Reaction kettle sampling detection device

Abstract

The invention relates to a reaction kettle sampling detection device in the technical field of chemical engineering. The reaction kettle sampling detection device comprises a reaction kettle, a lifting driving mechanism and a sampling detection mechanism, the sampling detection mechanism comprises a sampling rod, a sampling pump, a sampling valve, a sampling bottle and a spectral imaging analyzer, an inlet in the lower end of the sampling rod enters the kettle body from the top of the reaction kettle, the lifting driving mechanism drives the sampling rod to vertically move up and down relative to the reaction kettle, and a sample inlet of the sampling pump is communicated with an outlet in the upper end of the sampling rod; a sample outlet of the sampling pump is communicated with an inlet of the spectral imaging analyzer, and the sampling bottle is communicated with the sampling pump through the sampling valve. According to the device, on the basis of realizing closed normal-pressure quantitative residue-free sampling, the traditional off-line detection is upgraded into an on-line intelligent diagnosis system through a sampling-analysis-monitoring integrated design, so that the residue-free sampling standard under severe environments such as GMP (Good Manufacturing Practice) and the like is met, and the detection accuracy is improved through fusion analysis of spectral images and multi-parameter data; and industrial process monitoring is promoted to stride towards'visualization, intelligence and unmanned '.

Description

Technical Field

[0001] The present invention relates to the technical field of chemical industry, in particular to a sampling and detection device for a reactor. Background Art

[0002] Reactors are widely used in the petroleum, chemical, rubber, pesticide, dye, pharmaceutical, and food industries as pressure vessels for processes such as vulcanization, nitration, hydrogenation, hydrocarbonization, polymerization, and condensation. Monitoring the reaction progress of chemical solutions within reactors is a critical step in ensuring reaction efficiency, product quality, and production safety.

[0003] In current industrial practice, the main monitoring methods for chemical solutions in reactors include temperature monitoring, pressure monitoring, flow and liquid level monitoring, pH value and conductivity monitoring, etc., among which pH value detection is the main indicator of the reaction progress of chemical solutions in reactors. For example, publication number CN220238548U discloses a pH online monitoring device, wherein the pH online monitoring device includes: a feed pipe, a liquid return pipe, a circulation pump, a pH monitoring component and a monitoring pipe; one end of the feed pipe is located below the liquid level of the reactor, and a feed valve is provided on the feed pipe; one end of the liquid return pipe is connected to the reactor, and a liquid return valve is provided on the liquid return pipe; the liquid inlet end of the circulation pump is connected to the other end of the feed pipe, and the liquid outlet end of the circulation pump is connected to the other end of the liquid return pipe; both ends of the monitoring pipe are connected to the liquid return pipe, and the pH monitoring component is provided on the monitoring pipe. Although the system setting can automatically monitor the pH value of the solution in the reactor to infer the reaction progress of the chemical solution in the reactor, it cannot more accurately know the real-time reaction progress of the chemical solution in the reactor, such as its appearance during the reaction and the intermediate products in the reaction process. Summary of the Invention

[0004] In view of the defects in the prior art, the purpose of the present invention is to provide a reactor sampling and detection device.

[0005] According to the present invention, a reactor sampling and detection device includes a reactor, a lifting drive mechanism, and a sampling and detection mechanism; The sampling and detection mechanism includes a sampling rod, a sampling pump, a sampling valve, a sampling bottle, and a spectrum imaging analyzer. The sampling rod is a hollow cylindrical structure with open ends. The lower end inlet of the sampling rod enters the reactor from the top of the reactor. The lifting drive mechanism drives the sampling rod to move vertically up and down relative to the reactor. The sampling inlet of the sampling pump is connected to the upper end outlet of the sampling rod, and the sampling outlet of the sampling pump is connected to the inlet of the spectrum imaging analyzer. The sampling bottle is connected to the sampling pump through the sampling valve. The lifting drive mechanism drives the sampling rod to move vertically so that the lower end inlet reaches a predetermined depth, and the sampling pump is started. The solution in the reactor enters the spectrum imaging analyzer through the sampling rod. The sampling valve is opened for a predetermined time, and the sampling bottle obtains a predetermined amount of solution. The spectrum imaging analyzer performs online detection on the sample solution, and the sample solution in the sampling bottle passes offline detection.

[0006] In some embodiments, the sampling valve includes a first diaphragm valve and a second diaphragm valve, the first diaphragm valve and the second diaphragm valve are arranged in series, the upper inlet of the first diaphragm valve is connected to the pipeline between the sampling pump and the spectral imaging analyzer, and the lower outlet of the second diaphragm valve is connected to the sampling bottle, and the liquid in the pipeline between the sampling pump and the spectral imaging analyzer enters the sampling bottle through the high and low head difference.

[0007] In some embodiments, the sampling and detection mechanism further includes a detector, and the detector is installed on the spectral imaging analyzer.

[0008] In some embodiments, the detector is a pH meter, a viscometer, or a thermometer.

[0009] In some embodiments, a reflux assembly is further included, which includes a three-way sleeve, the lower port of the three-way sleeve is sealed and connected to the reactor, the lower end inlet of the sampling rod enters the cavity of the reactor from the upper port of the three-way sleeve, the side inlet of the three-way sleeve is connected to the liquid outlet of the spectrum imaging analyzer, and the solution detected by the spectrum imaging analyzer enters through the side inlet of the three-way sleeve and then flows back into the reactor.

[0010] In some embodiments, the reflux assembly further includes a horn connected between the three-way sleeve and the reactor, and the port area where the horn and the three-way sleeve are connected is smaller than the port area where the horn and the reactor are connected.

[0011] In some embodiments, a flushing assembly is further included, which includes a flushing pipe and a control valve. The flushing pipe is used to communicate with the sampling pump, the sampling valve and the spectral imaging analyzer respectively. The control valve is installed on the flushing pipe to control the on-off of the pipeline.

[0012] In some embodiments, a controller is further included, and the controller is electrically connected to the sampling pump, the sampling valve, the spectrum imaging analyzer, and the detector respectively.

[0013] Compared with the prior art, the present invention has the following beneficial effects: 1. The reactor sampling and detection device of the present invention, by synchronously detecting the appearance and internal properties of the sample solution, can not only verify the appearance and internal performance detection, but also obtain the corresponding relationship between the appearance and internal performance parameters of the reaction liquid at each stage during the reaction process and the solution of each layer after the reaction is completed, thereby realizing real-time and accurate monitoring of the reaction process of the chemical solution in the reactor, ensuring the safety of the reaction process and the accuracy of the results.

[0014] 2. The reactor sampling and detection device of the present invention sets a reflux component in the system, so that the solution detected by the sight glass can flow back into the reactor, thereby improving the utilization rate of materials and saving energy and reducing consumption.

[0015] 3. The reactor sampling and detection device of the present invention is provided with flushing components for pumps, valves, spectrum imaging analyzers, and pipelines, so as to promptly remove the solution remaining in the system and improve the accuracy of detection. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Other features, objects and advantages of the present invention will become more apparent upon reading the detailed description of non-limiting embodiments with reference to the following drawings: Figure 1 This is a schematic diagram of the overall structure of the reactor sampling and detection device of the present invention; Figure 2 This is a schematic diagram of the three-dimensional structure of the main body of the sampling and detection mechanism of the present invention in the front view direction; Figure 3 This is a schematic diagram of the three-dimensional structure of the main body of the sampling and detection mechanism of the present invention in the rear view direction; Figure 4 This is a schematic diagram of the three-dimensional structure of the sampling and detection mechanism body of the present invention when viewed from the side; Figure 5 This is a schematic diagram of the assembly structure of the lifting drive mechanism, sampling rod and reflux assembly of the present invention; Figure 6 for Figure 5 A partial enlarged view of . DETAILED DESCRIPTION

[0017] The present invention will be described in detail below with reference to specific embodiments. The following examples will help those skilled in the art to further understand the present invention, but are not intended to limit the present invention in any form. It should be noted that, for those skilled in the art, several changes and improvements can be made without departing from the scope of the present invention. These all fall within the scope of protection of the present invention.

[0018] Example 1 The present invention provides a reactor sampling and detection device, such as Figure 1-6As shown, it mainly includes a reactor 100 for mixing chemical liquids, a lifting drive mechanism 200 for driving the sampling structure to slide vertically, and a sampling and detection mechanism 300 for sampling and detection.

[0019] The sampling and detection mechanism 300 primarily comprises a sampling rod 310, a sampling pump 320, a sampling valve 330, a sampling bottle 340, and a spectral imaging analyzer 350. The sampling rod 310 is a long, cylindrical structure with open ends. The top shell of the reactor 100 is provided with a sampling hole. The lower end of the sampling rod 310 enters the reactor 100 through the hole. The sampling rod 310 and the sampling hole form a sliding, sealed fit. This sliding, sealed fit means that the sampling rod 310 can slide vertically up and down along the sampling hole, maintaining a substantially sealed state during the sliding process. The lifting drive mechanism 200 primarily comprises a drive motor 210, a stand 220, and a clamping jaw 230. When mounted, the stand 220 is parallel to the sampling rod 310. One end of the clamping jaw 230 is slidably connected to the support frame 220, while the other end is connected to the sampling rod 310. The drive motor 210 drives the clamping jaw 230 to slide up and down along the stand 220, thereby driving the sampling rod 310 to slide up and down relative to the reactor 100. This allows the lower inlet of the sampling rod 310 to move to a predetermined depth within the reactor 100, thereby collecting the reaction solution at the predetermined depth. A sampling pump 320, which can be a diaphragm pump, is mounted on the support frame 700 located outside the reactor 100 housing. The sampling pump 310 is connected to the upper outlet of the sampling rod 310 via a pipeline. At least a portion of the pipeline connecting the sampling pump 320 and the sampling rod 310 is a flexible tube to accommodate the upward and downward movement of the sampling rod 310. The sample outlet of the sampling pump 320 is connected to the spectral imaging analyzer 350 through a pipeline, and the spectral imaging analyzer 350 is also installed on the support frame 700. After the spectral imaging analyzer 350 obtains the sample solution delivered by the self-sampling pump 320, it performs real-time online detection on the sample solution, outputs visual indicators such as material color and turbidity in real time, and can generate dynamic data maps through system synchronization. This embodiment also provides an implementation method for effectively increasing the detection parameters, that is, a mounting hole is provided on the main structure of the spectral imaging analyzer 350, and a corresponding detector 360 is installed on the mounting hole, and the detector 360 is mainly a pH meter, a viscometer or a thermometer, etc. By installing the detector, the detection of solution performance can be further expanded, and the accuracy and efficiency of the detection can be further improved.

[0020] The outlet of the sampling valve 330 is connected to the inlet of the sampling bottle 340, and its inlet is connected to the sample outlet of the sampling pump 320. The amount of sample solution entering the sampling bottle 340 is controlled by the sampling valve 330. The solution in the sampling bottle 340 is used to be placed in a detection device for detection to obtain the response parameters of the sample solution. On the one hand, it can more accurately obtain the physical and chemical parameters of the sample solution in a certain period of time, and at the same time, it can also be mutually verified with the solution turbidity, solution color, etc. detected by the spectral imaging analyzer. In this embodiment, the sampling valve 330 is composed of two groups of diaphragm valves, which are respectively recorded as the first diaphragm valve 331 and the second diaphragm valve 332. The first diaphragm valve 331 and the second diaphragm valve 332 are arranged in series, that is, the outlet of the first diaphragm valve 331 is connected to the inlet of the second diaphragm valve 332. The first diaphragm valve 331 and the second diaphragm valve 332, which are arranged in series, are connected in an upright hanging manner and communicate with the pipeline between the sampling pump 320 and the spectral imaging analyzer 350. The inlet of the first diaphragm valve 331 is connected to the pipeline between the sampling pump 320 and the spectral imaging analyzer 350, while the outlet of the second diaphragm valve 332 is connected to the sampling bottle 340. As the sampling pump 320 delivers the sample solution into the spectral imaging analyzer 350 through the pipeline, the first diaphragm valve 331 is first opened, allowing some of the sample solution in the pipeline to flow into the vertical pipeline between the second diaphragm valve 332 and the first diaphragm valve 331. The first diaphragm valve 331 is then closed and the second diaphragm valve 332 is opened, allowing the sample solution to continue flowing toward the spectral imaging analyzer 350 and into the sampling bottle 340.

[0021] The operating principle of the reactor sampling and testing device provided in this embodiment is as follows: After the chemical solution reacts within the reactor 100 for a predetermined time, the drive motor 210 drives the gripper 230 to carry the sampling rod 310 in a vertical upward and downward motion, causing the lower inlet of the sampling rod 310 to reach a predetermined depth. The sampling pump 320 is activated, using negative pressure to draw the sample solution at the predetermined depth within the reactor 100 from the sampling rod 310 and transport it through a pipeline to the spectral imaging analyzer 350. As the sample solution enters the spectral imaging analyzer 350 through the pipeline, the first diaphragm valve 331 opens, allowing the sample solution to flow through the diaphragm valve 331 into the pipeline. The first diaphragm valve 331 then closes and the second diaphragm valve 332 opens, allowing the sample solution to flow into the sampling bottle 340 under the action of gravity. The spectral imaging analyzer 350 then tests the sample solution within its chamber for appearance, such as turbidity and color. Testing of the sample solution's composition and other physical and chemical properties is then completed by removing the sampling bottle 340 and transferring it to a testing instrument. Based on the realization of closed, normal-pressure quantitative residue-free sampling, this device upgrades traditional offline detection to an online intelligent diagnostic system through the integrated design of "sampling-analysis-monitoring". It not only meets the residue-free sampling standards in harsh environments such as GMP, but also promotes industrial process monitoring to "visualization, intelligence, and unmanned" through the fusion analysis of spectral images and multi-parameter data.

[0022] This embodiment further includes a controller 600, which is electrically connected to the sampling pump 320, the sampling valve 330, and the spectral imaging analyzer 350. The controller 600 is used to control the operation of the sampling pump 320, the sampling valve 330, the control mirror 350, the detector 360, etc., and receive parameters detected by the detection device.

[0023] Example 2 This embodiment 2 is formed on the basis of embodiment 1. By setting a reflux component in the system, the solution detected by the sight glass is refluxed into the reactor, thereby improving the utilization rate of materials and saving energy and reducing consumption. Specifically: like Figure 1 、 5As shown in Figure 6, the reflux assembly 400 mainly includes a three-way sleeve 410. The lower end of the three-way sleeve 410 is sealed and connected to the sampling hole of the reactor 100. After the lower end inlet of the sampling rod 310 enters the reactor 100 from the upper end of the three-way sleeve 410, the upper end of the three-way sleeve 410 is sealed and connected via a flange. At this time, the sampling rod 310 is sleeved with the three-way sleeve 410, and the sampling rod 310 can move vertically up and down relative to the three-way sleeve 410. At the same time, the outer diameter of the sampling rod 310 is smaller than the inner diameter of the three-way sleeve 410, forming an annular cavity for the sample solution to reflux. The side inlet of the three-way sleeve 410 is connected to the liquid outlet of the spectral imaging analyzer 350 through a pipeline. The sample solution detected by the spectral imaging analyzer 350 enters the annular cavity through the side inlet of the three-way sleeve 410 and refluxes into the reactor 100.

[0024] This embodiment also provides a preferred implementation in which the reflux assembly 400 further includes a trumpet 420, which is a cylindrical body with a trumpet-shaped internal structure. The trumpet 420 is connected between the three-way sleeve 410 and the sampling port of the reactor 100. The cross-sectional area of the upper end of the trumpet 420 where it interfaces with the three-way sleeve 410 is smaller than the cross-sectional area of the lower end of the trumpet 420 where it interfaces with the sampling port of the reactor 100. This trumpet-shaped structure reduces the resistance of the gas pressure at the top of the reactor to the reflux liquid, allowing the sample liquid to flow back into the reactor 100 more conveniently.

[0025] Example 3 This embodiment 3 is formed on the basis of embodiment 1 or 2, and by providing a flushing component for the pump valve, spectral imaging analyzer, and pipelines, the solution remaining in the system is promptly removed, thereby improving the accuracy of detection. Specifically: like Figure 1 and 4 As shown, a flushing assembly 500 is installed in the system pipeline. The flushing assembly 500 mainly consists of a flushing pipe 510 and a control valve 520. The flushing pipe 510 is connected to the sampling pump 320, sampling valve 330, and spectral imaging analyzer 350 through a main liquid inlet pipe and multiple branch pipes. The opening and closing of the pipeline is controlled by a control valve 520 installed in the connected pipeline. Through an external flushing device, flushing liquid is introduced into the pipeline and device components through the flushing pipe 510, flushing the pipeline and corresponding sampling and detection components to improve detection accuracy.

[0026] In the description of this application, it should be understood that the terms "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", etc., indicating the orientation or position relationship, are based on the orientation or position relationship shown in the accompanying drawings, and are only for the convenience of describing this application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on this application.

[0027] The above describes specific embodiments of the present invention. It should be understood that the present invention is not limited to the specific embodiments described above, and those skilled in the art may make various changes or modifications within the scope of the claims, which do not affect the essence of the present invention. The embodiments of this application and the features in the embodiments may be combined with each other in any manner unless there is a conflict.

Claims

1. A reactor sampling and detection device, characterized in that: It comprises a reaction kettle (100), a lifting drive mechanism (200), and a sampling and detection mechanism (300); The sampling and detection mechanism (300) includes a sampling rod (310), a sampling pump (320), a sampling valve (330), a sampling bottle (340), and a spectrum imaging analyzer (350). The sampling rod (310) is a hollow cylindrical structure with two ends open. The lower end inlet of the sampling rod (310) enters the reactor (100) from the top. The lifting drive mechanism (200) drives the sampling rod (310) to move vertically up and down relative to the reactor (100). The sampling inlet of the sampling pump (320) is connected to the upper end outlet of the sampling rod (310). The sampling outlet of the sampling pump (320) is connected to the inlet of the spectrum imaging analyzer (350). The sampling bottle (340) is connected to the sampling pump (320) through the sampling valve (330). The lifting drive mechanism (200) drives the sampling rod (310) to move vertically so that the lower end inlet reaches a predetermined depth, and the sampling pump (320) is started. The solution in the reactor (100) enters the spectrum imaging analyzer (350) through the sampling rod (310). The sampling valve (330) is opened for a predetermined time. The sampling bottle (340) obtains a predetermined amount of solution. The spectrum imaging analyzer (350) performs online detection on the sample solution, and the sample solution in the sampling bottle (340) passes offline detection.

2. The reactor sampling and detection device according to claim 1, characterized in that: The sampling valve (330) includes a first diaphragm valve (331) and a second diaphragm valve (332), wherein the first diaphragm valve (331) and the second diaphragm valve (332) are arranged in series, an upper inlet of the first diaphragm valve (331) is connected to the pipeline between the sampling pump (320) and the spectrum imaging analyzer (350), and a lower outlet of the second diaphragm valve (332) is connected to the sampling bottle (340), and the liquid in the pipeline between the sampling pump (320) and the spectrum imaging analyzer (350) enters the sampling bottle (340) through the high and low head difference.

3. The reactor sampling and detection device according to claim 1, characterized in that: The sampling and detection mechanism (300) further includes a detector (360), and the detector (360) is installed on the spectrum imaging analyzer (350).

4. The reactor sampling and detection device according to claim 3, characterized in that: The detector (360) is a pH meter, a viscometer or a thermometer.

5. The reactor sampling and detection device according to claim 1, characterized in that: The invention also includes a reflux component (400), wherein the reflux component (400) includes a three-way sleeve (410), the lower end of the three-way sleeve (410) is sealed and connected to the reactor (100), the lower end inlet of the sampling rod (310) enters the cavity of the reactor (100) from the upper end of the three-way sleeve (410), the side inlet of the three-way sleeve (410) is connected to the liquid outlet of the spectrum imaging analyzer (350), and the solution detected by the spectrum imaging analyzer (350) enters through the side inlet of the three-way sleeve (410) and flows back into the reactor (100).

6. The reactor sampling and detection device according to claim 5, characterized in that: The reflux assembly (400) further comprises a horn (420), the horn (420) being connected between the three-way sleeve (410) and the reactor (100), and the port area where the horn (420) and the three-way sleeve (410) are connected is smaller than the port area where the horn (420) and the reactor (100) are connected.

7. The reactor sampling and detection device according to claim 1, characterized in that: The system further comprises a flushing assembly (500), wherein the flushing assembly (500) comprises a flushing pipe (510) and a control valve (520). The flushing pipe (510) is used to communicate with the sampling pump (320), the sampling valve (330) and the spectrum imaging analyzer (350), respectively. The control valve (520) is installed on the flushing pipe (510) and is used to control the on-off of the pipeline.

8. The reactor sampling and detection device according to any one of claims 1 to 7, characterized in that: The system further comprises a controller (600), wherein the controller (600) is electrically connected to the sampling pump (320), the sampling valve (330), the spectrum imaging analyzer (350), and the detector (360).

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