Method for preparing ammonium salt by using metal cerium block

Abstract

The embodiment of the invention relates to the technical field of preparation of amino-containing compounds, in particular to a method for preparing ammonium salt by using a metal cerium block, which comprises the following steps: S10: treating the metal cerium block to enable the metal cerium block to be suitable for reaction; s20, the treated metal cerium block is placed in a sealed reaction container; s30, setting the reaction container in an inert atmosphere; s40, heating the reaction container to a preset temperature; s50, stopping inputting the inert gas into the reaction container, and inputting a mixed gas of H2O and N2 into the reaction container; s60, collecting gas from the reaction container, inputting the gas into dilute acid corresponding to the ammonium salt to be prepared, and reacting the gas with the dilute acid to obtain the ammonium salt; and S70, determining that the metal cerium block is completely reacted according to the gas in the step S60. By utilizing the method, the ammonia gas can be prepared in a relatively low temperature environment, the ammonium salt can be prepared without keeping a high-temperature and high-pressure reaction environment for a long time, the consumption of resources and energy is effectively reduced, and meanwhile, the safety risk of preparing the ammonium salt is reduced.

Description

Technical Field

[0001] The embodiments of the present application relate to the technical field of preparation of amino-containing compounds, and specifically to a method for preparing ammonium salts using metal cerium blocks. Background Art

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

[0003] Ammonium salt is a compound composed of ammonium ions and acid anions. Common ammonium salts include ammonium chloride, ammonium nitrate, ammonium sulfate, etc. They are widely used in agriculture, chemical industry, medicine and other fields. They are usually prepared by the reaction of ammonia and acid. However, the common methods for preparing ammonium salts currently require reactions to be carried out under high temperature and high pressure environments, which have certain risks and limitations. Summary of the invention

[0004] 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.

[0005] The embodiment of the present application provides a method for preparing ammonium salt using a metal cerium block, which comprises the following steps: S10: treating the metal cerium block to make it suitable for reaction; S20: placing the treated metal cerium block in a sealed reaction container; S30: setting the reaction container to an inert atmosphere; S40: heating the reaction container to a predetermined temperature; S50: stopping the inert gas input into the reaction container and inputting H into the reaction container. 2 O and N 2 mixed gas; S60: collecting the gas from the reaction container, and inputting the gas into the dilute acid corresponding to the ammonium salt to be prepared, and the gas reacts with the dilute acid to obtain the ammonium salt; S70: according to the gas in step S60, determining whether the reaction of the metal cerium block is complete.

[0006] The method in the embodiment of the present application uses a metal cerium block as a raw material, which is mixed with H in a sealed environment. 2 O and N 2 The mixed gas reacts to generate ammonia, so that the preparation of ammonia can be achieved under a relatively low temperature environment. The ammonium salt is then obtained by reacting the ammonia with a dilute acid corresponding to the ammonium salt to be prepared. Thus, the preparation of the ammonium salt can be achieved without maintaining a high temperature and high pressure reaction environment for a long time, thereby effectively reducing the consumption of resources and energy, and at the same time reducing the safety risk of preparing the ammonium salt. BRIEF DESCRIPTION OF THE DRAWINGS

[0007] 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.

[0008] Figure 1 The present invention is a flowchart of a method for preparing ammonium salt using a metal cerium block according to an embodiment of the present application.

[0009] 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

[0010] 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.

[0011] It is also necessary to explain here that, in order to avoid obscuring the present application due to unnecessary details, the accompanying drawings only show the device structure and / or processing steps that are closely related to the scheme according to the present application, while other details that are not closely related to the present application are omitted.

[0012] The inventors of the present application have discovered that the commonly used method for preparing ammonium salts is generally to synthesize ammonia gas by using nitrogen and hydrogen in the presence of a catalyst under a high temperature and high pressure environment, and then to generate ammonium salts by reacting the ammonia gas with an acid. The high temperature environment will cause the catalyst activity to decrease or become ineffective, resulting in a large consumption of the catalyst. In addition, since ammonium salts have poor thermal stability and are easily decomposed by heat, leading to explosion, there are certain safety risks in preparing them in a high temperature and high pressure environment.

[0013] Based on this, the embodiment of the present application provides a method for preparing ammonium salt using metal cerium block, such as Figure 1 As shown, Figure 1 A flow chart showing a method for preparing ammonium salt using a metal cerium block according to an embodiment of the present application is shown. The method comprises the following steps S10 to S70:

[0014] S10: Treating the metal cerium block to make it suitable for reaction.

[0015] S20: placing the treated metal cerium block in a sealed reaction container.

[0016] S30: The reaction container is set to an inert atmosphere.

[0017] S40: heating the reaction container to a predetermined temperature.

[0018] S50: Stop the inert gas input into the reaction vessel and input H 2 O and N 2 Mixed gas.

[0019] S60: collecting gas from the reaction container, and inputting the gas into the dilute acid corresponding to the ammonium salt to be prepared, and the gas reacts with the dilute acid to obtain the ammonium salt.

[0020] S70: Determine that the reaction of the metal cerium block is complete based on the gas in step S60.

[0021] The method provided in the embodiment of the present application uses a metal cerium block as a raw material, and makes it react with H in a sealed environment. 2 O and N 2 The mixed gas reacts to generate ammonia, so that the preparation of ammonia can be achieved under a relatively low temperature environment. The ammonium salt is then obtained by reacting the ammonia with a dilute acid corresponding to the ammonium salt to be prepared. Thus, the preparation of the ammonium salt can be achieved without maintaining a high temperature and high pressure reaction environment for a long time, thereby effectively reducing the consumption of resources and energy, and at the same time reducing the safety risk of preparing the ammonium salt.

[0022] In some embodiments, in step S10, the treatment of the metal cerium block is configured to remove the surface oxide layer of the metal cerium block to ensure that it is in contact with H. 2 O and N 2 The mixed gas reacts fully, and at the same time, the oxidation layer is prevented from affecting the quality and purity of the generated ammonium salt.

[0023] In some embodiments, step S10 may further include:

[0024] S101: placing a metal cerium block in an organic solvent.

[0025] S102: removing the surface oxide layer of the metal cerium block in an organic solvent.

[0026] In this embodiment, the metal cerium block is placed in an organic solvent to remove the oxide layer on its surface, so as to isolate the metal cerium block from the air to prevent it from burning during the process of removing the oxide layer, while improving the removal effect of the oxide layer to prevent it from being oxidized again during the removal of the oxide layer.

[0027] In some embodiments, after performing step S102, a step of removing the organic solvent and a step of detecting the removal of the organic solvent on the surface of the metal cerium block are also included to ensure that there is no organic solvent residue on the surface of the metal cerium block to avoid interference with the reaction and affect the quality and purity of the generated ammonium salt.

[0028] In some embodiments, in step S30, when the reaction vessel is set to an inert atmosphere, it can also include: collecting the gas exhausted from the reaction vessel, and determining whether the organic solvent in the metal cerium block is completely removed based on the weight of the gas, so as to further ensure the quality and purity of the generated ammonium salt.

[0029] Specifically, in step S30, a vacuum replacement method can be adopted, in which the interior of the reaction container is first evacuated, and then an inert gas is introduced into the reaction container to make the internal pressure of the reaction container reach a predetermined value, and then the reaction container is evacuated and an inert gas is introduced, and the above steps are repeated 2-3 times to completely replace the oxygen inside the reaction container; at this time, the gas discharged when the reaction container is evacuated can be collected, and the weight of the gas can be used. When the weight of the input gas is consistent with the weight of the collected output gas, it is determined that the organic solvent in the metal cerium block is completely removed.

[0030] In some embodiments, in step S40, when the reaction container is heated to a predetermined temperature, the predetermined temperature range is between 250°C and 350°C, so that the metal cerium block reacts with H in the temperature range. 2 O and N 2 The mixed gas reacts to generate ammonia, thereby achieving the preparation of ammonia under a lower temperature environment.

[0031] In some embodiments, in step S50, H is introduced into the reaction vessel. 2 O and N 2 During the mixing process, the interior of the reaction vessel is kept at normal pressure so that the metal cerium block can react with H 2 O and N 2 The mixed gas reacts to generate ammonia, thereby achieving the preparation of ammonia without maintaining a high-pressure environment.

[0032] H in the mixed gas 2 The proportion of O can be in the range of 30%-70%, so as to adjust the generation rate of ammonia according to the needs, thereby avoiding the reduction of the generation rate of ammonium salt due to insufficient ammonia or the waste of ammonia due to excessive ammonia. 2 On the contrary, when the generation rate of ammonia needs to be reduced, the proportion of H 2 The proportion of O.

[0033] In step S60, the composition of the dilute acid can be determined according to the ammonium salt to be prepared. For example, when the ammonium salts to be obtained are ammonium chloride, ammonium nitrate and ammonium sulfate, the composition of the dilute acid is hydrochloric acid, nitric acid and sulfuric acid.

[0034] In some embodiments, in step S70, the gas from the reaction container includes hydrogen. Based on the hydrogen, it is determined that the reaction of the metal cerium block is complete to ensure full utilization of the metal cerium block, improve resource utilization, and avoid waste.

[0035] Specifically, in step S70, since the metal cerium block is in contact with H 2 O and N 2 When the mixed gas reacts, the generated gases include ammonia and hydrogen. When it is determined that the gas from the reaction container does not include hydrogen, it can be determined that the metal cerium block has reacted completely.

[0036] In some embodiments, in step S70, the speed of the mixed gas input can be determined according to the rate of change of hydrogen in the gas from the reaction container.

[0037] In this embodiment, the change rate of hydrogen in the gas discharged from the current reaction container is used to determine whether the current reaction rate meets the predetermined requirements. For example, when the change rate of hydrogen is large, that is, the rate at which the amount of hydrogen increases is fast, it means that the current reaction rate is high. Therefore, the speed of inputting the mixed gas can be reduced or increased according to the actual needs of the current reaction process, thereby adjusting the reaction rate.

[0038] In the method for preparing ammonium salt using metal cerium block in the embodiment of the present application, the metal cerium block can be prepared by the following method, which includes the following steps S1 to S8:

[0039] S1: molten cerium material.

[0040] S2: The melt obtained in step S1 is cast into an ingot.

[0041] S3: Divide the molded product obtained in step S2.

[0042] S4: storing the fraction obtained in step S3 in a first organic solvent.

[0043] S5: removing surface oxides from the partitioned product in the first organic solvent.

[0044] S6: taking out the product obtained in step S5 from the first organic solvent, and removing the first organic solvent on the surface of the product by using a second organic solvent.

[0045] S7: removing the second organic solvent on the surface of the product.

[0046] S8: Determine that the second organic solvent is completely removed.

[0047] The method provided in the embodiment of the present application is to store the obtained split products by melt-casting and splitting the cerium material in a first organic solvent, and treat the split products in the first organic solvent to remove the oxides on the surface of the split products while isolating the split products from the air to prevent them from burning; then, use a second organic solvent to remove the first organic solvent on the surface of the product, and completely remove the second organic solvent to minimize the impurity content in the metal cerium block finally obtained, effectively improve the purity of the metal cerium block, and thus ensure the accuracy of subsequent experiments.

[0048] In some embodiments, in step S1, the following steps are also included:

[0049] S11: Determine the temperature of the melt in real time.

[0050] S12: Determine the heating power of the melting operation according to the temperature determined in step S11 and the predetermined temperature.

[0051] 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.

[0052] In step S12, the predetermined temperature is the temperature at which the cerium material melts and at which the purity of the obtained melt is the highest.

[0053] In step S2, the molten ingot obtained in step S1 may be formed into a cake-like object so as to be subsequently divided into shapes and sizes that meet predetermined requirements.

[0054] In some embodiments, in step S3, the segmentation operation may be performed under an inert gas atmosphere to prevent the molded product obtained in step S2 from reacting with oxygen to generate oxides during the segmentation process.

[0055] 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.

[0056] In some embodiments, in step S3, the following steps may also be included:

[0057] S31: Cutting the molded product obtained in step S2 into columns of a predetermined size.

[0058] S32: Segment the columnar material obtained in step S31.

[0059] In this embodiment, the formed object obtained in step S2 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 metal cerium block that meets predetermined requirements.

[0060] In step S4, after obtaining the partition, 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.

[0061] In step S5, the surface of the partition may be polished with sandpaper in the first organic solvent to remove oxides on the surface of the partition.

[0062] In step S6, 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.

[0063] In some embodiments, in step S7, 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.

[0064] 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 metal cerium block.

[0065] In some embodiments, step S7 may further include the following steps:

[0066] S71: Place the product in a sealed container.

[0067] S72: Evacuate the sealed container.

[0068] S73: Introduce inert gas into the sealed container to purge the product.

[0069] 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.

[0070] Before step S71, 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.

[0071] In some embodiments, in step S7, the following steps may also be included:

[0072] S74: Collect exhaust gas discharged from the sealed container.

[0073] S75: Determine the composition of the exhaust gas.

[0074] In step S8, it is determined that the second organic solvent is completely removed according to the components of the tail gas determined in step S75.

[0075] 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.

[0076] Specifically, in step S74, 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 S75. In step S8, when the exhaust gas components do not contain the second organic solvent, it is determined that the second organic solvent has been completely removed.

[0077] In some embodiments, step S8 may further include the following steps:

[0078] S81: After the product is placed in the sealed container but before the inert gas is introduced, weigh the sealed container.

[0079] S82: In step S73, the sealed container is continuously weighed.

[0080] S83: According to the weighing result in step S82 and the weighing result in step S81, it is determined whether the second organic solvent is completely removed.

[0081] 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.

[0082] Specifically, in step S81, after placing the product in a sealed container and evacuating the sealed container, the sealed container is weighed, and then an inert gas is input into the sealed container; in step S82, after inputting the inert gas, the sealed container is continuously weighed to obtain multiple weighing results of the sealed container after inputting the inert gas; in step S83, the multiple weighing results obtained in step S82 are compared with the weighing results in step S81 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.

[0083] In some embodiments, step S8 may further include the following steps:

[0084] S84: In step S73, the sealed container is continuously weighed.

[0085] S85: According to the weighing result in step S84, it is determined whether the second organic solvent is completely removed.

[0086] 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.

[0087] Specifically, in step S84, after the inert gas is input into the sealed container, the sealed container is continuously weighed to obtain multiple weighing results; in step S85, 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.

[0088] 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.

[0089] The following is a specific example to further illustrate the process of preparing ammonium salt using metal cerium blocks in the present application.

[0090] The metal cerium block is placed in an organic solvent, and the surface oxide layer of the metal cerium block is removed in the organic solvent, and the organic solvent is removed, and the removal of the organic solvent on the surface of the metal cerium block is detected; the treated metal cerium block is placed in a sealed reaction container; the reaction container is set to an inert atmosphere, and the inside of the reaction container is first evacuated by vacuum replacement, and then an inert gas is introduced into the reaction container to make the pressure inside the reaction container reach a predetermined value, and then the reaction container is evacuated and then an inert gas is introduced, and the above steps are repeated 2-3 times to completely replace the oxygen inside the reaction container; the reaction container is heated to between 250°C and 350°C; the inert gas is stopped from being introduced into the reaction container, and H is introduced into the reaction container 2 O and N 2 Mixed gas, H 2 O molar ratio is 30%-70%, and this process keeps the interior of the reaction container at normal pressure; collecting the gas from the reaction container, and inputting the gas into the dilute acid corresponding to the ammonium salt to be prepared, and the gas reacts with the dilute acid to obtain the ammonium salt; according to the gas in step S60, when it is determined that the gas from the reaction container does not include hydrogen, it is determined that the reaction of the metal cerium block is complete.

[0091] 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.

[0092] 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 preparing ammonium salt using metal cerium block, characterized in that: It includes the following steps: S10: treating the metal cerium block to make it suitable for reaction; S20: placing the treated metal cerium block in a sealed reaction container; S30: setting the reaction container to an inert atmosphere; S40: heating the reaction container to a predetermined temperature; S50: stop inputting the inert gas into the reaction container, and input a mixed gas of H2O and N2 into the reaction container; S60: collecting gas from the reaction container, and inputting the gas into a dilute acid corresponding to the ammonium salt to be prepared, wherein the gas reacts with the dilute acid to obtain the ammonium salt; S70: Determine, based on the gas in step S60, whether the reaction of the metal cerium block is complete.

2. The method according to claim 1, characterized in that In the step S40, the predetermined temperature range is between 250°C and 350°C.

3. The method according to claim 1, characterized in that In the step S50, during the process of inputting the mixed gas, the interior of the reaction container is maintained at normal pressure.

4. The method according to claim 1, characterized in that: In the step S70, the gas includes hydrogen, and the completion of the reaction of the metal cerium block is determined based on the hydrogen.

5. The method according to claim 4, characterized in that In the step S70, the speed of the mixed gas input is determined according to the change rate of the hydrogen.

6. The method according to claim 1, characterized in that In the step S10, the treatment is configured to remove a surface oxide layer of the metal cerium block.

7. The method according to claim 6, characterized in that The step S10 further includes: S11: placing the metal cerium block in an organic solvent; S12: removing the surface oxide layer of the metal cerium block in the organic solvent.

8. The method according to claim 7, characterized in that After the step S12 is performed, the method further includes the steps of removing the organic solvent and detecting the removal status of the organic solvent on the surface of the metal cerium block.

9. The method according to claim 8, characterized in that In step S30, it also includes: collecting the gas exhausted from the reaction vessel, Whether the organic solvent in the metal cerium block is completely removed is determined based on the weight of the gas.

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