ECH automatic recycling system
By introducing automatic circulating reflux and online detection control in the ECH recycling system, the problem of manual adjustment of the liquid level of the liquid separator tank is solved, efficient recycling of ECH and product quality improvement, and meet industrial production needs.
Patent Information
- Application Number
- CN202422374802.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-27
- Publication Date
- 2025-07-29
- Estimated Expiration
- 2034-09-27
AI Technical Summary
In the prior art, the ECH recycling process requires operators to always pay attention to the liquid level of the liquid separator tank, consume a lot of manpower and make mistakes, affecting the reaction efficiency and product quality, and it is difficult to meet production requirements.
An automatic circulation and recovery system consisting of a reactor, a condenser and a condensing liquid separation tank is used to realize the automatic circulation and reflux of ECH using a differential pressure position gauge and a check valve. Combined with an online water content detector, an aqueous phase solution is automatically replenished, and a water phase overflow tube and a visual mirror are set to observe the liquid separation situation, and a steam jet pump is used to evacuate and improve the separation efficiency.
Realize automatic recycling of ECH, reduce manual operation difficulty, improve recovery rate and product quality, save energy, and improve production efficiency.
Smart Images

Figure CN223159239U_ABST
Abstract
Description
Technical Field
[0001] The utility model belongs to the field of chemical production equipment, and particularly relates to an automatic circulation recovery system for ECH. Background Technique
[0002] Glycidyl ether is produced by using an alcohol or phenolic substance containing active hydrogen and epichlorohydrin (ECH) as raw materials through a process of etherification first and then ring closure. During this production process, water needs to be continuously discharged to ensure the smooth progress of the reaction. However, during the discharge of water, epichlorohydrin (ECH) will also be discharged together, so ECH needs to be continuously replenished to ensure production.
[0003] In industrial production, a separation tank is usually used, and the reflux of ECH is adjusted by relying on the opening of the reflux proportional control valve. However, this method requires operators to always monitor the liquid level of the separation tank for real-time adjustment, consuming a large amount of manpower. At the same time, it is inevitable for workers to make mistakes, resulting in waste of ECH. Seriously, it affects the reaction efficiency and product quality, and also affects the recovery rate, causing pollution and making it difficult to meet the actual production requirements. Content of the Utility Model
[0004] In order to improve the recovery and treatment efficiency of ECH and product quality, and reduce the operation difficulty of the device, this application provides an automatic circulation recovery system for ECH, which can significantly improve the yield and quality of ECH products, is easy to operate, reduces manpower consumption, and saves energy.
[0005] This application provides an automatic circulation recovery system for ECH, which adopts the following technical solutions:
[0006] An automatic circulation recovery system for ECH includes a reaction kettle, the reaction kettle is connected to a condenser through a liquid pipeline, the condenser is connected to a condensation separation tank, a check valve is arranged at the bottom of the condensation separation tank, the check valve is connected to a reflux pipeline, the reflux pipeline is connected to the reaction kettle, a differential pressure level gauge is also arranged on the condensation separation tank, and the differential pressure level gauge is connected to the check valve.
[0007] By adopting the above technical solutions, the materials in the reaction kettle react by heating the reaction kettle. During the reaction process, the water and ECH generated are azeotroped into steam, which is condensed by connecting to the condenser through a pipeline. The condensed mixed liquid enters the condensation separation tank and is separated into an aqueous solution and an oil-phase solution. Through the differential pressure level gauge arranged on the condensation separation tank and the connection of the check valve arranged at the bottom of the reaction kettle, the separation tank automatically interlocks the check valve at the bottom of the reaction kettle through the differential pressure liquid level gauge, and the organic-phase ECH is refluxed to the reaction kettle for continuous cyclic reaction, improving the cyclic utilization efficiency of ECH.
[0008] In a specific feasible implementation, a plurality of aqueous-phase overflow pipes are provided on one side of the condensation and separation tank. The aqueous-phase overflow pipes are connected to a water receiving tank, and each aqueous-phase overflow pipe is connected to a water valve. A sight glass is also provided on the condensation and separation tank.
[0009] By adopting the above technical solution, by providing a plurality of aqueous-phase overflow pipes on the condensation and separation tank, the aqueous phase in the separation tank can be discharged in time and enter the water receiving tank, further improving the separation efficiency and reducing the separation time. The sight glass can be used to observe the separation situation inside the condensation and separation tank, avoiding uneven separation and preventing the organic phase ECH from flowing out through the aqueous-phase overflow pipe, resulting in waste of resources and reducing the recovery rate.
[0010] In a specific feasible implementation, a water inlet pipe is provided at the top of the condensation and separation tank, and the pipeline of the water inlet pipe extends to the middle and lower part of the condensation and separation tank.
[0011] By adopting the above technical solution, by inserting the pipeline of the water inlet pipe into the middle and lower part of the separation tank, it can prevent the disturbance of stratification during feeding and improve the separation and recovery efficiency.
[0012] In a specific feasible implementation, a hydraulic valve is further provided at the bottom of the condensation and separation tank, and the hydraulic valve is connected to an ECH receiving tank.
[0013] By adopting the above technical solution, by providing a hydraulic valve and connecting it to an ECH receiving tank, after the glycidyl ether preparation reaction is completed, the remaining ECH can be recovered, reducing the waste of ECH and improving the recovery rate.
[0014] In a specific feasible implementation, the bottom of the water receiving tank is connected to a water-phase valve through an aqueous-phase overflow pipe, the end of the aqueous-phase overflow pipe is connected to a reflux pipe, and an on-line water content detector is provided at the bottom of the reaction kettle. The on-line water content detector is connected to the water-phase valve.
[0015] By adopting the above technical solution, by providing an on-line water content detector at the bottom of the kettle, when the aqueous-phase liquid is lower than the set value, the aqueous-phase solution is automatically supplemented to participate in the reaction and a new round of purification is continued.
[0016] In a specific feasible implementation, one end of the condenser is provided with a water inlet, and the other end is provided with a water return port. Both the water inlet and the water return port are connected to a cooling water tank.
[0017] By adopting the above technical solution, by setting the cooling water to return, the cooling of the condenser is accelerated, so that the water vapor and the co-boiling ECH in the production process are quickly cooled, improving the production efficiency.
[0018] In a specific feasible implementation, a steam jet pump is further connected to the condensation and separation tank through a pipeline, and the steam jet pump is connected to a vacuum system.
[0019] By adopting the above technical solution, a steam jet pump is used to evacuate the air, making the liquid separation efficiency of the condensation and liquid separation tank higher, the separation interface more obvious, the separation effect better, further saving the residence time and improving the production efficiency.
[0020] In a specific feasible embodiment, a vent valve is further provided at the top of the condensation and liquid separation tank.
[0021] By adopting the above technical solution, after passing through the reaction kettle and the condenser, a small amount of non-condensable gas is discharged through the vent valve, making the liquid separation of water and ECH faster and the production efficiency of ECH in the system higher.
[0022] In summary, the present application includes at least one of the following beneficial technical effects:
[0023] 1. The mixed materials in the reaction kettle react by heating the reaction kettle. During the reaction process, the water and ECH generated form an azeotrope and turn into steam, which is connected to the condenser through a pipeline for condensation. The condensed mixed liquid enters the condensation and liquid separation tank and is separated into an aqueous solution and an oil-phase solution. Through the differential pressure level gauge provided on the condensation and liquid separation tank and the one-way valve provided at the bottom of the reaction kettle, the liquid separation tank automatically interlocks the one-way valve at the bottom of the reaction kettle through the differential pressure level gauge, and the organic phase ECH is refluxed to the reaction kettle for continuous cyclic reaction, improving the recycling efficiency of ECH.
[0024] 2. By providing a plurality of aqueous-phase overflow pipes on the condensation and liquid separation tank, the aqueous phase in the liquid separation tank is discharged in time and enters the water receiving tank, further improving the liquid separation efficiency and reducing the liquid separation time. A sight glass is provided to observe the liquid separation situation inside the condensation and liquid separation tank, avoiding uneven liquid separation and causing the organic phase ECH to flow out from the aqueous-phase overflow pipe, resulting in waste of resources and reducing the recovery utilization rate.
[0025] 3. By providing an on-line water content detector at the bottom of the kettle, when the aqueous-phase liquid is lower than the set value, the aqueous-phase solution is automatically supplemented to participate in the reaction and a new round of purification is continued. BRIEF DESCRIPTION OF THE DRAWINGS
[0026] Figure 1 is a schematic structural diagram of Embodiment 1 of the present application.
[0027] Figure 2 is a schematic structural diagram of Embodiment 2 of the present application.
[0028] Description of reference numerals: 1, reactor; 11, condenser; 12, condensate separation tank; 13, check valve; 131, reflux pipeline; 14, differential pressure level gauge; 2, aqueous phase overflow pipe; 21, water receiving tank; 22, water valve; 23, sight glass; 3, water inlet pipe; 33, hydraulic valve; 331, ECH receiving tank; 4, aqueous phase valve; 44, on-line water content detector; 441, water inlet; 442, water return port; 5, steam ejector pump; 51, vacuum system; 511, vent valve. Detailed implementation manners
[0029] The following further describes the present application in conjunction with Figure 1-2 accompanying drawings.
[0030] The embodiment of the present application discloses an automatic ECH recycling system.
[0031] Embodiment 1
[0032] Referring to Figure 1 , an automatic ECH recycling system includes a reactor 1, a condenser 11 and a condensate separation tank 12 connected in sequence through pipelines, and an ECH receiving tank 331 and a water receiving tank 21 respectively connected to the condensate separation tank 12. Three aqueous phase overflow pipes 2 with different water level heights are arranged on one side of the condensate separation tank 12. The three aqueous phase overflow pipes 2 are communicated and connected to the water receiving tank 21, and each aqueous phase overflow pipe 2 is connected with a water valve 22. A sight glass 23 is also arranged on the condensate separation tank 12. The sight glass 23 can observe the liquid separation situation inside the condensate separation tank 12, avoiding uneven liquid separation and causing the organic phase ECH to flow out from the aqueous phase overflow pipe 2, resulting in waste of resources and reducing the recycling utilization rate.
[0033] The bottom of the water receiving tank 21 is connected with an aqueous phase overflow pipe 2, and the aqueous phase overflow pipe 2 is connected with an aqueous phase valve 4 and connected to the reactor 1. An on-line water content detector 44 is arranged on the reactor 1. Through the on-line water content detector 44, the aqueous phase valve 4 can be controlled, and then the content of the aqueous phase in the reactor 1 can be controlled. When the aqueous phase liquid is lower than the set value, the aqueous phase solution is automatically supplemented to participate in the reaction and continue a new round of purification.
[0034] The discharge port of the reactor 1 is connected with a condenser 11 through a pipeline. The right side of the condenser 11 is connected with a water inlet 441, and the other end is provided with a water return port 442. The water inlet 441 and the water return port 442 are both connected to a cooling water tank, which is used to supply water vapor and the ECH mixture azeotroped with it that enter the condenser 11 during the production process to the condenser 11; a water inlet pipe 3 is arranged at the top of the condensate separation tank 12. The discharge port of the condenser 11 is connected to the water inlet pipe 3, and the pipeline of the water inlet pipe 3 extends to the middle and lower part of the condensate separation tank 12 to prevent the stratification from being disturbed during feeding and improve the separation and recycling efficiency.
[0035] A one-way valve 13 is provided at the bottom of the condensation and separation tank 12. The one-way valve 13 is connected to the reaction kettle 1 through a reflux pipeline 131. A differential pressure level gauge 14 is also provided on the condensation and separation tank 12. The differential pressure level gauge 14 is connected to the one-way valve 13, so that the separation tank automatically interlocks the one-way valve 13 at the bottom of the reaction kettle 1 through the differential pressure level gauge, and the organic phase ECH is refluxed to the reaction kettle 1 for continuous cyclic reaction, improving the recycling efficiency of ECH. A hydraulic valve 33 is also provided at the bottom of the condensation and separation tank 12. The hydraulic valve 33 is connected to an ECH receiving tank 331, which is convenient for draining the remaining ECH in the separation tank into the ECH receiving tank 331 after the reaction is completed, and it can be reused during the next production.
[0036] The implementation principle of Example 1 is as follows: The mixed materials in the reaction kettle 1 react by heating the reaction kettle 1. During the reaction process, the water and ECH generated form an azeotrope and turn into steam, which is condensed by being connected to the condenser 11 through a pipeline. The condensed mixed liquid enters the condensation and separation tank 12 and is separated into an aqueous solution and an oil-phase solution. Through the differential pressure level gauge 14 provided on the condensation and separation tank 12 and the one-way valve 13 provided at the bottom of the reaction kettle 1, the separation tank automatically interlocks the one-way valve 13 at the bottom of the reaction kettle 1 through the differential pressure level gauge, and the organic phase ECH is refluxed to the reaction kettle 1 for continuous cyclic reaction, avoiding the original method of adjusting the reflux of ECH by relying on the opening of the proportional control valve for reflux. Furthermore, it is not necessary for the operator to always pay attention to the real-time adjustment of the liquid level in the separation tank, realizing automatic cyclic control of the reaction. Furthermore, through the on-line water content detector 44 provided on the reaction kettle 1, the water phase valve 4 can be controlled, and thus the water content in the reaction kettle 1 can be controlled. When the aqueous liquid is lower than the set value, the aqueous solution is automatically supplemented to participate in the reaction, and a new round of purification is continued. Thus, the automatic cyclic recovery of ECH is realized.
[0037] Example 2
[0038] Refer to Figure 2 , the difference between this embodiment and Example 1 is that a steam jet pump 5 is also connected to the condensation and separation tank 12 through a pipeline. The steam jet pump 5 is connected to a vacuum system 51, and a vent valve 511 is also provided at the top of the condensation and separation tank 12.
[0039] The implementation principle of Example 2 is as follows: Using the steam jet pump 5 to evacuate, the separation efficiency of the condensation and separation tank 12 is higher, the separation interface is more obvious, the separation effect is better, and the residence time is further saved. The small amount of non-condensable gas in the reaction kettle 1 and the condenser 11 is discharged through the vent valve 511, making the separation of water and ECH faster and the production efficiency of ECH higher.
[0040] The above are all the preferred embodiments of this application. The protection scope of this application is not limited accordingly. Therefore, all equivalent changes made according to the structure, shape, and principle of this application should be covered within the protection scope of this application.
Claims
1. An automatic recycling system for ECH, characterized in that, It includes a reactor (1). The reactor (1) is connected to a condenser (11) through a liquid pipeline. The condenser (11) is connected to a condensation separation tank (12). A check valve (13) is provided at the bottom of the condensation separation tank (12). The check valve (13) is connected to a reflux pipeline (131). The reflux pipeline (131) is connected to the reactor (1). A differential pressure level gauge (14) is also provided on the condensation separation tank (12). The differential pressure level gauge (14) is connected to the check valve (13).
2. The ECH automatic recycling system according to claim 1, characterized in that, On one side of the condensation separation tank (12), there are a number of aqueous phase overflow pipes (2). The aqueous phase overflow pipes (2) are connected to a water receiving tank (21). Each aqueous phase overflow pipe (2) is connected to a water valve (22). A sight glass (23) is also provided on the condensation separation tank (12).
3. An ECH automatic recycling system according to claim 1, characterized in that, An inlet pipe (3) is provided at the top of the condensation separation tank (12). The pipeline of the inlet pipe (3) extends to the middle and lower part of the condensation separation tank (12).
4. An ECH automatic recycling system according to claim 1, characterized in that A hydraulic valve (33) is also provided at the bottom of the condensation separation tank (12). The hydraulic valve (33) is connected to an ECH receiving tank (331).
5. An ECH automatic recycling system according to claim 2, characterized in that, The bottom of the water receiving tank (21) is connected to an aqueous phase valve (4) through the aqueous phase overflow pipe (2). The end of the aqueous phase overflow pipe (2) is connected to a reflux pipe. An on-line water content detector (44) is provided at the bottom of the reactor (1). The on-line water content detector (44) is connected to the aqueous phase valve (4).
6. The ECH automatic recycling system according to claim 1, wherein One end of the condenser (11) is provided with a water inlet (441), and the other end is provided with a water return port (442). Both the water inlet (441) and the water return port (442) are connected to a cooling water tank.
7. An ECH automatic recycling system according to claim 1, characterized in that, The condensation separation tank (12) is also connected to a steam jet pump (5) through a pipeline. The steam jet pump (5) is connected to a vacuum system (51).
8. An ECH automatic circulation recovery system according to claim 7, characterized in that, A vent valve (511) is also provided at the top of the condensation separation tank (12).