Method for determining the temperature of the interior of a reaction furnace and method for converting a sample of cerium (Ce) into an oxide using the method

Abstract

Embodiments of the present application relate to the technical field of temperature measurement of flowing gas, and particularly to a method for determining the temperature of the interior of a reaction furnace and a method for converting a sample of cerium (Ce) into an oxide using the method. In a first aspect, embodiments of the present application provide a method for determining the temperature of the interior of a reaction furnace. In a second aspect, embodiments of the present application also provide a method for converting a sample of cerium (Ce) into an oxide, which uses the method for determining the temperature of the interior of a reaction furnace according to any one of the embodiments of the first aspect. Through the method of the present application, the current temperature in the reaction furnace can be accurately determined by obtaining the temperature of the heating element in actual use, without the need to set a temperature measuring element in the reaction furnace, thereby avoiding interference with the normal reaction in the furnace, and achieving accurate and timely regulation of the temperature in the reaction furnace, while avoiding affecting the quality and performance of the product generated by the reaction furnace.

Description

TECHNICAL FIELD

[0001] Embodiments of the present application relate to the technical field of temperature measurement of flowing gas, and in particular to a method for determining the temperature of the interior of a reaction furnace and a method for converting a sample of cerium (Ce) into an oxide using the method. BACKGROUND

[0002] The statements herein are merely provided to give a basic understanding of the present application and are not necessarily intended to constitute the prior art.

[0003] The reaction furnace is widely used in industrial production as a device for promoting chemical reactions under high temperature, high pressure or other conditions, and is suitable for large-scale and high-efficiency production requirements.

[0004] During the normal operation of the reaction furnace, the reaction conditions, such as the temperature in the furnace, need to be controlled and adjusted, but due to the high temperature and high pressure in the reaction space, the currently commonly used method for measuring the temperature in the furnace still has many problems such as great difficulty in measurement and low accuracy of measurement results. SUMMARY

[0005] A brief summary of the present application is given in the following to provide a basic understanding of some aspects of the present application. It should be understood that this summary is not an exhaustive overview of the present application. It is not intended to identify key or important parts of the present application nor is it intended to limit the scope of the present application. Its purpose is merely to present some concepts in a simplified form as a prelude to the more detailed description to be discussed later.

[0006] In a first aspect, embodiments of the present application provide a method for determining the temperature of the interior of a reaction furnace, wherein a heating element is provided outside the reaction furnace, and the heating element is configured to heat the reaction furnace. The method comprises the following steps: S10: providing a plurality of temporary temperature measuring elements in the reaction furnace, configured to measure the temperature in the reaction furnace; S20: providing a plurality of temperature measuring elements on the heating element, configured to measure the temperature of the heating element; S30: starting the heating element to heat the reaction furnace to a predetermined temperature; S40: using the measuring elements, determining the temperature in the reaction furnace when the heating element reaches the predetermined temperature and remains constant, using the temporary temperature measuring elements; S50: changing the predetermined temperature of step S30 within the design temperature range of the heating element, and repeating step S40 to obtain a plurality of predetermined temperatures of the heating element and the corresponding temperatures in the reaction furnace; S60: determining the relationship between the predetermined temperature of the heating element and the temperature in the reaction furnace according to the predetermined temperature of the heating element and the temperature in the reaction furnace obtained in step S50; S70: removing the temporary temperature measuring elements; S80: in actual use, obtaining the current temperature of the heating element, and determining the temperature of the interior of the reaction furnace according to the relationship determined in step S60.

[0007] In a second aspect, the embodiments of the present application further provide a method for converting a sample of cerium (Ce) into an oxide, which method employs the method for determining the temperature inside a reaction furnace according to any of the embodiments of the first aspect of the present application.

[0008] By the method in the embodiments of the present application, the current temperature inside the reaction furnace can be accurately determined by obtaining the temperature of the heating member in actual use, without the need to set a temperature measuring member inside the reaction furnace, thereby avoiding interference with the normal reaction in the furnace, so that accurate and timely regulation of the temperature inside the reaction furnace is realized, while the quality and performance of the product generated by the reaction furnace are avoided from being affected. BRIEF DESCRIPTION OF DRAWINGS

[0009] Other objects and advantages of the present application will become apparent from the following description of the embodiments of the present application, when viewed in conjunction with the accompanying drawings.

[0010] Figure 1 is a flow chart of the method for determining the temperature inside a reaction furnace according to an embodiment of the present application.

[0011] It should be noted that the drawings are not necessarily drawn to scale, but are merely intended to illustrate the concept in a schematic manner without affecting the understanding of the reader. DETAILED DESCRIPTION

[0012] In the following, exemplary embodiments of the present application will be described with reference to the drawings. In the description of the embodiments, not all features of the actual implementation are described in the specification for the sake of clarity and conciseness. It should be appreciated, however, that many implementation-specific decisions can have to be made in order to develop any such actual implementation, to implement developer-specific goals, such as compliance with system- and business-related constraints, which will vary from one implementation to another. Moreover, it should be appreciated that, while the development work can be very complex and time-consuming, such development work would be a routine undertaking for those of ordinary skill in the art having the benefit of this disclosure.

[0013] It should also be noted that, in order to avoid obscuring the present application with unnecessary details, only the device structures and / or processing steps closely related to the solution according to the present application are shown in the drawings, while other details not closely related to the present application are omitted.

[0014] The inventor of the present application finds that, since the temperature inside the reaction furnace is the space temperature, the heating temperature set by the heating member for heating the reaction furnace cannot reflect the temperature inside the reaction furnace in real time, and there is a large error with the actual temperature, and directly measuring the temperature inside the reaction furnace by the temperature measuring member is easy to damage the temperature measuring member, and is easy to interfere with the reaction material in the furnace, therefore, at present, there is no method that can accurately and timely determine the temperature inside the reaction furnace without interfering with the normal reaction in the furnace.

[0015] Based on this, the embodiment of the present application provides a method for determining the temperature inside the reaction furnace, wherein a heating member is arranged outside the reaction furnace, the heating member is arranged to heat the reaction furnace, such as Figure 1 as shown, Figure 1 The flow chart of the method for determining the temperature inside the reaction furnace of one embodiment of the present application is shown, and the method comprises the following steps S10 to S80:

[0016] S10: A plurality of temporary temperature measuring members are arranged in the reaction furnace, which are arranged to measure the temperature inside the reaction furnace.

[0017] S20: A plurality of temperature measuring members are arranged on the heating member, which are used to measure the temperature of the heating member.

[0018] S30: Start the heating member to heat the reaction furnace to a predetermined temperature.

[0019] S40: When the heating member reaches the predetermined temperature and keeps constant, determine the temperature inside the reaction furnace when the constant is kept by the temporary temperature measuring member by using the temperature measuring member.

[0020] S50: Change the predetermined temperature of step S30 in the design temperature range of the heating member, and repeat step S40 to obtain a plurality of predetermined temperatures of the heating member and the corresponding temperatures inside the reaction furnace.

[0021] S60: According to the predetermined temperature of the heating member and the temperature inside the reaction furnace obtained in step S50, determine the relationship between the predetermined temperature of the heating member and the temperature inside the reaction furnace.

[0022] S70: Remove the temporary temperature measuring member.

[0023] S80: In actual use, obtain the current temperature of the heating member, and determine the temperature inside the reaction furnace according to the relationship determined in step S60.

[0024] The method provided in the embodiments of this application utilizes temporary temperature measuring elements and temperature measuring elements to measure the temperatures of the reactor and heating elements respectively. After adjusting the set temperature of the heating elements, the predetermined temperatures of multiple heating elements and their corresponding temperatures inside the reactor are obtained. Based on this, the relationship between the predetermined temperatures of the heating elements and the temperatures inside the reactor is determined. In practical use, the current temperature inside the reactor can be accurately determined based on this relationship by obtaining the temperatures of the heating elements, eliminating the need to install temperature measuring elements inside the reactor and avoiding interference with the normal reaction inside the reactor. Thus, precise and timely control of the temperature inside the reactor is achieved, while avoiding affecting the quality and performance of the products generated in the reactor.

[0025] In some embodiments, in step S10, temporary temperature measuring elements are set up in the following manner: a temporary temperature measuring element is set up at predetermined intervals within the range from the center of the reactor to the furnace wall, so as to measure the temperature at different locations in the transverse space inside the reactor and ensure that the temperature measurement results can reflect the actual temperature inside the reactor.

[0026] For example, based on the radius of the reactor, a temporary temperature measuring element can be installed at intervals of 1 / 4 of the radius value within the range from the center of the reactor to the furnace wall, so that the temporary temperature measuring elements are evenly distributed in the transverse space inside the reactor.

[0027] In some embodiments, in step S10, temporary temperature measuring elements are set up in the following manner: a temporary temperature measuring element is set up at predetermined intervals from the bottom to the top of the reactor to measure the temperature at different heights inside the reactor, ensuring that the temperature measurement results can reflect the actual temperature inside the reactor.

[0028] For example, based on the height of the reactor, a temporary temperature measuring element can be installed at intervals of 1 / 4 of the height value along the center line of the reactor from the bottom to the top of the reactor, so that the temporary temperature measuring elements are evenly distributed in the longitudinal space inside the reactor.

[0029] In some embodiments, in step S20, the temperature measuring elements are set up as follows: a temperature measuring element is set at predetermined intervals within the range from the bottom to the top of the heating element to measure the temperature at different heights of the heating element, ensuring that the temperature measurement results can reflect the actual temperature of the heating element.

[0030] For example, based on the height value of the heating element, a temperature measuring element can be set at intervals of 1 / 4 of the height value within the range from the bottom to the top of the heating element, so that the temperature measuring elements are evenly distributed at different heights of the heating element.

[0031] In some embodiments, in step S30, when the heating element is started to heat the reactor to a predetermined temperature, the heating rate is less than a predetermined value to avoid the heating rate being too fast, which would cause the temperature inside the reactor to be unstable at the predetermined temperature.

[0032] For example, the predetermined heating rate can be set to 10°C / min, and the heating element is set to heat at a rate of less than 10°C / min when heating the reactor to the predetermined temperature.

[0033] In step S40, the temperature sensor determines that the heating element has reached the predetermined temperature T. i Furthermore, when the temperature remains constant, multiple temporary temperature sensors installed inside the reactor are used to determine the constant temperature T inside the reactor. j For example, the temperature should be kept constant for at least 30 minutes.

[0034] In some embodiments, in steps S30-S40, the heating method is set to be the same as when operating the reaction in the reactor, so as to simulate the working conditions in actual use as much as possible, making the temperature inside the reactor closer to the temperature in actual use, thereby making the relationship between the heating element and the temperature inside the reactor more reliable.

[0035] In some embodiments, steps S30-S40 further include introducing an inert gas at a predetermined pressure into the reactor in the same manner as when the reactor is being operated, to further simulate the working conditions during actual use, thereby making the relationship between the heating element and the temperature inside the reactor more reliable.

[0036] In step S50, the predetermined temperature of step S30 can be changed within the design temperature range of the heating element, and the heating rate can be set to be less than a predetermined value, for example, less than 10°C / min; and step S40 can be repeated to obtain the predetermined temperatures of multiple heating elements and the temperatures in multiple corresponding reaction furnaces.

[0037] In step S60, the relationship between the predetermined temperature of the heating element and the temperature inside the reactor can be determined based on the predetermined temperatures of the multiple heating elements obtained in step S50 and the temperatures inside the multiple reactors. The predetermined temperature of the heating element can be the temperature of the heating element measured by a temperature measuring element.

[0038] In some embodiments, step S60 may further include the following steps:

[0039] S61: Based on the predetermined temperature of the heating element and the temperature inside the reactor obtained in step S50, determine the relationship curve between the predetermined temperature of the heating element and the temperature inside the reactor.

[0040] S62: Determine the relationship between the predetermined temperature of the heating element and the temperature inside the reactor based on the relationship curve.

[0041] S63: Based on the formula, determine the relationship curve between the predetermined temperature of the heating element and the temperature inside the reactor.

[0042] In this embodiment, the predetermined temperatures of multiple heating elements and their corresponding temperatures in multiple reaction furnaces are used to determine the relationship curve between the predetermined temperatures of the heating elements and the temperatures in the reaction furnaces. Based on the relationship curve, the relationship formula between the predetermined temperatures of the heating elements and the temperatures in the reaction furnaces is determined, and the relationship curve is determined through this formula to obtain a curve that can accurately reflect the relationship between the predetermined temperatures of the heating elements and the temperatures in the reaction furnaces. This improves the accuracy of obtaining the current temperature in the reaction furnace from the current temperature of the heating elements in actual use.

[0043] Specifically, in step S61, the predetermined temperatures of multiple heating elements and the corresponding temperatures inside the reactor are fitted to obtain a curve reflecting the relationship between the predetermined temperatures of the heating elements and the temperatures inside the reactor. In step S62, the relationship between the predetermined temperatures of the heating elements and the temperatures inside the reactor is determined based on the relationship curve, and it is judged whether the goodness of fit of the relationship meets the predetermined requirements. If the requirements are not met, the fitting method and data can be optimized and adjusted, and a new relationship can be obtained. In step S63, the relationship curve is plotted based on the new relationship so that the curve can more accurately reflect the relationship between the predetermined temperatures of the heating elements and the temperatures inside the reactor.

[0044] In some embodiments, step S60 further includes the following steps:

[0045] S64: Correct the relationship curve obtained in step S63 based on the predetermined temperature of the heating element and the temperature inside the reactor obtained in step S50.

[0046] S65: Update the relationship curve based on the correction results of step S64.

[0047] S66: Based on the updated relationship curve from step S65, determine the updated relationship between the predetermined temperature of the heating element and the temperature inside the reactor.

[0048] S67: Based on the updated relationship in step S66, determine the updated relationship curve between the predetermined temperature of the heating element and the temperature inside the reactor.

[0049] In this embodiment, the predetermined temperature of the heating element and the temperature inside the reactor obtained in step S50 are used to verify whether the relationship curve determined by the formula in step S63 can accurately reflect the relationship between the predetermined temperature of the heating element and the temperature inside the reactor. The relationship curve is updated according to the correction result, the formula is re-determined, and a new relationship curve is obtained according to the formula to further improve the accuracy of the relationship curve.

[0050] Specifically, in step S64, the accuracy of the relationship curve can be verified by using the values ​​of the predetermined heating element temperature and the reactor temperature that were not used when the relationship curve was initially determined in step S61, and the parts of the relationship curve that need to be corrected, such as the slope and intercept of the curve, can be determined. In step S65, according to the specific requirements of curve correction, an appropriate method is selected to refit the data to update the relationship curve. In step S66, the updated relationship formula between the predetermined heating element temperature and the reactor temperature is determined based on the updated relationship curve, and it is judged whether the goodness of fit of the relationship formula meets the predetermined requirements. In step S67, the relationship curve is plotted again based on the updated relationship formula to obtain a curve that can more accurately reflect the relationship between the predetermined heating element temperature and the reactor temperature.

[0051] Embodiments of this application also provide a method for converting a cerium (Ce) sample into an oxide, the method employing the method for determining the internal temperature of the reactor according to any embodiment of the first aspect of this application. The method includes the following steps S1 to S8:

[0052] S1: Place the sample in a sealed reaction furnace.

[0053] S2: Set the reactor to an inert atmosphere.

[0054] S3: Determine the current pressure of the reactor.

[0055] S4: During the reaction process, determine the exhaust volume of the reactor tail gas based on the pressure determined in step S3.

[0056] S5: Heat the reactor to the predetermined temperature.

[0057] S6: Stop feeding inert gas and feed reaction gas into the reactor.

[0058] S7: Monitor the exhaust gas from the reactor to determine when the reaction is complete.

[0059] S8: After confirming that the reaction is complete, introduce inert gas into the reactor until the reactor cools down.

[0060] The method provided in the embodiments of this application involves setting the reactor to an inert atmosphere before the reaction begins, determining the pressure of the reactor under the inert atmosphere, and determining the exhaust volume of the reactor tail gas based on the pressure value. This pre-determining of the reactor exhaust volume allows for control of the internal pressure of the reactor during the reaction, thereby controlling the conversion rate and ensuring that the cerium sample reacts fully with oxygen. Simultaneously, it avoids excessive internal pressure that could cause the container to rupture and lead to an accident. Furthermore, by monitoring the exhaust gas discharged from the reactor, the reaction progress is determined based on changes in the exhaust gas composition to avoid excessively long reaction times, thus obtaining a stable and high-purity cerium oxide product.

[0061] In step S2, when setting the reactor to an inert atmosphere, a vacuum replacement method can be used. First, the inside of the reactor is evacuated, then inert gas is introduced to bring the internal pressure of the reactor to a predetermined value. The reactor is then evacuated again and inert gas is introduced again. This process is repeated 2-3 times to completely replace the oxygen inside the reactor. For example, the introduced inert gas can be argon, nitrogen, or helium.

[0062] Following step S2, the process may further include: determining the expected pressure of the reactor in order to adjust the current pressure of the reactor based on that expected pressure.

[0063] The expected pressure can be the pressure control range of the reactor, that is, the range between the maximum and minimum values ​​allowed when controlling the pressure of the reactor to ensure the quality and performance of the reaction products.

[0064] In step S3, when determining the current pressure of the reactor, a pressure monitoring device can be installed in the reactor to obtain the current pressure inside the reactor in real time.

[0065] In some embodiments, in step S4, the exhaust volume of the tail gas can be determined based on the current pressure of the reactor and the expected pressure, so as to control the internal pressure of the reactor within the expected pressure range by controlling and adjusting the current exhaust volume of the tail gas, thereby achieving control of the conversion rate during the reaction process.

[0066] Specifically, when the current pressure of the reactor is greater than the expected pressure, the exhaust gas volume is increased; when the current pressure of the reactor is less than the expected pressure, the exhaust gas volume is decreased.

[0067] In some embodiments, in step S4, a suction device can be used to extract the exhaust gas, thereby changing the exhaust volume. In this embodiment, the suction device provides power for exhaust gas discharge, accelerating the exhaust speed and increasing the exhaust volume when the current pressure of the reactor is greater than the expected pressure, thereby achieving timely adjustment of the internal pressure of the reactor and reducing the gap between the internal pressure of the reactor and the expected pressure.

[0068] In some embodiments, in step S4, the opening degree of the valve in the exhaust gas pipeline can be controlled to change the exhaust gas discharge rate. In this embodiment, by controlling the opening degree of the valve in the exhaust gas pipeline, the valve opening degree is reduced when the current pressure of the reactor is lower than the expected pressure, or the valve opening degree is increased when the current pressure of the reactor is higher than the expected pressure, thereby changing the exhaust gas discharge rate and achieving precise control of the internal pressure of the reactor, reducing the difference between the internal pressure of the reactor and the expected pressure.

[0069] Furthermore, in step S4, the suction device can work in conjunction with the valve controlling the exhaust gas pipeline. When the current pressure of the reactor is greater than the expected pressure, the valve opening degree is increased, and the exhaust gas is sucked in conjunction with the suction device to further accelerate the exhaust speed, increase the exhaust volume, and further accelerate the rate of adjustment of the internal pressure of the reactor, thereby ensuring precise control of the conversion rate during the reaction process.

[0070] In some embodiments, in step S4, a regulating valve is installed on the tail gas pipeline of the reactor to regulate the tail gas emission rate, thereby improving the regulation accuracy of the tail gas emission rate and further realizing precise control of the internal pressure of the reactor.

[0071] In some embodiments, in step S4, the amount of input reaction gas can be reduced according to the determined pressure to avoid the tail gas concentration from exceeding a predetermined value, which would lead to excessively high pressure inside the reactor and excessively fast conversion rate.

[0072] In some embodiments, in step S4, the amount of inert gas input can be increased according to a determined pressure to avoid the tail gas concentration from exceeding a predetermined value, which would lead to excessively high pressure inside the reactor and excessively fast conversion rate.

[0073] In some embodiments, in step S5, the reaction temperature inside the reactor is monitored in real time, and based on the real-time temperature, it is determined whether heating has ended so that the reaction temperature inside the reactor reaches a predetermined temperature.

[0074] For example, thermocouples can be used to control the heating temperature of the reactor and to monitor the reaction temperature inside the reactor in real time.

[0075] In step S6, the input of inert gas is stopped, and a reaction gas, such as a mixture of steam and nitrogen, a mixture of steam and argon, or a mixture of steam and air, is introduced into the reactor.

[0076] In some embodiments, in step S7, the reaction rate is determined based on the rate of change of a predetermined component in the exhaust gas, so as to judge the reaction progress based on the current reaction rate, thereby determining whether the conversion of the cerium sample into oxide has ended, and avoiding excessively long reaction time.

[0077] In step S7, since the reaction gas input to the reactor in step S6 is a mixture of steam and nitrogen, or a mixture of steam and argon, or a mixture of steam and air, the reaction rate can be determined based on the rate of change of hydrogen in the tail gas. Furthermore, when the rate of change of hydrogen approaches 0 within a certain time, it can be determined that the conversion of the sample into oxide is complete. When the reaction gas is a mixture of steam and nitrogen, the reaction rate can also be determined based on the rate of change of ammonia in the tail gas.

[0078] In some embodiments, in step S7, reaction parameters can be determined based on the determined reaction rate and the expected reaction rate. In this embodiment, reaction parameters are determined by comparing the current reaction rate with the expected reaction rate, so that when the current reaction rate cannot meet the expected requirements, the current reaction parameters can be adjusted according to the determined reaction parameters, thereby adjusting the current conversion rate to reach the expected conversion rate.

[0079] The reaction parameters may include reaction temperature, vapor concentration, gas composition, gas flow rate, and pressure.

[0080] In some embodiments, step S7 may further include the following steps:

[0081] S71: Determine the relationship between conversion rate and reaction temperature.

[0082] S72: Determine the desired reaction temperature based on the relationship.

[0083] In this embodiment, the relationship between the conversion rate and the reaction temperature during the reaction process is established, and the desired reaction temperature is determined based on this relationship. This facilitates the adjustment of the current reaction temperature to reduce the difference between the current conversion rate and the desired conversion rate.

[0084] In some embodiments, step S71 may further include the following steps:

[0085] S711: Obtain multiple conversion rates and the corresponding reaction temperature for each conversion rate.

[0086] S712: Based on the conversion rate and reaction temperature obtained in step S711, determine the relationship curve between the conversion rate and the reaction temperature.

[0087] S713: Determine the relationship between conversion rate and reaction temperature based on the relationship curve.

[0088] S714: Determine the relationship curve between conversion rate and reaction temperature based on the formula.

[0089] In this embodiment, the relationship curve between conversion rate and reaction temperature is determined by using multiple conversion rates and their corresponding multiple reaction temperatures. The relationship formula between conversion rate and reaction temperature is determined based on the relationship curve, and the relationship curve is determined by the formula to obtain a curve that can accurately reflect the relationship between conversion rate and reaction temperature. Thus, it is convenient to accurately obtain the current reaction temperature based on the current conversion rate.

[0090] Specifically, in step S712, the obtained multiple conversion rates and the corresponding reaction temperatures for each conversion rate are fitted to obtain a curve reflecting the relationship between the conversion rate and the reaction temperature; in step S713, the relationship between the conversion rate and the reaction temperature is determined based on the relationship curve, and it is judged whether the goodness of fit of the relationship meets the predetermined requirements. If the requirements are not met, the fitting method and data can be optimized and adjusted, and a new relationship can be obtained; in step S714, the relationship curve is plotted based on the new relationship so that the curve can more accurately reflect the relationship between the conversion rate and the reaction temperature.

[0091] In some embodiments, step S71 may further include the following steps:

[0092] S715: Correct the relationship curve obtained in step S714 using the value between the conversion rate and the reaction temperature obtained from the experiment.

[0093] S716: Update the relationship curve based on the correction results of step S715.

[0094] S717: Based on the updated relationship curve from step S716, determine the updated relationship between conversion rate and reaction temperature.

[0095] S718: Based on the updated relationship in step S717, determine the updated relationship curve between conversion rate and reaction temperature.

[0096] In this embodiment, the conversion rate and reaction temperature values ​​obtained in the experiment are used to verify whether the relationship curve determined by the formula in step S714 can accurately reflect the relationship between the conversion rate and the reaction temperature. The relationship curve is updated according to the correction results, the formula is re-determined, and a new relationship curve is obtained according to the formula to further improve the accuracy of the relationship curve.

[0097] Specifically, in step S715, the accuracy of the relationship curve can be verified using the conversion rate and reaction temperature values ​​not used in step S711, and the parts of the relationship curve that need correction, such as the slope and intercept of the curve, can be determined. In step S716, according to the specific requirements of curve correction, an appropriate method is selected to refit the data to update the relationship curve. In step S717, the updated relationship between the conversion rate and reaction temperature is determined based on the updated relationship curve, and it is judged whether the goodness of fit of the relationship meets the predetermined requirements. In step S718, the relationship curve is plotted again based on the updated relationship to obtain a curve that can more accurately reflect the relationship between the conversion rate and reaction temperature.

[0098] In some embodiments, in step S8, the humidity of the exhaust gas is monitored, and the complete discharge of the reaction gas is determined based on the humidity of the exhaust gas, so as to avoid affecting the subsequent reaction of cerium sample to oxide, which would lead to a decrease in the performance and quality of the oxidation product.

[0099] Specifically, in step S8, after the reaction is complete, inert gas is introduced into the reactor and the humidity of the tail gas is monitored. When the humidity of the tail gas drops to a predetermined value, it indicates that the tail gas is dry and free of moisture, and it can be determined that the reaction gas, i.e., the steam, in the reactor has been completely discharged.

[0100] The cerium (Ce) sample in this application can be prepared by the following steps S100 to S800:

[0101] S100: Molten cerium material.

[0102] S200: Cast the molten material obtained in step S100 into an ingot.

[0103] S300: The molded part obtained in step S200.

[0104] S400: The fraction obtained in step S300 is stored in a first organic solvent.

[0105] S500: Remove surface oxides from the fraction in a first organic solvent.

[0106] S600: Remove the product obtained in step S500 from the first organic solvent and remove the first organic solvent from the surface of the product using a second organic solvent.

[0107] S700: A second organic solvent for removing the surface of the product.

[0108] S800: Ensure complete removal of the second organic solvent.

[0109] In this embodiment, the cerium material is melted, cast, and divided to obtain a fraction, which is then stored in a first organic solvent and treated in the first organic solvent to remove the oxides on its surface while isolating the fraction from air and preventing it from burning. Then, a second organic solvent is used to remove the first organic solvent from the surface of the product and completely remove the second organic solvent, so as to minimize the impurity content in the final cerium sample, effectively improve the purity of the cerium sample, and thus ensure the accuracy of subsequent experiments.

[0110] In some embodiments, step S100 further includes the following step:

[0111] S101: Determine the temperature of the melt in real time.

[0112] S102: Determine the heating power for the melting operation based on the temperature determined in step S101 and the predetermined temperature.

[0113] In this embodiment, the current temperature of the melt is determined in real time and compared with a predetermined temperature to determine the heating power required for the melting operation. This facilitates the adjustment of the heating power and further removes impurities from the melt.

[0114] In step S102, the predetermined temperature is when the cerium material melts, resulting in the highest purity of the melt.

[0115] In step S200, the molten ingot obtained in step S100 can be molded into a disc shape so that it can be subsequently divided into shapes and sizes that meet predetermined requirements.

[0116] In some embodiments, the slitting operation in step S300 can be performed under an inert gas atmosphere to prevent the molded article obtained in step S200 from reacting with oxygen during the slitting process and generating oxides.

[0117] For example, dry ice can be used to create an inert gas atmosphere to isolate the molded part from oxygen, while simultaneously cooling the slitting operation to prevent the molded part from spontaneously combusting.

[0118] In some embodiments, step S300 may further include the following steps:

[0119] S301: Cut the molded article obtained in step S200 into a columnar object of a predetermined size.

[0120] S302: Divide the columnar material obtained in step S301.

[0121] In this embodiment, the molded material obtained in step S200 is cut into columnar objects of a predetermined size, and then the columnar objects are divided into small segments of a predetermined size in order to obtain cerium samples that meet the predetermined requirements.

[0122] In step S400, after obtaining the fraction, the fraction is immediately transferred to a first organic solvent for preservation to isolate it from oxygen and prevent combustion. For example, the first organic solvent may be kerosene.

[0123] In step S500, the surface of the segment can be sanded with sandpaper in a first organic solvent to remove oxides from the surface of the segment.

[0124] In step S600, the product obtained after removing surface oxides is removed from the first organic solvent and placed in a second organic solvent to remove the first organic solvent from the surface of the product. For example, the second organic solvent may be ethanol.

[0125] In some embodiments, in step S700, an inert gas can be used to continuously purge the product surface to remove the second organic solvent from the product surface, thereby preventing the product from undergoing an oxidation reaction and generating oxides again.

[0126] The second organic solvent is a volatile solvent, which is easy to evaporate when the product surface is continuously purged with inert gas, thereby facilitating the complete removal of the second organic solvent and improving the purity of the cerium sample.

[0127] In some embodiments, step S700 may further include the following steps:

[0128] S701: Place the product in a sealed container.

[0129] S702: Vacuum the sealed container.

[0130] S703: Inert gas is introduced into a sealed container to purge the product.

[0131] In this embodiment, the product is placed in a sealed container, the air in the sealed container is extracted, and an inert gas is introduced into it to continuously purge the surface of the product with the inert gas, thereby removing the second organic solvent in an oxygen-isolated environment and minimizing the oxidation of the product during the process.

[0132] Before step S701, before placing the product in the sealed container, the inside of the sealed container can be converted to an inert gas atmosphere to prevent the product from being oxidized by the air inside the sealed container when it is placed in the sealed container.

[0133] In some embodiments, step S700 may further include the following steps:

[0134] S704: Collect exhaust gases emitted from sealed containers.

[0135] S705: Determine the composition of exhaust gas.

[0136] In step S800, the complete removal of the second organic solvent is determined based on the composition of the exhaust gas identified in step S705.

[0137] In this embodiment, the exhaust gas discharged from the sealed container is collected and its composition is determined in order to determine whether the second organic solvent has been completely removed. The determination result is highly accurate and effectively avoids the residue of the second organic solvent.

[0138] Specifically, in step S704, the exhaust gas discharged from the sealed container can be continuously collected during the process of introducing inert gas into the sealed container, and the components in the exhaust gas can be determined in step S705. In step S800, when the exhaust gas components do not contain the second organic solvent, it is determined that the second organic solvent has been completely removed.

[0139] In some embodiments, step S800 may further include the following steps:

[0140] S801: Weigh the sealed container after the product has been placed in it and before an inert gas has been introduced.

[0141] S802: In step S703, the sealed container is continuously weighed.

[0142] S803: Based on the weighing results in step S802 and step S801, determine that the second organic solvent has been completely removed.

[0143] In this embodiment, the weight of the sealed container before and after the product is purged with inert gas is compared to efficiently and directly determine whether the second organic solvent has been completely removed.

[0144] Specifically, in step S801, after placing the product in a sealed container and evacuating the container, the sealed container is weighed, and then an inert gas is introduced into the sealed container; in step S802, after introducing the inert gas, the sealed container is continuously weighed to obtain multiple weighing results of the sealed container after introducing the inert gas; in step S803, the multiple weighing results obtained in step S802 are compared with the weighing results in step S801 to obtain multiple comparison results. When the comparison results meet the condition of remaining unchanged within a predetermined time range, it can be determined that the second organic solvent has been completely removed.

[0145] In some embodiments, step S800 may further include the following steps:

[0146] S804: In step S703, the sealed container is continuously weighed.

[0147] S805: Based on the weighing results in step S804, confirm that the second organic solvent has been completely removed.

[0148] In this embodiment, by continuously weighing the sealed container and judging from the weight change, it is possible to determine more efficiently and directly whether the second organic solvent has been completely removed.

[0149] Specifically, in step S804, after introducing inert gas into the sealed container, the sealed container is continuously weighed to obtain multiple weighing results; in step S805, when it is observed that multiple weighing results meet the condition of remaining unchanged within a predetermined time range, it can be determined that the second organic solvent has been completely removed.

[0150] In some embodiments, the first organic solvent can be dissolved in the second organic solvent so that the second organic solvent can remove the first organic solvent from the surface of the product.

[0151] The process of determining the internal temperature of the reactor in this application is further illustrated below with specific embodiments.

[0152] Based on the radius of the reactor, temporary temperature measuring elements are installed at intervals of 1 / 4 of the radius along the center of the reactor to the reactor wall. Based on the height of the reactor, temporary temperature measuring elements are also installed at intervals of 1 / 4 of the height along the centerline from the bottom to the top of the reactor to measure the temperature inside the reactor. Based on the height of the heating element, a temperature measuring element is installed at intervals of 1 / 4 of the height from the bottom to the top of the heating element to measure its temperature. The heating element is activated to heat the reactor to the predetermined temperature at a rate less than 10°C / min. The temperature is measured after the temperature measuring elements confirm that the heating element has reached the predetermined temperature T. i Furthermore, when the temperature remains constant, multiple temporary temperature sensors installed inside the reactor are used to determine the constant temperature T inside the reactor. j The temperature must be kept constant for at least 30 minutes; within the design temperature range of the heating element, the predetermined temperature of the heating element must be changed at a rate of less than 10℃ / min, and the heating element must be confirmed to have reached the predetermined temperature T by a temperature measuring device. i+1 Furthermore, when the temperature remains constant, multiple temporary temperature sensors installed inside the reactor are used to determine the constant temperature T inside the reactor. j+1 Repeat this process multiple times to obtain the predetermined temperatures of multiple heating elements and the corresponding temperatures inside the reactor; based on the predetermined temperatures of multiple heating elements and the temperatures inside the reactor obtained in step S50, determine the relationship between the predetermined temperatures of the heating elements and the temperatures inside the reactor; remove the temporary temperature measuring element, obtain the current temperature of the heating element in actual use, and determine the internal temperature of the reactor based on the determined relationship between the predetermined temperatures of the heating elements and the temperatures inside the reactor.

[0153] Regarding the embodiments of this application, it should also be noted that, without conflict, the embodiments of this application and the features in the embodiments can be combined with each other to obtain new embodiments.

[0154] The above are merely specific embodiments of this application, but the scope of protection of this application is not limited thereto. The scope of protection of this application shall be determined by the scope of the claims.

Claims

1. A method for determining the internal temperature of a reactor, wherein, A heating element is provided outside the reactor, and the heating element is configured to heat the reactor, characterized by comprising the following steps: S10: Multiple temporary temperature measuring elements are installed inside the reactor to measure the temperature inside the reactor. S20: Multiple temperature measuring elements are provided on the heating element for measuring the temperature of the heating element; S30: Start the heating element to heat the reactor to a predetermined temperature; S40: Using the temperature measuring element, when the heating element reaches a predetermined temperature and remains constant, the temporary temperature measuring element is used to determine the temperature inside the reactor when it remains constant. S50: Change the predetermined temperature in step S30 within the design temperature range of the heating element, and repeat step S40 to obtain the predetermined temperatures of multiple heating elements and the corresponding temperatures inside the reactor. S60: Based on the predetermined temperature of the heating element and the temperature inside the reactor obtained in step S50, determine the relationship between the predetermined temperature of the heating element and the temperature inside the reactor. S70: Remove the temporary temperature measuring element; S80: In actual use, the current temperature of the heating element is obtained, and the internal temperature of the reactor is determined according to the relationship determined in step S60.

2. The method according to claim 1, characterized in that, In step S10, the temporary temperature measuring element is set up in the following manner: Within the range from the center of the reactor to the furnace wall, a temporary temperature measuring element is installed at predetermined intervals.

3. The method according to claim 1, characterized in that, In step S10, the temporary temperature measuring element is set up in the following manner: A temporary temperature measuring element is installed at predetermined intervals from the bottom to the top of the reactor.

4. The method according to claim 1, characterized in that, In step S20, the temperature measuring element is set up as follows: A temperature measuring element is provided at predetermined intervals from the bottom to the top of the heating element.

5. The method according to claim 1, characterized in that, In step S30, the rate of temperature increase is less than the predetermined value.

6. The method according to claim 1, characterized in that, In steps S30-S40, the heating method is set to be the same as when operating the reaction using the reactor.

7. The method according to claim 6, characterized in that, In steps S30-S40, an inert gas at a predetermined pressure is introduced into the reactor in the same manner as when the reactor is operated.

8. The method according to claim 1, characterized in that, Step S60 also includes the following steps: S61: Based on the predetermined temperature of the heating element and the temperature inside the reactor obtained in step S50, determine the relationship curve between the predetermined temperature of the heating element and the temperature inside the reactor. S62: Determine the relationship between the predetermined temperature of the heating element and the temperature inside the reactor based on the relationship curve; S63: Based on the given formula, determine the relationship curve between the predetermined temperature of the heating element and the temperature inside the reactor.

9. The method according to claim 8, characterized in that, Step S60 also includes the following steps: S64: Based on the predetermined temperature of the heating element and the temperature inside the reactor obtained in step S50, correct the relationship curve obtained in step S63. S65: Update the relationship curve based on the correction result of step S64; S66: Based on the updated relationship curve in step S65, determine the updated relationship between the predetermined temperature of the heating element and the temperature inside the reactor. S67: Based on the updated relationship formula in step S66, determine the updated relationship curve between the predetermined temperature of the heating element and the temperature inside the reactor.

10. A method for converting a cerium (Ce) sample into an oxide, characterized in that, The method described herein employs the method for determining the internal temperature of the reactor as described in any one of claims 1-9.

Images