An azide reagent wastewater continuous quenching device based on a kettle reactor and a working method thereof

Abstract

The application discloses an azide reagent wastewater continuous quenching device and method based on a kettle reactor, which comprises a first pipeline, a second pipeline, a third pipeline, a fourth pipeline, a PLC control box, a nitrogen pipeline, a venting pipeline and a quenching kettle, a neutralization kettle and a receiving tank arranged from high to low in sequence. The application is based on the modularization of the kettle reactor and the matched pipeline, has high integration, small liquid holding capacity in the quenching reaction section, high heat and mass transfer efficiency, realizes online continuous quenching of the azide reagent wastewater in the production workshop, can be flexibly transferred and conveniently disassembled and adapted to multiple industrial production scenes, can improve the quenching treatment capacity and treatment efficiency of the wastewater, and can be widely applied to industrial large-scale production.

Description

Technical Field

[0001] This invention relates to the field of pharmaceutical and chemical equipment technology, specifically to a continuous quenching device for azide reagent wastewater based on a batch reactor and its working method. Background Technology

[0002] In the chemical and pharmaceutical production process, excipients or by-reactants are usually in excess. For reactions involving some highly active or high-risk excipients or by-reactants, after the reaction is completed, the excipients or by-reactants need to be quenched to make them lose their activity and transform them into safer and more stable substances, so as to carry out post-treatment and 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. During the preparation of azide compounds, side reactions produce waste liquid containing azide reagents. 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] Therefore, there is an urgent need in this field for a continuous quenching device and method for azide reagent wastewater based on a batch reactor, which has a small liquid holdup, high adaptability, and can greatly reduce the risks in the production process, ensuring high efficiency and safety in production. Summary of the Invention

[0006] To solve the above technical problems, the present invention provides a continuous quenching device for azide reagent wastewater based on a batch reactor, including a first pipeline, a second pipeline, a third pipeline, a fourth pipeline, a PLC control box, a nitrogen pipeline, a venting pipeline, and a quenching tank, a neutralization tank, and a receiving tank arranged in descending order of height;

[0007] The interiors of the quenching vessel, neutralization vessel, and receiving vessel are connected sequentially by pipelines. The installation height of the quenching vessel is higher than that of the neutralization vessel, and the installation height of the neutralization vessel is higher than that of the receiving vessel. An online ion chromatograph is fixedly installed between the neutralization vessel and the receiving vessel.

[0008] The second and fourth pipelines enter the interior of the quenching vessel through the liquid inlet at the top of the quenching vessel, and the ends of the second and fourth pipelines that enter the interior of the quenching vessel extend to the bottom of the quenching vessel.

[0009] The fourth pipeline, which does not extend into the quenching vessel, is equipped with a tee, and the first pipeline is connected to the fourth pipeline and the interior of the quenching vessel through the tee.

[0010] One end of the third pipeline enters the interior of the neutralization vessel through the liquid inlet at the top of the neutralization vessel and extends to the bottom of the neutralization vessel;

[0011] The first pipeline is used to transport sodium nitrite solution, the second pipeline is used to transport sulfuric acid aqueous solution, the third pipeline is used to transport liquid alkali, and the fourth pipeline is used to transport azide reagent wastewater.

[0012] One end of the nitrogen pipeline is connected to a nitrogen source, and the other end of the nitrogen pipeline is divided into three branches, which are respectively connected to the interior of the quenching vessel, the neutralization vessel and the receiving tank.

[0013] One end of the venting pipeline is equipped with a tail gas processor, and the other end of the venting pipeline is divided into three branches, which are respectively connected to the interior of the quenching vessel, the neutralization vessel and the receiving tank.

[0014] The PLC control box is electrically connected to the first pipeline, the second pipeline, the third pipeline, the fourth pipeline, the nitrogen pipeline, the venting pipeline, the quenching kettle, the neutralization kettle, and the receiving tank, respectively.

[0015] Specifically, the quenching vessel is equipped with a first thermometer, a first level gauge, a first pressure gauge, and a first pH meter. The first thermometer, the first level gauge, the first pressure gauge, and the first pH meter are all electrically connected to the PLC control box. The side of the quenching vessel is provided with a quenching vessel overflow port, and the quenching vessel overflow port is connected to the liquid inlet of the neutralization vessel through a pipeline.

[0016] Specifically, the neutralization vessel is equipped with a second thermometer, a second level gauge, a second pressure gauge, and a second pH meter. The second thermometer, the second level gauge, the second pressure gauge, and the second pH meter are all electrically connected to the PLC control box. The side of the neutralization vessel is provided with a neutralization vessel overflow port, and the neutralization vessel overflow port is connected to the liquid inlet of the receiving tank through a pipeline.

[0017] Specifically, the receiving tank is equipped with a third level gauge, and the outlet of the receiving tank is equipped with a transfer pump. Both the third level gauge and the transfer pump are electrically connected to the PLC control box.

[0018] Specifically, both the quenching vessel and the neutralization vessel are equipped with a temperature control jacket and a stirrer. The inner surfaces of both the quenching vessel and the neutralization vessel are coated with a fluorine material layer. Cooling water is circulated in the temperature control jacket to regulate the temperature inside the vessel.

[0019] Specifically, an azide acid detector is fixedly installed at one end of the venting pipeline where the exhaust gas processor is located. The azide acid detector is used to detect the content of azide acid in the exhaust gas, and the azide acid detector is electrically connected to the PLC control box.

[0020] Specifically, a first metering pump and a first flow meter are installed on the first pipeline, a second metering pump and a second flow meter are installed on the second pipeline, a third metering pump and a third flow meter are installed on the third pipeline, and a fourth metering pump is installed on the fourth pipeline. The first metering pump, the second metering pump, the third metering pump, the fourth metering pump, the first flow meter, the second flow meter, and the third flow meter are all electrically connected to the PLC control box.

[0021] Specifically, the first metering pump, the second metering pump, the third metering pump, and the fourth metering pump are all diaphragm metering pumps.

[0022] Specifically, the transfer pump is a pneumatic diaphragm pump.

[0023] In another aspect, the present invention provides a method for continuously quenching azide reagent wastewater based on the aforementioned continuous quenching device for azide reagent wastewater using a batch reactor, the method comprising the following steps:

[0024] S1. Start-up: Introduce nitrogen into the device through the nitrogen pipeline to inertize it, turn on the stirrers of the quenching vessel and the neutralization vessel, input cooling water into the temperature control jackets of the quenching vessel and the neutralization vessel, and turn on the online ion chromatograph and the azido acid detector.

[0025] S2. Continuous quenching: Turn on the third metering pump to introduce liquid alkali into the neutralization vessel. After the liquid alkali flow rate stabilizes, turn on the second metering pump to introduce sulfuric acid solution into the quenching vessel. After the sulfuric acid solution flow rate stabilizes, turn on the first metering pump to introduce sodium nitrite solution into the quenching vessel. After the sodium nitrite solution flow rate stabilizes, turn on the fourth metering pump to mix the azide reagent wastewater with the sodium nitrite solution and send it into the quenching vessel for continuous online quenching.

[0026] S3. pH Adjustment: After the liquid level of the mixture in the quenching kettle rises to the overflow port of the quenching kettle, it automatically flows into the neutralization kettle and mixes with the alkaline solution in the neutralization kettle to adjust the pH. After the liquid level of the mixture in the neutralization kettle rises to the overflow port of the neutralization kettle, it automatically flows into the receiving tank. The third liquid level gauge in the receiving tank converts the liquid level value into an electrical signal and transmits it to the PLC control box. The PLC control box starts the transfer pump to discharge the quenching wastewater from the receiving tank.

[0027] Specifically, in steps S2 and S3, temperature alarm interlock, pressure alarm interlock, liquid level alarm interlock, pH alarm interlock, tail gas azido acid alarm interlock and discharge azide ion alarm interlock are set.

[0028] The temperature alarm interlock is as follows: the first thermometer converts the temperature of the liquid in the quenching kettle into an electrical signal and transmits it to the PLC control box; the second thermometer converts the temperature of the liquid in the neutralization kettle into an electrical signal and transmits it to the PLC control box; when the temperature of the quenching kettle or the neutralization kettle exceeds 40°C or falls below 10°C, the PLC control box 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 pressure alarm interlock is as follows: the first pressure gauge converts the pressure of the quenching kettle into an electrical signal and transmits it to the PLC control box; the second pressure gauge converts the pressure of the neutralization kettle into an electrical signal and transmits it to the PLC control box; when the pressure of the quenching kettle or the neutralization kettle exceeds the set value, the PLC control box shuts down the first metering pump, the second metering pump, the third metering pump and the fourth metering pump and alarms.

[0030] The liquid level alarm interlock is as follows: the first liquid level gauge converts the liquid level height of the quenching kettle into an electrical signal and transmits it to the PLC control box; the second liquid level gauge converts the liquid level height of the neutralization kettle into an electrical signal and transmits it to the PLC control box; the third liquid level gauge converts the liquid level height of the receiving tank into an electrical signal and transmits it to the PLC control box. When the liquid level height of the quenching kettle or neutralization kettle is higher than the set value, the PLC control box shuts down the first metering pump, the second metering pump, the third metering pump, and the fourth metering pump and alarms. When the liquid level height of the receiving tank is higher than the set value, the PLC control box shuts down the first metering pump, the second metering pump, the third metering pump, and the fourth metering pump, starts the transfer pump, and alarms.

[0031] The pH alarm interlock is as follows: the first pH meter converts the pH value of the quenching vessel into an electrical signal and transmits it to the PLC control box. When the pH value of the quenching vessel exceeds 3, the PLC control box shuts down the fourth metering pump and triggers an alarm.

[0032] The exhaust gas azido acid alarm interlock is as follows: the azido acid detector converts the azido acid concentration in the venting pipeline into an electrical signal and transmits it to the PLC control box. When the azido acid concentration in the venting pipeline exceeds 3ppm, the PLC control box shuts down the first metering pump, the second metering pump, the third metering pump and the fourth metering pump and alarms.

[0033] The azide ion alarm interlock is as follows: the online ion chromatograph converts the concentration of azide ions in the discharged liquid into an electrical signal and transmits it to the PLC control box. When the concentration of azide ions in the discharged liquid exceeds 3 ppm, the PLC control box shuts down the first metering pump, the second metering pump, the third metering pump and the fourth metering pump and alarms.

[0034] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0035] 1. The continuous quenching device for azide reagent wastewater based on a batch reactor provided by the present invention is based on a modular skid-mounted batch reactor and supporting pipelines, with high integration, small liquid hold-up in the quenching reaction section, and high heat and mass transfer efficiency. It realizes online continuous quenching of azide reagent wastewater in the production workshop. It can be flexibly transferred and easily disassembled to adapt to multiple industrial production scenarios. It can also improve the quenching treatment capacity and treatment efficiency of wastewater, and can be widely used in large-scale industrial production.

[0036] 2. The continuous quenching device for azide reagent wastewater based on a batch reactor provided by this invention uses a PLC control box to control multiple metering pumps and transfer pumps based on data from multiple thermometers, level gauges, pH meters, and pressure gauges. This enables automatic monitoring and adjustment of temperature, level, pH, and pressure during the quenching process. Furthermore, it can promptly alarm and control the quenching process based on the detection results from an azide acid detector and an online ion chromatograph. This automatic and stable detection and operation avoids the safety risks and labor costs associated with frequent manual operations in intermittent quenching processes.

[0037] 3. The continuous quenching device for azide reagent wastewater based on a batch reactor provided by the present invention has a fourth pipeline for conveying azide reagent wastewater that can 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 does not require large-scale temporary storage, has a small liquid holding capacity, and greatly improves the wastewater treatment efficiency.

[0038] 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

[0039] Figure 1 This is a schematic diagram of the overall structure of the continuous quenching device for azide reagent wastewater based on a batch reactor provided by the present invention in Example 1.

[0040] In the diagram, 1-quenching vessel, 2-neutralization vessel, 3-receiving tank, 4-first pipeline, 5-second pipeline, 6-third pipeline, 7-fourth pipeline, 8-nitrogen pipeline, 9-venting pipeline, 10-online ion chromatograph, 11-first metering pump, 12-second metering pump, 13-third metering pump, 14-fourth metering pump, 15-transfer pump. Detailed Implementation

[0041] 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.

[0042] 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.

[0043] Example 1

[0044] like Figure 1 As shown in the figure, this embodiment illustrates a continuous quenching device for azide reagent wastewater based on a batch reactor, including a first pipeline 4, a second pipeline 5, a third pipeline 6, a fourth pipeline 7, a PLC control box, a nitrogen pipeline 8, a venting pipeline 9, and a quenching tank 1, a neutralization tank 2, and a receiving tank 3 arranged sequentially from high to low. The PLC control box, quenching tank 1, neutralization tank 2, and receiving tank 3 are all fixedly installed on a frame or bracket, forming a modular skid-mounted device that is easy to move and can also be nested into other production lines for flexible use.

[0045] The interiors of the quenching vessel 1, neutralization vessel 2, and receiving vessel 3 are connected sequentially by pipelines. The installation height of the quenching vessel 1 is higher than that of the neutralization vessel 2, and the installation height of the neutralization vessel 2 is higher than that of the receiving vessel 3. An online ion chromatograph 10 is fixedly installed between the neutralization vessel 2 and the receiving vessel 3. The online ion chromatograph 10 can monitor the residual concentration of azide ions in the feed liquid overflowing from the neutralization vessel 2 to the receiving vessel 3 in real time.

[0046] In this embodiment, the bottom of the quenching vessel 1 is higher than the top of the neutralization vessel 2, and the bottom of the neutralization vessel 2 is higher than the top of the receiving tank 3, making full use of the positional difference between the devices to facilitate the transfer of materials.

[0047] The second pipe 5 and the fourth pipe 7 enter the interior of the quenching vessel 1 through the inlet at the top of the quenching vessel 1, and one end of each pipe extends to the bottom of the quenching vessel 1. One end of the third pipe 6 enters the interior of the neutralization vessel 2 through the inlet at the top of the neutralization vessel 2 and extends to the bottom of the neutralization vessel 2. The azide wastewater is first mixed with the sodium nitrite solution before entering the quenching vessel 1. The bottom-inserted feeding method in the quenching vessel 1 not only avoids the risk of the azide wastewater directly contacting sulfuric acid and generating azidoic acid, but also ensures sufficient residence time for the azide wastewater in the quenching vessel 1, thus facilitating sufficient quenching. Similarly, the neutralization vessel 2 also uses a bottom-inserted feeding method to ensure sufficient neutralization reaction of the liquid.

[0048] A tee is installed on the fourth pipeline 7 that does not extend into the quenching vessel 1. The first pipeline 4 is connected to the fourth pipeline 7 and the interior of the quenching vessel 1 through the tee.

[0049] Pipeline 4 is used to transport sodium nitrite solution, pipeline 5 is used to transport sulfuric acid solution, pipeline 6 is used to transport liquid alkali, and pipeline 7 is used to transport azide reagent wastewater.

[0050] One end of the nitrogen pipeline 8 is connected to a nitrogen source, and the other end of the nitrogen pipeline 8 is divided into three branches and connected to the interior of the quenching vessel 1, the neutralization vessel 2 and the receiving tank 3 respectively; one end of the vent pipeline 9 is equipped with a tail gas processor, and the other end of the vent pipeline 9 is divided into three branches and connected to the interior of the quenching vessel 1, the neutralization vessel 2 and the receiving tank 3 respectively.

[0051] The PLC control box is electrically connected to the first pipeline 4, the second pipeline 5, the third pipeline 6, the fourth pipeline 7, the nitrogen pipeline 8, the venting pipeline 9, the quenching vessel 1, the neutralization vessel 2, and the receiving tank 3, respectively.

[0052] The PLC control box is equipped with a human-machine interface that displays information transmitted to the PLC control box from each component electrically connected to it in real time. It can also set alarm prompts and safety interlocks.

[0053] The quenching vessel 1 is equipped with a first thermometer, a first level gauge, a first pressure gauge, and a first pH meter. The first thermometer, the first level gauge, the first pressure gauge, and the first pH meter are all electrically connected to the PLC control box. The side of the quenching vessel 1 is provided with an overflow port. The overflow port of the quenching vessel 1 is connected to the liquid inlet of the neutralization vessel 2 through a pipeline.

[0054] The neutralization vessel 2 is equipped with a second thermometer, a second level gauge, a second pressure gauge, and a second pH meter. The second thermometer, the second level gauge, the second pressure gauge, and the second pH meter are all electrically connected to the PLC control box. The side of the neutralization vessel 2 is provided with an overflow port, which is connected to the liquid inlet of the receiving tank 3 through a pipeline.

[0055] The receiving tank 3 is equipped with a third level gauge, and the outlet of the receiving tank 3 is equipped with a transfer pump 15, which is a pneumatic diaphragm pump. Both the third level gauge and the transfer pump 15 are electrically connected to the PLC control box.

[0056] Both the quenching vessel 1 and the neutralization vessel 2 are equipped with temperature control jackets and stirrers. The inner surfaces of both the quenching vessel 1 and the neutralization vessel 2 are coated with a fluorine material layer. Cooling water is circulated in the temperature control jacket to regulate the temperature inside the vessel.

[0057] A azido acid detector is fixedly installed at one end of the vent pipe 9 where the exhaust gas processor is located. The azido acid detector is used to detect the content of azido acid in the exhaust gas. The azido acid detector is electrically connected to the PLC control box.

[0058] The first pipeline 4 is equipped with a first metering pump 11 and a first flow meter; the second pipeline 5 is equipped with a second metering pump 12 and a second flow meter; the third pipeline 6 is equipped with a third metering pump 13 and a third flow meter; and the fourth pipeline 7 is equipped with a fourth metering pump 14. The first metering pump 11, the second metering pump 12, the third metering pump 13, the fourth metering pump 14, the first flow meter, the second flow meter, and the third flow meter are all electrically connected to the PLC control box. The on / off status and flow rate of the four pipelines can be displayed on the display interface of the PLC control box. The on / off status and flow rate can also be adjusted through the PLC control box to ensure stable material flow.

[0059] The first metering pump 11, the second metering pump 12, the third metering pump 13, and the fourth metering pump 14 are all diaphragm metering pumps.

[0060] This embodiment illustrates a method for quenching azide reagent wastewater using the aforementioned continuous quenching device for azide reagent wastewater based on a batch reactor. In this embodiment, the pH value in the quenching vessel 1 is controlled to be below 3, the temperature in the quenching vessel 1 and the neutralization vessel 2 is maintained at 10-40°C, and the azide acid content measured by the azide acid detector on the venting pipeline 9 should be less than 3 ppm.

[0061] The specific steps are as follows:

[0062] S1. Start-up: Introduce nitrogen into the device through nitrogen pipeline 8 to inertize it, turn on the stirrers of quenching vessel 1 and neutralization vessel 2, input cooling water into the temperature control jackets of quenching vessel 1 and neutralization vessel 2, and turn on the online ion chromatograph 10 and azido acid detector.

[0063] S2. Continuous quenching: Turn on the third metering pump 13 to introduce liquid alkali into the neutralization vessel 2. After the liquid alkali flow rate stabilizes, turn on the second metering pump 12 to introduce sulfuric acid aqueous solution into the quenching vessel 1. After the sulfuric acid aqueous solution flow rate stabilizes, turn on the first metering pump 11 to introduce sodium nitrite solution into the quenching vessel 1. After the sodium nitrite solution flow rate stabilizes, turn on the fourth metering pump 14 to mix the azide reagent wastewater with the sodium nitrite solution and send it into the quenching vessel 1 for continuous online quenching.

[0064] S3. pH Adjustment: After the liquid level of the mixture in quenching vessel 1 rises to the overflow port of quenching vessel 1, it automatically flows into neutralizing vessel 2 and mixes with the alkaline solution in neutralizing vessel 2 to adjust the pH to neutral. After the liquid level of the mixture in neutralizing vessel 2 rises to the overflow port of neutralizing vessel 2, it automatically flows into receiving tank 3. The third liquid level gauge in receiving tank 3 converts the liquid level value into an electrical signal and transmits it to the PLC control box. The PLC control box starts the transfer pump 15 to discharge the quenching wastewater into receiving tank 3.

[0065] After the aforementioned settings are completed, in steps S2 and S3, temperature alarm interlock, pressure alarm interlock, liquid level alarm interlock, pH alarm interlock, tail gas azido acid alarm interlock and discharge azide ion alarm interlock are set.

[0066] The temperature alarm interlock is as follows: the first thermometer converts the temperature of the liquid in the quenching vessel 1 into an electrical signal and transmits it to the PLC control box; the second thermometer converts the temperature of the liquid in the neutralization vessel 2 into an electrical signal and transmits it to the PLC control box; when the temperature of the quenching vessel 1 or the neutralization vessel 2 exceeds 40℃ or falls below 10℃, the PLC control box shuts down the first metering pump 11, the second metering pump 12, the third metering pump 13 and the fourth metering pump 14 and triggers an alarm.

[0067] The pressure alarm interlock is as follows: the first pressure gauge converts the pressure of quenching vessel 1 into an electrical signal and transmits it to the PLC control box; the second pressure gauge converts the pressure of neutralization vessel 2 into an electrical signal and transmits it to the PLC control box; when the pressure of quenching vessel 1 or neutralization vessel 2 exceeds the set value, the PLC control box shuts down the first metering pump 11, the second metering pump 12, the third metering pump 13 and the fourth metering pump 14 and alarms.

[0068] The liquid level alarm interlock is as follows: the first liquid level gauge converts the liquid level of quenching vessel 1 into an electrical signal and transmits it to the PLC control box; the second liquid level gauge converts the liquid level of neutralizing vessel 2 into an electrical signal and transmits it to the PLC control box; the third liquid level gauge converts the liquid level of receiving tank 3 into an electrical signal and transmits it to the PLC control box. When the liquid level of quenching vessel 1 or neutralizing vessel 2 is higher than the set value, the PLC control box shuts down the first metering pump 11, the second metering pump 12, the third metering pump 13 and the fourth metering pump 14 and alarms. When the liquid level of receiving tank 3 is higher than the set value, the PLC control box shuts down the first metering pump 11, the second metering pump 12, the third metering pump 13 and the fourth metering pump 14, starts the transfer pump 15 and alarms.

[0069] The pH alarm interlock is as follows: the first pH meter converts the pH value of the quenching vessel 1 into an electrical signal and transmits it to the PLC control box. When the pH value of the quenching vessel 1 exceeds 3, the PLC control box shuts down the fourth metering pump 14 and triggers an alarm.

[0070] The exhaust gas azido acid alarm interlock is as follows: the azido acid detector converts the azido acid concentration in the venting pipeline 9 into an electrical signal and transmits it to the PLC control box. When the azido acid concentration in the venting pipeline 9 exceeds 3ppm, the PLC control box shuts down the first metering pump 11, the second metering pump 12, the third metering pump 13 and the fourth metering pump 14 and alarms.

[0071] The azide ion alarm interlock is as follows: the online ion chromatograph 10 converts the concentration of azide ions in the discharged liquid into an electrical signal and transmits it to the PLC control box. When the concentration of azide ions in the discharged liquid exceeds 3 ppm, the PLC control box shuts down the first metering pump 11, the second metering pump 12, the third metering pump 13 and the fourth metering pump 14 and alarms.

[0072] 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 30-300 min, which can ensure that the azide residue after quenching is less than 3 ppm.

[0073] 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 continuous quenching device for azide reagent wastewater based on a batch reactor, characterized in that, It includes a first pipeline, a second pipeline, a third pipeline, a fourth pipeline, a PLC control box, a nitrogen pipeline, a venting pipeline, and a quenching vessel, a neutralization vessel, and a receiving tank arranged in descending order of height; wherein, the first pipeline has a first metering pump, the second pipeline has a second metering pump, the third pipeline has a third metering pump, and the fourth pipeline has a fourth metering pump, and the first, second, third, and fourth metering pumps are all electrically connected to the PLC control box; The interiors of the quenching vessel, neutralization vessel, and receiving vessel are connected sequentially by pipelines. The installation height of the quenching vessel is higher than that of the neutralization vessel, and the installation height of the neutralization vessel is higher than that of the receiving vessel. An online ion chromatograph is fixedly installed between the neutralization vessel and the receiving vessel. The second and fourth pipelines enter the interior of the quenching vessel through the liquid inlet at the top of the quenching vessel, and the ends of the second and fourth pipelines that enter the interior of the quenching vessel extend to the bottom of the quenching vessel. The fourth pipeline, which does not extend into the quenching vessel, is equipped with a tee, and the first pipeline is connected to the fourth pipeline and the interior of the quenching vessel through the tee. One end of the third pipeline enters the interior of the neutralization vessel through the liquid inlet at the top of the neutralization vessel and extends to the bottom of the neutralization vessel; The first pipeline is used to transport sodium nitrite solution, the second pipeline is used to transport sulfuric acid aqueous solution, the third pipeline is used to transport liquid alkali, and the fourth pipeline is used to transport azide reagent wastewater. One end of the nitrogen pipeline is connected to a nitrogen source, and the other end of the nitrogen pipeline is divided into three branches, which are respectively connected to the interior of the quenching vessel, the neutralization vessel and the receiving tank. One end of the venting pipeline is equipped with a tail gas processor, and the other end of the venting pipeline is divided into three branches, which are respectively connected to the interior of the quenching vessel, the neutralization vessel and the receiving tank. The PLC control box is electrically connected to the first pipeline, the second pipeline, the third pipeline, the fourth pipeline, the nitrogen pipeline, the venting pipeline, the quenching kettle, the neutralization kettle, and the receiving tank, respectively. During continuous quenching, the third metering pump is turned on to introduce liquid alkali into the neutralization kettle. After the liquid alkali flow rate stabilizes, the second metering pump is turned on to introduce sulfuric acid solution into the quenching kettle. After the sulfuric acid solution flow rate stabilizes, the first metering pump is turned on to introduce sodium nitrite solution into the quenching kettle. After the sodium nitrite solution flow rate stabilizes, the fourth metering pump is turned on to mix the azide reagent wastewater with the sodium nitrite solution and send it into the quenching kettle for continuous online quenching. Both the quenching vessel and the neutralization vessel are equipped with a temperature control jacket and a stirrer. The inner surfaces of both the quenching vessel and the neutralization vessel are coated with a fluorine material layer. Cooling water is circulated in the temperature control jacket to regulate the temperature inside the vessel.

2. The continuous quenching device for azide reagent wastewater based on a batch reactor according to claim 1, characterized in that, The quenching vessel is equipped with a first thermometer, a first level gauge, a first pressure gauge, and a first pH meter. The first thermometer, the first level gauge, the first pressure gauge, and the first pH meter are all electrically connected to the PLC control box. The side of the quenching vessel is provided with a quenching vessel overflow port, and the quenching vessel overflow port is connected to the liquid inlet of the neutralization vessel through a pipeline.

3. The continuous quenching device for azide reagent wastewater based on a batch reactor according to claim 1, characterized in that, The neutralization vessel is equipped with a second thermometer, a second level gauge, a second pressure gauge, and a second pH meter. The second thermometer, the second level gauge, the second pressure gauge, and the second pH meter are all electrically connected to the PLC control box. The side of the neutralization vessel is provided with a neutralization vessel overflow port, which is connected to the liquid inlet of the receiving tank through a pipeline.

4. The continuous quenching device for azide reagent wastewater based on a batch reactor according to claim 1, characterized in that, The receiving tank is equipped with a third level gauge, and the outlet of the receiving tank is equipped with a transfer pump. Both the third level gauge and the transfer pump are electrically connected to the PLC control box.

5. The continuous quenching device for azide reagent wastewater based on a batch reactor according to claim 1, characterized in that, A azido acid detector is fixedly installed at one end of the venting pipeline where the exhaust gas processor is located. The azido acid detector is used to detect the content of azido acid in the exhaust gas. The azido acid detector is electrically connected to the PLC control box.

6. The continuous quenching device for azide reagent wastewater based on a batch reactor according to claim 1, characterized in that, A first flow meter is installed on the first pipeline, a second flow meter is installed on the second pipeline, and a third flow meter is installed on the third pipeline. The first flow meter, the second flow meter, and the third flow meter are all electrically connected to the PLC control box.

7. The continuous quenching device for azide reagent wastewater based on a batch reactor according to claim 6, characterized in that, The first metering pump, the second metering pump, the third metering pump, and the fourth metering pump are all diaphragm metering pumps.

8. The continuous quenching device for azide reagent wastewater based on a batch reactor according to claim 4, characterized in that, The transfer pump is a pneumatic diaphragm pump.

9. A method for continuously quenching azide reagent wastewater based on a continuous quenching device for azide reagent wastewater using a batch reactor as described in any one of claims 1-8, characterized in that, The method includes the following steps: S1. Start-up: Introduce nitrogen into the device through the nitrogen pipeline to inertize it, turn on the stirrers of the quenching vessel and the neutralization vessel, input cooling water into the temperature control jackets of the quenching vessel and the neutralization vessel, and turn on the online ion chromatograph and the azido acid detector. S2. Continuous quenching: Turn on the third metering pump to introduce liquid alkali into the neutralization vessel. After the liquid alkali flow rate stabilizes, turn on the second metering pump to introduce sulfuric acid solution into the quenching vessel. After the sulfuric acid solution flow rate stabilizes, turn on the first metering pump to introduce sodium nitrite solution into the quenching vessel. After the sodium nitrite solution flow rate stabilizes, turn on the fourth metering pump to mix the azide reagent wastewater with the sodium nitrite solution and send it into the quenching vessel for continuous online quenching. S3. pH Adjustment: After the liquid level of the mixture in the quenching kettle rises to the overflow port of the quenching kettle, it automatically flows into the neutralization kettle and mixes with the alkaline solution in the neutralization kettle to adjust the pH. After the liquid level of the mixture in the neutralization kettle rises to the overflow port of the neutralization kettle, it automatically flows into the receiving tank. The third liquid level gauge in the receiving tank converts the liquid level value into an electrical signal and transmits it to the PLC control box. The PLC control box starts the transfer pump to discharge the quenching wastewater from the receiving tank.

10. The method for continuously quenching azide reagent wastewater according to claim 9, characterized in that, In steps S2 and S3, temperature alarm interlock, pressure alarm interlock, liquid level alarm interlock, pH alarm interlock, tail gas azido acid alarm interlock and discharge azide ion alarm interlock are set. The temperature alarm interlock is as follows: the first thermometer converts the temperature of the liquid in the quenching kettle into an electrical signal and transmits it to the PLC control box; the second thermometer converts the temperature of the liquid in the neutralization kettle into an electrical signal and transmits it to the PLC control box; when the temperature of the quenching kettle or the neutralization kettle exceeds 40°C or falls below 10°C, the PLC control box shuts down the first metering pump, the second metering pump, the third metering pump, and the fourth metering pump and triggers an alarm. The pressure alarm interlock is as follows: the first pressure gauge converts the pressure of the quenching kettle into an electrical signal and transmits it to the PLC control box; the second pressure gauge converts the pressure of the neutralization kettle into an electrical signal and transmits it to the PLC control box; when the pressure of the quenching kettle or the neutralization kettle exceeds the set value, the PLC control box shuts down the first metering pump, the second metering pump, the third metering pump and the fourth metering pump and alarms. The liquid level alarm interlock is as follows: the first liquid level gauge converts the liquid level height of the quenching kettle into an electrical signal and transmits it to the PLC control box; the second liquid level gauge converts the liquid level height of the neutralization kettle into an electrical signal and transmits it to the PLC control box; the third liquid level gauge converts the liquid level height of the receiving tank into an electrical signal and transmits it to the PLC control box. When the liquid level height of the quenching kettle or neutralization kettle is higher than the set value, the PLC control box shuts down the first metering pump, the second metering pump, the third metering pump, and the fourth metering pump and alarms. When the liquid level height of the receiving tank is higher than the set value, the PLC control box shuts down the first metering pump, the second metering pump, the third metering pump, and the fourth metering pump, starts the transfer pump, and alarms. The pH alarm interlock is as follows: the first pH meter converts the pH value of the quenching vessel into an electrical signal and transmits it to the PLC control box. When the pH value of the quenching vessel exceeds 3, the PLC control box shuts down the fourth metering pump and triggers an alarm. The exhaust gas azido acid alarm interlock is as follows: the azido acid detector converts the azido acid concentration in the venting pipeline into an electrical signal and transmits it to the PLC control box. When the azido acid concentration in the venting pipeline exceeds 3ppm, the PLC control box shuts down the first metering pump, the second metering pump, the third metering pump and the fourth metering pump and alarms. The azide ion alarm interlock is as follows: the online ion chromatograph converts the concentration of azide ions in the discharged liquid into an electrical signal and transmits it to the PLC control box. When the concentration of azide ions in the discharged liquid exceeds 3 ppm, the PLC control box shuts down the first metering pump, the second metering pump, the third metering pump and the fourth metering pump and alarms.

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