, a plurality of condensing tubes inside the condensation chamber, rising holes through the partition plate along its thickness direction, rising tubes inside the rising holes, the rising tubes connecting the upper and lower ends of the partition plate, flow guides distributed below the partition plate, a plurality of outflow holes on the sidewall of the rising tubes above the partition plate, a recovery pipe connected to the sidewall of the condensation chamber, and a distillate separation mechanism connected to the other end of the recovery pipe.

2. The distillation and recovery apparatus for the preparation of ethylene glycol butyl ether according to claim 1, characterized in that: The distillate separation mechanism includes a settling and layering tower, a drain valve, a drain valve, an intermediate tower, and a recovery tower. The settling and layering tower is connected to the recovery pipe. A cooling module is installed inside the settling and layering tower. The drain valve is connected to the side wall of the settling and layering tower, and the drain valve is connected to the bottom wall of the settling and layering tower. The intermediate tower is connected to the end of the drain valve away from the settling and layering tower. A loading container is installed inside the intermediate tower. The loading container is connected to the drain valve. A metering valve is installed at the connection between the drain valve and the loading container. A weight sensing module is installed at the bottom of the loading container. The metering valve is communicatively connected to the weight sensing module. The loading container is connected to a discharge pipe and a reflux pipe. The discharge pipe is connected to the recovery tower, and the other end of the reflux pipe is connected to the settling and layering tower.

3. The distillation recovery apparatus for preparing ethylene glycol butyl ether according to claim 2, characterized in that: A temperature control module is installed at the top of the interior of the intermediate tower.

4. The distillation recovery apparatus for preparing ethylene glycol butyl ether according to claim 2, characterized in that: The sidewall of the condensation chamber is connected to several recovery pipes, and the other end of each recovery pipe is connected to a distillate separation mechanism. Each recovery pipe is equipped with an on / off valve.

5. The distillation recovery apparatus for preparing ethylene glycol butyl ether according to claim 1, characterized in that: A negative pressure module is installed at the top of the riser pipe.

6. The distillation and recovery apparatus for the preparation of ethylene glycol butyl ether according to claim 1, characterized in that: The bottom wall of the condensation chamber is provided with a flow guiding slope, which is inclined toward the direction of the recovery pipe.

7. The distillation and recovery apparatus for the preparation of ethylene glycol butyl ether according to claim 1, characterized in that: The inner wall of the flow guide is provided with a number of support rods, all of which are arranged in a horizontal direction and distributed along the circumferential direction of the flow guide. At one end of each of the support rods that is close to each other, a number of rotating parts are provided. The output shaft of the rotating parts is arranged in a vertical direction, and a stirring shaft is provided on the output shaft of the rotating parts. The stirring shaft is inserted into the reaction liquid tank.

8. The distillation recovery apparatus for preparing ethylene glycol butyl ether according to claim 7, characterized in that: An isolation cover is provided on the surface of the support rod, the isolation cover covers the rotating part, and the side wall of the isolation cover has a flow slope.

9. The distillation recovery apparatus for preparing ethylene glycol butyl ether according to claim 1, characterized in that: The reaction tank is surrounded by a barrier cover.

10. The distillation recovery apparatus for preparing ethylene glycol butyl ether according to claim 9, characterized in that: The side wall of the reaction tank is connected to an outlet pipe, which passes through a barrier cover and a distillation column in sequence. The other end of the outlet pipe is connected to a recovery tank, and a molecular sieve is installed on the outlet pipe.

Images