Reaction kettle
By designing the diverting structure and temperature control of the circulation and sampling pipeline in the reactor, the impact of temperature changes on the online detection of SEBS hydrogenation is solved, and higher detection accuracy and stability are achieved.
Patent Information
- Application Number
- CN202422152243.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-03
- Publication Date
- 2025-07-04
- Estimated Expiration
- 2034-09-03
AI Technical Summary
In the online detection of SEBS hydrogenation degree, temperature changes lead to deviations in Raman spectroscopic detection results, affecting the detection accuracy.
Design a reactor, through the diversion structure of the circulation pipeline and the sampling pipeline, combined with the temperature control mechanism and the Raman probe, to stabilize the temperature environment and reduce the impact of temperature on the detection results.
It significantly improves the accuracy of SEBS hydrogenation degree detection, reduces the impact of temperature on the detection results, and improves the stability and accuracy of the detection.
Smart Images
Figure CN223065161U_ABST
Abstract
Description
Technical Field
[0001] This application belongs to the technical field of on-line process detection of SEBS hydrogenation degree. Specifically, it relates to a reaction kettle. Background Art
[0002] SEBS is the selectively hydrogenated product of SBS (styrene-butadiene-styrene triblock copolymer), and its performance is closely related to the degree of hydrogen addition. The evaluation index of the degree of hydrogen addition is the hydrogenation degree. The higher the hydrogenation degree of SEBS, the better its tensile strength, heat resistance, antioxidant property, and aging resistance.
[0003] For on-line detection of the SEBS hydrogenation degree, Raman spectroscopy detection technology based on laser inelastic scattering can be used. This method first needs to establish a reference model for SEBS with different hydrogenation degrees, and then compare the spectral detection results of the Raman probe with the reference model to obtain the SEBS hydrogenation degree. The detection process has advantages such as being fast and non-destructive. Moreover, compared with infrared spectroscopy, Raman spectroscopy is less affected by free OH bonds such as water molecules, making it more suitable for the detection of liquid samples. In addition, the fiber optic probe can be made of materials suitable for different uses, so it can be directly applied to acidic, alkaline, and corrosive environments.
[0004] However, the Raman spectrum of SEBS is not only affected by its hydrogenation degree but also sensitive to temperature. The change in temperature will cause the shift of the Raman spectral peak. When the temperature difference between the on-line detection temperature environment and the temperature environment during reference model establishment is large, it will cause measurement deviation. Summary of the Invention
[0005] The purpose of this application is to provide a reaction kettle to stabilize the temperature environment of the Raman probe and improve the accuracy of on-line detection of the Raman probe.
[0006] To achieve the above purpose, this application provides a reaction kettle, which includes:
[0007] A kettle body for SEBS hydrogenation reaction;
[0008] A circulation pipeline, the inlet end and the outlet end of which are both communicated with the inner cavity of the kettle body, and a circulation pump is provided;
[0009] A sampling pipeline, which is connected in parallel to the circulation pipeline;
[0010] A Raman probe, which is arranged on the sampling pipeline and is used to detect the SEBS rubber solution in the sampling pipeline.
[0011] In some embodiments, the sampling pipeline includes a temperature control mechanism for controlling the temperature of the SEBS rubber solution. The temperature control mechanism and the Raman probe are sequentially arranged after the inlet of the sampling pipeline.
[0012] In some embodiments, the temperature control mechanism is a water cooler.
[0013] In some embodiments, the sampling pipeline further includes a sampling valve, and the sampling valve is used for sampling the SEBS rubber solution in the sampling pipeline.
[0014] In some embodiments, the circulation pipeline includes a first stop valve, and the first stop valve is used to control the flow rate of the circulation pipeline.
[0015] In some embodiments, the sampling pipeline includes a second stop valve, and the second stop valve provided at the inlet of the sampling pipeline is used to control the flow rate of the sampling pipeline.
[0016] In some embodiments, the Raman probe is detachably inserted into the sampling pipeline, and the sampling pipeline includes a third stop valve. The third stop valve provided at the outlet of the sampling pipeline is used to control the on-off of the sampling pipeline.
[0017] In some embodiments, both the feed end and the discharge end of the circulation pipeline are connected to the kettle body through maintenance valves. The maintenance valves are used to control the on-off of the circulation pipeline. The circulation pipeline further includes an openable and closable air blowing port and an openable and closable evacuation port. The air blowing port is arranged adjacent to the discharge end, and the evacuation port is arranged adjacent to the feed end.
[0018] In some embodiments, the reaction kettle further includes a temperature sensor arranged adjacent to the sensitive element of the Raman probe.
[0019] In some embodiments, the circulation pipeline is detachably connected to the kettle body.
[0020] In the technical solution of the present application, the circulation pipeline can draw out a part of the SEBS colloid from the kettle body for SEBS hydrogenation reaction, and a small amount of SEBS colloid can be shunted from the circulation pipeline through the sampling pipeline connected in parallel to the circulation pipeline. The Raman probe arranged on the sampling pipeline is used to perform spectral detection on the SEBS colloid to determine the hydrogenation degree of the SEBS colloid. Through two shunts of "kettle body - circulation pipeline" and "circulation pipeline - sampling pipeline", the flow rate of the SEBS colloid used for hydrogenation degree detection can be significantly reduced, which is beneficial to cooling the SEBS colloid to room temperature, thereby reducing the influence of the temperature on the spectrum of the SEBS colloid, and further improving the accuracy of SEBS hydrogenation degree detection.
[0021] Other features and advantages of the embodiments of the present application will be described in detail in the subsequent specific embodiment part. Brief Description of the Drawings
[0022] The accompanying drawings are used to provide a further understanding of the embodiments of the present application, and constitute a part of the specification. Together with the following specific embodiments, they are used to explain the embodiments of the present application, but do not constitute a limitation to the embodiments of the present application. For those of ordinary skill in the art, other drawings can be obtained based on the structures shown in these drawings without creative efforts. In the drawings:
[0023] Figure 1 It is a schematic structural diagram of a reactor according to a specific embodiment of the present application.
[0024] Explanation of reference numerals in the drawings
[0025] 1 Reactor body 8 First stop valve
[0026] 2 Circulation pump 7 Second stop valve
[0027] 3 Water cooler 9 Third stop valve
[0028] 4 Sampling valve A Circulation pipeline
[0029] 5 Raman probe B Sampling pipeline Specific embodiments
[0030] The following will describe in detail the specific embodiments of the present application with reference to the accompanying drawings. It should be understood that the specific embodiments described herein are only used to illustrate and explain the present application, and are not used to limit the present application.
[0031] The reactor according to the present application will be described below with reference to the drawings.
[0032] The present application discloses a novel reactor, as Figure 1 shown, a reactor in a specific embodiment includes:
[0033] Reactor body 1, which is used for the hydrogenation reaction of SEBS;
[0034] Circulation pipeline A, both the inlet end and the outlet end of the circulation pipeline A are communicated with the inner cavity of the reactor body 1, and a circulation pump 2 is provided;
[0035] Sampling pipeline B, which is connected in parallel to the circulation pipeline A;
[0036] Raman probe 5, which is arranged on the sampling pipeline B, and the Raman probe 5 is used to detect the SEBS rubber solution in the sampling pipeline B.
[0037] Specifically, refer to Figure 1, the circulation pipeline A is connected in parallel to the reactor body 1, and the sampling pipeline B equipped with the Raman probe 5 is connected in parallel to the circulation pipeline A (that is, both ends of the sampling pipeline B are arranged on the circulation pipeline A). Considering the balance between the side reaction ratio and the reaction rate, the reaction temperature in the reactor body 1 for SEBS hydrogenation reaction is generally set between 40 °C and 90 °C, which is much higher than the laboratory temperature for the reference modeling of SEBS with different hydrogenation degrees (i.e., the calibration ambient temperature, such as 25 °C), so that the results of on-line detection are greatly affected by temperature. To reduce the temperature influence, a certain amount of SEBS colloid can be drawn out from the reactor body 1 through the circulation pipeline A driven by a circulation pump 2 with a certain power, and then a small amount of SEBS colloid is further diverted from the circulation pipeline A through the sampling pipeline B and then used by the Raman probe 5 for Raman spectroscopy detection of SEBS. After two-stage diversion through "reactor body 1 - circulation pipeline A" and "circulation pipeline A - sampling pipeline B", the flow rate of the SEBS colloid in the sampling pipeline B is more controllable and is significantly reduced, that is, the cooling effect after leaving the reactor body 1 is better. Compared with the prior art method of directly performing Raman spectroscopy detection on the SEBS colloid, the present application can stabilize the temperature environment of the Raman probe 5 and improve the accuracy of on-line detection of the Raman probe 5.
[0038] Among them, the temperature in the reactor body 1 for SEBS hydrogenation reaction is not limited to the above-mentioned range of 40 °C to 90 °C, and can also be other temperature ranges, such as between 60 °C and 90 °C, etc.; the temperature for the reference modeling of SEBS with different hydrogenation degrees is not limited to the above-mentioned 25 °C, and can also be other temperatures, such as 60 °C.
[0039] To further reduce the influence of the detection ambient temperature on the detection results. In this embodiment, as Figure 1 shown, the sampling pipeline B may include a temperature control mechanism for controlling the temperature of the SEBS colloidal solution, and the temperature control mechanism and the Raman probe 5 are sequentially arranged after the inlet of the sampling pipeline B.
[0040] Specifically, referring to Figure 1 , after the SEBS colloidal solution enters the sampling pipeline B, it is first stabilized to the calibration ambient temperature by the temperature control mechanism, and then the Raman spectroscopy detection is performed by the Raman probe 5. With such a setting, the accuracy of on-line detection can be greatly improved.
[0041] In this embodiment, as Figure 1 shown, the temperature control mechanism is a water cooler 3.
[0042] Specifically, referring to Figure 1 , after the SEBS colloidal solution is cooled by the water cooler 3, it can be detected by the Raman probe 5. With such a setting, the structure is simple and it is beneficial to reduce the manufacturing cost and the maintenance cost, and can also improve the accuracy of on-line detection of the Raman probe 5.
[0043] Of course, those skilled in the art can understand that the temperature control mechanism is not limited to the above-mentioned water cooler 3, and can also be other cooling elements, such as a semiconductor cooler, etc. Moreover, the temperature control mechanism can even include a cooling element and / or a heating element, such as a combination of a semiconductor cooler and / or a resistance wire, etc.
[0044] In this embodiment, as Figure 1 shown, the sampling pipeline B further includes a sampling valve 4, and the sampling valve 4 is used for sampling the SEBS rubber solution in the sampling pipeline B.
[0045] Specifically, referring to Figure 1 , the sampling valve 4 is arranged between the temperature control mechanism and the Raman probe 5. With such an arrangement, a part of the cooled SEBS rubber solution in the sampling pipeline B can be obtained through the sampling valve 4, so that the SEBS rubber solution can be sampled. Among them, the installation position of the sampling valve 4 is not limited to between the above-mentioned temperature control mechanism and the Raman probe 5, and can also be other positions.
[0046] In this embodiment, as Figure 1 shown, the circulation pipeline A includes a first stop valve 8, and the first stop valve 8 is used to control the flow rate of the circulation pipeline A.
[0047] Specifically, referring to Figure 1 , by controlling the opening and closing degree of the first stop valve 8, the flow rate of the circulation pipeline A can be restricted, so as to realize the adjustment of the split flow rate of the sampling pipeline B from the circulation pipeline A. After further controlling the flow rate of the SEBS rubber solution in the sampling pipeline B, it is beneficial to further stabilize the temperature environment of the Raman probe 5. Among them, the installation position of the first stop valve 8 is not limited to between the parallel port of the sampling pipeline B and the circulation pipeline A, and can also be other positions.
[0048] In this embodiment, as Figure 1 shown, the sampling pipeline B includes a second stop valve 7, and the second stop valve 7 arranged at the inlet of the sampling pipeline B is used to control the flow rate of the sampling pipeline B.
[0049] Specifically, referring to Figure 1 , the second stop valve 7 can directly realize the flow rate adjustment of the sampling pipeline B, so as to control the SEBS rubber solution in the sampling pipeline B to the expected flow rate, so as to stabilize the temperature environment of the Raman probe 5, thereby improving the accuracy of on-line detection of the Raman probe 5.
[0050] On the basis of providing the second stop valve 7, in this embodiment, as Figure 1 shown, the Raman probe 5 is detachably inserted into the sampling pipeline B, and the sampling pipeline B includes a third stop valve 9, and the third stop valve 9 arranged at the outlet of the sampling pipeline B is used to control the on-off of the sampling pipeline B.
[0051] Specifically, referring toFigure 1 When the Raman probe 5 needs to be repaired, the second stop valve 7 and the third stop valve 9 can be closed simultaneously to close the sampling pipeline B, facilitating the disassembly and assembly of the Raman probe 5 without affecting the production of the reactor.
[0052] In this embodiment, both the feeding end and the discharging end of the circulation pipeline A are connected to the kettle body 1 through maintenance valves (not shown in the figure). The maintenance valves are used to control the on-off of the circulation pipeline A. The circulation pipeline A further includes an openable and closable air blowing port (not shown in the figure) and an openable and closable emptying port (not shown in the figure). The air blowing port is arranged adjacent to the discharging end, and the emptying port is arranged adjacent to the feeding end.
[0053] Specifically, when maintenance is required, the air blowing port and the emptying port can be opened. At the same time, the maintenance valves at both the feeding end and the discharging end of the circulation pipeline A are closed, and high-pressure gas, such as nitrogen, is introduced from the air blowing port, so that the materials in the circulation pipeline A can be emptied, and the process of emptying the materials will not affect the reactor after the maintenance valves are closed.
[0054] In this embodiment, the reactor further includes a temperature sensor (not shown in the figure) arranged adjacent to the sensitive component of the Raman probe 5.
[0055] Specifically, the temperature sensor arranged adjacent to the sensitive component of the Raman probe 5 can accurately obtain the measurement environment temperature, thereby obtaining the temperature difference between the measurement environment temperature and the calibration environment temperature. By setting the compensation amount required for the reference model through this temperature difference, the accuracy of the on-line detection of the Raman probe 5 can be greatly improved after temperature compensation of the reference model.
[0056] In this embodiment, the circulation pipeline A is detachably connected to the kettle body 1.
[0057] Specifically, such a setting is beneficial to the processing, maintenance, and transportation of the reactor.
[0058] In the description of the present application, it should be understood that the terms "first" and "second" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance or implicitly indicating the quantity of the indicated technical features. Thus, the features defined with "first" and "second" may explicitly or implicitly include at least one of these features. In the description of the present application, "a plurality" means at least two, such as two, three, etc., unless otherwise specifically defined.
[0059] In this application, unless otherwise clearly stipulated or defined, terms such as "installed", "connected", "linked", "fixed", etc. shall be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or integrated; it can be a mechanical connection, an electrical connection, or communication with each other; it can be directly connected, or indirectly connected through an intermediate medium, and can be the communication inside two components or the interaction relationship between two components, unless otherwise clearly defined. For those of ordinary skill in the art, the specific meanings of the above terms in this application can be understood according to specific circumstances.
[0060] In the description of this specification, the description with reference to terms such as "one embodiment", "some embodiments", "examples", "specific examples", or "some examples", etc. means that the specific features, structures, materials, or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of this application. In this specification, the schematic expressions of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials, or characteristics described can be combined in a suitable manner in any one or more embodiments or examples. In addition, without contradiction, those skilled in the art can combine and combine the different embodiments or examples described in this specification and the features of different embodiments or examples.
Claims
1. Reactor, characterized in that, The reactor includes: A reactor body (1) for the hydrogenation reaction of SEBS; A circulation pipeline (A) whose inlet end and outlet end are both communicated with the inner cavity of the reactor body (1), and a circulation pump (2) is provided; A sampling pipeline (B) which is connected in parallel to the circulation pipeline (A); A Raman probe (5) provided on the sampling pipeline (B), and the Raman probe (5) is used to detect the SEBS rubber solution in the sampling pipeline (B).
2. The reactor according to claim 1, characterized in that, The sampling pipeline (B) includes a temperature control mechanism for controlling the temperature of the SEBS rubber solution. The temperature control mechanism and the Raman probe (5) are sequentially arranged after the inlet of the sampling pipeline (B).
3. The reactor according to claim 2, characterized in that, The temperature control mechanism is a water cooler (3).
4. The reactor according to claim 1, wherein, The sampling pipeline (B) further includes a sampling valve (4) for sampling the SEBS rubber solution in the sampling pipeline (B).
5. The reactor according to any one of claims 1 to 4, characterized in that, The circulation pipeline (A) includes a first stop valve (8) for controlling the flow rate of the circulation pipeline (A).
6. The reactor according to claim 5, characterized in that, The sampling pipeline (B) includes a second stop valve (7). The second stop valve (7) provided at the inlet of the sampling pipeline (B) is used to control the flow rate of the sampling pipeline (B).
7. The reactor according to claim 6, characterized in that, The Raman probe (5) is detachably inserted into the sampling pipeline (B). The sampling pipeline (B) includes a third stop valve (9). The third stop valve (9) provided at the outlet of the sampling pipeline (B) is used to control the on-off of the sampling pipeline (B).
8. The reactor according to claim 5, characterized in that, Both the inlet end and the outlet end of the circulation pipeline (A) are connected to the reactor body (1) through maintenance valves. The maintenance valves are used to control the on-off of the circulation pipeline (A). The circulation pipeline (A) further includes an openable and closable air blowing port and an openable and closable evacuation port. The air blowing port is arranged adjacent to the outlet end, and the evacuation port is arranged adjacent to the inlet end.
9. The reactor according to claim 5, characterized in that, The reactor further includes a temperature sensor arranged adjacent to the sensitive component of the Raman probe (5).
10. The reactor according to claim 1, characterized in that, The circulation pipeline (A) is detachably connected to the reactor body (1).