A tubular rapid quenching device for azide wastewater and its working method

Abstract

This invention discloses a tubular rapid quenching device for azide wastewater and its operating method, comprising a water bath, a quenching coil reactor, a neutralization coil reactor, a coil heat exchanger, a PLC controller, and multiple pipelines, including a feed pipeline group, an alkali solution pipeline, a discharge pipeline, a heat exchange pipeline, and a circulation pipeline. The tubular rapid quenching device for azide wastewater provided by this invention, based on a tubular reaction disc, can significantly increase the speed of the entire quenching process, completing quenching in just 5-50 minutes. Furthermore, the device can withstand pressures up to 1-2 MPa, far exceeding conventional reactors. The entire quenching process takes place within the pipelines, achieving zero leakage during quenching, which not only reduces costs but also greatly lowers the probability of industrial production safety issues.

Description

Technical Field

[0001] This invention relates to the field of pharmaceutical and chemical equipment technology, specifically to a tubular rapid quenching device for azide wastewater and its working method. Background Technology

[0002] In chemical and pharmaceutical production processes, excipients or by-reactants are usually in excess. For reactions involving highly reactive or high-risk excipients or by-reactants, quenching is necessary after the reaction to deactivate them and transform them into safer and more stable substances, followed by post-treatment before discharge. In the preparation of azide compounds, by-reactions generate waste liquid containing azide reagents, causing serious environmental pollution; therefore, treatment is essential before discharge.

[0003] Azide compounds are a class of highly reactive chemical raw materials and pharmaceutical intermediates, widely used in fine chemicals, aerospace, biotechnology, and pharmaceuticals. Commonly used azide reagents include inorganic sodium azide and other organic azide compounds, all of which hydrolyze in water to form azidoic acid (HN3). HN3 is explosive and highly toxic. my country has strict regulations regarding the use of azide ions (N3). - There are strict controls. According to the current emission standards, the maximum allowable emission concentration of azide in wastewater is 3 mg / L.

[0004] In current technologies, the conventional quenching method involves slowly adding quenching reagents into the reaction device. This method requires large equipment, is time-consuming, inefficient, involves complex procedures, and has a low degree of automation. It requires manual sampling to monitor the quenching process, which can lead to untimely feedback of results. In addition, due to the long processing time, azide wastewater needs to be temporarily stored in large quantities, which can cause a series of safety hazards or accidents.

[0005] For batch quenching, the batch reactor is large, has many joints, and includes components such as motor stirrers. It has poor sealing and overall pressure resistance, and the speed is relatively slow. Therefore, the risk of azidoic acid or other liquids overflowing during the process is unavoidable, which wastes costs and easily causes safety hazards.

[0006] Therefore, there is an urgent need in this field for a tubular rapid quenching device for azide wastewater that can improve the speed, efficiency and safety of azide wastewater quenching. Summary of the Invention

[0007] To solve the above technical problems, the present invention provides a tubular rapid quenching device for azide wastewater, including a water bath, a quenching coil reactor, a neutralization coil reactor, a coil heat exchanger, a PLC controller, and multiple pipelines, wherein the pipelines include a feed pipeline group, an alkali pipeline, a discharge pipeline, a heat exchange pipeline, and a circulation pipeline.

[0008] The water bath contains heat exchange process water. The bottom of the water bath has an outlet. One end of the circulation pipe is fixedly connected to the outlet, and the other end of the circulation pipe is inserted into the water bath. A circulation pump is installed on the circulation pipe.

[0009] The quenching coil reactor, neutralizing coil reactor, and coil heat exchanger are all fixedly installed inside the water bath. The quenching coil reactor is fixedly installed at the lower end of the neutralizing coil reactor, and the outlet of the quenching coil reactor and the inlet of the neutralizing coil reactor are connected by a pipeline. Both ends of the coil heat exchanger are connected to the heat exchange pipeline, which is used to input and output heat exchange medium into and out of the coil heat exchanger.

[0010] The feed pipeline assembly is located on one side of the water bath and extends into the water bath, and the feed pipeline assembly is fixedly connected to the feed inlet of the quenching coil reactor.

[0011] One end of the alkali solution pipeline is connected to the alkali solution source, and the other end of the alkali solution pipeline is connected to the feed end of the neutralization coil reactor.

[0012] One end of the discharge pipeline is fixedly connected to the discharge port of the neutralization coil reactor, and the other end of the discharge pipeline is connected to a wastewater collection device. An online ion chromatograph is installed on the discharge pipeline.

[0013] The PLC controller is electrically connected to the water bath, feed pipeline group, discharge pipeline, heat exchange pipeline and circulation pipeline.

[0014] Specifically, the coil of the quenching coil reactor is wound from bottom to top.

[0015] Specifically, the coil of the neutralizing coil reactor is wound from bottom to top.

[0016] Specifically, the feed pipeline assembly includes a main pipeline, a first branch pipeline, and a second branch pipeline. One end of the main pipeline is connected to the first branch pipeline and the second branch pipeline via a tee. The other end of the main pipeline is connected to the bottom end of the quenching coil reactor. A first static mixer is installed on the main pipeline.

[0017] Specifically, the first branch consists of a sodium nitrite pipeline and an azide wastewater pipeline. One end of the sodium nitrite pipeline is connected to a sodium nitrite solution source, and the other end of the sodium nitrite pipeline is connected to the azide wastewater pipeline. One end of the azide wastewater pipeline is connected to an azide wastewater source, and the other end of the azide wastewater pipeline is connected to the sodium nitrite pipeline. A second static mixer is installed at the connection end of the sodium nitrite pipeline and the azide wastewater pipeline. The second branch is a sulfuric acid pipeline. One end of the sulfuric acid pipeline is connected to a sulfuric acid solution source, and the other end of the sulfuric acid pipeline is connected to the main pipeline.

[0018] Specifically, a first metering pump and a first flow meter are fixedly installed on the sodium nitrite pipeline, and both the first metering pump and the first flow meter are electrically connected to the PLC controller. A second metering pump and a second flow meter are fixedly installed on the sulfuric acid pipeline, and both the second metering pump and the second flow meter are electrically connected to the PLC controller. A third metering pump and a third flow meter are fixedly installed on the alkali pipeline, and both the third metering pump and the third flow meter are electrically connected to the PLC controller. A fourth metering pump and a fourth flow meter are fixedly installed on the azide wastewater pipeline, and both the fourth metering pump and the fourth flow meter are electrically connected to the PLC controller.

[0019] Specifically, a resistance temperature detector (RTD) is fixedly installed in the water bath, and the RTD is electrically connected to the PLC controller.

[0020] Specifically, both the quenching coil reactor and the neutralizing coil reactor are made of PFA material, and the coil heat exchanger is made of metal.

[0021] Specifically, the PLC controller is equipped with a human-machine interface, which is used to display device operating parameters and alarm prompts.

[0022] Another aspect of the present invention provides a quenching method based on the aforementioned tubular rapid quenching device for azide wastewater, the method comprising the following steps:

[0023] S1. Start-up: Purge nitrogen into the quenching coil reactor and the neutralization coil reactor to inertize the device, open the heat exchange pipeline, add heat exchange process water into the water bath to submerge the quenching coil reactor and the neutralization coil reactor, and start the circulation pump and the online ion chromatograph.

[0024] S2. Continuous quenching: Turn on the third metering pump to introduce liquid alkali into the neutralization coil reactor. After the liquid alkali flow rate stabilizes, turn on the second metering pump to introduce sulfuric acid solution into the quenching coil reactor. After the sulfuric acid solution flow rate stabilizes, turn on the first metering pump to introduce sodium nitrite solution into the quenching coil reactor. After the sodium nitrite solution flow rate stabilizes, turn on the fourth metering pump to mix the azide wastewater with the sodium nitrite solution and send it into the quenching coil reactor for continuous online quenching.

[0025] S3. pH Adjustment: After the mixture in the quenching coil reactor is quenched, it enters the neutralization coil reactor and is mixed with the alkaline solution in the neutralization coil reactor to adjust the pH. After the pH adjustment is completed, it is discharged through the discharge pipeline. The online ion chromatograph on the discharge pipeline detects the azide ion content in the feed solution online and transmits the results to the PLC control box.

[0026] Specifically, temperature alarm interlock, flow alarm interlock and discharge azide ion alarm interlock are set in steps S2 and S3;

[0027] The temperature alarm interlock is as follows: the resistance thermometer converts the temperature of the liquid in the quenching coil reactor into an electrical signal and transmits it to the PLC controller. When the temperature of the quenching coil reactor exceeds 30°C or falls below 20°C, the PLC controller shuts down the first metering pump, the second metering pump, the third metering pump, and the fourth metering pump and issues an alarm.

[0028] The flow alarm interlock is as follows: the first flow meter converts the flow rate of the sodium nitrite pipeline into an electrical signal and transmits it to the PLC controller; the second flow meter converts the flow rate of the sulfuric acid pipeline into an electrical signal and transmits it to the PLC controller; the third flow meter converts the flow rate of the alkali pipeline into an electrical signal and transmits it to the PLC controller; and the fourth flow meter converts the flow rate of the azide wastewater pipeline into an electrical signal and transmits it to the PLC controller. When any flow meter is higher or lower than the set value, the PLC controller shuts down the first metering pump, the second metering pump, the third metering pump, and the fourth metering pump and triggers an alarm.

[0029] The discharge azide ion alarm interlock is as follows: the online ion chromatograph converts the concentration of azide ions in the discharge solution into an electrical signal and transmits it to the PLC controller. When the concentration of azide ions in the discharge solution exceeds 3 ppm, the PLC controller shuts down the first metering pump, the second metering pump, the third metering pump and the fourth metering pump and alarms.

[0030] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0031] 1. The azide wastewater tubular rapid quenching device provided by the present invention, based on a tubular reaction plate, can increase the speed of the entire quenching process, which can be completed in only 5-50 minutes. Moreover, the whole device can withstand pressure up to 1-2 MPa, far exceeding that of conventional reaction vessels. The quenching process is carried out entirely in the pipeline, achieving zero leakage during quenching. This not only helps to reduce costs but also greatly reduces the probability of industrial production safety problems.

[0032] 2. The azide wastewater tubular rapid quenching device provided by the present invention has a PLC controller that can monitor and adjust the feed flow rate, pressure, quenching and neutralization reaction temperature, and azide ion concentration of the effluent in real time. It has a high degree of automation and timely and accurate feedback.

[0033] 3. The azide wastewater tubular rapid quenching device provided by the present invention allows the azide wastewater pipeline to be directly and seamlessly connected to the front-end reaction unit or separation and extraction unit to achieve online continuous quenching of azide reagent wastewater in the production workshop. It eliminates the need for large-scale temporary storage, has a small liquid holding capacity, and greatly improves the wastewater treatment efficiency.

[0034] 4. The method for continuously quenching azide reagent wastewater provided by this invention has a high degree of automation, timely and accurate feedback of monitoring results, simple operation and wide applicability. It can be flexibly nested and used with upstream or downstream production units, greatly expanding the application space and scenarios. Attached Figure Description

[0035] Figure 1 This is a schematic diagram of the overall structure of the tubular rapid quenching device for azide wastewater provided by the present invention in Embodiment 1.

[0036] In the diagram, 1-quenching coil reactor, 2-neutralization coil reactor, 3-coil heat exchanger, 4-circulation pipeline, 5-discharge pipeline, 6-alkali solution pipeline, 7-main pipeline, 8-sodium nitrite pipeline, 9-azide wastewater pipeline, 10-sulfuric acid pipeline, 11-online ion chromatography detector, 12-first metering pump, 13-second metering pump, 14-third metering pump, 15-fourth metering pump, 16-circulation pump, 17-resistance thermometer, 18-water bath, 19-first static mixer, 20-second static mixer. Detailed Implementation

[0037] The technical solution of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. Unless otherwise specified, the materials, instruments, and reagents used in the following embodiments can be obtained commercially. Unless otherwise specified, the technical means used in the embodiments are conventional means well known to those skilled in the art.

[0038] The structures, proportions, sizes, etc., illustrated in the accompanying drawings of this specification are only for illustrative purposes to aid those skilled in the art and are not intended to limit the implementation conditions of this invention. Therefore, they have no substantial technical significance. Any modifications to the structure, changes in proportions, or adjustments to size, without affecting the effectiveness and purpose of this invention, should still fall within the scope of the technical content disclosed in this invention. Furthermore, the terms such as "upper," "lower," "left," "right," "middle," and "one" used in this specification are merely for clarity of description and are not intended to limit the scope of this invention. Changes or adjustments to their relative relationships, without substantially altering the technical content, should also be considered within the scope of this invention.

[0039] In the following examples, the alkaline solution is a sodium hydroxide solution, and the sulfuric acid is a dilute aqueous sulfuric acid solution.

[0040] Example 1

[0041] like Figure 1 As shown in the figure, this embodiment illustrates a tubular rapid quenching device for azide wastewater, including a water bath 18, a quenching coil reactor 1, a neutralization coil reactor 2, a coil heat exchanger 3, a PLC controller, and multiple pipelines, including a feed pipeline group, an alkali solution pipeline 6, a discharge pipeline 5, a heat exchange pipeline, and a circulation pipeline 4.

[0042] The water bath 18 contains heat exchange process water. The bottom of the water bath 18 is provided with a water outlet. One end of the circulation pipe 4 is fixedly connected to the water outlet, and the other end of the circulation pipe 4 is inserted into the water bath 18. A circulation pump 16 is provided on the circulation pipe 4.

[0043] The circulating pump 16 circulates the heat exchange process water in the water bath 18 to enhance the disturbance of the water flow. On the one hand, it can improve the heat transfer coefficient outside the tubes of the quenching coil reactor 1 and the neutralizing coil reactor 2. On the other hand, the circulating flow keeps the temperature of each point in the water bath 18 uniform.

[0044] Quenching coil reactor 1, neutralizing coil reactor 2 and coil heat exchanger 3 are all fixedly installed inside water bath 18. Quenching coil reactor 1 is fixedly installed at the lower end of neutralizing coil reactor 2, and the outlet of quenching coil reactor 1 and the inlet of neutralizing coil reactor 2 are connected by a pipeline. Both ends of coil heat exchanger 3 are connected to heat exchange pipeline, which is used to input and output heat exchange medium into coil heat exchanger 3.

[0045] The feed pipeline assembly is located on one side of the water bath 18 and extends into the water bath 18, and the feed pipeline assembly is fixedly connected to the feed inlet of the quenching coil reactor 1.

[0046] One end of the alkali solution pipeline 6 is connected to the alkali solution source, and the other end of the alkali solution pipeline 6 is connected to the feed end of the neutralization coil reactor 2.

[0047] One end of the discharge pipe 5 is fixedly connected to the discharge port of the neutralization coil reactor 2, and the other end of the discharge pipe 5 is connected to a wastewater collection device. An online ion chromatograph 11 is installed on the discharge pipe 5.

[0048] The PLC controller is electrically connected to the water bath 18, the feed pipeline group, the discharge pipeline 5, the heat exchange pipeline and the circulation pipeline 4.

[0049] Since the quenching reaction produces gas, in order to reduce the pressure difference in the system pipeline and allow the generated gas in the pipe to flow smoothly upward, the coil of the quenching coil reactor 1 is wound from bottom to top, and the coil of the neutralization coil reactor 2 is also wound from bottom to top.

[0050] The feed pipeline assembly includes a main pipeline 7, a first branch pipeline and a second branch pipeline. One end of the main pipeline 7 is connected to the first branch pipeline and the second branch pipeline via a tee. The other end of the main pipeline 7 is connected to the bottom end of the quenching coil reactor 1. A first static mixer 19 is installed on the main pipeline 7.

[0051] The first branch consists of a sodium nitrite pipeline 8 and an azide wastewater pipeline 9. One end of the sodium nitrite pipeline 8 is connected to a sodium nitrite solution source, and the other end of the sodium nitrite pipeline 8 is connected to the azide wastewater pipeline 9. One end of the azide wastewater pipeline 9 is connected to an azide wastewater source, and the other end of the azide wastewater pipeline 9 is connected to the sodium nitrite pipeline 8. A second static mixer 20 is installed at the connection end of the sodium nitrite pipeline 8 and the azide wastewater pipeline 9. The second branch is a sulfuric acid pipeline 10. One end of the sulfuric acid pipeline 10 is connected to a sulfuric acid solution source, and the other end of the sulfuric acid pipeline 10 is connected to the main pipeline 7.

[0052] The first static mixer 19 is used to mix azide wastewater and sodium nitrite solution, and the second static mixer 20 is used to mix the reaction solution after the first stage reaction with sulfuric acid.

[0053] A first metering pump 12 and a first flow meter are fixedly installed on the sodium nitrite pipeline 8. Both the first metering pump 12 and the first flow meter are electrically connected to the PLC controller. A second metering pump 13 and a second flow meter are fixedly installed on the sulfuric acid pipeline 10. Both the second metering pump 13 and the second flow meter are electrically connected to the PLC controller. A third metering pump 14 and a third flow meter are fixedly installed on the alkali pipeline 6. Both the third metering pump 14 and the third flow meter are electrically connected to the PLC controller. A fourth metering pump 15 and a fourth flow meter are fixedly installed on the azide wastewater pipeline 9. Both the fourth metering pump 15 and the fourth flow meter are electrically connected to the PLC controller. The first metering pump 12, the second metering pump 13, the third metering pump 14, and the fourth metering pump 15 are all diaphragm metering pumps. The first metering pump 12 is used to transport sodium nitrite, so it is made of 316L material. The third metering pump 14 is used to transport alkaline solution, so it is also made of 316L material. The second metering pump 13 is made of corrosion-resistant and non-metallic PTFE because it transports sulfuric acid. Similarly, the fourth metering pump 15, which is used to transport azide reagent, is also made of corrosion-resistant and non-metallic PTFE material.

[0054] A resistance thermometer 17 is fixedly installed in the water bath 18, and the resistance thermometer 17 is electrically connected to the PLC controller.

[0055] Both the quenching coil reactor 1 and the neutralization coil reactor 2 are made of PFA material, while the coil heat exchanger 3 is made of metal.

[0056] The PLC controller is equipped with a human-machine interface, which is used to display device operating parameters and alarm prompts.

[0057] The specific implementation method for quenching using the tubular rapid quenching device for azide wastewater shown in this embodiment is as follows:

[0058] S1. Start-up: Purge nitrogen into quenching coil reactor 1 and neutralization coil reactor 2 to inertize the device, turn on the heat exchange pipeline, add heat exchange process water into water bath 18 to submerge quenching coil reactor 1 and neutralization coil reactor 2, and turn on circulation pump 16 and online ion chromatograph 11.

[0059] S2. Continuous quenching: Turn on the third metering pump 14 to introduce liquid alkali into the neutralization coil reactor 2. After the liquid alkali flow rate stabilizes, turn on the second metering pump 13 to introduce sulfuric acid solution into the quenching coil reactor 1. After the sulfuric acid solution flow rate stabilizes, turn on the first metering pump 12 to introduce sodium nitrite solution into the quenching coil reactor 1. After the sodium nitrite solution flow rate stabilizes, turn on the fourth metering pump 15 to mix the azide wastewater with the sodium nitrite solution and send it into the quenching coil reactor 1 for continuous online quenching.

[0060] S3. pH Adjustment: After the mixture in the quenching coil reactor 1 is quenched, it enters the neutralization coil reactor 2 and is mixed with the alkaline solution in the neutralization coil reactor 2 to adjust the pH. After the pH adjustment is completed, it is discharged through the discharge pipeline 5. The online ion chromatograph 11 on the discharge pipeline 5 performs online detection of the azide ion content in the feed solution and transmits the result to the PLC control box.

[0061] In steps S2 and S3, temperature alarm interlock, flow alarm interlock, and discharge azide ion alarm interlock are set.

[0062] The temperature alarm interlock is as follows: The resistance thermometer 17 converts the temperature of the liquid in the quenching coil reactor 1 into an electrical signal and transmits it to the PLC controller. When the temperature of the quenching coil reactor 1 exceeds 30°C or falls below 20°C, the PLC controller shuts down the first metering pump 12, the second metering pump 13, the third metering pump 14 and the fourth metering pump 15 and triggers an alarm.

[0063] The flow alarm interlock is as follows: the first flow meter converts the flow of sodium nitrite pipeline 8 into an electrical signal and transmits it to the PLC controller; the second flow meter converts the flow of sulfuric acid pipeline 10 into an electrical signal and transmits it to the PLC controller; the third flow meter converts the flow of alkali solution pipeline 6 into an electrical signal and transmits it to the PLC controller; and the fourth flow meter converts the flow of azide wastewater pipeline 9 into an electrical signal and transmits it to the PLC controller. When any flow meter is higher or lower than the set value, the PLC controller shuts down the first metering pump 12, the second metering pump 13, the third metering pump 14, and the fourth metering pump 15 and triggers an alarm.

[0064] The azide ion alarm interlock is as follows: the online ion chromatograph 11 converts the concentration of azide ions in the discharged liquid into an electrical signal and transmits it to the PLC controller. When the concentration of azide ions in the discharged liquid exceeds 3 ppm, the PLC controller shuts down the first metering pump 12, the second metering pump 13, the third metering pump 14 and the fourth metering pump 15 and triggers an alarm.

[0065] In this embodiment, the ratio of sodium nitrite to azide residue during the treatment process is 2-50, the ratio of sulfuric acid to azide residue is 2-50, and the quenching residence time is 5-50 minutes, which can ensure that the azide residue after quenching is less than 3 ppm.

[0066] In summary, the above embodiments are merely preferred embodiments of the present invention and are not intended to limit the scope of protection of the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A tubular rapid quenching device for azide wastewater, characterized in that, It includes a water bath, a quenching coil reactor, a neutralization coil reactor, a coil heat exchanger, a PLC controller, and multiple pipelines, including a feed pipeline group, an alkali solution pipeline, a discharge pipeline, a heat exchange pipeline, and a circulation pipeline; The water bath contains heat exchange process water. The bottom of the water bath has an outlet. One end of the circulation pipe is fixedly connected to the outlet, and the other end of the circulation pipe is inserted into the water bath. A circulation pump is installed on the circulation pipe. The quenching coil reactor, neutralizing coil reactor, and coil heat exchanger are all fixedly installed inside the water bath. The quenching coil reactor is fixedly installed at the lower end of the neutralizing coil reactor, and the outlet of the quenching coil reactor and the inlet of the neutralizing coil reactor are connected by a pipeline. Both ends of the coil heat exchanger are connected to heat exchange pipelines, which are used to input and output heat exchange medium into and out of the coil heat exchanger. The coils of the quenching coil reactor are wound from bottom to top, and the coils of the neutralizing coil reactor are wound from bottom to top. The feed pipeline assembly is located on one side of the water bath and extends into the water bath, and the feed pipeline assembly is fixedly connected to the feed inlet of the quenching coil reactor. One end of the alkali solution pipeline is connected to the alkali solution source, and the other end of the alkali solution pipeline is connected to the feed end of the neutralization coil reactor. One end of the discharge pipeline is fixedly connected to the discharge port of the neutralization coil reactor, and the other end of the discharge pipeline is connected to a wastewater collection device. An online ion chromatograph is installed on the discharge pipeline. The PLC controller is electrically connected to the water bath, feed pipeline group, discharge pipeline, heat exchange pipeline and circulation pipeline.

2. The tubular rapid quenching device for azide wastewater according to claim 1, characterized in that, The feed pipeline assembly includes a main pipeline, a first branch pipeline, and a second branch pipeline. One end of the main pipeline is connected to the first branch pipeline and the second branch pipeline via a tee. The other end of the main pipeline is connected to the bottom end of the quenching coil reactor. A first static mixer is installed on the main pipeline.

3. The tubular rapid quenching device for azide wastewater according to claim 2, characterized in that, The first branch consists of a sodium nitrite pipeline and an azide wastewater pipeline. One end of the sodium nitrite pipeline is connected to a sodium nitrite solution source, and the other end of the sodium nitrite pipeline is connected to the azide wastewater pipeline. One end of the azide wastewater pipeline is connected to an azide wastewater source, and the other end of the azide wastewater pipeline is connected to the sodium nitrite pipeline. A second static mixer is installed at the connection end of the sodium nitrite pipeline and the azide wastewater pipeline. The second branch is a sulfuric acid pipeline. One end of the sulfuric acid pipeline is connected to a sulfuric acid solution source, and the other end of the sulfuric acid pipeline is connected to the main pipeline.

4. The tubular rapid quenching device for azide wastewater according to claim 3, characterized in that, A first metering pump and a first flow meter are fixedly installed on the sodium nitrite pipeline, and both the first metering pump and the first flow meter are electrically connected to the PLC controller. A second metering pump and a second flow meter are fixedly installed on the sulfuric acid pipeline, and both the second metering pump and the second flow meter are electrically connected to the PLC controller. A third metering pump and a third flow meter are fixedly installed on the alkali pipeline, and both the third metering pump and the third flow meter are electrically connected to the PLC controller. A fourth metering pump and a fourth flow meter are fixedly installed on the azide wastewater pipeline, and both the fourth metering pump and the fourth flow meter are electrically connected to the PLC controller.

5. The tubular rapid quenching device for azide wastewater according to claim 1, characterized in that, A resistance temperature detector (RTD) thermometer is fixedly installed in the water bath, and the RTD thermometer is electrically connected to the PLC controller.

6. The tubular rapid quenching device for azide wastewater according to claim 1, characterized in that, Both the quenching coil reactor and the neutralizing coil reactor are made of PFA material, and the coil heat exchanger is made of metal.

7. The tubular rapid quenching device for azide wastewater according to claim 1, characterized in that, The PLC controller is equipped with a human-machine interface, which is used to display device operating parameters and alarm prompts.

8. A quenching method based on the tubular rapid quenching device for azide wastewater as described in any one of claims 1-7, characterized in that, The method includes the following steps: S1. Start-up: Purge nitrogen into the quenching coil reactor and the neutralization coil reactor to inertize the device, open the heat exchange pipeline, add heat exchange process water into the water bath to submerge the quenching coil reactor and the neutralization coil reactor, and start the circulation pump and the online ion chromatograph. S2. Continuous quenching: Turn on the third metering pump to introduce liquid alkali into the neutralization coil reactor. After the liquid alkali flow rate stabilizes, turn on the second metering pump to introduce sulfuric acid solution into the quenching coil reactor. After the sulfuric acid solution flow rate stabilizes, turn on the first metering pump to introduce sodium nitrite solution into the quenching coil reactor. After the sodium nitrite solution flow rate stabilizes, turn on the fourth metering pump to mix the azide wastewater with the sodium nitrite solution and send it into the quenching coil reactor for continuous online quenching. S3. pH Adjustment: After the mixture in the quenching coil reactor is quenched, it enters the neutralization coil reactor and is mixed with the alkaline solution in the neutralization coil reactor to adjust the pH. After the pH adjustment is completed, it is discharged through the discharge pipeline. The online ion chromatograph on the discharge pipeline detects the azide ion content in the feed solution online and transmits the results to the PLC control box.

9. The quenching method according to claim 8, characterized in that, In steps S2 and S3, temperature alarm interlock, flow alarm interlock, and discharge azide ion alarm interlock are set. The temperature alarm interlock is as follows: the resistance thermometer converts the temperature of the liquid in the quenching coil reactor into an electrical signal and transmits it to the PLC controller. When the temperature of the quenching coil reactor exceeds 30°C or falls below 20°C, the PLC controller shuts down the first metering pump, the second metering pump, the third metering pump, and the fourth metering pump and issues an alarm. The flow alarm interlock is as follows: the first flow meter converts the flow rate of the sodium nitrite pipeline into an electrical signal and transmits it to the PLC controller; the second flow meter converts the flow rate of the sulfuric acid pipeline into an electrical signal and transmits it to the PLC controller; the third flow meter converts the flow rate of the alkali pipeline into an electrical signal and transmits it to the PLC controller; and the fourth flow meter converts the flow rate of the azide wastewater pipeline into an electrical signal and transmits it to the PLC controller. When any flow meter is higher or lower than the set value, the PLC controller shuts down the first metering pump, the second metering pump, the third metering pump, and the fourth metering pump and issues an alarm. The discharge azide ion alarm interlock is as follows: the online ion chromatograph converts the concentration of azide ions in the discharge solution into an electrical signal and transmits it to the PLC controller. When the concentration of azide ions in the discharge solution exceeds 3 ppm, the PLC controller shuts down the first metering pump, the second metering pump, the third metering pump and the fourth metering pump and alarms.

Images