A phosphate ester fire-resistant oil micro-oxidation system and oxidation monitoring method

Abstract

The present invention relates to the technical field of phosphate fire-resistant oil production, and in particular to a phosphate fire-resistant oil micro-oxidation system and an oxidation monitoring method. The phosphate fire-resistant oil micro-oxidation system comprises a micro-oxidation module, an oxygen supply module, a conveying module, a circulation module and a sampling module, wherein the micro-oxidation module comprises an oxidation kettle and a catalytic layer filled with a ball ring filler, the oxygen supply module is used to monitor the oxygen concentration, and inject oxygen into the oxidation kettle according to a preset pressure, the conveying module is used to input and output the phosphate fire-resistant oil, the circulation module is used to quantitatively circulate the phosphate fire-resistant oil for multiple times for treatment, and the sampling module is used to sample and perform performance testing on the treated phosphate fire-resistant oil. The present invention enables the phosphate fire-resistant oil to fully contact with oxygen under the catalytic action of the ball ring filler through precise oxygen supply and stable reaction pressure, and performs repeated micro-oxidation treatment, so as to efficiently remove easily deteriorated components such as phenols in the phosphate fire-resistant oil, and improve the stability of the phosphate fire-resistant oil.

Description

Technical Field

[0001] The invention relates to the technical field of phosphate fire-resistant oil production, in particular to a phosphate fire-resistant oil micro-oxidation system and an oxidation monitoring method. Background Art

[0002] Phosphate ester fire-resistant oil is a fire-resistant hydraulic oil. With the rapid development of electric power, some large-scale thermal power plants, nuclear power plants, and large-capacity high-parameter steam turbine generator sets are also increasing. In order to meet the high-parameter requirements of the speed control systems of these units and avoid fire accidents caused by high-pressure oil leakage in the system, their speed control systems have generally adopted phosphate ester fire-resistant oil as hydraulic medium.

[0003] The main component of phosphate fire-resistant oil is triaryl phosphate, which is not easily oxidized. In the production process of phosphate fire-resistant oil, the prepared phosphate fire-resistant oil often also includes easily degradable components such as phenols. The presence of these easily degradable components may have a negative impact on the performance and stability of phosphate fire-resistant oil, such as causing oil quality deterioration, acid value increase, darker color, etc. At present, there is no established process for the treatment of easily degradable components in phosphate fire-resistant oil, so it is impossible to effectively improve the stability of phosphate fire-resistant oil during the production of phosphate fire-resistant oil. Summary of the invention

[0004] The object of the present invention is to provide a phosphate fire-resistant oil micro-oxidation system and an oxidation monitoring method to solve the problem of poor stability of phosphate fire-resistant oils prepared in the prior art due to the presence of easily degradable components such as phenols.

[0005] In order to achieve the above object, the present invention adopts the following technical solution:

[0006] The present invention discloses a phosphate fire-resistant oil micro-oxidation system, comprising:

[0007] A micro-oxidation module, the micro-oxidation module comprising an oxidation kettle and a catalytic layer arranged in the oxidation kettle, the catalytic layer is filled with a ball ring filler, and the phosphate fire-resistant oil is contacted with oxygen through the ball ring filler for micro-oxidation treatment;

[0008] An oxygen supply module, which is connected to the oxidation kettle and is used to monitor the oxygen concentration in the oxidation kettle and inject oxygen into the oxidation kettle at a preset pressure;

[0009] A conveying module, the conveying module is connected to the oxidation kettle, and is used to inject phosphate fire-resistant oil into the oxidation kettle, and output the phosphate fire-resistant oil after micro-oxidation treatment;

[0010] A circulation module, the circulation module is connected to the oxidation kettle and is used to quantitatively circulate the phosphate fire-resistant oil below the catalytic layer to the top of the catalytic layer multiple times;

[0011] A sampling module is connected to the oxidation kettle and is used to sample and test the phosphate fire-resistant oil after micro-oxidation treatment and upload the test results. The start and stop control of the sampling module and the circulation module are linked.

[0012] Optionally, the catalytic layer divides the internal space of the oxidation kettle into a fire-resistant oil collecting chamber and an exhaust gas collecting chamber from bottom to top;

[0013] The oxygen supply module, the transport module and the sampling module are all connected to the fire-resistant oil collection chamber;

[0014] An atomization module is arranged in the exhaust gas collection chamber, the circulation module connects the fire-resistant oil collection chamber and the atomization module, and the phosphate fire-resistant oil in the fire-resistant oil collection chamber is sprayed toward the catalytic layer through the circulation module and the atomization module.

[0015] Optionally, the atomization module includes a plurality of spray pipes parallel to the upper surface of the catalytic layer, and a plurality of atomization nozzles arranged on the spray pipes, the plurality of spray pipes are distributed side by side along the width direction of the catalytic layer, and the plurality of atomization nozzles on the spray pipes cover the area of ​​the catalytic layer in the length direction, wherein the spray pipes and the circulation module are docked.

[0016] Optionally, the oxygen supply module includes an oxygen storage tank, an oxygen pressure reducing valve, an oxygen concentration detection unit and a pressure transmitter, an oxygen supply pipeline is provided between the oxygen storage tank and the fire-resistant oil collecting chamber, and the oxygen pressure reducing valve is provided on the oxygen supply pipeline;

[0017] The oxygen concentration detection unit is arranged on the exhaust gas collecting chamber, and is used to detect the oxygen concentration in the exhaust gas collecting chamber and upload the detection result, and the oxygen concentration detection unit is linked to the opening and closing control of the oxygen pressure reducing valve;

[0018] The pressure transmitter is arranged on the oxygen supply pipeline, and is used for detecting the pressure inside the oxidation kettle and uploading the detection result. The pressure transmitter is linked to the pressure control of the oxygen pressure reducing valve.

[0019] Optionally, the phosphate ester fire-resistant oil micro-oxidation system also includes an exhaust gas treatment module, which includes an exhaust gas delivery pipe, and an exhaust solenoid valve and an activated carbon oil and gas adsorption box arranged on the exhaust gas delivery pipe, and one end of the exhaust gas delivery pipe is connected to the exhaust gas collecting chamber.

[0020] Optionally, the delivery module includes an oil inlet unit and an oil outlet unit;

[0021] The oil inlet unit comprises an oil inlet pipeline connected to the fire-resistant oil collecting chamber, and an oil inlet pump and a pump body inlet solenoid valve arranged on the oil inlet pipeline;

[0022] The oil discharge unit comprises an oil discharge pipeline communicated with the fire-resistant oil collecting chamber, and an oil discharge pump and a pump body outlet electromagnetic valve arranged on the oil discharge pipeline.

[0023] Optionally, a liquid level gauge is provided on the oxidation kettle, and a liquid level transmitter is provided on the liquid level gauge. The liquid level transmitter is used to detect the capacity of the phosphate anti-oil in the oxidation kettle and upload the detection result, and the liquid level transmitter is linked to the opening and closing control of the pump body inlet solenoid valve.

[0024] Optionally, the circulation module includes a circulation pipe, and a variable frequency circulation pump and a flow meter arranged on the circulation pipe, one end of the circulation pipe is connected to the fire-resistant oil collection chamber, and the other end of the circulation pipe is connected to the atomization module, the flow meter is used to detect the circulation flow of the phosphate fire-resistant oil and upload the detection result, and the start and close control of the flow meter and the variable frequency circulation pump are linked.

[0025] Optionally, the phosphate fire-resistant oil micro-oxidation system also includes a heating module, which includes a heater and a temperature transmitter arranged on the circulation pipeline, and the temperature transmitter is used to detect the temperature of the phosphate fire-resistant oil after heating and upload the detection result, and the temperature control of the temperature transmitter and the heater is linked.

[0026] The present invention also discloses an oxidation monitoring method, which uses the above-mentioned phosphate fire-resistant oil micro-oxidation system and comprises:

[0027] Prepare the phosphate ester fire-resistant oil and oxygen source to be treated;

[0028] In response to the input monitoring of the phosphate ester fire-resistant oil, the phosphate ester fire-resistant oil is injected into the chamber below the catalytic layer in the oxidation kettle through the delivery module, and the liquid level information of the phosphate ester fire-resistant oil in the oxidation kettle is obtained at the same time;

[0029] In response to the monitored liquid level information reaching a preset liquid level, the delivery module is controlled to close the injection of phosphate fire-resistant oil, and oxygen is injected into the chamber below the catalytic layer in the oxidation kettle through the oxygen supply module, and at the same time, oxygen concentration information in the chamber above the catalytic layer in the oxidation kettle is obtained;

[0030] In response to the monitored oxygen concentration information reaching a preset concentration, the circulation module is controlled to circulate the phosphate fire-resistant oil below the catalytic layer to above the catalytic layer, and evenly spray the catalytic layer, so that the phosphate fire-resistant oil is fully in contact with oxygen under the catalytic action of the ball ring packing for micro-oxidation treatment;

[0031] After the circulation module circulates the phosphate fire-resistant oil below the catalytic layer for a preset number of times, the circulation module is controlled to stop the circulation, and the sampling module is used to quantitatively sample the phosphate fire-resistant oil after micro-oxidation treatment in the oxidation kettle to detect the performance of the oil sample;

[0032] In response to the oil sample detection performance reaching the preset index, the phosphate anti-oil after micro-oxidation treatment in the oxidation kettle is discharged through the conveying module and filled into the finished product barrel; or in response to the oil sample detection performance not reaching the preset index, the circulation module is controlled to continue to circulate the phosphate anti-oil in the oxidation kettle for a preset number of times until the oil sample detection performance reaches the preset index.

[0033] Compared with the prior art, the phosphate fire-resistant oil micro-oxidation system and oxidation monitoring method provided by the embodiment of the present invention have the following beneficial effects:

[0034] By introducing the micro-oxidation process in the production process of fire-resistant oil, that is, monitoring the oxygen concentration in the oxidation kettle through the oxygen supply module, and injecting oxygen into the oxidation kettle according to the preset pressure, accurate oxygen concentration control can be achieved, thereby promoting the oxidation reaction during the micro-oxidation treatment of fire-resistant oil, improving the reaction rate and conversion rate, and shortening the production cycle. At the same time, the circulation module is used to quantitatively circulate the phosphate fire-resistant oil below the catalytic layer to the top of the catalytic layer for multiple times, and through the ball ring filler in the catalytic layer, the phosphate fire-resistant oil is fully contacted with oxygen under the catalytic action of the ball ring filler for micro-oxidation treatment, so as to remove phenols and other easily deteriorated components in the phosphate fire-resistant oil. Based on the characteristic that the phosphate fire-resistant oil itself is not easily oxidized, the stability of the phosphate fire-resistant oil is effectively improved. In addition, the sampling module is used to sample and test the phosphate fire-resistant oil after micro-oxidation treatment to ensure that the phosphate fire-resistant oil after micro-oxidation treatment reaches the ideal performance index and avoids excessive oxidation of the phosphate fire-resistant oil itself. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] The technical solution of the present invention will be further described in detail below with reference to the accompanying drawings and embodiments, in which:

[0036] Figure 1 A schematic block diagram of the connection structure of each module of the phosphate fire-resistant oil micro-oxidation system provided in an embodiment of the present invention;

[0037] Figure 2 A schematic block diagram of the overall structure of a phosphate fire-resistant oil micro-oxidation system provided in an embodiment of the present invention.

[0038] The reference numerals in the figures are:

[0039] 1. Micro-oxidation module; 11. Oxidation kettle; 111. Fire-resistant oil collection chamber; 112. Waste gas collection chamber; 113. Spray pipe; 114. Atomizing nozzle; 115. Liquid level meter; 116. Liquid level transmitter; 12. Catalytic layer; 2. Oxygen supply module; 21. Oxygen storage tank; 22. Oxygen pressure reducing valve; 23. Oxygen concentration detection unit; 24. Pressure transmitter; 3. Delivery module; 31. Oil inlet pipeline; 32. Oil inlet pump; 3 3. Pump body inlet solenoid valve; 34. Oil discharge pipeline; 35. Oil discharge pump; 36. Pump body outlet solenoid valve; 4. Circulation module; 41. Circulation pipeline; 42. Frequency conversion circulation pump; 43. Flow meter; 5. Sampling module; 6. Electrical control cabinet; 7. Waste gas treatment module; 71. Waste gas delivery pipeline; 72. Exhaust solenoid valve; 73. Activated carbon oil and gas adsorption box; 8. Heating module; 81. Heater; 82. Temperature transmitter. DETAILED DESCRIPTION

[0040] It should be noted that, in the absence of conflict, the embodiments and features in the embodiments of the present application can be combined with each other. Now, in conjunction with the accompanying drawings, the preferred embodiments of the present invention are described in detail.

[0041] The present invention discloses a phosphate fire-resistant oil micro-oxidation system, such as Figure 1 and Figure 2 As shown, it includes a micro-oxidation module 1, an oxygen supply module 2, a conveying module 3, a circulation module 4 and a sampling module 5. The micro-oxidation module 1 includes an oxidation kettle 11, and a catalytic layer 12 arranged in the oxidation kettle 11. The catalytic layer 12 is filled with ball ring fillers, which are used for the phosphate fire-resistant oil to be micro-oxidized through the ball ring fillers and oxygen contact. The oxygen supply module 2 is docked with the oxidation kettle 11 to monitor the oxygen concentration in the oxidation kettle 11 and inject oxygen into the oxidation kettle 11 according to a preset pressure. The conveying module 3 is docked with the oxidation kettle 11 to inject the phosphate fire-resistant oil into the oxidation kettle and output the phosphate fire-resistant oil after micro-oxidation treatment. The circulation module 4 is docked with the oxidation kettle 11 to circulate the phosphate fire-resistant oil below the catalytic layer 12 to the top of the catalytic layer 12 multiple times. The sampling module 5 is docked with the oxidation kettle 11 to sample and detect the phosphate fire-resistant oil after micro-oxidation treatment and upload the test results, and the start and stop control of the sampling module 5 and the circulation module 4 are linked.

[0042] Through the implementation method of the above-mentioned phosphate fire-resistant oil micro-oxidation system, by introducing the micro-oxidation process in the production process of fire-resistant oil, that is, first monitoring the oxygen concentration in the oxidation kettle 11 through the oxygen supply module 2, and injecting oxygen into the oxidation kettle 11 according to the preset pressure to achieve accurate oxygen control, thereby promoting the oxidation reaction during the micro-oxidation treatment of fire-resistant oil, improving the reaction rate and conversion rate, and shortening the production cycle. At the same time, the circulation module 4 is used to quantitatively circulate the phosphate fire-resistant oil below the catalytic layer 12 to the top of the catalytic layer 12 for multiple times, and through the ball ring filler in the catalytic layer 12, the phosphate fire-resistant oil is fully contacted with oxygen under the catalytic action of the ball ring filler for repeated micro-oxidation treatment, so as to efficiently remove the phenols and other easily deteriorated components in the phosphate fire-resistant oil, based on the characteristic that the phosphate fire-resistant oil itself is not easily oxidized, the stability of the phosphate fire-resistant oil is effectively improved. In addition, the sampling module 5 is used to sample and detect the phosphate fire-resistant oil after micro-oxidation treatment to ensure that the phosphate fire-resistant oil after micro-oxidation treatment reaches the ideal performance index and avoids the phosphate fire-resistant oil itself from being over-oxidized. Therefore, the phosphate ester fire-resistant oil micro-oxidation system according to the embodiment of the present invention can be applied to various industrial equipments that need to use phosphate ester fire-resistant oil to perform micro-oxidation treatment on phosphate ester fire-resistant oil.

[0043] Preferably, the ball ring filler adopts copper ball ring, which is usually made of copper and is a highly efficient filler. It is an improvement on the Raschig ring, a ring filler with many windows on the ring wall of the ordinary Raschig ring, one or two layers of windows on the side wall of the ring, and the blades of the windows are bent into the ring. Due to the opening of the ring wall, the distribution performance of gas and liquid is greatly improved compared with the Raschig ring, especially the inner surface area of ​​the ring can be fully utilized. At the same time, the active sites on its surface can promote the oxidation reaction, and make the phosphate fire-resistant oil move irregularly in the copper ball ring, so that the copper ball ring can not only expand the area of ​​contact with oxygen for the phosphate fire-resistant oil, but also play a role in catalyzing the oxidation of the phosphate fire-resistant oil and oxygen, thereby ensuring that the phosphate fire-resistant oil can be fully contacted with oxygen for micro-oxidation treatment under the catalytic action of the ball ring filler.

[0044] Furthermore, the catalytic layer 12 divides the internal space of the oxidation kettle 11 into a fire-resistant oil collection chamber 111 and an exhaust gas collection chamber 112 from bottom to top. The oxygen supply module 2, the conveying module 3 and the sampling module 5 are all connected to the fire-resistant oil collection chamber 111. An atomization module is provided in the exhaust gas collection chamber 112, and the circulation module 4 connects the fire-resistant oil collection chamber 111 and the atomization module, and the phosphate fire-resistant oil in the fire-resistant oil collection chamber 111 is sprayed to the catalytic layer 12 through the circulation module 4 and the atomization module.

[0045] According to the implementation method of the phosphate fire-resistant oil micro-oxidation system, the oxidation kettle 11 is a tank container, and the catalytic layer 12 is composed of a ball ring filler filled in a metal frame, and is fixed above the liquid level of the phosphate fire-resistant oil in the oxidation kettle 11, so that it divides the internal space of the oxidation kettle 11 into a fire-resistant oil collection chamber 111 and an exhaust gas collection chamber 112 from bottom to top, and the phosphate fire-resistant oil is injected into the fire-resistant oil collection chamber 111, and the exhaust gas generated during the micro-oxidation treatment of the phosphate fire-resistant oil is collected and discharged from the exhaust gas collection chamber 112, so as to avoid the mixing of the exhaust gas and the phosphate fire-resistant oil to affect the stability of the phosphate fire-resistant oil. In addition, the atomization module is used to enable the phosphate fire-resistant oil to be sprayed onto the ball ring filler of the catalytic layer 12 in the form of atomization, further expanding the contact area between the phosphate fire-resistant oil and the catalytic layer 12, thereby improving the efficiency of the phosphate fire-resistant oil in full contact with oxygen for micro-oxidation treatment under the catalytic action of the ball ring filler.

[0046] Furthermore, the atomization module includes a plurality of spray pipes 113 parallel to the upper surface of the catalyst layer 12, and a plurality of atomization nozzles 114 arranged on the spray pipes 113. The plurality of spray pipes 113 are arranged side by side along the width direction of the catalyst layer 12, and the plurality of atomization nozzles 114 on the spray pipes 113 cover the area of ​​the catalyst layer 12 in the length direction. The spray pipes 113 are connected to the circulation module 4.

[0047] Through the implementation of the above-mentioned phosphate fire-resistant oil micro-oxidation system, using a number of spray pipes 113 distributed side by side and a number of atomizing nozzles 114 covering the length direction area of ​​the catalyst layer 12, it is possible to ensure the uniformity of the distribution of the phosphate fire-resistant oil on the catalyst layer 12 when spraying, so that the phosphate fire-resistant oil can be fully contacted with the catalyst layer 12, increasing the contact opportunity between the phosphate fire-resistant oil and the ball ring filler, which is conducive to improving the efficiency of the phosphate fire-resistant oil in fully contacting with oxygen for micro-oxidation treatment under the catalytic action of the ball ring filler, and avoiding that some areas are not sprayed by the phosphate fire-resistant oil, thereby improving the treatment efficiency of the phosphate fire-resistant oil. At the same time, in the oxidation reaction, uniform spraying helps to evenly distribute heat on the catalyst layer 12, realize uniform heat exchange, thereby better controlling the reaction temperature, and improving the stability and safety of the phosphate fire-resistant oil micro-oxidation treatment. Preferably, the arrangement of a number of spray pipes 113 and a number of atomizing nozzles 114 can be adjusted according to actual needs, such as increasing or decreasing the number of spray pipes 113 and atomizing nozzles 114 to adapt to different treatment requirements and process conditions.

[0048] Furthermore, the oxygen supply module 2 includes an oxygen storage tank 21, an oxygen pressure reducing valve 22, an oxygen concentration detection unit 23 and a pressure transmitter 24. An oxygen supply pipeline is provided between the oxygen storage tank 21 and the fire-resistant oil collection chamber 111, and the oxygen pressure reducing valve 22 is provided on the oxygen supply pipeline. The oxygen concentration detection unit 23 is provided on the exhaust gas collection chamber 112, and is used to detect the oxygen concentration in the exhaust gas collection chamber 112 and upload the detection result, and the opening and closing control of the oxygen concentration detection unit 23 and the oxygen pressure reducing valve 22 are linked. The pressure transmitter 24 is provided on the oxygen supply pipeline, and is used to detect the pressure inside the oxidation kettle and upload the detection result, and the pressure transmitter 24 and the pressure control of the oxygen pressure reducing valve 22 are linked.

[0049] According to the implementation method of the phosphate fire-resistant oil micro-oxidation system, since the phosphate fire-resistant oil is initially injected into the fire-resistant oil collection chamber 111 of the oxidation kettle for storage, the circulation module 4 circulates the phosphate fire-resistant oil in the fire-resistant oil collection chamber 111 to a plurality of spray pipes 113, and a plurality of atomizing nozzles 114 evenly spray the fire-resistant oil on the ball ring packing in the catalyst layer 12 in the exhaust gas collection chamber 112. The oxygen concentration detection unit 23 is used to detect the oxygen concentration in the exhaust gas collection chamber 112 in real time, that is, to detect the oxygen concentration in the upper space of the oxidation kettle 11, and the detection result is uploaded to the equipped electrical control cabinet 6 for display, so as to accurately obtain whether the oxygen concentration in the entire oxidation kettle 11 is saturated. Then, the electrical control cabinet 6 automatically adjusts the opening of the oxygen pressure reducing valve 22 according to the set oxygen concentration value, accurately controls the oxygen flow entering the oxidation kettle, and ensures that the micro-oxidation treatment is fully carried out. At the same time, the pressure inside the oxidation kettle is detected in real time by the pressure transmitter 24, and the detection result is uploaded to the electrical control cabinet 6 for display, and then the electrical control cabinet 6 automatically adjusts the opening of the oxygen pressure reducing valve 22 according to the set pressure value to keep the pressure inside the oxidation kettle stable, thereby improving the safety and stability of the reaction. Then the phosphate fire-resistant oil micro-oxidation system of the embodiment of the present invention improves the efficiency of the oxidation reaction through accurate oxygen supply and stable reaction pressure, making the micro-oxidation treatment of the phosphate fire-resistant oil more thorough. In addition, the linkage control of the oxygen concentration detection unit 23 and the pressure transmitter 24 can timely discover and handle abnormal conditions, such as excessive or low oxygen concentration, abnormal pressure, etc., so that key parameters such as oxygen concentration and pressure can be monitored and recorded in real time, which is convenient for tracing and analyzing the processing process, improving the quality management level, and ensuring the safety of the reaction process. On this basis, the entire oxygen supply module 2 can realize intelligent control, without the need for manual frequent adjustment of oxygen supply and pressure, reducing the complexity and error of manual operation, and improving work efficiency.

[0050] Furthermore, the phosphate ester fire-resistant oil micro-oxidation system also includes an exhaust gas treatment module 7. The exhaust gas treatment module 7 includes an exhaust gas delivery pipeline 71, and an exhaust solenoid valve 72 and an activated carbon oil and gas adsorption box 73 arranged on the exhaust gas delivery pipeline 71, and one end of the exhaust gas delivery pipeline 71 is connected to the exhaust gas collection chamber 112.

[0051] Through the implementation of the above-mentioned phosphate fire-resistant oil micro-oxidation system, the waste gas generated in the waste gas collection chamber 112 during the micro-oxidation treatment of the phosphate fire-resistant oil is discharged in time by the waste gas delivery pipe 71, so as to avoid the mixing of the waste gas and the phosphate fire-resistant oil to affect the stability of the phosphate fire-resistant oil. At the same time, the activated carbon oil and gas adsorption box 73 can effectively adsorb and remove harmful components in the waste gas, such as oil mist and organic pollutants, thereby reducing the emission of pollutants in the waste gas, which helps to improve the air quality of the working environment. In addition, the waste gas treatment module 7 is also linked with the oxygen supply module 2. That is, when oxygen is injected into the oxidation kettle 11 through the oxygen storage tank 21, the exhaust solenoid valve 72 is automatically opened. With the injection of oxygen, the waste gas or excess gas in the waste gas collection chamber 112 is discharged through the waste gas delivery pipe 71, and when the oxygen concentration in the oxidation kettle 11 reaches the set concentration, the exhaust solenoid valve 72 is automatically closed to ensure that the oxygen concentration in the entire oxidation kettle 11 can fully carry out the micro-oxidation treatment.

[0052] Furthermore, the delivery module 3 includes an oil inlet unit and an oil discharge unit. The oil inlet unit includes an oil inlet pipeline 31 connected to the fire-resistant oil collection chamber 111, and an oil inlet pump 32 and a pump body inlet solenoid valve 33 arranged on the oil inlet pipeline 31. The oil discharge unit includes an oil discharge pipeline 34 connected to the fire-resistant oil collection chamber 111, and an oil discharge pump 35 and a pump body outlet solenoid valve 36 arranged on the oil discharge pipeline 34.

[0053] Through the implementation of the above-mentioned phosphate ester fire-resistant oil micro-oxidation system, the oil inlet pipeline 31 connects the oxidation kettle 11 and the upper-level processing system for the production of phosphate ester fire-resistant oil, and the oil discharge pipeline 34 connects the oxidation kettle 11 and the finished barrel. By utilizing the functions of the oil inlet pump 32 and the oil discharge pump 35, the flow rate of the phosphate ester fire-resistant oil can be accurately controlled to achieve accurate oil supply and oil discharge to the system to meet the process requirements. At the same time, the pump body inlet solenoid valve 33 and the pump body outlet solenoid valve 36 can effectively prevent the backflow and contamination of the phosphate ester fire-resistant oil, and ensure the quality and performance of the fire-resistant oil. The phosphate ester fire-resistant oil micro-oxidation system of the embodiment of the present invention can improve the oil supply efficiency of the fire-resistant oil and reduce the pressure fluctuation and energy loss in the system through the coordinated work of the oil inlet unit and the oil discharge unit. Preferably, the setting of the pump body inlet solenoid valve 33 and the pump body outlet solenoid valve 36 can be controlled by the electrical control cabinet 6 to cut off the oil circuit in time when the system fails or is abnormal, so as to avoid leakage of the fire-resistant oil and other safety problems.

[0054] Furthermore, the oxidation kettle 11 is provided with a level gauge 115, and the level gauge 115 is provided with a level transmitter 116. The level transmitter 116 is used to detect the capacity of the phosphate fire-resistant oil in the oxidation kettle and upload the detection result, and the level transmitter 116 is linked to the opening and closing control of the pump body inlet electromagnetic valve 33.

[0055] Through the implementation method of the above-mentioned phosphate ester fire-resistant oil micro-oxidation system, the liquid level meter 115 can reflect the capacity of the phosphate ester fire-resistant oil in the oxidation kettle in real time, so that the operator can observe it intuitively. And the liquid level information is obtained by the liquid level transmitter 116 and uploaded to the electrical control cabinet 6 for display. Through the linkage control with the pump body inlet solenoid valve 33, the oil intake of the fire-resistant oil can be accurately controlled to ensure that the liquid level in the oxidation kettle is kept within a suitable range, and to avoid excessive injection of the phosphate ester fire-resistant oil to cause oil spills. Among them, accurate liquid level control helps to optimize the reaction process, ensure that the ratio of oxygen to phosphate ester fire-resistant oil is appropriate, improve reaction efficiency and product quality, and when the liquid level is abnormal, the electrical control cabinet 6 can promptly issue an alarm to remind the operator to take measures to avoid failures or accidents.

[0056] Furthermore, the circulation module 4 includes a circulation pipeline 41, and a variable frequency circulation pump 42 and a flow meter 43 arranged on the circulation pipeline 41. One end of the circulation pipeline 41 is connected to the fire-resistant oil collection chamber 111, and the other end of the circulation pipeline 41 is connected to the atomization module. The flow meter 43 is used to detect the circulation flow of the phosphate fire-resistant oil and upload the detection result, and the flow meter 43 and the variable frequency circulation pump 42 are linked to the on-off control.

[0057] Through the implementation of the above-mentioned phosphate ester fire-resistant oil micro-oxidation system, the circulation flow of the phosphate ester fire-resistant oil can be detected in real time by using the flow meter 43, and the detection result can be uploaded to the electrical control cabinet 6 for display. The electrical control cabinet 6 can automatically adjust the opening and closing of the variable frequency circulation pump 42 according to the set value or process requirements, accurately control the circulation flow of the fire-resistant oil, ensure the normal operation of the system, and the stable flow control helps to reduce the impact and wear on the equipment and extend the service life of the equipment. When the flow is abnormal, the electrical control cabinet 6 can issue an alarm in time to remind the operator to take measures to avoid failures or accidents.

[0058] Furthermore, the phosphate fire-resistant oil micro-oxidation system also includes a heating module 8. The heating module 8 includes a heater 81 and a temperature transmitter 82 arranged on the circulation pipe 41. The temperature transmitter 82 is used to detect the temperature of the phosphate fire-resistant oil after heating and upload the detection result, and the temperature transmitter 82 and the temperature control of the heater 81 are linked.

[0059] Through the implementation of the above-mentioned phosphate fire-resistant oil micro-oxidation system, the temperature of the phosphate fire-resistant oil after heating can be detected in real time by using the temperature transmitter 82, and the detection result can be uploaded to the electrical control cabinet 6 for display. The electrical control cabinet 6 can automatically adjust the power of the heater 81 according to the set value or process requirements, accurately control the temperature of the fire-resistant oil, and ensure the normal operation of the system. Through the heating effect of the heater 81, the phosphate fire-resistant oil can be quickly heated during the circulation process to increase the chemical reaction activity of the phosphate fire-resistant oil, promote the phosphate fire-resistant oil to fully contact with oxygen under the catalytic action of the ball ring filler for micro-oxidation treatment, and help remove phenols and other easily deteriorated components in the phosphate fire-resistant oil. At the same time, the appropriate temperature can reduce the viscosity of the phosphate fire-resistant oil, improve its fluidity, make it easier to circulate and process in the system, and ensure good heat transfer and mass transfer effects. And the heating rate can be adjusted as needed, the heating efficiency is improved, and the heating time is reduced.

[0060] Furthermore, the sampling module 5 preferably includes a sampling pipeline, a sampling valve, a filtering device and a detection instrument. The sampling pipeline connects the oxidation kettle 11 and the detection instrument, and is used to transport the sampled phosphate fire-resistant oil. The sampling valve is installed on the sampling pipeline, and is used to control the opening and closing of the sampling process so as to take out the phosphate fire-resistant oil sample from the oxidation kettle 11. The filtering device can be located in the sampling pipeline, and is used to remove impurities and particulate matter in the sample to ensure the purity of the sample. The detection instrument is used to perform performance analysis and detection on the collected phosphate fire-resistant oil sample, such as a chemical analysis instrument, a chromatograph, etc., and upload the test results to the equipped electrical control cabinet 6 for display.

[0061] The present invention also discloses an oxidation monitoring method, which uses the above-mentioned phosphate fire-resistant oil micro-oxidation system and comprises:

[0062] Prepare the phosphate ester fire-resistant oil and oxygen source to be treated;

[0063] In response to the input monitoring of the phosphate ester fire-resistant oil, the phosphate ester fire-resistant oil is injected into the chamber below the catalytic layer 12 in the oxidation kettle 11 through the delivery module 3, and the liquid level information of the phosphate ester fire-resistant oil in the oxidation kettle 11 is obtained at the same time;

[0064] In response to the monitored liquid level information reaching a preset liquid level, the delivery module 3 is controlled to close the injection of the phosphate fire-resistant oil, and oxygen is injected into the chamber below the catalytic layer 12 in the oxidation kettle 11 through the oxygen supply module 2, and at the same time, the oxygen concentration information in the chamber above the catalytic layer 12 in the oxidation kettle 11 is obtained;

[0065] In response to the monitored oxygen concentration information reaching a preset concentration, the control circulation module 4 circulates the phosphate fire-resistant oil below the catalyst layer 12 to the top of the catalyst layer 12, and evenly sprays the catalyst layer 12, so that the phosphate fire-resistant oil is fully in contact with oxygen under the catalytic action of the ball ring packing for micro-oxidation treatment;

[0066] After the circulation module 4 circulates the phosphate fire-resistant oil below the catalytic layer 12 for a preset number of times, the circulation module 4 is controlled to stop the circulation, and the sampling module 5 quantitatively samples the phosphate fire-resistant oil after micro-oxidation treatment in the oxidation kettle 11 to detect the performance of the oil sample;

[0067] In response to the oil sample detection performance reaching the preset index, the phosphate anti-oil after micro-oxidation treatment in the oxidation kettle 11 is discharged through the conveying module 3 and filled into the finished product barrel; or in response to the oil sample detection performance not reaching the preset index, the control circulation module 4 continues to circulate the phosphate anti-oil in the oxidation kettle for a preset number of times until the oil sample detection performance reaches the preset index.

[0068] Through the implementation of the above oxidation monitoring method, the phosphate ester fire-resistant oil to be slightly oxidized is injected into the fire-resistant oil collection chamber 111 of the oxidation kettle 11 through the oil inlet pump 32 and the pump body inlet solenoid valve 33. The amount of oil injected can be directly observed through the liquid level meter 115, and can also be displayed on the electrical control cabinet 6 through the liquid level transmitter 116. When the oxygen concentration detection unit 23 detects that the oxygen concentration in the exhaust gas collection chamber 112 of the oxidation kettle 11 is lower than the set value, the exhaust solenoid valve 72 automatically opens, and the oxygen in the oxygen storage tank 21 enters the oxidation kettle 11 through the oxygen pressure reducing valve 22. When the set oxygen concentration is reached, the exhaust solenoid valve 72 automatically closes, and the variable frequency circulation pump 42 is started to circulate the phosphate ester fire-resistant oil in the fire-resistant oil collection chamber 111. At the same time, the heater 81 heats the phosphate ester fire-resistant oil (finally to 80℃±2), and the operation of the heater 81 is controlled by the temperature transmitter 82 to maintain the temperature of the phosphate ester fire-resistant oil. The phosphate fire-resistant oil is pumped into the spray pipe 113 through the variable frequency circulation pump 42, and is evenly sprayed onto the ball ring filler in the catalytic layer 12 by the atomizing nozzle 114. The phosphate fire-resistant oil is fully contacted with oxygen under the catalytic action of the ball ring filler for micro-oxidation. After multiple cycles, when the oxygen concentration in the exhaust gas collection chamber 112 of the oxidation kettle 11 decreases, the exhaust solenoid valve 72 automatically opens, and the exhaust gas in the exhaust gas collection chamber 112 enters the activated carbon oil and gas adsorption box 73 through the exhaust solenoid valve 72 for adsorption treatment to remove harmful exhaust gas and then discharge it into the atmosphere. When sampling is performed through the sampling module 5 and it is detected that the performance index of the phosphate fire-resistant oil after micro-oxidation reaches the ideal effect, the micro-oxidation work is completed, and the phosphate fire-resistant oil in the oxidation kettle 11 is filled into the finished barrel through the oil discharge pump 35 and the pump body outlet solenoid valve 36.

[0069] The phosphate fire-resistant oil micro-oxidation system and oxidation monitoring method provided in the embodiments of the present invention efficiently remove easily deteriorated components such as phenols in the phosphate fire-resistant oil by introducing a micro-oxidation process in the production process of the fire-resistant oil, thereby effectively improving the stability of the phosphate fire-resistant oil and avoiding excessive oxidation of the phosphate fire-resistant oil itself.

[0070] It should be understood that the above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit it. For those skilled in the art, the technical solutions described in the above embodiments can be modified, or some of the technical features therein can be replaced by equivalents; and all these modifications and replacements should fall within the scope of protection of the claims attached to the present invention.

Claims

1. A phosphate ester fire-resistant oil micro-oxidation system, characterized in that: The phosphate ester fire-resistant oil micro-oxidation system comprises: A micro-oxidation module, the micro-oxidation module comprises an oxidation kettle and a catalytic layer arranged in the oxidation kettle, the catalytic layer is filled with ball ring fillers, and the phosphate fire-resistant oil is contacted with oxygen through the ball ring fillers for micro-oxidation treatment, and the catalytic layer divides the internal space of the oxidation kettle into a fire-resistant oil collection chamber and an exhaust gas collection chamber from bottom to top; An oxygen supply module, which is connected to the oxidation kettle and is used to monitor the oxygen concentration in the oxidation kettle and inject oxygen into the oxidation kettle at a preset pressure, and includes an oxygen storage tank, an oxygen pressure reducing valve and an oxygen concentration detection unit. An oxygen supply pipeline is provided between the oxygen storage tank and the fire-resistant oil collection chamber. The oxygen pressure reducing valve is provided on the oxygen supply pipeline. The oxygen concentration detection unit is provided on the exhaust gas collection chamber and is used to detect the oxygen concentration in the exhaust gas collection chamber and upload the detection result. The oxygen concentration detection unit and the oxygen pressure reducing valve are controlled in conjunction with each other for opening and closing; A conveying module, the conveying module is connected to the oxidation kettle, and is used to inject phosphate fire-resistant oil into the oxidation kettle, and output the phosphate fire-resistant oil after micro-oxidation treatment; A circulation module, the circulation module is connected to the oxidation kettle and is used to quantitatively circulate the phosphate fire-resistant oil below the catalytic layer to the top of the catalytic layer multiple times; A sampling module, which is connected to the oxidation kettle and is used to sample and test the phosphate fire-resistant oil after micro-oxidation treatment and upload the test results, and the start and stop control of the sampling module and the circulation module are linked; The oxygen supply module, the transport module and the sampling module are all connected to the fire-resistant oil collection chamber; The exhaust gas treatment module is controlled in linkage with the oxygen supply module, and comprises an exhaust gas delivery pipeline and an exhaust solenoid valve arranged on the exhaust gas delivery pipeline. One end of the exhaust gas delivery pipeline is connected to the exhaust gas collecting chamber.

2. The phosphate ester fire-resistant oil micro-oxidation system according to claim 1, characterized in that: An atomization module is arranged in the exhaust gas collection chamber, the circulation module connects the fire-resistant oil collection chamber and the atomization module, and the phosphate fire-resistant oil in the fire-resistant oil collection chamber is sprayed toward the catalytic layer through the circulation module and the atomization module.

3. The phosphate ester fire-resistant oil micro-oxidation system according to claim 2, characterized in that: The atomization module includes a plurality of spray pipes parallel to the upper surface of the catalyst layer, and a plurality of atomization nozzles arranged on the spray pipes, wherein the plurality of spray pipes are distributed side by side along the width direction of the catalyst layer, and the plurality of atomization nozzles on the spray pipes cover the area of ​​the catalyst layer in the length direction, wherein the spray pipes are connected to the circulation module.

4. The phosphate ester fire-resistant oil micro-oxidation system according to claim 2, characterized in that: The oxygen supply module includes a pressure transmitter, which is arranged on the oxygen supply pipeline and is used to detect the pressure inside the oxidation kettle and upload the detection result. The pressure transmitter is linked to the pressure control of the oxygen pressure reducing valve.

5. The phosphate fire-resistant oil micro-oxidation system according to any one of claims 2 to 4, characterized in that: The exhaust gas treatment module includes an activated carbon oil and gas adsorption box arranged on the exhaust gas delivery pipeline.

6. The phosphate ester fire-resistant oil micro-oxidation system according to claim 2, characterized in that: The delivery module includes an oil inlet unit and an oil discharge unit; The oil inlet unit comprises an oil inlet pipeline connected to the fire-resistant oil collecting chamber, and an oil inlet pump and a pump body inlet solenoid valve arranged on the oil inlet pipeline; The oil discharge unit comprises an oil discharge pipeline communicated with the fire-resistant oil collecting chamber, and an oil discharge pump and a pump body outlet electromagnetic valve arranged on the oil discharge pipeline.

7. The phosphate ester fire-resistant oil micro-oxidation system according to claim 6, characterized in that: The oxidation kettle is provided with a liquid level meter, and the liquid level meter is provided with a liquid level transmitter. The liquid level transmitter is used to detect the capacity of the phosphate anti-oil in the oxidation kettle and upload the detection result, and the liquid level transmitter is linked to the opening and closing control of the pump body inlet solenoid valve.

8. The phosphate ester fire-resistant oil micro-oxidation system according to claim 2, characterized in that: The circulation module includes a circulation pipeline, and a variable frequency circulation pump and a flow meter arranged on the circulation pipeline. One end of the circulation pipeline is connected to the fire-resistant oil collection chamber, and the other end of the circulation pipeline is connected to the atomization module. The flow meter is used to detect the circulation flow of phosphate fire-resistant oil and upload the detection result, and the flow meter and the variable frequency circulation pump are linked in start and stop control.

9. The phosphate ester fire-resistant oil micro-oxidation system according to claim 8, characterized in that: The phosphate fire-resistant oil micro-oxidation system also includes a heating module, which includes a heater and a temperature transmitter arranged on the circulation pipeline. The temperature transmitter is used to detect the temperature of the phosphate fire-resistant oil after heating and upload the detection result, and the temperature transmitter and the temperature control of the heater are linked.

10. An oxidation monitoring method, using the phosphate fire-resistant oil micro-oxidation system according to any one of claims 1 to 9, characterized in that: The oxidation monitoring method comprises: Prepare the phosphate ester fire-resistant oil and oxygen source to be treated; In response to the input monitoring of the phosphate ester fire-resistant oil, the phosphate ester fire-resistant oil is injected into the chamber below the catalytic layer in the oxidation kettle through the delivery module, and the liquid level information of the phosphate ester fire-resistant oil in the oxidation kettle is obtained at the same time; In response to the monitored liquid level information reaching a preset liquid level, the delivery module is controlled to close the injection of phosphate fire-resistant oil, and oxygen is injected into the chamber below the catalytic layer in the oxidation kettle through the oxygen supply module, and at the same time, oxygen concentration information in the chamber above the catalytic layer in the oxidation kettle is obtained; In response to the monitored oxygen concentration information reaching a preset concentration, the circulation module is controlled to circulate the phosphate fire-resistant oil below the catalytic layer to above the catalytic layer, and evenly spray the catalytic layer, so that the phosphate fire-resistant oil is fully in contact with oxygen under the catalytic action of the ball ring packing for micro-oxidation treatment; After the circulation module circulates the phosphate fire-resistant oil below the catalytic layer for a preset number of times, the circulation module is controlled to stop the circulation, and the sampling module is used to quantitatively sample the phosphate fire-resistant oil after micro-oxidation treatment in the oxidation kettle to detect the performance of the oil sample; In response to the oil sample detection performance reaching the preset index, the phosphate anti-oil after micro-oxidation treatment in the oxidation kettle is discharged through the conveying module and filled into the finished product barrel; or in response to the oil sample detection performance not reaching the preset index, the circulation module is controlled to continue to circulate the phosphate anti-oil in the oxidation kettle for a preset number of times until the oil sample detection performance reaches the preset index.

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