Reaction solution separation device for fine chemical engineering
The reaction solution separation device, controlled by a detector and a pneumatic valve, solves the problem of separation difficulties caused by unclear interfaces, and achieves automatic separation and efficient production.
Patent Information
- Application Number
- CN202522670506.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-17
- Publication Date
- 2026-01-16
- Estimated Expiration
- 2035-12-17
AI Technical Summary
In existing technologies, the interfaces between the solvent layer, intermediate layer, and aqueous phase layer in the reaction solution are unclear, making manual separation difficult. This requires repeated operations, resulting in low production efficiency, easy misjudgment, and significant material loss.
The interface position is detected in real time by a detector, and combined with pneumatic valve for coordinated control, the solvent layer, intermediate layer and aqueous phase layer are automatically separated. The inlet is designed to be curved to avoid static electricity and foam generation, and an observation window is provided for easy operation.
It achieves precise and automatic separation of reaction solutions, improves production efficiency, reduces material loss, and simplifies the operation process.
Smart Images
Figure CN223800116U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model belongs to the technical field of reaction solution separation, specifically relates to a reaction solution separation device for fine chemical industry. BACKGROUND
[0002] In the production of fine chemical and new chemical material, many reaction processes involve the synergistic reaction of solvent and water or water-containing raw material, or water is generated in the reaction process, resulting in the existence of mutually insoluble solvent layer, water phase layer and interface blurred intermediate layer in the final reaction solution. At present, the traditional separation technology usually removes insoluble solid impurities first, and then relies on gravity sedimentation and manual operation of oil-water separator for separation.
[0003] But in actual production, due to the existence of impurities, by-product, emulsifier or trace solid in raw material, the reaction solution is not clear after standing, but presents a complex state of solvent layer, intermediate layer and water phase layer interface, which makes it difficult for artificial observation and judgment, resulting in the difficulty of one-time complete separation of solvent layer or water layer, and the need for repeated standing and liquid separation operation, thereby the problems of low production efficiency and occupation of manpower exist, and the precision of separation by manpower is poor, and misjudgment is easy to occur in operation, thereby causing material loss. UTILITY MODEL CONTENT
[0004] Based on the above technical problems, the utility model aims to provide a reaction solution separation device for fine chemical industry, which realizes the function of automatically separating the solvent layer, intermediate layer and water phase layer in the reaction liquid accurately, thereby improving the production efficiency and reducing the material loss.
[0005] The specific technical scheme is as follows:
[0006] A reaction solution separation device for fine chemical industry, comprising: a separator, an automatic liquid separation device and a detector; the top of the separator is provided with a liquid inlet, and the bottom is provided with a main liquid outlet; the automatic liquid separation device comprises a main connecting pipe, a first branch pipe, a second branch pipe, a main pneumatic valve, an upper layer medium pneumatic valve, a middle layer medium pneumatic valve and a lower layer medium pneumatic valve, the main connecting pipe is in communication with the main liquid outlet, the first branch pipe and the second branch pipe are in communication with the main connecting pipe respectively, the main pneumatic valve is arranged on the main connecting pipe, the upper layer medium pneumatic valve is arranged on the first branch pipe, and the middle layer medium pneumatic valve and the lower layer medium pneumatic valve are arranged on the two sides of the second branch pipe respectively; the detector is arranged on the main connecting pipe.
[0007] In addition, the reaction solution separation device for fine chemical industry provided by the above technical scheme of the utility model can also have the following additional technical features:
[0008] In the above technical scheme, the top of the separator is further provided with a temperature detection port, an exhaust port, a protective gas inlet, a liquid level detection port and an inspection port, and the bottom of the separator is provided with a middle layer liquid outlet standby port and a lower layer liquid outlet standby port.
[0009] In the above technical scheme, the bottom of the liquid inlet port extends into the separator, and the bottom of the liquid inlet port is bent towards the inner wall of the separator.
[0010] In the above technical scheme, a plurality of observation mirrors and a plurality of mirror lamps are further included; the mirror lamps are arranged on the inner wall of the separator, and the observation mirrors are arranged on the outer wall of the separator.
[0011] In the above technical scheme, the plurality of observation mirrors are staggered, and the observation mirrors are opposite to the positions of the mirror lamps.
[0012] In the above technical scheme, the five-way mirror is arranged on the main connecting pipe, and the probe of the detector is inserted into the five-way mirror.
[0013] Compared with the prior art, the reaction solution separation device for fine chemical industry has the beneficial effects that:
[0014] 1. The interface positions of the solvent layer, the intermediate layer and the water layer are detected in real time by the detector, and the detector is used in cooperation with the upper layer medium pneumatic valve, the intermediate layer medium pneumatic valve and the lower layer medium pneumatic valve, so that automatic separation of the medium from the lower layer to the upper layer is realized, the problem of manual separation difficulty caused by the existence of the intermediate layer and unclear interface and the problem of the need for repeated operation are solved, the production efficiency is improved, and the material loss is reduced.
[0015] 2. The liquid inlet port is designed to be bent towards the inner wall of the separator, so that the solvent reaction liquid flows down along the inner wall, static electricity and foam caused by direct impact on the liquid surface are avoided, and the layered interface is disturbed.
[0016] 3. A plurality of observation mirrors and mirror lamps are arranged, so that the operator can observe the internal layering condition. BRIEF DESCRIPTION OF DRAWINGS
[0017] Fig. 1 It is a structure schematic view of the reaction solution separation device for fine chemical industry;
[0018] Fig. 2 It is a sectional view of the separator;
[0019] Fig. 3 It is a top view of the separator;
[0020] Among them, Figs. 1-3 The correspondence between the reference signs and the component names in the above table is as follows:
[0021] 10 Separator, 11 Liquid Inlet, 12 Main Liquid Outlet, 13 Main Connecting Pipe, 14 First Branch Pipe, 15 Second Branch Pipe, 16 Main Pneumatic Valve, 17 Upper Layer Medium Pneumatic Valve, 18 Middle Layer Medium Pneumatic Valve, 19 Lower Layer Medium Pneumatic Valve, 20 Detector, 21 Temperature Detection Port, 22 Exhaust Port, 23 Protective Gas Inlet, 24 Liquid Level Detection Port, 25 Inspection Port, 26 Middle Layer Liquid Outlet Backup Port, 27 Lower Layer Liquid Outlet Backup Port, 28 Observation Sight Glass, 29 Sight Glass Light, 30 Five-Way Sight Glass. Detailed Implementation
[0022] The following are specific implementation cases and appendices. Figs. 1-3 The present invention will be further described below, but the present invention is not limited to these embodiments. Example 1:
[0023] A reaction solution separation device for fine chemical industry, such as Figs. 1-3 As shown, the system includes: a separator 10, an automatic liquid separation device, and a detector 20; the separator 10 has an inlet 11 at the top and a main outlet 12 at the bottom; the automatic liquid separation device includes a main connecting pipe 13, a first branch pipe 14, a second branch pipe 15, a main pneumatic valve 16, an upper medium pneumatic valve 17, a middle medium pneumatic valve 18, and a lower medium pneumatic valve 19. The main connecting pipe 13 is connected to the main outlet 12, and the first branch pipe 14 and the second branch pipe 15 are respectively connected to the main connecting pipe 13. The main pneumatic valve 16 is installed on the main connecting pipe 13, the upper medium pneumatic valve 17 is installed on the first branch pipe 14, and the middle medium pneumatic valve 18 and the lower medium pneumatic valve 19 are respectively installed on both sides of the second branch pipe 15; the detector 20 is installed on the main connecting pipe 13.
[0024] When using the above structure for automatic liquid separation, the detector 20 detects the interface position of the solvent layer, intermediate layer and water layer in real time, and works in conjunction with the upper medium pneumatic valve 17, the middle medium pneumatic valve 18 and the lower medium pneumatic valve 19 to achieve automatic separation of the medium from the lower layer to the upper layer. This solves the problem of difficulty in manual liquid separation due to the presence of the intermediate layer and unclear interface, which requires repeated operations, thereby improving production efficiency and reducing material loss.
[0025] The specific implementation process is as follows:
[0026] First, open the main pneumatic valve 16. After waiting for 15 seconds, the detector 20 checks whether the liquid is the lower layer medium. If it is the lower layer medium, the lower layer medium pneumatic valve 19 opens to discharge the lower layer medium. If it is not the lower layer medium, the main pneumatic valve 16 is closed, and the staff checks whether there is any abnormality.
[0027] In the process of liquid separation, when the detector 20 detects that the characteristic of the lower medium changes more than the judgment threshold r1, delay 1s, close the lower medium pneumatic valve 19. The solution continues to separate, after the delay time t1, the detector 20 detects whether the solution is the lower medium again, if it is the lower medium, open the lower medium pneumatic valve 19, continue to discharge the lower medium; when the detection of the lower medium characteristic changes more than the judgment threshold r1, delay 1s, close the lower medium pneumatic valve 19, and the lower medium separation is completed.
[0028] After a delay of 10s, the detector 20 detects whether the liquid is the middle medium, if so, open the middle medium pneumatic valve 18, discharge the middle medium, when the detection of the middle medium characteristic changes more than the judgment threshold r2, delay 1s, close the middle medium pneumatic valve 18; The solution continues to separate, after the delay time t2, detect whether the solution is the middle medium again, if so, open the middle medium pneumatic valve 18, continue to discharge the middle medium; when the detection of the middle medium characteristic changes more than the judgment threshold r2, delay 1s, close the middle medium valve, and the middle medium separation is completed.
[0029] After a delay of 10s, the detector 20 detects whether the liquid is the upper medium, if so, open the upper medium valve, discharge the upper medium, when the detection of the pipeline has no liquid, delay 10s, close the upper medium valve, and the liquid separation is completed.
[0030] Specifically, the upper medium of the reaction solution is the solvent layer, and the lower medium is generally the aqueous phase layer, wherein the difference between the characteristic data of the aqueous phase layer and the solvent layer is greater than or equal to 500.
[0031] Specifically, the detector 20, the main pneumatic valve 16, the upper medium pneumatic valve 17, the middle medium pneumatic valve 18 and the lower medium pneumatic valve 19 are controlled by the access control system to realize automatic liquid separation.
[0032] Specifically, the detector 20 is an ultrasonic detector 20, which is not affected by the chroma, turbidity, density and conductivity of the medium, and the model of the ultrasonic detector 20 can be a conventional model purchased on the market.
[0033] Specifically, the layering device is a cylindrical structure, and the bottom of the layering device is a conical structure. The height and diameter ratio of the cylinder and the cone can be adjusted according to the layering speed of the reaction liquid and the feeding amount.
[0034] In the embodiment of the utility model, the top of the separator 10 is also provided with a temperature detection port 21, an exhaust port 22, a protective gas inlet 23, a liquid level detection port 24 and an inspection port 25, and the bottom of the separator 10 is provided with a middle layer liquid outlet standby port 26 and a lower layer liquid outlet standby port 27.
[0035] A temperature sensor is installed through the temperature detection port 21 for monitoring the temperature of the reaction solution separation process in the separator 10; the exhaust port 22 is used to release gas when the feed or temperature changes, balance the pressure inside the separator 10, and maintain normal pressure; the protector inlet is used to access ammonia or other protective gas to establish an inert atmosphere when needed to prevent solution oxidation; the liquid level detection port 24 is used to install a liquid level measuring instrument to achieve the purpose of remotely monitoring the liquid level of the solution in the separator 10; the inspection port 25 is designed to facilitate the staff to conduct daily inspection and internal cleaning of the inside of the separator 10.
[0036] The main liquid outlet 12, the middle layer liquid outlet standby port 26 and the lower layer liquid outlet standby port 27 can be connected to an automatic liquid distribution device and installed with a detection instrument 20, so that the optimal liquid outlet can be selected flexibly according to the characteristics of different reaction liquids, such as a certain phase layer volume ratio being too large, high viscosity or easy to block.
[0037] Specifically, when the liquid level measuring instrument detects that the liquid level changes exceed the threshold range or the separation time exceeds the set range, and the lower layer medium separation is completed but no signal is sent that the lower layer medium separation is completed, the main pneumatic valve 16 and the lower layer medium pneumatic valve 19 are automatically closed to stop the separation operation, so that the operator can check the abnormality.
[0038] In the embodiment of the utility model, the bottom of liquid inlet 11 extends into separator 10, and the bottom of liquid inlet 11 is bent towards the inner wall of separator 10.
[0039] By bending the bottom of the liquid inlet 11 towards the inner wall of the separator 10, the solvent reaction liquid flows down along the inner wall, avoiding direct impact on the liquid surface to generate static electricity and foam, and disturbing the already layered interface.
[0040] In the embodiment of the utility model, a plurality of observation mirrors 28 and a plurality of mirror lamps 29 are further included; the mirror lamp 29 is arranged on the inner wall of the separator 10, and the observation mirror 28 is arranged on the outer wall of the separator 10.
[0041] By arranging the observation mirror 28 and the mirror lamp 29, the staff can observe the layered interface and abnormal conditions in the separator 10.
[0042] In the embodiment of the utility model, the plurality of observation mirrors 28 are staggered, and the observation mirror 28 is opposite to the mirror lamp 29 in position.
[0043] In the embodiment of the utility model, the five-way mirror 30 is arranged on the main connecting pipe 13, and the probe of the detection instrument 20 is inserted into the five-way mirror 30.
[0044] The five-way mirror 30 is arranged to facilitate the staff to observe the solution flowing through the main connecting pipe 13. Embodiment 2:
[0045] This embodiment takes the treatment of the condensed reaction material as an example. After pressure filtration of the condensed reaction material of fine chemical intermediates, the obtained filtrate contains chlorobenzene, aluminum chloride aqueous solution and suspended solids. The chlorobenzene is the upper medium, the aluminum chloride aqueous solution is the lower medium, and the suspended solids are the intermediate medium.
[0046] The technical solution of Example 1 is used for separation treatment. First, the characteristic signal range of each phase medium on the detector is determined by the experimental detector. The aluminum chloride aqueous solution is 14000-14800, the suspended solids are 0, and the chlorobenzene is 9400-9900. According to this, the threshold value r1 for identifying the lower medium is set to 14000-15000, and the threshold value r2 for identifying the intermediate medium is set to 0-500.
[0047] Since the mixed liquid is slowly layered, and the process requires that the lower and intermediate media be completely separated as much as possible, the standing time t1 after lower layer separation is set to 1800s, and the standing time t2 after intermediate layer separation is set to 1800s.
[0048] The use of this technology to separate the solution can reduce the amount of chlorobenzene in the lower aqueous solution to a minimum, and can control the amount of suspended solids in chlorobenzene to a minimum, thereby reducing the amount of hazardous solid waste generated during chlorobenzene recovery. Example 3:
[0049] This embodiment takes the n-hexane solvent used in the extraction and refining process of electronic materials as an example. Since the raw material contains moisture, a three-phase system is formed after reaction. The upper layer is n-hexane dissolved with the target product, the intermediate layer is a transition layer formed by impurity suspended solids, and the lower layer is the water phase.
[0050] The technical solution of Example 1 is used for separation treatment. First, the characteristic signal range of each phase is determined by the experimental detector. After detection, the threshold value is set to identify the threshold value r1 of the lower water phase, which is 11000-12000, and the threshold value r2 of the intermediate layer suspended solids, which is 0-500.
[0051] In view of the fast layering speed of the material, the standing time t1 after lower layer separation is set to 600s, and the standing time t2 after intermediate layer separation is set to 1200s.
[0052] The use of this technology to separate the solution can reduce the amount of chlorobenzene in the lower aqueous solution to a minimum, and can control the amount of suspended solids in chlorobenzene to a minimum, thereby reducing the amount of hazardous solid waste generated during chlorobenzene recovery.
[0053] In the description of the utility model, the term "a plurality of" refers to two or more than two, unless otherwise expressly limited, the orientation or position relationship indicated by the terms "upper", "lower" and the like is based on the orientation or position relationship shown in the drawings, and is only for the convenience of describing the utility model and simplifying the description, and does not indicate or imply that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as limiting the utility model; the terms "connection", "installation", "fixation" and the like should be understood broadly, for example, "connection" can be fixed connection, can also be detachable connection, or integral connection; can be directly connected, or indirectly connected through an intermediate medium. For ordinary skilled persons in the art, the specific meaning of the above terms in the utility model can be understood according to the specific circumstances.
[0054] The above only describes preferred embodiments of the utility model and is not used to limit the utility model. For those skilled in the art, the utility model can have various changes and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the utility model should be included in the protection scope of the utility model.
Claims
1. A separation apparatus for reaction solutions used in fine chemicals, characterized by comprising: The application relates to a separator, an automatic liquid distribution device and a detector. The top of the separator is provided with a liquid inlet, and the bottom is provided with a main liquid outlet; the automatic liquid distribution device comprises a main connecting pipe, a first branch pipe, a second branch pipe, a main pneumatic valve, an upper-layer medium pneumatic valve, a middle-layer medium pneumatic valve and a lower-layer medium pneumatic valve, the main connecting pipe is communicated with the main liquid outlet, the first branch pipe and the second branch pipe are respectively communicated with the main connecting pipe, the main pneumatic valve is arranged on the main connecting pipe, the upper-layer medium pneumatic valve is arranged on the first branch pipe, and the middle-layer medium pneumatic valve and the lower-layer medium pneumatic valve are respectively arranged on the two sides of the second branch pipe; and the detector is arranged on the main connecting pipe.
2. The device for separating a reaction solution for fine chemicals according to claim 1, wherein The top of the separator is further provided with a temperature detection port, an exhaust port, a protective gas inlet, a liquid level detection port and an inspection port, and the bottom of the separator is provided with a middle-layer liquid outlet standby port and a lower-layer liquid outlet standby port.
3. The device for separating a reaction solution for fine chemicals according to claim 1, wherein The bottom of the liquid inlet extends into the separator, and the bottom of the liquid inlet is bent towards the inner wall of the separator.
4. The device for separating a reaction solution for fine chemicals according to claim 1, wherein The application further relates to a device for separating and detecting liquid. A plurality of observation mirrors and a plurality of mirror lamps are arranged; the mirror lamps are arranged on the inner wall of the separator, and the observation mirrors are arranged on the outer wall of the separator.
5. The device for separating a reaction solution used in fine chemicals according to claim 4, wherein The plurality of observation mirrors are staggered, and the observation mirrors are opposite to the positions of the mirror lamps.
6. The device for separating a reaction solution for fine chemicals according to claim 1, wherein A five-way mirror is arranged on the main connecting pipe, and the probe of the detector is inserted into the five-way mirror.