A system and method for detecting the oxidative stability of phosphate ester fire-resistant oil

Abstract

This invention provides a system and method for detecting the oxidation stability of phosphate ester fire-resistant oil. The system includes a pressure vessel cavity for holding a sample bottle containing phosphate ester fire-resistant oil. The pressure vessel cavity is housed within a constant-temperature heating device. The sample bottle is placed into the pressure vessel cavity through a first opening, which is sealed by a sealing ring and a pressure vessel top cover. A second opening of the pressure vessel cavity is connected to an oxygen injection device via a pipe. A pressure sensor is installed within the pressure vessel cavity. A third opening of the pressure vessel cavity is open to the atmosphere. The constant-temperature heating device, pressure sensor, oxygen injection device, and single-arm composite robot are all connected to a detection and control system. This system can accurately detect the oxidation stability of phosphate ester fire-resistant oil without requiring any chemical reagents, offering advantages such as environmental friendliness, increased efficiency, and labor savings.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of chemical analysis, and particularly relates to a system and method for detecting oxidation stability of phosphate ester fire-resistant oil. BACKGROUND

[0002] The phosphate ester fire-resistant oil (hereinafter referred to as fire-resistant oil) for power plants is mainly deteriorated due to oxidation reaction in the use process, and the generated deterioration products can cause the poor oxidation resistance, further accelerate the deterioration speed of the oil product, increase the acid value of the oil product, reduce the resistivity, generate sludge, reduce the flexibility of the turbine part sleeve action, cause the corrosion and jam of the servo valve of the speed regulation system, and even cause the abnormal shutdown accident of the unit. Therefore, the oxidation stability of the new oil and the running oil needs to be closely monitored to master the change trend of the oxidation resistance of the oil product, and when the oxidation resistance of the running oil is obviously reduced, appropriate measures are taken to ensure the safe operation of the unit.

[0003] The new fire-resistant oil oxidation stability detection method adopts EN 14832:2005 Petroleum and related products-Determination of oxidation stability and corrosivity of phosphate ester fire-resistant oils, and DL / T 1654-2016 is equivalent to EN 14832. The method is to continuously pass in oxygen for 164h under heating to cause the oxidation reaction of the oil product, the detection period is long, the cost is high, the flow of the oxygen participating in the reaction will fluctuate or have a large deviation in the test process, the result deviates, and in addition, the high-pressure steel cylinder needs to be used for a long time, and there is a safety hazard.

[0004] There is no test method for the oxidation stability of the running fire-resistant oil at present, and the oil product will be deteriorated in the operation process of the unit, small molecule acids are generated in the deterioration process, if the oxidation stability is detected by using the EN 14832 method, the gas will carry the small molecule acids from the oil into the absorption tube in the detection process, if the water in the absorption tube cannot absorb all the small molecule acids in time, part of the small molecule acids will be discharged into the atmosphere, which reduces the acceleration effect of the small molecule acids on the oxidation on one hand, and directly reduces the total acid value tested after the oxidation on the other hand. Directly and indirectly, the oxidation stability result deviates from the actual situation.

[0005] Therefore, it is necessary to develop a system capable of detecting the oxidation stability of the new fire-resistant oil and the running fire-resistant oil. SUMMARY

[0006] In order to solve the problems in the prior art, the application provides a system and method for detecting the oxidation stability of the phosphate ester fire-resistant oil, which can accurately detect the oxidation stability of the phosphate ester fire-resistant oil, does not need any chemical reagent, and has the effects of environmental protection, efficiency improvement and labor saving.

[0007] In order to achieve the above object, the present application provides the following technical scheme: a system for detecting the oxidation stability of phosphate ester fire-resistant oil, comprising a pressure container cavity for placing a sample bottle containing phosphate ester fire-resistant oil, the pressure container cavity being arranged in a constant temperature heating device, the sample bottle being placed in the pressure container cavity through a first opening of the pressure container cavity, the first opening of the pressure container cavity being sealed by a sealing ring and a pressure container top cover, a second opening of the pressure container cavity being communicated with an oxygen injection device through a pipeline, a pressure sensor being arranged in the pressure container cavity, and a third opening of the pressure container cavity being communicated with the atmosphere;

[0008] The constant temperature heating device, the pressure sensor, the oxygen injection device and the single-arm composite robot are connected with a detection control system, which is used for controlling the single-arm composite robot to place or take out the sample bottle from the pressure container cavity, controlling the opening and closing of the oxygen injection device according to the pressure detected by the pressure sensor, controlling the constant temperature heating device to heat the pressure container cavity, and obtaining the time required for the pressure in the pressure container cavity to drop to a set pressure value when the oxidation stability is determined, which represents the oxidation stability of the phosphate ester fire-resistant oil.

[0009] Further, when the oxidation stability test is performed, the water content of the phosphate ester fire-resistant oil in the sample bottle is not more than 600 mg / L, the addition amount is 2 g to 10 g, the heating range of the constant temperature heating device is 150 DEG C to 200 DEG C, and the pressure range in the pressure container cavity 9 is 300 kPa to 600 kPa.

[0010] Further, the constant temperature heating device comprises a constant temperature control system, a temperature sensor and a metal bath heating device, the detection control system is connected with the constant temperature control system, the temperature sensor and the metal bath heating device, is used for obtaining the temperature in the pressure container cavity through the temperature sensor, and controlling the temperature of the metal bath heating device to be constant through the constant temperature control system.

[0011] Further, the oxygen injection device comprises an electromagnetic control valve, an oxygen source and a one-way electromagnetic control valve, the oxygen source is communicated with the second opening of the pressure container cavity through a pipeline, the electromagnetic control valve is arranged on the pipeline, the one-way electromagnetic control valve is arranged at the third opening of the pressure container cavity, the detection control system is connected with the electromagnetic control valve and is used for controlling the opening and closing of the oxygen source, and the detection control system is connected with the one-way electromagnetic control valve and is used for controlling the opening and closing of the third opening to discharge the oxygen in the pressure container cavity.

[0012] Further, the detection control system is connected with the single-arm composite robot and is used for controlling the single-arm composite robot to place or remove the sealing ring and the pressure container top cover for the first opening of the pressure container cavity, so as to realize the sealing or opening of the first opening of the pressure container cavity.

[0013] Further, the rotating function end of the single-arm composite robot is a hexagonal column, the middle of the upper part of the pressure container top cover is an inner hexagonal column, the size of which is suitable for the hexagonal column of the single-arm composite robot end to achieve the grasping and fastening of the pressure container top cover.

[0014] Further, the grasping outer diameter of the single-arm composite robot clamping end is 0.5cm-6cm, the clamping end is used to clamp the sealing ring in the sealing ring placement from the sealing ring placement 11 to the first opening of the pressure container cavity or clamp the sealing ring at the first opening of the pressure container cavity to the sealing ring placement; the clamping end is used to clamp the sample bottle in the sample placement to the pressure container cavity or clamp the sample bottle in the pressure container cavity to the waste oil cup recovery.

[0015] The application also provides a method for detecting the oxidation stability of phosphate ester fire-resistant oil by using the above system, and the specific steps are as follows:

[0016] S1, the detection control system controls the single-arm composite robot to clamp the sample bottle containing the phosphate ester fire-resistant oil in the pressure container cavity, and closes the first outlet of the pressure container cavity;

[0017] S2, the third opening of the pressure container cavity is opened, the detection control system controls the oxygen injection device to open and inject oxygen into the pressure container cavity to discharge the air in the pressure container cavity;

[0018] S3, the third opening of the pressure container cavity is closed, the detection control system controls the oxygen injection device to open and inject oxygen into the pressure container cavity, when the pressure sensor detects that the pressure reaches the set value, the feedback is fed back to the detection control system, and the detection control system controls the oxygen injection device to close;

[0019] S4, the detection control system controls the constant temperature heating device to heat the pressure container cavity to the set temperature, and the pressure sensor detects the pressure data in the pressure container cavity, when the pressure sensor detects that the pressure in the pressure container cavity decreases to the set pressure value, the detection control system records the required time, and the time represents the oxidation stability of the phosphate ester fire-resistant oil.

[0020] Further, in S1, when the first outlet of the pressure container cavity is closed, the detection control system controls the single-arm composite robot to clamp the sealing ring at the first opening position of the pressure container cavity and fasten the pressure container top cover at the first opening of the pressure container cavity.

[0021] Further, a one-way electromagnetic control valve is arranged at the third opening of the pressure container cavity, and the detection control system is connected with the one-way electromagnetic control valve to realize the opening and closing of the third opening by controlling the one-way electromagnetic control valve.

[0022] Compared with the prior art, the application has at least the following beneficial effects:

[0023] The system for detecting the oxidation stability of phosphate ester fire-resistant oil provided by the application can continuously test the oxidation stability without waiting for the sample to cool down, and the sample bottle is placed into the pressure container cavity by the single-arm composite robot, which avoids errors caused by manual operation and improves the accuracy and repeatability of the test. The constant-temperature heating device can accurately control the heating temperature, ensuring that the test process is carried out under constant temperature conditions, and further improving the accuracy of the test. At the same time, the pressure sensor can monitor the pressure change in the pressure container cavity in real time, ensuring accurate control of the oxygen injection amount. The injection of oxygen and the monitoring of pressure are accurately controlled by the pressure sensor and the detection control system, which reduces the operation risk and improves the safety of the test process. The detection control system has the functions of automatically recording data and automatically storing data, which can conveniently save and check the test results, providing convenience for the monitoring and evaluation of oil quality.

[0024] When the system is used for detection, the weighed sample is placed into the pressure container by the single-arm composite robot, oxygen is filled to a set pressure, the constant-temperature heating device is started to heat to a certain temperature, and the detection control system starts timing while heating. The pressure of the pressure container is continuously recorded during the period until the pressure value in the pressure container cavity decreases by a fixed value from the highest pressure, and the timing is stopped. The recorded time is used as the basis for evaluating the oxidation resistance of the oil. The system can accurately check the oxidation stability of phosphate ester fire-resistant oil, and has the effects of fast speed, environmental protection, high efficiency and labor saving.

[0025] The system for detecting the oxidation stability of phosphate ester fire-resistant oil provided by the application can continuously test the oxidation stability without waiting for the sample to cool down, and the sample bottle is placed into the pressure container cavity by the single-arm composite robot, which avoids errors caused by manual operation and improves the accuracy and repeatability of the test. The constant-temperature heating device can accurately control the heating temperature, ensuring that the test process is carried out under constant temperature conditions, and further improving the accuracy of the test. At the same time, the pressure sensor can monitor the pressure change in the pressure container cavity in real time, ensuring accurate control of the oxygen injection amount. The injection of oxygen and the monitoring of pressure are accurately controlled by the pressure sensor and the detection control system, which reduces the operation risk and improves the safety of the test process. The detection control system has the functions of automatically recording data and automatically storing data, which can conveniently save and check the test results, providing convenience for the monitoring and evaluation of oil quality.

[0026] When the system is used for detection, the weighed sample is placed into the pressure container by the single-arm composite robot, oxygen is filled to a set pressure, the constant-temperature heating device is started to heat to a certain temperature, and the detection control system starts timing while heating. The pressure of the pressure container is continuously recorded during the period until the pressure value in the pressure container cavity decreases by a fixed value from the highest pressure, and the timing is stopped. The recorded time is used as the basis for evaluating the oxidation resistance of the oil. The system can accurately check the oxidation stability of phosphate ester fire-resistant oil, and has the effects of fast speed, environmental protection, high efficiency and labor saving. BRIEF DESCRIPTION OF DRAWINGS

[0027] Figure 1 is a schematic view of a system for detecting the oxidation stability of phosphate ester fire-resistant oil;

[0028] Among them, 1 is the detection and control system, 2 is the constant temperature control system, 3 is the temperature sensor, 4 is the metal bath heating device, 5 is the pressure sensor, 6 is the electromagnetic control valve, 7 is the oxygen source, 8 is the one-way electromagnetic control valve, 9 is the pressure vessel cavity, 10 is the single-arm composite robot, 11 is the sealing ring placement area, 12 is the pressure vessel top cover placement area, 13 is the waste oil cup recycling area, and 14 is the sample placement area. Detailed Implementation

[0029] The present invention will be further described below with reference to the accompanying drawings and specific embodiments.

[0030] like Figure 1 As shown, this invention provides a system for detecting the oxidation stability of phosphate ester fire-resistant oil, comprising: a detection and control system 1, a constant temperature control system 2, a temperature sensor 3, a metal bath heating device 4, a pressure sensor 5, an electromagnetic control valve 6, an oxygen source 7, a one-way electromagnetic control valve 8, a pressure vessel chamber 9, a single-arm composite robot 10, a sealing ring placement area 11, a pressure vessel top cover placement area 12, a waste oil cup recycling area 13, and a sample placement area 14, wherein: the sample placement area 14 is numbered for placing sample bottles containing phosphate ester fire-resistant oil according to the number; the sample bottles containing phosphate ester fire-resistant oil are placed in the pressure vessel chamber. The oxidation reaction takes place in pressure vessel cavity 9. Pressure vessel cavity 9 is set in metal bath heating device 4. Metal bath heating device 4 is connected to temperature sensor 3 and constant temperature control system 2 to control the temperature in pressure vessel cavity 9 to be constant. The first opening of pressure vessel cavity 9 is set at the top. The first opening of pressure vessel cavity 9 is sealed by setting pressure vessel top cover and sealing ring. The second opening of pressure vessel cavity 9 is connected to oxygen source 7 through pipeline. Electromagnetic control valve 6 is set on pipeline to control the on and off of oxygen source 7. A one-way electromagnetic control valve 8 is set at the third opening of pressure vessel cavity 9 to discharge oxygen in pressure vessel cavity 9.

[0031] A pressure sensor 5 is installed in the pressure vessel cavity 9 to detect the pressure data in the pressure vessel cavity 9;

[0032] The constant temperature control system 2, temperature sensor 3, metal bath heating device 4, pressure sensor 5, and electromagnetic control valve 6 are all connected to the detection and control system 1. The detection and control system 1 obtains the temperature in the pressure vessel cavity 9 through the temperature sensor 3 and controls the temperature of the metal bath heating device 4 to be constant through the constant temperature control system 2. The detection and control system 1 obtains the pressure data in the pressure vessel cavity 9 through the pressure sensor 5 and controls the opening and closing of the electromagnetic control valve 6 and the one-way electromagnetic control valve 8 to achieve the purpose of introducing oxygen into the pressure vessel cavity 9.

[0033] The single-arm compound robot 10 is connected with the detection control system 1, the detection control system 1 controls the single-arm compound robot 10 to transfer the sample bottle in the sample placement position 14 to the pressure container cavity 9, and controls the single-arm compound robot 10 to place the sealing ring on the first opening of the pressure container cavity 9, and then tightens the pressure container top cover, so that the pressure container cavity 9 is sealed.

[0034] The specific steps of the system for detecting the oxidation stability of phosphate ester fire-resistant oil according to the present application are as follows:

[0035] Step 1, the water content of the phosphate ester fire-resistant oil is regulated to be not more than 600 mg / L, and the phosphate ester fire-resistant oil is new phosphate ester fire-resistant oil or running phosphate ester fire-resistant oil;

[0036] Step 2, a set amount of phosphate ester fire-resistant oil is weighed and placed in a sample bottle, the sample bottle is placed in the pressure container cavity 9, the single-arm compound robot 10 places a sealing ring on the first opening of the pressure container cavity 9, the single-arm compound robot 10 places the pressure container top cover on the sealing ring and tightens the pressure container top cover, so that the pressure container cavity 9 is sealed;

[0037] Step 3, under room temperature conditions, the electromagnetic control valve 6 is opened to introduce oxygen into the pressure container cavity 9, when the pressure sensor 5 detects that the pressure in the pressure container cavity 9 reaches 300 kPa, the electromagnetic control valve 6 is closed, the one-way electromagnetic control valve 8 is opened, and the gas in the pressure container 9 is discharged, which is repeated three times, after the residual air in the pressure container cavity is discharged, the oxygen pressure in the pressure container 9 reaches a certain fixed value in 300 kPa-600 kPa, the electromagnetic control valve 6 is closed to stop the introduction of oxygen, and the pressure value of the pressure container cavity 9 is detected, and it is considered to reach the set pressure within a deviation of ±0.05 kPa;

[0038] Step 4, the constant temperature control system 2 controls the metal bath heating device 4 to heat the pressure container cavity 9, and keeps the temperature constant at a certain fixed value in 150℃-200℃, the temperature of the pressure container cavity 9 is detected, and it is considered to reach the set temperature within a deviation of ±0.5℃. At this time, the phosphate ester fire-resistant oil and oxygen react;

[0039] Step 5, from the start of heating, the pressure sensor 5 detects the pressure of the pressure container cavity 9, and timing is performed, when the pressure sensor 5 detects that the oxygen pressure in the pressure container cavity 9 drops to a certain percentage of the highest pressure, the time is recorded, and the time value represents the oxidation stability of the phosphate ester fire-resistant oil;

[0040] Wherein, the reaction rate v = kc, if the reactant concentration c is the same at the same temperature, the rate constant k is constant for a particular substance. For different phosphate ester fire-resistant oils, the value of k is different, the reaction rate v is different, the method limits the same temperature and reactant concentration, and the oxidation rate of the oil sample is characterized by the rate of reactant content reduction, and then the oxidation stability of the oil sample is characterized.

[0041] The value of k is related to the reaction temperature, the higher the temperature, the larger the value of k, the faster the reaction speed, and the shorter the time to distinguish the oxidation stability difference of the oil sample. However, if the temperature is too high, the oil sample will carbonize and stick to the test equipment, making it difficult to clean. Therefore, the test is conducted at 180℃, and the reaction time required by the phosphate ester fire-resistant oil is about 500min when the pressure drop reaches 10%, achieving the requirement of rapid detection of the oxidation stability of the phosphate ester fire-resistant oil.

[0042] Repeat steps 2-5 to perform repeated measurements, and take the arithmetic mean of the two measurement results that meet the repeatability requirements as the measurement result of the oxidation stability of the phosphate ester fire-resistant oil.

[0043] In step 2, take 2g-10g of the treated new phosphate ester fire-resistant oil or the running phosphate ester fire-resistant oil, and optimally take 4.000g+0.020g of the treated new phosphate ester fire-resistant oil or the running phosphate ester fire-resistant oil; when detecting the oxidation stability of multiple phosphate ester fire-resistant oils, ensure that each phosphate ester fire-resistant oil is tested under the same detection environment under the condition of the same sampling amount, so as to obtain horizontal comparison data;

[0044] In step 2, the material of the pressure vessel cavity 9 is a corrosion-resistant material such as lead, aluminum, and stainless steel, the volume is 20ml, the inner diameter is 50±0.15mm, the pressure resistance is not less than 1000kPa, the inner surface is polished, and it is equipped with a filling valve, a safety valve, a gas discharge valve, and an integrated cooling fan, wherein the valve is a dead volume and a small size electromagnetic valve, and the cooling fan can blow the bottom of the pressure vessel with external air to accelerate the cooling of the test temperature to room temperature after the test.

[0045] In step 2, the volume ratio of the amount of phosphate ester fire-resistant oil to the volume of the pressure vessel cavity 9 can be (2-10)g / 20ml.

[0046] In step 2, the sample bottle containing the phosphate ester fire-resistant oil is placed in the pressure vessel cavity 9, and the electromagnetic control valve 6 and the one-way electromagnetic control valve 8 are used to repeatedly charge and discharge oxygen into the pressure vessel cavity 9 at room temperature for 3 times to discharge the residual air in the pressure vessel cavity 9, and then charge oxygen until the set pressure is reached and maintained stable for not less than 30s, and the optimal set pressure is 300kPa±0.05kPa.

[0047] In steps 3-5, the pressure sensor 5 is used to detect the pressure in the pressure vessel cavity 9, the test range of the pressure sensor 5 is not less than 0-1000 kPa, the deviation is within ±1%, the accuracy is 0.01 kPa; the sensitivity is not less than 10 mV / kPa;

[0048] In step 4, the optimal set temperature is 180℃±0.5℃, and the temperature of the pressure vessel cavity 9 should be raised to the set temperature in less than 10 min;

[0049] In step 4, the power of the metal bath heating device 4 is 500w, which is sealed at the bottom of the pressure vessel cavity 9, the temperature control range is room temperature-200℃, the accuracy is ±0.5℃, and the precision is 0.1℃; the temperature sensor 3 is used to detect the temperature in the pressure vessel cavity 9, the temperature sensor is a platinum resistance thermometer, the test range is room temperature-200℃, the accuracy is ±0.1℃, and t is the actual temperature;

[0050] In step 5, the time required for the best oxygen pressure in the pressure vessel cavity 9 to drop by 10% from the highest pressure is used to represent the oxidation stability of the phosphate ester fire-resistant oil;

[0051] In step 5, if the pressure continues to drop within 5 min of the initial reaction, the test should be stopped.

[0052] When the above system is used to detect the oxidation stability of phosphate ester fire-resistant oil, no chemical reagents and catalysts are needed during the implementation process, and by limiting the water content of the oil sample, the interference of oil hydrolysis on oxidation stability is avoided, the entire reaction process is close to the use environment of phosphate ester, which is high pressure, and the amount of phosphate ester fire-resistant oil used for testing is small, the testing speed is fast, and the oxidation stability of new and running phosphate ester fire-resistant oil can be quickly and accurately evaluated.

[0053] The process of automatically controlling the operation of the system for detecting the oxidation stability of fire-resistant oil provided by the present application is as follows:

[0054] S1 turns on the detection control system 1, sets the position parameters of the single-arm composite robot 10 from the pressure vessel cavity 9, the sealing ring placement place 11, the pressure vessel top cover placement place 12, the waste oil cup recovery place 13, and the sample placement place 14, and inputs the detection control system 1; sets the test temperature, the filling pressure limit, the number of pre-test inflation and deflation, and the maximum pressure drop data for oxidation stability detection;

[0055] Further, the position parameters of the sample placement place 14 include the position parameters of the sample;

[0056] Further, the single-arm composite robot 10 adopts a ViperX 300 Robot Arm mechanical arm, which has the functions of automatic grabbing, positioning, rotating, laser scanning obstacles, visual obstacle avoidance, force sensor, and emergency stop safety protection,

[0057] Further, the external interface of the single-arm composite robot includes a network port, a USB port, and an HDMI port, and the master control module includes four USB interfaces.

[0058] Further, the rotating function end shape of the single-arm composite robot 10 matches the shape on the pressure container top cover, achieving the grasping and fastening of the pressure container top cover.

[0059] Further, the rotating function end of the single-arm composite robot 10 is a hexagonal column, and the middle part of the upper part of the pressure container top cover is an inner hexagonal body, the size of which is adapted to the hexagonal column of the end of the single-arm composite robot 10, so that the pressure container top cover can be screwed on the first opening of the pressure container cavity 9, and the torque limit of the rotating function end is 15 N·m.

[0060] Further, the outer diameter of the automatic grasping of the single-arm composite robot 10 can be freely adjusted between 0.5 cm and 6 cm, and the positioning accuracy is not greater than 0.1 cm.

[0061] Further, the working environment of the single-arm composite robot 10 is temperature: -10℃ to +40℃, relative humidity less than 85%;

[0062] S2 uses an analytical balance to weigh 4.000±0.0020g of the phosphate ester anti-flame oil sample to be detected in the sample bottle, covers the bottle plug, and numbers the sample, and inputs the sample information corresponding to the number into the detection control system 1;

[0063] Further, the outer diameter of the sample bottle is 5cm±0.3cm;

[0064] Further, the sample bottle is made of borosilicate glass material, and the wall thickness is not less than 5mm;

[0065] Further, the overlapping part of the pressure container top cover and the sample bottle of the sample bottle is a ground opening, and the height of the ground opening is 0.3cm±0.1cm.

[0066] S3 places the sample bottle according to the number in the numbered position in the sample placement place 14;

[0067] S4 places the sealing ring corresponding to the test sample in the sealing ring placement place 11;

[0068] Further, the material of the sealing ring is fluorine rubber;

[0069] Further, a single sealing ring is placed horizontally, and multiple sealing rings are placed vertically;

[0070] S5 places a plastic cup in the waste oil cup recycling place 13;

[0071] S6 The test begins, the detection control system 1 controls the single-arm compound robot 10 to remove the cap of the sample bottle in order according to the preset position parameters, and place it in the waste oil cup 13, then pick up a sealing ring from the sealing ring placement 11 and place it in the groove on the upper edge of the first opening of the pressure container cavity 9, then pick up the pressure container top cover and place it on the pressure container cavity 9, put the outer hexagonal column at the end of the single-arm compound robot 10 into the inner hexagonal groove on the pressure container top cover, and rotate the pressure container top cover clockwise, stop rotating when the torque reaches 10 N·m, and send a signal to the detection control system 1.

[0072] S8 The detection control system 1 opens the data recording function of the pressure sensor 5 and opens the electromagnetic control valve 6 to make oxygen from the oxygen source 7 enter the pressure container cavity 9, when the pressure sensor 5 detects that the pressure reaches the set value, the detection control system 1 closes the electromagnetic control valve 6 and opens the one-way control electromagnetic valve 8 to discharge the gas in the pressure container cavity 9, when the pressure sensor 5 detects that the pressure reaches atmospheric pressure, the detection control system 1 closes the one-way control electromagnetic valve 8, and repeats the above steps 3 times. After discharging the air in the pressure container cavity 9, the detection control system 1 opens the electromagnetic control valve 6 to make oxygen from the oxygen source 7 enter the pressure container cavity 9, when the pressure sensor 5 detects that the pressure reaches the set value, the detection control system 1 closes the electromagnetic control valve 6.

[0073] S9 The detection control system 1 opens the constant temperature control system 2 and further opens the metal bath heating device 4, at the same time, the detection control system 1 opens the timing function and the pressure data recording function, and records the pressure data returned by the pressure sensor 5 in real time, when the pressure data decreases from the highest point to the set value, stop timing, and close the metal bath heating device 4 and the constant temperature control system 2, record the test time, which is the oxidation stability test result of the sample.

[0074] S10 The detection control system 1 opens the one-way control electromagnetic valve 8 to discharge the gas in the pressure container cavity 9, when the pressure sensor 5 detects that the pressure reaches atmospheric pressure, the one-way control electromagnetic valve 8 is closed.

[0075] S11 The detection control system 1 controls the outer hexagonal column at the end of the single-arm compound robot 10 to be placed in the inner hexagonal groove on the pressure container top cover, and after opening the cap counterclockwise, place the cap on the pressure container top cover placement 12.

[0076] S12 The detection control system 1 controls the single-arm compound robot 10 to take out the sample bottle containing the sample and place it in the plastic cup in the waste oil cup 13.

[0077] S13 The detection control system 1 repeats S1-S12 to test other phosphate ester fire-resistant oil samples.

[0078] S14 After the detection control system 1 detects that all the tests of the samples set by the system 1 are completed, the system 1 automatically turns off the power.

Claims

1. A method for detecting the oxidation stability of a phosphate ester fire-resistant oil, characterized by, The oxidation stability detection system for phosphate ester fire-resistant oil is used, and the system includes a pressure container cavity (9) for placing a sample bottle containing phosphate ester fire-resistant oil, the pressure container cavity (9) is arranged in a constant temperature heating device, the sample bottle is placed into the pressure container cavity (9) through a first opening of the pressure container cavity (9), the first opening of the pressure container cavity (9) is sealed by a sealing ring and a pressure container top cover, a second opening of the pressure container cavity (9) is communicated with an oxygen injection device through a pipeline, a pressure sensor (5) is arranged in the pressure container cavity (9), and a third opening of the pressure container cavity (9) is communicated with the atmosphere; The constant temperature heating device, the pressure sensor (5), the oxygen injection device and the single-arm composite robot (10) are connected with a detection control system (1), the detection control system (1) is used for controlling the single-arm composite robot (10) to place or take out the sample bottle from the pressure container cavity (9), acquiring the opening and closing of the oxygen injection device controlled by the pressure detected by the pressure sensor (5), controlling the constant temperature heating device to heat the pressure container cavity (9), and acquiring the time required for the pressure in the pressure container cavity (9) to drop to a set pressure value detected by the pressure sensor (5) during the oxidation stability measurement, the time indicating the oxidation stability of the phosphate ester fire-resistant oil; When the oxidation stability test is performed, the water content of the phosphate ester fire-resistant oil in the sample bottle is not more than 600 mg / L, the addition amount is 2 g to 10 g, the heating range of the constant temperature heating device is 150 DEG C to 200 DEG C, and the pressure range in the pressure container cavity (9) is 300 kPa to 600 kPa; The constant temperature heating device includes a constant temperature control system (2), a temperature sensor (3) and a metal bath heating device (4), the detection control system (1) is connected with the constant temperature control system (2), the temperature sensor (3) and the metal bath heating device (4) to acquire the temperature in the pressure container cavity (9) through the temperature sensor (3) and control the temperature of the metal bath heating device (4) to be constant through the constant temperature control system (2); The oxygen injection device includes an electromagnetic control valve (6), an oxygen source (7) and a one-way electromagnetic control valve (8), the oxygen source (7) is communicated with the second opening of the pressure container cavity (9) through a pipeline, the electromagnetic control valve (6) is arranged on the pipeline, the one-way electromagnetic control valve (8) is arranged at the third opening of the pressure container cavity (9), the detection control system (1) is connected with the electromagnetic control valve (6) to control the opening and closing of the oxygen source (7), and the detection control system (1) is connected with the one-way electromagnetic control valve (8) to control the opening and closing of the third opening to discharge the oxygen in the pressure container cavity (9); The detection control system (1) is connected with the single-arm composite robot (10) to control the single-arm composite robot (10) to place or remove the sealing ring and the pressure container top cover for the first opening of the pressure container cavity (9), so that the first opening of the pressure container cavity (9) is sealed or opened; When the oxidation stability of the phosphate ester fire-resistant oil is detected by using the above system, the specific steps are as follows: S1, the detection control system (1) controls the single-arm composite robot (10) to clamp the sample bottle containing phosphate ester fire-resistant oil and place it in the pressure container cavity (9), and closes the first opening of the pressure container cavity (9); S2, the third opening of the pressure container cavity (9) is opened, the detection control system (1) controls the oxygen injection device to open and inject oxygen into the pressure container cavity (9) to discharge the air in the pressure container cavity (9); S3, the third opening of the pressure container cavity (9) is closed, the detection control system (1) controls the oxygen injection device to open and inject oxygen into the pressure container cavity (9), and when the pressure sensor (5) detects that the pressure reaches the set value, it feeds back to the detection control system (1), and the detection control system (1) controls the oxygen injection device to close; S4, the detection control system (1) controls the constant temperature heating device to heat the pressure container cavity (9) to the set temperature, and the pressure sensor (5) detects the pressure data in the pressure container cavity (9), and when the pressure sensor (5) detects that the pressure in the pressure container cavity (9) drops to the set pressure value, the detection control system (1) records the required time, which represents the oxidation stability of the phosphate ester fire-resistant oil; In S1, when the first opening of the pressure container cavity (9) is closed, the detection control system (1) controls the single-arm composite robot (10) to grab the sealing ring and place it at the first opening position of the pressure container cavity (9), and to grab the pressure container top cover and fasten it at the first opening of the pressure container cavity (9).

2. The method for detecting oxidation stability of phosphate ester fire-resistant oil according to claim 1, characterized in that, The rotating end of the single-arm composite robot (10) is a hexagonal column, and the upper middle part of the pressure container top cover is an inner hexagonal body with a size suitable for the hexagonal column end of the single-arm composite robot (10) to realize the grabbing and fastening of the pressure container top cover.

3. The method for detecting oxidation stability of phosphate ester fire-resistant oil according to claim 1, characterized in that, The grabbing outer diameter of the clamping end of the single-arm composite robot (10) is 0.5cm-6cm, and the clamping end is used to clamp the sealing ring from the sealing ring placement place (11) and place it at the first opening of the pressure container cavity (9), or to clamp the sealing ring at the first opening of the pressure container cavity (9) to the sealing ring placement place (11); the clamping end is used to clamp the sample bottle in the sample placement place (14) and place it in the pressure container cavity (9), or to clamp the sample bottle in the pressure container cavity (9) and place it in the waste oil cup recovery place (13).

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