Method for converting cerium (Ce) sample into oxide based on reaction tail gas

Abstract

The embodiment of the invention relates to the technical field of preparation or treatment of rare earth metal, in particular to a method for converting a cerium (Ce) sample into an oxide based on reaction tail gas, and the method comprises the following steps: placing the sample in a sealed reaction container; setting the container in an inert atmosphere; determining the current pressure of the container; determining the exhaust amount of the tail gas of the container according to the determined current pressure in the reaction process; heating the container to a predetermined temperature; stopping inputting the inert gas, and inputting reaction gas into the container; monitoring tail gas of the reaction container and determining that the reaction is finished; and after determining that the reaction is finished, inputting inert gas into the reaction container until the reaction container is cooled. According to the method, the gas displacement of the reaction container can be determined in advance before the reaction is started, so that the internal pressure of the container is conveniently controlled, the conversion rate is controlled, and meanwhile bursting caused by too large internal pressure of the container is avoided; and the reaction process is determined through tail gas component change, so that the reaction time is prevented from being too long, and the cerium oxide product with stable properties and high purity is obtained.

Description

Technical Field

[0001] The embodiments of the present application relate to the technical field of preparation or treatment of rare earth metals, and more particularly to a method for converting a cerium (Ce) sample into oxides based on reaction tail gas. Background Art

[0002] The statements herein merely provide background information related to the present application and do not necessarily constitute prior art.

[0003] Cerium is a rare earth element with good chemical stability and high corrosion resistance. The oxides generated by its reaction also have a variety of unique chemical and physical properties. Cerium oxide has high catalytic activity, oxygen storage and release functions, and good optical properties, and is widely used in chemical industry, energy, materials science, optics and other fields. When converting cerium samples into oxides, air oxidation, chemical oxidation and other methods are usually used.

[0004] However, the currently commonly used method of converting cerium into oxide still has many problems in controlling and regulating the reaction process during actual application, resulting in the quality and performance of the converted cerium oxide being difficult to meet the predetermined requirements. Summary of the invention

[0005] A brief overview of the present application is provided below in order to provide a basic understanding of certain aspects of the present application. It should be understood that this overview is not an exhaustive overview of the present application. It is not intended to identify the 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 certain concepts in a simplified form as a prelude to a more detailed description discussed later.

[0006] An embodiment of the present application provides a method for converting a cerium (Ce) sample into an oxide based on reaction exhaust gas, which includes the following steps: S1: placing the sample in a sealed reaction container; S2: setting the reaction container to an inert atmosphere; S3: determining the current pressure of the reaction container; S4: during the reaction, determining the exhaust volume of the exhaust gas of the reaction container according to the pressure determined in step S3; S5: heating the reaction container to a predetermined temperature; S6: stopping the input of inert gas and inputting reaction gas into the reaction container; S7: monitoring the exhaust gas of the reaction container to determine the end of the reaction; S8: after determining that the reaction is over, inputting inert gas into the reaction container until the reaction container is cooled.

[0007] The method in the embodiments of the present application sets the reaction container to an inert atmosphere before the reaction starts, determines the pressure of the reaction container when it is in the inert atmosphere, and determines the exhaust volume of the tail gas of the reaction container based on the pressure value, so as to determine the exhaust volume of the reaction container in advance before the reaction starts, so as to control the internal pressure of the reaction container during the reaction, thereby controlling the conversion rate, ensuring that the cerium sample reacts fully with the water vapor, and at the same time, avoiding the internal pressure of the reaction container from being too high, causing the container to burst and cause an accident; and, by monitoring the tail gas discharged from the reaction container, determining the reaction progress according to the change of the tail gas composition, so as to avoid too long a reaction time, thereby obtaining a cerium oxide product with stable properties and high purity. BRIEF DESCRIPTION OF THE DRAWINGS

[0008] Other objects and advantages of the present application will become apparent from the following description of the embodiments of the present application with reference to the accompanying drawings, and will help to provide a comprehensive understanding of the present application.

[0009] Figure 1 The present invention is a flowchart of a method for converting a sample of cerium (Ce) into oxides based on reaction tail gas according to one embodiment of the present application.

[0010] It should be noted that the drawings are not necessarily drawn to scale, but are merely shown in a schematic manner that does not affect the reader's understanding. DETAILED DESCRIPTION

[0011] Exemplary embodiments of the present application will be described below in conjunction with the accompanying drawings. For the sake of clarity and conciseness, not all features of the actual implementation are described in the specification. However, it should be understood that many implementation-specific decisions must be made in the process of developing any such actual implementation in order to achieve the developer's specific goals, such as meeting those constraints related to the system and business, and these constraints may vary from implementation to implementation. In addition, it should be understood that although the development work may be very complex and time-consuming, it is only a routine task for those skilled in the art who benefit from the content of this application.

[0012] It is also necessary to explain here that, in order to avoid obscuring the present application due to unnecessary details, only the device structure and / or processing steps closely related to the scheme according to the present application are shown in the accompanying drawings, while other details that are not very relevant to the present application are omitted.

[0013] The inventors of the present application have discovered that the currently commonly used method for converting cerium samples into oxides still has problems such as difficulty in controlling the conversion rate and difficulty in determining the reaction progress during actual application, which makes it impossible for the cerium sample to fully react with water vapor, resulting in an incomplete reaction, or it is impossible to determine whether the reaction has been completed, resulting in a too long reaction time, thereby affecting the quality and performance of the generated oxidation product.

[0014] Based on this, the embodiment of the present application provides a method for converting a sample of cerium (Ce) into oxides based on the reaction tail gas, such as Figure 1 As shown, Figure 1 A flow chart showing a method for converting a sample of cerium (Ce) into oxides based on reaction tail gas according to an embodiment of the present application is shown. The method includes the following steps S1 to S8:

[0015] S1: Place the sample in a sealed reaction container.

[0016] S2: Set the reaction vessel to an inert atmosphere.

[0017] S3: Determine the current pressure of the reaction vessel.

[0018] S4: During the reaction process, the exhaust volume of the tail gas from the reaction container is determined according to the pressure determined in step S3.

[0019] S5: heating the reaction container to a predetermined temperature.

[0020] S6: Stop the inert gas input and input the reaction gas into the reaction container.

[0021] S7: Monitor the tail gas from the reaction vessel to determine the end of the reaction.

[0022] S8: After determining that the reaction is complete, an inert gas is introduced into the reaction container until the reaction container is cooled.

[0023] The method provided in the embodiments of the present application sets the reaction container to an inert atmosphere before the reaction starts, determines the pressure of the reaction container when it is in the inert atmosphere, and determines the exhaust volume of the tail gas of the reaction container based on the pressure value, so as to determine the exhaust volume of the reaction container in advance before the reaction starts, so as to control the internal pressure of the reaction container during the reaction, thereby controlling the conversion rate, ensuring that the cerium sample reacts fully with water vapor, and at the same time, avoiding excessive pressure inside the reaction container that causes the container to burst and cause an accident; and, by monitoring the tail gas discharged from the reaction container, determining the reaction progress based on the change in the tail gas composition, so as to avoid too long a reaction time, thereby obtaining a cerium oxide product with stable properties and high purity.

[0024] In step S2, when the reaction container is set to an inert atmosphere, a vacuum replacement method can be used, first the reaction container is vacuumed, then an inert gas is input therein, so that the pressure inside the reaction container reaches a predetermined value, and then the reaction container is vacuumed and then an inert gas is input, and the above steps are repeated 2-3 times to completely replace the oxygen inside the reaction container. For example, the input inert gas can be argon, nitrogen, helium, etc.

[0025] After step S2, the method may further include: determining an expected pressure of the reaction container, so as to adjust the current pressure of the reaction container according to the expected pressure.

[0026] The expected pressure may be a pressure control range of the reaction vessel, that is, a numerical range between a maximum value and a minimum value allowed when the pressure of the reaction vessel is controlled in order to ensure the quality and performance of the reaction product.

[0027] In step S3, when determining the current pressure of the reaction container, a pressure monitoring device may be provided in the reaction container to obtain the current pressure inside the reaction container in real time.

[0028] In some embodiments, in step S4, the exhaust volume of the exhaust gas can be determined based on the current pressure of the reaction container and the expected pressure, so that the internal pressure of the reaction container can be controlled to be maintained within the expected pressure range by controlling and adjusting the current exhaust volume of the exhaust gas, thereby achieving control of the conversion rate during the reaction process.

[0029] Specifically, when the current pressure of the reaction container is greater than the expected pressure, the exhaust volume of the tail gas is increased, and when the current pressure of the reaction container is less than the expected pressure, the exhaust volume of the tail gas is reduced.

[0030] In some embodiments, in step S4, the exhaust gas may be sucked by a suction device to change the exhaust volume of the exhaust gas. In this embodiment, the exhaust device is used to provide power for exhaust gas discharge, so that when the current pressure of the reaction container is greater than the expected pressure, the exhaust speed is accelerated and the exhaust volume is increased, thereby achieving timely adjustment of the internal pressure of the reaction container and reducing the gap between the internal pressure of the reaction container and the expected pressure.

[0031] In some embodiments, in step S4, the opening and closing degree of the valve of the tail gas pipeline can also be used to control the exhaust volume of the tail gas. In this embodiment, by controlling the opening and closing degree of the valve of the tail gas pipeline, when the current pressure of the reaction vessel is less than the expected pressure, the opening and closing degree of the valve is reduced, or, when the current pressure of the reaction vessel is greater than the expected pressure, the opening and closing degree of the valve is increased, thereby changing the exhaust volume of the tail gas, achieving accurate control of the internal pressure of the reaction vessel, and reducing the gap between the internal pressure of the reaction vessel and the expected pressure.

[0032] Furthermore, in step S4, the suction device can cooperate with the valve that controls the exhaust gas pipeline. When the current pressure of the reaction container is greater than the expected pressure, the opening degree of the valve is increased, and the exhaust gas is sucked together with the suction device to further increase the exhaust speed, increase the exhaust volume, and further accelerate the adjustment rate of the internal pressure of the reaction container, thereby ensuring precise control of the conversion rate during the reaction process.

[0033] In some embodiments, in step S4, a regulating valve is provided on the exhaust pipe of the reaction container, and the regulating valve is used to adjust the exhaust gas emission to improve the regulation accuracy of the exhaust gas emission, thereby further achieving precise control of the internal pressure of the reaction container.

[0034] 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 being greater than a predetermined value, resulting in excessive pressure in the reaction container and excessively fast conversion rate.

[0035] In some embodiments, in step S4, the amount of inert gas input can be increased according to the determined pressure to avoid the tail gas concentration being greater than a predetermined value, which would result in excessive pressure in the reaction container and excessively fast conversion rate.

[0036] In some embodiments, in step S5, the reaction temperature in the reaction container is monitored in real time, and based on the real-time temperature, it is determined whether the heating is terminated, so that the reaction temperature in the reaction container reaches a predetermined temperature.

[0037] For example, a thermocouple may be used to control the heating temperature of the reaction container and monitor the reaction temperature inside the reaction container in real time.

[0038] In step S6, the inert gas is stopped from being supplied, and a reaction gas, for example, a mixture of steam and nitrogen, a mixture of steam and argon, or a mixture of steam and air, is supplied to the reaction container.

[0039] In some embodiments, in step S7, the reaction rate of the reaction is determined based on the change rate of the predetermined component in the exhaust gas, so as to judge the reaction progress based on the current reaction rate, thereby judging whether the conversion of the cerium sample into oxide is completed, and avoiding excessive reaction time.

[0040] In step S7, since the reaction gas input into the reaction container 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 of the reaction can be determined based on the change rate of hydrogen in the exhaust gas, and when the change rate of hydrogen approaches 0 within a certain period of time, it can be determined that the conversion of the sample into oxides is complete; when the reaction gas is a mixture of steam and nitrogen, the reaction rate of the reaction can also be determined based on the change rate of ammonia in the exhaust gas.

[0041] In some embodiments, in step S7, the reaction parameters may be determined according to the determined reaction rate and the expected reaction rate. In this embodiment, the reaction parameters are determined by the current reaction rate and the expected reaction rate, so that when the current reaction rate cannot meet the expected requirements, the current reaction parameters are adjusted according to the determined reaction parameters, thereby adjusting the current conversion rate to achieve the expected conversion rate.

[0042] Among them, the reaction parameters may include reaction temperature, steam concentration, gas composition, gas flow rate, pressure, etc.

[0043] In some embodiments, step S7 may further include the following steps:

[0044] S71: Determine the relationship between conversion rate and reaction temperature.

[0045] S72: Determine the desired reaction temperature based on the relationship.

[0046] In this embodiment, a relationship between the conversion rate and the reaction temperature during the reaction process is established to determine the desired reaction temperature of the reaction process based on this relationship, thereby facilitating adjustment of the current reaction temperature to reduce the difference between the current conversion rate and the desired conversion rate.

[0047] In some embodiments, in step S71, the following steps may also be included:

[0048] S711: Obtain multiple conversion rates and the reaction temperature corresponding to each conversion rate.

[0049] S712: According to the conversion rate and reaction temperature obtained in step S711, a relationship curve between the conversion rate and the reaction temperature is determined.

[0050] S713: Determine the relationship between the conversion rate and the reaction temperature according to the relationship curve.

[0051] S714: Determine a relationship curve between conversion rate and reaction temperature according to the relationship.

[0052] In this embodiment, a relationship curve between conversion rate and reaction temperature is determined through multiple conversion rates and their corresponding multiple reaction temperatures, a relationship equation between conversion rate and reaction temperature is determined based on the relationship curve, and the relationship curve is determined through the relationship equation to obtain a curve that can accurately reflect the relationship between conversion rate and reaction temperature, thereby facilitating accurate acquisition of the current reaction temperature through the current conversion rate.

[0053] Specifically, in step S712, the multiple conversion rates obtained and the reaction temperatures corresponding to 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 it does not meet the requirements, the fitting method and data can be optimized and adjusted, and a new relationship can be obtained again; in step S714, a relationship curve is drawn based on the new relationship so that the curve can more accurately reflect the relationship between the conversion rate and the reaction temperature.

[0054] In some embodiments, in step S71, the following steps may also be included:

[0055] S715: Using the value between the conversion rate and the reaction temperature obtained in the experiment, calibrate the relationship curve obtained in step S714.

[0056] S716: Update the relationship curve according to the correction result of step S715.

[0057] S717: Determine an updated relationship between the conversion rate and the reaction temperature according to the relationship curve updated in step S716.

[0058] S718: Determine an updated relationship curve between conversion rate and reaction temperature according to the relationship equation updated in step S717.

[0059] In this embodiment, the values ​​of conversion rate and reaction temperature obtained in the experiment are used to verify whether the relationship curve determined according to the relationship formula in step S714 can accurately reflect the relationship between the conversion rate and the reaction temperature, and the relationship curve is updated according to the correction result, the relationship formula is re-determined, and then a new relationship curve is obtained according to the relationship formula to further improve the accuracy of the relationship curve.

[0060] Specifically, in step S715, the values ​​of conversion rate and reaction temperature not used in step S711 can be used to verify the accuracy of the relationship curve, and determine the parts of the relationship curve that need to be corrected, such as the slope and intercept of the curve; in step S716, according to the specific needs of the curve correction, a suitable method is selected to refit the data to update the relationship curve; in step S717, the updated relationship between the conversion rate and the reaction temperature is determined according to the updated relationship curve, and it is determined whether the goodness of fit of the relationship meets the predetermined requirements; in step S718, the relationship curve is drawn according to the updated relationship to obtain a curve that can further accurately reflect the relationship between the conversion rate and the reaction temperature.

[0061] In some embodiments, in step S8, the humidity of the tail gas is monitored, and based on the humidity of the tail gas, it is determined that the reaction gas has been completely discharged to avoid affecting the subsequent reaction of converting the cerium sample into oxides, resulting in a decrease in the performance and quality of the oxidation product.

[0062] Specifically, in step S8, after the reaction is completed, an inert gas is input into the reaction container 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 does not contain moisture, and it can be determined that the reaction gas, i.e., steam, in the reaction container has been completely discharged.

[0063] Before step S1, the method may further include preparing a sample of the cerium (Ce) material.

[0064] Specifically, when the cerium (Ce) material is made into a sample, the following steps S100 to S800 may be included:

[0065] S100: molten cerium material.

[0066] S200: The melt obtained in step S100 is cast into an ingot.

[0067] S300: Divide the molded product obtained in step S200.

[0068] S400: storing the fraction obtained in step S300 in a first organic solvent.

[0069] S500: removing surface oxides from the partitioned product in a first organic solvent.

[0070] S600: taking out the product obtained in step S500 from the first organic solvent, and removing the first organic solvent on the surface of the product by using a second organic solvent.

[0071] S700: removing the second organic solvent on the surface of the product.

[0072] S800: Determine whether the second organic solvent is completely removed.

[0073] In this embodiment, the cerium material is melt-cast and divided to obtain the divided product, which is stored in a first organic solvent and treated in the first organic solvent to remove the oxide on its surface while isolating the divided product from the air to prevent it from burning. Thereafter, the first organic solvent is removed from the surface of the product using a second organic solvent, and the second organic solvent is completely removed to minimize the impurity content in the finally obtained cerium sample, effectively improving the purity of the cerium sample and thus ensuring the accuracy of subsequent experiments.

[0074] In some embodiments, in step S100, the following steps are also included:

[0075] S101: Determine the temperature of the melt in real time.

[0076] S102: Determine the heating power of the melting operation according to the temperature determined in step S101 and the predetermined temperature.

[0077] In this embodiment, the current temperature of the melt is determined in real time and compared with the predetermined temperature to determine the heating power required for the melting operation, thereby facilitating adjustment of the heating power and further removing impurities in the melt.

[0078] In step S102, the predetermined temperature is the temperature at which the cerium material melts and at which the purity of the obtained melt is the highest.

[0079] In step S200, the molten ingot obtained in step S100 may be formed into a cake-like object so as to be subsequently divided into shapes and sizes that meet predetermined requirements.

[0080] In some embodiments, in step S300, the segmentation operation may be performed under an inert gas atmosphere to prevent the molded object obtained in step S200 from reacting with oxygen to generate oxides during the segmentation process.

[0081] For example, dry ice may be used to create an inert gas atmosphere to isolate the molded object from oxygen, while cooling the cutting operation to prevent the molded object from self-igniting.

[0082] In some embodiments, in step S300, the following steps may also be included:

[0083] S301: Cutting the molded object obtained in step S200 into a columnar object of a predetermined size.

[0084] S302: Segment the columnar material obtained in step S301.

[0085] In this embodiment, the formed object obtained in step S200 is cut into columns of a predetermined size, and then the columns are divided into small segments of a predetermined size, so as to obtain a cerium sample that meets the predetermined requirements.

[0086] In step S400, after the partition is obtained, the partition is immediately transferred to a first organic solvent for storage to isolate oxygen and prevent the partition from burning. For example, the first organic solvent may be kerosene.

[0087] In step S500 , the surface of the partition may be polished with sandpaper in the first organic solvent to remove oxides on the surface of the partition.

[0088] In step S600, the product obtained after removing the surface oxide is taken out from the first organic solvent and placed in a second organic solvent to remove the first organic solvent on the surface of the product. For example, the second organic solvent may be ethanol.

[0089] In some embodiments, in step S700, an inert gas may be used to continuously purge the surface of the product to remove the second organic solvent on the surface of the product, thereby preventing the product from undergoing an oxidation reaction and generating oxides again.

[0090] The second organic solvent is a volatile solvent, which is easy to volatilize when the surface of the product is continuously purged with an inert gas, thereby facilitating complete removal of the second organic solvent and improving the purity of the cerium sample.

[0091] In some embodiments, step S700 may further include the following steps:

[0092] S701: Place the product in a sealed container.

[0093] S702: Evacuate the sealed container.

[0094] S703: Introduce inert gas into the sealed container to purge the product.

[0095] 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 therein, so as to continuously purge the surface of the product with the inert gas, remove the second organic solvent in an environment isolated from oxygen, and avoid oxidation of the product in the process as much as possible.

[0096] Before step S701, before placing the product in a sealed container, the sealed container may be converted into an inert gas atmosphere to prevent the product from being oxidized by the air inside the sealed container when placed in the sealed container.

[0097] In some embodiments, in step S700, the following steps may also be included:

[0098] S704: Collect exhaust gas discharged from the sealed container.

[0099] S705: Determine the components in the exhaust gas.

[0100] In step S800, it is determined that the second organic solvent is completely removed according to the components of the tail gas determined in step S705.

[0101] In this embodiment, the tail gas discharged from the sealed container is collected and its components are determined to facilitate judgment on whether the second organic solvent is completely removed. The judgment result is highly accurate and effectively avoids residual components of the second organic solvent.

[0102] Specifically, in step S704, while introducing inert gas into the sealed container, the exhaust gas discharged from the sealed container can be continuously collected, and the components of 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.

[0103] In some embodiments, step S800 may further include the following steps:

[0104] S801: After the product is placed in the sealed container but before the inert gas is introduced, weigh the sealed container.

[0105] S802: In step S703, the sealed container is continuously weighed.

[0106] S803: According to the weighing result in step S802 and the weighing result in step S801, it is determined whether the second organic solvent is completely removed.

[0107] In this embodiment, by comparing the weight of the sealed container before and after the product is purged with the inert gas, it is convenient to efficiently and directly determine whether the second organic solvent is completely removed.

[0108] Specifically, in step S801, after the product is placed in a sealed container and the sealed container is evacuated, the sealed container is weighed, and then an inert gas is input into the sealed container; in step S802, after the inert gas is input, the sealed container is continuously weighed to obtain multiple weighing results of the sealed container after the inert gas is input; 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.

[0109] In some embodiments, step S800 may further include the following steps:

[0110] S804: In step S703, the sealed container is continuously weighed.

[0111] S805: According to the weighing result in step S804, it is determined whether the second organic solvent is completely removed.

[0112] In this embodiment, the sealed container is continuously weighed, and the weight change thereof is used to more efficiently and directly determine whether the second organic solvent has been completely removed.

[0113] Specifically, in step S804, after the inert gas is input into the sealed container, the sealed container is continuously weighed to obtain multiple weighing results; in step S805, when it is observed that the 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.

[0114] In some embodiments, the first organic solvent is soluble in the second organic solvent, so that the second organic solvent can remove the first organic solvent from the surface of the product.

[0115] In some embodiments, in step S5, when the reaction container is heated to a predetermined temperature, the following method for determining the temperature inside the reaction container can be used to determine whether the temperature inside the reaction container has reached the predetermined temperature. The method includes the following steps S10 to S80:

[0116] S10: multiple temporary temperature measuring components are arranged in the reaction container, and are arranged to measure the temperature in the reaction container.

[0117] S20: multiple temperature measuring elements are arranged on the heating element to measure the temperature of the heating element.

[0118] S30: Start the heating element to heat the reaction container to a predetermined temperature.

[0119] S40: using a temperature measuring element to determine when the heating element reaches a predetermined temperature and remains constant, and using a temporary temperature measuring element to determine the temperature in the reaction container when the temperature remains constant.

[0120] S50: changing the predetermined temperature of step S30 within the design temperature range of the heating element, and repeating step S40 to obtain the predetermined temperatures of the plurality of heating elements and the corresponding temperatures in the reaction container.

[0121] S60: Determine the relationship between the predetermined temperature of the heating element and the temperature in the reaction container according to the predetermined temperature of the heating element and the temperature in the reaction container obtained in step S50.

[0122] S70: Remove the temporary temperature measuring device.

[0123] S80: In actual use, the current temperature of the heating element is obtained, and the temperature inside the reaction container is determined according to the relationship determined in step S60.

[0124] The method provided in the embodiments of the present application utilizes a temporary temperature measuring device and a temperature measuring device to respectively measure the temperature of a reaction container and a heating device, so as to obtain predetermined temperatures of a plurality of heating devices and the temperature in the corresponding reaction container after adjusting the set temperature of the heating device, and determine the relationship between the predetermined temperature of the heating device and the temperature in the reaction container accordingly, so that in actual use, the current temperature in the reaction container can be accurately determined based on the relationship by obtaining the temperature of the heating device, without setting a temperature measuring device in the reaction container to avoid interfering with the normal reaction in the furnace, thereby achieving accurate and timely regulation of the temperature in the reaction container, while avoiding affecting the quality and performance of the product generated in the reaction container.

[0125] In some embodiments, in step S10, a temporary temperature measuring device is set up in the following manner: within the range from the center of the reaction container to the furnace wall of the reaction container, a temporary temperature measuring device is set at a predetermined interval to measure the temperature at different positions in the lateral space of the reaction container to ensure that the temperature measurement result can reflect the actual temperature in the reaction container.

[0126] For example, according to the radius value of the reaction container, a temporary temperature measuring component can be set at every interval of 1 / 4 of the radius value within the range from the center of the reaction container to the furnace wall of the reaction container, so that the temporary temperature measuring components are evenly distributed in the lateral space within the reaction container.

[0127] In some embodiments, in step S10, a temporary temperature measuring component is set up in the following manner: a temporary temperature measuring component is set at a predetermined interval in the range from the bottom to the top of the reaction container to measure the temperature at different heights in the reaction container to ensure that the temperature measurement result can reflect the actual temperature in the reaction container.

[0128] For example, according to the height value of the reaction container, a temporary temperature measuring component can be set at every interval of 1 / 4 of the height value along the center line of the reaction container within the range from the bottom to the top of the reaction container, so that the temporary temperature measuring components are evenly distributed in the longitudinal space within the reaction container.

[0129] In some embodiments, in step S20, the temperature measuring element is set in the following manner: a temperature measuring element is set at a predetermined distance from the bottom to the top of the heating element to measure the temperature at different heights of the heating element to ensure that the temperature measurement result can reflect the actual temperature of the heating element.

[0130] For example, according to the height value of the heating element, a temperature measuring element can be set at every 1 / 4 of the height value 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.

[0131] In some embodiments, in step S30, when the heating element is started to heat the reaction container to a predetermined temperature, the heating rate is less than a predetermined value to avoid the heating rate being too fast, which may cause the temperature in the reaction container to be unable to stabilize at the predetermined temperature.

[0132] For example, the predetermined value of the heating rate may be set to 10° C. / min. When the reaction container is heated to the predetermined temperature, the heating element is set to heat at a rate less than 10° C. / min.

[0133] In step S40, after the temperature measuring element determines that the heating element has reached a predetermined temperature T i When the temperature T in the reaction container is kept constant, a plurality of temporary temperature measuring devices arranged in the reaction container are used to determine the temperature T in the reaction container when the temperature is kept constant. j For example, the temperature is kept constant for no less than 30 minutes.

[0134] In some embodiments, in steps S30 to S40, the heating method is set to be the same as that in the reaction operation using a reaction container, so as to simulate the working conditions during actual use as much as possible, so that the temperature in the reaction container is closer to the temperature during actual use, thereby making the relationship between the heating element and the temperature in the reaction container determined subsequently more reliable.

[0135] In some embodiments, in steps S30 to S40, it also includes inputting an inert gas of a predetermined pressure into the reaction container. The method of inputting the inert gas is the same as that of using the reaction container for reaction operation, so as to further simulate the working conditions during actual use, thereby making the subsequently determined relationship between the heating element and the temperature in the reaction container more reliable.

[0136] 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 is set to be less than a predetermined value, for example, less than 10°C / min; and step S40 is repeated to obtain the predetermined temperatures of multiple heating elements and the temperatures in multiple reaction containers corresponding thereto.

[0137] In step S60, the relationship between the predetermined temperature of the heating element and the temperature in the reaction container can be determined based on the predetermined temperatures of the multiple heating elements obtained in step S50 and the temperatures in the multiple reaction containers, wherein the predetermined temperature of the heating element can be the temperature of the heating element measured by a temperature measuring element.

[0138] In some embodiments, step S60 may further include the following steps:

[0139] S61: Determine a relationship curve between the predetermined temperature of the heating element and the temperature in the reaction container according to the predetermined temperature of the heating element and the temperature in the reaction container obtained in step S50.

[0140] S62: Determine a relationship between the predetermined temperature of the heating element and the temperature in the reaction container according to the relationship curve.

[0141] S63: Determine the predetermined temperature of the heating element and the relationship curve in the reaction container according to the relationship expression.

[0142] In this embodiment, the predetermined temperatures of multiple heating elements and the corresponding temperatures in multiple reaction containers are used to determine a relationship curve between the predetermined temperature of the heating element and the temperature in the reaction container. The relationship equation between the predetermined temperature of the heating element and the temperature in the reaction container is determined based on the relationship curve, and the relationship curve is determined through the relationship equation to obtain a curve that can accurately reflect the relationship between the predetermined temperature of the heating element and the temperature in the reaction container, thereby improving the accuracy of the current temperature in the reaction container obtained by the current temperature of the heating element in actual use.

[0143] Specifically, in step S61, the predetermined temperatures of the multiple heating elements and the temperature in the reaction container corresponding to each predetermined temperature are fitted to obtain a curve reflecting the relationship between the predetermined temperature of the heating element and the temperature in the reaction container; in step S62, the relationship between the predetermined temperature of the heating element and the temperature in the reaction container is determined according to the relationship curve, and it is judged whether the goodness of fit of the relationship meets the predetermined requirements. If it does not meet the requirements, the fitting method and data can be optimized and adjusted, and a new relationship can be obtained again; in step S63, a relationship curve is drawn according to the new relationship so that the curve can more accurately reflect the relationship between the predetermined temperature of the heating element and the temperature in the reaction container.

[0144] In some embodiments, in step S60, the following steps are also included:

[0145] S64: Correcting the relationship curve obtained in step S63 according to the predetermined temperature of the heating element obtained in step S50 and the temperature in the reaction container.

[0146] S65: Update the relationship curve according to the correction result of step S64.

[0147] S66: Determine an updated relationship between the predetermined temperature of the heating element and the temperature in the reaction container according to the relationship curve updated in step S65.

[0148] S67: According to the relationship equation updated in step S66, an updated relationship curve between the predetermined temperature of the heating element and the temperature in the reaction container is determined.

[0149] In this embodiment, the predetermined temperature of the heating element and the temperature in the reaction container obtained in step S50 are used to verify whether the relationship curve determined according to the relationship formula in step S63 can accurately reflect the relationship between the predetermined temperature of the heating element and the temperature in the reaction container, and the relationship curve is updated according to the correction result, the relationship formula is re-determined, and then a new relationship curve is obtained according to the relationship formula to further improve the accuracy of the relationship curve.

[0150] Specifically, in step S64, the values ​​of the predetermined temperature of the heating element and the temperature in the reaction vessel that were not used when the relationship curve was initially determined in step S61 can be used to verify the accuracy of the relationship curve and determine the part of the relationship curve that needs to be corrected, such as the slope and intercept of the curve; in step S65, according to the specific needs of the curve correction, a suitable method is selected to refit the data to update the relationship curve; in step S66, the updated relationship equation of the predetermined temperature of the heating element and the temperature in the reaction vessel is determined according to the updated relationship curve, and it is determined whether the goodness of fit of the relationship equation meets the predetermined requirements; in step S67, the relationship curve is drawn based on the updated relationship equation to obtain a curve that can further accurately reflect the relationship between the predetermined temperature of the heating element and the temperature in the reaction vessel.

[0151] The following is a specific example to further illustrate the process of converting a cerium (Ce) sample into oxides in the present application.

[0152] Place the sample in a sealed reaction container; set the reaction container to an inert atmosphere, and use a vacuum replacement method to first evacuate the interior of the reaction container, then input inert gas into it to make the internal pressure of the reaction container reach a predetermined value, then evacuate the reaction container and input inert gas, and repeat the above steps 2-3 times to completely replace the oxygen inside the reaction container; determine the pressure control range value of the reaction container; use a pressure monitoring device to determine the current pressure inside the reaction container; determine the exhaust volume of the exhaust gas based on the determined current pressure of the reaction container and the expected pressure, and use a suction device and a valve that controls the exhaust gas pipeline to adjust the current exhaust volume of the exhaust gas; heat the reaction container, and monitor the reaction temperature in the reaction container in real time, and determine whether the heating is completed based on the real-time temperature, until The temperature in the reaction container reaches a predetermined temperature; the input of inert gas is stopped, and a mixture of steam and nitrogen, or a mixture of steam and argon, or a mixture of steam and air is input into the reaction container; the tail gas of the reaction container is monitored, and the reaction rate of the reaction is determined according to the rate of change of the predetermined components in the tail gas, and the reaction progress is determined according to the current reaction rate, thereby determining the end of the reaction; when the current reaction rate cannot meet the expected requirements, the reaction parameters are determined according to the determined reaction rate and the expected reaction rate, and the current reaction parameters are adjusted according to the determined reaction parameters; after determining that the reaction is over, an inert gas is input into the reaction container, and the humidity of the tail gas is monitored at the same time, and it is determined that the reaction gas is completely discharged according to the humidity of the tail gas. After determining that the reaction gas is completely discharged, the inert gas is continuously input into the reaction container until the reaction container is cooled.

[0153] Regarding the embodiments of the present application, it should also be noted that, in the absence of conflict, the embodiments of the present application and the features therein can be combined with each other to obtain new embodiments.

[0154] The above are only specific implementation methods of the present application, but the protection scope of the present application is not limited thereto. The protection scope of the present application shall be based on the protection scope of the claims.

Claims

1. A method for converting a sample of cerium (Ce) into oxides based on reaction tail gas, characterized in that: It includes the following steps: S1: placing the sample in a sealed reaction container; S2: setting the reaction vessel to an inert atmosphere; S3: Determine the current pressure of the reaction container; S4: during the reaction process, determining the exhaust volume of the tail gas of the reaction container according to the pressure determined in step S3; S5: heating the reaction container to a predetermined temperature; S6: stop inputting the inert gas, and input the reaction gas into the reaction container; S7: monitoring the tail gas of the reaction container to determine the end of the reaction; S8: After determining that the reaction is finished, an inert gas is introduced into the reaction container until the reaction container is cooled.

2. The method according to claim 1, characterized in that In step S4, the exhaust volume of the exhaust gas is determined according to the determined pressure and the expected pressure.

3. The method according to claim 2, characterized in that In step S4, the exhaust gas is sucked by a suction device to change the exhaust volume of the exhaust gas.

4. The method according to claim 2, characterized in that: In step S4, the exhaust volume of the exhaust gas is changed by controlling the opening and closing degree of the valve of the exhaust gas pipeline.

5. The method according to claim 1, characterized in that: In step S5, the reaction temperature in the reaction container is monitored in real time, and whether the heating is finished is determined based on the real-time temperature.

6. The method according to claim 1, characterized in that In step S7, the reaction rate of the reaction is determined according to the change rate of the predetermined component in the exhaust gas.

7. The method according to claim 6, characterized in that In step S7, reaction parameters are determined according to the determined reaction rate and the expected reaction rate.

8. The method according to claim 1, characterized in that In step S8, the humidity of the tail gas is monitored, and based on the humidity of the tail gas, it is determined that the exhaust of the reaction gas is complete.

9. The method according to claim 6, characterized in that In step S7, the following steps are also included: S71: Determine the relationship between conversion rate and reaction temperature; S72: Determine the desired reaction temperature according to the relationship.

10. The method according to claim 6, characterized in that In step S71, the following steps are also included: S711: Obtain multiple conversion rates and a reaction temperature corresponding to each conversion rate; S712: Determine a relationship curve between the conversion rate and the reaction temperature according to the conversion rate and the reaction temperature obtained in step S711; S713: Determine a relationship between the conversion rate and the reaction temperature according to the relationship curve; S714: Determine a relationship curve between the conversion rate and the reaction temperature according to the relationship equation.

11. The method according to claim 10, characterized in that In step S71, the following steps are also included: S715: using the value between the conversion rate and the reaction temperature obtained in the experiment, calibrating the relationship curve obtained in step S714; S716: updating the relationship curve according to the correction result of step S715; S717: Determine an updated relationship between the conversion rate and the reaction temperature according to the relationship curve updated in step S716; S718: Determine an updated relationship curve between the conversion rate and the reaction temperature according to the relationship equation updated in step S717.

12. The method according to claim 1, characterized in that In step S4, a regulating valve is provided on the tail gas pipeline of the reaction container, and the tail gas emission is regulated by the regulating valve.

13. The method according to claim 1, characterized in that In step S4, the amount of input reaction gas is reduced according to the determined pressure to prevent the tail gas concentration from being greater than a predetermined value.

14. The method according to claim 1, characterized in that In step S4, the amount of inert gas input is increased according to the determined pressure to prevent the tail gas concentration from being greater than a predetermined value.

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