CN114107772A - Preparation equipment and preparation method of sodium-potassium alloy - Google Patents
Preparation equipment and preparation method of sodium-potassium alloy Download PDFInfo
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- CN114107772A CN114107772A CN202111433144.2A CN202111433144A CN114107772A CN 114107772 A CN114107772 A CN 114107772A CN 202111433144 A CN202111433144 A CN 202111433144A CN 114107772 A CN114107772 A CN 114107772A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C24/00—Alloys based on an alkali or an alkaline earth metal
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
The invention provides a preparation device and a preparation method of a sodium-potassium alloy, wherein the preparation device of the sodium-potassium alloy comprises the following steps: the sodium-potassium alloy preparation container is used for preparing sodium-potassium alloy; the sodium storage device is connected with the sodium-potassium alloy preparation container to convey sodium to the sodium-potassium alloy preparation container; the potassium storage device is connected with the sodium-potassium alloy preparation container to convey potassium to the sodium-potassium alloy preparation container; an inert gas supply device which is communicated with the sodium-potassium alloy preparation container, the sodium storage device and the potassium storage device to provide inert gas; the sodium-potassium alloy proportion measuring device is connected with the sodium-potassium alloy preparation container so as to detect the proportion of the sodium-potassium alloy in the sodium-potassium alloy preparation container; and the adjusting device is used for adjusting the ratio of sodium and potassium conveyed to the sodium-potassium alloy preparation container.
Description
Technical Field
The invention belongs to the technical field of alloy preparation, and particularly relates to a preparation device and a preparation method of a sodium-potassium alloy.
Background
The sodium-potassium alloy is widely used in the industries of reactors, batteries and the like, and the physical properties of the sodium-potassium alloy have great difference along with the change of the sodium-potassium ratio, so the sodium-potassium ratio needs to be controlled in the preparation process. The related preparation method of the sodium-potassium alloy is to obtain sodium and potassium in a set proportion by adopting a weighing mode and then mix the sodium and the potassium, but the matching degree of the actual proportion of the sodium-potassium alloy prepared by the related preparation method and the set proportion is not high, and the proportion of the sodium-potassium alloy cannot be adjusted after the sodium-potassium alloy is prepared, so that the proportion accuracy of the sodium-potassium alloy preparation is low.
Disclosure of Invention
In view of this, the invention provides a preparation device and a preparation method of a sodium-potassium alloy, so as to solve the technical problem of how to improve the accuracy of the sodium-potassium ratio of the sodium-potassium alloy.
The technical scheme of the invention is realized as follows:
the embodiment of the invention provides a preparation device of a sodium-potassium alloy, which comprises:
the sodium-potassium alloy preparation container is used for preparing sodium-potassium alloy;
the sodium storage device is connected with the sodium-potassium alloy preparation container to convey sodium to the sodium-potassium alloy preparation container;
the potassium storage device is connected with the sodium-potassium alloy preparation container to convey potassium to the sodium-potassium alloy preparation container;
an inert gas supply device which is communicated with the sodium-potassium alloy preparation container, the sodium storage device and the potassium storage device to provide inert gas;
the sodium-potassium alloy proportion measuring device is connected with the sodium-potassium alloy preparation container so as to detect the proportion of the sodium-potassium alloy in the sodium-potassium alloy preparation container;
and the adjusting device is used for adjusting the ratio of sodium and potassium conveyed to the sodium-potassium alloy preparation container.
In some embodiments, further comprising:
and the sodium-potassium alloy purification device is connected with the sodium-potassium alloy preparation container and is used for removing impurities in the sodium-potassium alloy preparation container.
In some embodiments, further comprising:
and the electromagnetic pump is connected between the sodium-potassium alloy preparation container and the sodium-potassium alloy purification device and between the sodium-potassium alloy preparation container and the sodium-potassium alloy proportion measurement device so as to drive the sodium-potassium alloy in the sodium-potassium alloy preparation container to be conveyed to the sodium-potassium alloy purification device and the sodium-potassium alloy proportion measurement device.
In some embodiments, the adjustment device comprises:
the sodium adjusting piece is arranged between the sodium storage device and the sodium-potassium alloy preparation container and is used for opening and closing the communication between the sodium storage device and the sodium-potassium alloy preparation container;
and the potassium adjusting piece is arranged between the potassium storage device and the sodium-potassium alloy preparation container and is used for opening and closing the communication between the potassium storage device and the sodium-potassium alloy preparation container.
In some embodiments, the sodium conditioner comprises:
a first metering barrel communicated with the sodium-potassium alloy preparation container;
the first one-way valve is communicated with the sodium storage device and the first metering barrel so as to adjust the volume of sodium entering the first metering barrel from the sodium storage device;
the potassium regulating member includes:
the second metering barrel is communicated with the sodium-potassium alloy preparation container;
and the second one-way valve is communicated with the potassium storage device and the second metering barrel so as to adjust the volume of potassium entering the second metering barrel from the potassium storage device.
In some embodiments, level gauges are arranged in the sodium storage device and the potassium storage device.
The embodiment of the invention also provides a preparation method of the sodium-potassium alloy by adopting the preparation equipment, which comprises the following steps:
s1, opening the inert gas supply device, and filling inert gas into the sodium-potassium alloy preparation container, the sodium storage device and the potassium storage device to enable H in the gas in the sodium-potassium alloy preparation container, the sodium storage device and the potassium storage device2The content of O is less than or equal to 50 mu L/L, and O2The content of the (D) is less than or equal to 50 mu L/L;
s2, opening the sodium storage device and the potassium storage device, and closing the sodium storage device and the potassium storage device after conveying a first set amount of potassium and a second set amount of sodium into the sodium-potassium alloy preparation container according to the set proportion of the sodium-potassium content;
s3, preparing a sodium-potassium alloy in the sodium-potassium alloy preparation container;
s4, conveying the sodium-potassium alloy to the sodium-potassium alloy proportion measuring device to detect the current proportion of the sodium-potassium content in the sodium-potassium alloy;
s5, determining the supplement amount of sodium or potassium to be supplemented according to the difference value between the current proportion and the set proportion;
and S6, correspondingly opening the sodium storage device and the potassium storage device, and conveying the supplement amount of sodium or potassium to the sodium-potassium alloy preparation container.
In some embodiments, after step S3 and before step S4, further comprising:
and S35, sending the sodium-potassium alloy in the sodium-potassium alloy preparation container to a sodium-potassium alloy purification device at a set flow rate.
In some embodiments, the set flow rate is 0.1-1 m3/h。
In some embodiments, before step S2, the method further includes:
and heating the sodium-potassium alloy preparation container, the sodium storage device and the potassium storage device to 100-250 ℃.
The sodium-potassium alloy preparation equipment provided by the embodiment of the invention comprises a sodium-potassium alloy preparation container, a sodium storage device, a potassium storage device, an inert gas supply device, a sodium-potassium alloy proportion measuring device and an adjusting device, wherein sodium and potassium are introduced into the sodium-potassium alloy preparation container by adopting the sodium storage device and the potassium storage device so as to prepare the sodium-potassium alloy in the sodium-potassium alloy preparation container, the inert gas supply device is used for providing a stable inert gas reaction environment, the sodium-potassium alloy proportion measuring device can measure the proportion of the prepared sodium-potassium alloy in real time, and the adjusting device can adjust the sodium storage device or the potassium storage device to supplement sodium or potassium into the sodium-potassium alloy preparation container according to the difference value between the measured actual sodium-potassium proportion and the set proportion so as to adjust the actual sodium-potassium proportion. The embodiment of the invention realizes the detection of the proportion of the prepared sodium-potassium alloy through the sodium-potassium alloy proportion measuring device, can feed back the detected actual proportion of the sodium-potassium alloy to the adjusting device, and supplements sodium or potassium to the sodium-potassium alloy preparation container through the adjusting device according to the difference value of the actual proportion and the set proportion to realize the adjustment of the proportion of the sodium-potassium alloy, so that the actual proportion is consistent with the set proportion, and the accuracy of the proportion of the sodium and the potassium for preparing the sodium-potassium alloy is improved.
Drawings
FIG. 1 is a schematic structural diagram of a sodium-potassium alloy preparation apparatus according to an embodiment of the present invention;
FIG. 2 is a flow chart of the steps of a method for preparing a sodium-potassium alloy according to an embodiment of the present invention;
fig. 3 is a schematic structural diagram of a sodium-potassium alloy ratio measuring device in the embodiment of the present invention.
Description of reference numerals:
1. a sodium-potassium alloy preparation container; 2. a sodium storage device; 3. a potassium storage device; 4. an inert gas supply device; 5. a sodium-potassium alloy proportion measuring device; 51. a body; 52. a vibrating member; 53. a signal processing device; 6. an adjustment device; 61. a sodium adjustment member; 611. a first metering bucket; 612. a first check valve; 62. a potassium regulating member; 621. a second metering bucket; 622. a second one-way valve; 7. a sodium potassium alloy purification device; 8. an electromagnetic pump; 9. a liquid level meter; 10. an outlet conduit.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The individual features described in the embodiments can be combined in any suitable manner without departing from the scope, for example different embodiments and aspects can be formed by combining different features. In order to avoid unnecessary repetition, various possible combinations of the specific features of the invention will not be described further.
In the following description, the term "first/second/so" is used merely to distinguish different objects and does not mean that there is a common or relationship between the objects. It should be understood that the description of the "upper", "lower", "outer" and "inner" directions as related to the orientation in the normal use state, and the "left" and "right" directions indicate the left and right directions indicated in the corresponding schematic drawings, and may or may not be the left and right directions in the normal use state.
It should be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element. "plurality" means greater than or equal to two.
The embodiment of the invention provides a preparation device of a sodium-potassium alloy, wherein the sodium-potassium alloy is an alloy of sodium and potassium and is in a liquid state at room temperature. As shown in fig. 1, the manufacturing apparatus in the embodiment of the present invention includes a sodium-potassium alloy manufacturing vessel 1, a sodium storage device 2, a potassium storage device 3, an inert gas supply device 4, a sodium-potassium alloy ratio measuring device 5, and an adjusting device 6. The sodium-potassium alloy preparation container 1 is used for preparing sodium-potassium alloy, the sodium-potassium alloy is prepared by setting the proportion of sodium and potassium of the sodium-potassium alloy to be prepared according to the requirement, and quantitative sodium and potassium are added into the sodium-potassium alloy preparation container 1 and heated to a certain temperature, so that the sodium and the potassium are melted to prepare the sodium-potassium alloy. Wherein, the sodium-potassium alloy preparation container 1 is provided with an outlet pipeline 10 for leading out the prepared sodium-potassium alloy. Because the activity of the sodium-potassium alloy is very high and the danger coefficient is high, the airtightness of the sodium-potassium alloy preparation container 1 needs to be maintained in the preparation process of the sodium-potassium alloy so as to reduce the explosion risk of the sodium-potassium alloy. In the process of preparing the sodium-potassium alloy, the whole preparation equipment of the sodium-potassium alloy is in a sealed state, so that the risk that an operator directly contacts the sodium-potassium alloy can be avoided or reduced; and the pipeline and the container in the whole preparation equipment for the sodium-potassium alloy are filled with inert gas, so that the sodium-potassium alloy is prevented from contacting air, the risk of directly operating the sodium-potassium alloy can be reduced, and the safety is improved.
The sodium-potassium alloy preparation container 1 in the embodiment of the invention can be continuously used, and the original sodium-potassium alloy does not need to be emptied before the sodium-potassium alloy with a new proportion is prepared, so that the waste caused by excessive preparation at one time is avoided, and the risk of treating the sodium-potassium alloy waste liquid is reduced.
The sodium storage device 2 is connected with the sodium-potassium alloy preparation container 1, the sodium storage device 2 is used for storing sodium, and the sodium storage device 2 is used for conveying sodium to the sodium-potassium alloy preparation container 1, wherein the sodium storage device 2 and the sodium-potassium alloy preparation container 1 can be connected through a pipeline, and the pipeline can be set as a metal hose. The potassium storage device 3 is connected with the sodium-potassium alloy preparation container 1, and the potassium storage device 3 is used for conveying potassium to the sodium-potassium alloy preparation container 1, wherein the potassium storage device 3 is connected with the sodium-potassium alloy preparation container 1 through a pipeline which can be set as a metal hose.
The inert gas supply device 4 is communicated with the sodium-potassium alloy preparation container 1, the sodium storage device 2 and the potassium storage device 3, the inert gas supply device 4 is used for supplying inert gas, and the chemical properties of the sodium-potassium alloy are relatively active, so that in the embodiment of the invention, the inert gas in the inert gas supply device 4 needs to be introduced into the sodium-potassium alloy preparation container 1, the sodium storage device 2 and the potassium storage device 3, so that the sodium in the sodium storage device 2 and the potassium in the potassium storage device 3 can be stored in an inert gas environment, and the sodium and the potassium in the sodium-potassium alloy preparation container 1 can react in the inert gas environment. The inert gas supply device 4 introduces inert gas into the sodium-potassium alloy preparation container 1, the sodium storage device 2 and the potassium storage device 3 before the sodium-potassium alloy is prepared, so that the proportion requirement of the inert gas and the air in the sodium-potassium alloy preparation container 1, the sodium storage device 2 and the potassium storage device 3 is larger than a certain value, the purity of the inert gas in the sodium-potassium alloy preparation container 1, the sodium storage device 2 and the potassium storage device 3 is higher, and the stability of sodium, potassium and sodium-potassium alloy in the sodium-potassium alloy preparation container 1, the sodium storage device 2 and the potassium storage device 3 is favorably improved. The inert gas supply device 4 can be respectively connected with the sodium-potassium alloy preparation container 1, the sodium storage device 2 and the potassium storage device 3 through pipelines, and valves can be arranged on the pipelines to realize the control of the conduction of the inert gas. It should be noted that the inert gas in the embodiment of the present invention includes, but is not limited to, argon, nitrogen, helium, etc., as long as the inert gas does not react with sodium, potassium, and sodium-potassium alloy.
The sodium-potassium alloy proportion measuring device 5 is connected with the sodium-potassium alloy preparation container 1, the sodium-potassium alloy proportion measuring device 5 is used for detecting the sodium-potassium proportion of the sodium-potassium alloy prepared in the sodium-potassium alloy preparation container 1, the actual sodium-potassium proportion of the sodium-potassium alloy prepared in the sodium-potassium alloy preparation container 1 is detected by arranging the sodium-potassium alloy proportion measuring device 5 because the physical properties of the sodium-potassium alloys with different proportions have larger differences, the detected actual sodium-potassium proportion of the sodium-potassium alloy is compared with the set sodium-potassium proportion of the sodium-potassium alloy, the comparison result is fed back to the adjusting device 6, the adjusting device 6 correspondingly supplements sodium or potassium to the sodium-potassium alloy preparation container 1, the sodium-potassium alloy with updated sodium-potassium proportion is obtained by reflecting the sodium-potassium alloy preparation container 1 again, and the sodium-potassium alloy with the set sodium-potassium proportion can be prepared, so as to realize the stable control of the physical properties of the sodium-potassium alloy. Wherein, the sodium-potassium alloy proportion measuring device 5 can be connected with the sodium-potassium alloy preparation container 1 through a pipeline, and the pipeline can be a metal hose. The pipeline can be provided with a valve, and the delivery of the sodium-potassium alloy from the sodium-potassium alloy preparation container 1 to the sodium-potassium alloy proportion measuring device 5 is controlled by controlling the on-off state of the valve. For example, as shown in fig. 1, two pipelines are provided between the sodium-potassium alloy preparation vessel 1 and the sodium-potassium alloy preparation vessel 1, the first pipeline is used for communicating the outlet of the sodium-potassium alloy preparation vessel 1 with the inlet of the sodium-potassium alloy proportion measuring device 5, the second pipeline is used for communicating the outlet of the sodium-potassium alloy proportion measuring device 5 with the inlet of the sodium-potassium alloy preparation vessel 1, and one-way valves are provided on both pipelines. In general, the valves on the two pipelines are closed, after the sodium-potassium alloy is prepared, the valve of the first pipeline is opened, the sodium-potassium alloy in the sodium-potassium alloy preparation container 1 enters the sodium-potassium alloy proportion measuring device 5, and the valve of the first pipeline is closed until the sodium-potassium alloy in the sodium-potassium alloy proportion measuring device 5 reaches a set amount; the ratio of the sodium-potassium alloy is detected by the sodium-potassium alloy ratio measuring device 5, and the ratio of the sodium-potassium alloy detected by the sodium-potassium alloy ratio measuring device 5 can be used for representing the actual sodium-potassium ratio of the sodium-potassium alloy prepared in the sodium-potassium alloy preparation container 1; after the detection is finished, the valve of the second pipeline is opened, the sodium-potassium alloy in the sodium-potassium alloy proportion measuring device 5 flows back to the sodium-potassium alloy preparation container 1, and finally the valve of the second pipeline is closed to wait for the next sodium-potassium proportion detection of the sodium-potassium alloy.
There are various measuring methods of the sodium-potassium alloy ratio measuring device 5, and as shown in fig. 3, the sodium-potassium alloy ratio measuring device 5 may be provided with a main body 51, a vibrating piece 52, and a signal processing device 53. The ratio of the sodium-potassium alloy in the cavity is measured by using the difference of the resonance frequency of the vibration member 52 in the sodium-potassium alloy of different ratio. The vibration member 52 extends into the sodium-potassium alloy to be measured, the body 51 can provide an electric signal for the vibration of the vibration member 52, the vibration member 52 can convert the electric energy into the mechanical energy, the vibration member 52 can convert the mechanical energy in the resonance state into the electric energy in the resonance state of the vibration member 52, and the electric signal of the resonance frequency is transmitted to the body 51. The main body 51 can transmit an electric signal of a resonance frequency to the signal processing device 53, and the signal processing device 53 calculates an initial ratio of sodium to potassium in the sodium-potassium alloy from the received resonance frequency.
The following description is given of a method for calculating the ratio of sodium to potassium in a sodium-potassium alloy:
wherein D is the ratio of the sodium-potassium alloy (i.e. the mass percentage of potassium), f is the resonant frequency of the vibrating piece in the sodium-potassium alloy, and k is1、k2、k3Is a constant.
From the above formula, the ratio of the sodium-potassium alloy is related to the resonance frequency in the sodium-potassium alloy. k is a radical of1、k2、k3Is a constant related to the characteristics of the measuring device itself, where k1、k2、k3The mass of the vibrating piece in the measuring device of the sodium-potassium alloy proportion and the volume, the temperature and other characteristic parameters of the vibrating piece are related. At the same temperature, under the condition of structure size determination of a measuring device of the ratio of the sodium-potassium alloy, the 3 parameters k are1、k2、k3To determine the value.
The calculation formula of the ratio of sodium to potassium in the sodium-potassium alloy in the embodiment of the invention is obtained by fitting a large amount of experimental data and then simplifying, a large amount of sodium-potassium alloys with known ratio are adopted under the condition of set temperature, and the resonance frequency of each sodium-potassium alloy with known ratio is measured by using a measuring device of the ratio of the sodium-potassium alloys. Substituting multiple sets of data into the calculation formula of the ratio of sodium to potassium in the sodium-potassium alloyWhere the parameter k is calculated1、k2And k3Wherein, the data are the proportion of the sodium-potassium alloy and the corresponding resonance frequency, and the data are at least three groups.
In some embodiments, the sodium-potassium alloy proportion measuring device can realize dynamic measurement of the sodium-potassium alloy, that is, the sodium-potassium alloy can enter the sodium-potassium alloy proportion measuring device and flow out of the sodium-potassium alloy proportion measuring device according to a set flow rate, and the sodium-potassium alloy proportion measuring device can directly measure the flowing sodium-potassium alloy.
The adjusting device 6 is used for adjusting the ratio of sodium and potassium delivered to the sodium-potassium alloy preparation vessel 1. With reference to fig. 1, the following description is made of the process for preparing a sodium-potassium alloy:
before the sodium-potassium alloy is prepared, the inert gas supply device 4 is started firstly, and inert gas is introduced into the sodium-potassium alloy preparation container 1, the sodium storage device 2 and the potassium storage device, so that the purity of the inert gas in the preparation device meets certain preparation requirements, and the stability requirements of the preparation device in the reaction process are met. Then, opening a sodium storage device 2 and a potassium storage device 3, introducing a first set amount of sodium into a sodium-potassium alloy preparation container 1 through the sodium storage device 2 according to a set sodium-potassium ratio of a required sodium-potassium alloy, introducing a second set amount of potassium into the sodium-potassium alloy preparation container 1 through the potassium storage device 3, preparing the sodium-potassium alloy in the sodium-potassium alloy preparation container 1 after closing the sodium storage device 2 and the potassium storage device 3, introducing the sodium-potassium alloy into a sodium-potassium alloy ratio measuring device 5 after the sodium-potassium alloy is prepared, detecting an actual sodium-potassium ratio of the sodium-potassium alloy through the sodium-potassium alloy ratio measuring device 5, and determining a sodium or potassium supplementing amount to be supplemented according to a difference value between the actual sodium-potassium ratio of the sodium-potassium alloy and the set sodium-potassium ratio; and (3) starting a corresponding part in the adjusting device 6 to start the communication between the sodium storage device or the potassium storage device and the sodium-potassium alloy preparation container, and controlling and supplementing the sodium or potassium with a corresponding amount to the sodium-potassium alloy preparation container by the adjusting device 6 to finish the preparation of the sodium-potassium alloy again, so that the actual sodium-potassium ratio of the sodium-potassium alloy is adjusted. Of course, after the first adjustment, the sodium-potassium alloy ratio measuring device 5 may be adopted to detect the actual sodium-potassium ratio of the adjusted sodium-potassium alloy again, and the second sodium-potassium ratio adjustment is continued, so that the sodium-potassium ratio adjustment may be performed repeatedly until the matching degree between the actual sodium-potassium ratio of the sodium-potassium alloy and the set sodium-potassium ratio of the sodium-potassium alloy meets the actual requirement.
The sodium-potassium alloy preparation equipment provided by the embodiment of the invention comprises a sodium-potassium alloy preparation container, a sodium storage device, a potassium storage device, an inert gas supply device, a sodium-potassium alloy proportion measuring device and an adjusting device, wherein sodium and potassium are introduced into the sodium-potassium alloy preparation container by adopting the sodium storage device and the potassium storage device so as to prepare the sodium-potassium alloy in the sodium-potassium alloy preparation container, the inert gas supply device is used for providing a stable inert gas reaction environment, the sodium-potassium alloy proportion measuring device can measure the actual sodium-potassium proportion of the prepared sodium-potassium alloy, and the adjusting device can adjust the sodium storage device or the potassium storage device to supplement sodium or potassium into the sodium-potassium alloy preparation container according to the difference value of the actual sodium-potassium proportion and the set proportion so as to adjust the actual sodium-potassium proportion of the sodium-potassium alloy. The embodiment of the invention realizes the detection of the proportion of the prepared sodium-potassium alloy through the sodium-potassium alloy proportion measuring device, can feed back the detected actual proportion of the sodium-potassium alloy to the adjusting device, and supplements sodium or potassium to the sodium-potassium alloy preparation container through the adjusting device according to the difference value of the actual proportion and the set proportion to realize the adjustment of the proportion of the sodium-potassium alloy, so that the actual proportion is consistent with the set proportion, and the accuracy of the proportion of the sodium and the potassium for preparing the sodium-potassium alloy is improved.
In some embodiments, as shown in fig. 1, the apparatus for preparing a sodium-potassium alloy further includes a sodium-potassium alloy purification device 7. The sodium-potassium alloy purification device 7 is connected with the sodium-potassium alloy preparation container 1. The sodium-potassium alloy purification device 7 is used for removing impurities in the sodium-potassium alloy preparation container 1, and it should be noted that in the sodium-potassium alloy preparation and crystallization process, chemical components in the solidified metal cannot be diffused in time due to the high cooling speed, and the distribution of each component element in the sodium-potassium alloy is not uniform during crystallization, so that segregation is generated, and the physical properties of the alloy are affected.
The sodium-potassium alloy purification device 7 in the embodiment of the invention is used for removing metal and nonmetal impurities in the sodium-potassium alloy, so that the risk of proportional segregation of the sodium-potassium alloy is reduced, the corrosion risk of preparation equipment for the sodium-potassium alloy is reduced, and meanwhile, the impurity pollution in raw materials can be avoided, so that the high-purity sodium-potassium alloy is prepared.
The purification principle of the sodium-potassium alloy purification device in the embodiment of the present invention is explained below:
according to the principle of liquid metal purification, because the solubility of each compound is different, consequently can set up the cold source in sodium potassium alloy purifier, make the temperature reduction in the sodium potassium alloy purifier through the cold source, the temperature reduction after the sodium potassium alloy enters into sodium potassium alloy purifier, the impurity crystallization that adopts the mode of physics condensation to be lower with the solubility is appeared. And then the crystallized impurities are screened out in a filtering mode, so that the sodium-potassium alloy is purified.
As shown in fig. 1, two pipelines are also provided between the sodium-potassium alloy purification device 7 and the sodium-potassium alloy preparation container 1 for connection, and in the same way as the connection between the sodium-potassium alloy proportion measurement device 5 and the sodium-potassium alloy preparation container 1, the sodium-potassium alloy prepared in the sodium-potassium alloy preparation container 1 can be introduced into the sodium-potassium alloy purification device 7 for purification by controlling the opening and closing of valves on the two pipelines, and then the purified sodium-potassium alloy is guided back into the sodium-potassium alloy preparation container 1 by the sodium-potassium alloy purification device 7, so that the segregation risk is reduced. In some embodiments, as shown in fig. 1, the apparatus for preparing a sodium-potassium alloy further comprises an electromagnetic pump 8. The electromagnetic pump 8 is connected between the sodium-potassium alloy preparation container 1 and the sodium-potassium alloy purification device 7, and the electromagnetic pump 8 is also connected between the sodium-potassium alloy preparation container 1 and the sodium-potassium alloy proportion measurement device 5. The electromagnetic pump 8 is used for driving the sodium-potassium alloy in the sodium-potassium alloy preparation container 1 to be conveyed to the sodium-potassium alloy purification device 7 and the sodium-potassium alloy proportion measuring device 5. As shown in fig. 1, the sodium-potassium alloy purification device 7 and the sodium-potassium alloy ratio measurement device 5 need to be separately operated, for example, in the case where the sodium-potassium alloy purification device 7 is operated, the sodium-potassium alloy ratio measurement device 5 needs to be turned off, and in the case where the sodium-potassium alloy ratio measurement device 5 is operated, the sodium-potassium alloy purification device 7 needs to be turned off. Correspondingly, as shown in fig. 1, the sodium-potassium alloy purification device 7 is connected in parallel with the sodium-potassium alloy proportion measurement device 5, that is, the sodium-potassium alloy purification device 7 and the sodium-potassium alloy proportion measurement device 5 are respectively connected in parallel to a loop of the sodium-potassium alloy preparation container, the electromagnetic pump 8 can be arranged on a main path of the parallel line, a valve can be arranged between the electromagnetic pump 8 and the sodium-potassium alloy preparation container, and each branch can be independently provided with a valve. In the actual preparation process, the sodium-potassium alloy purifying device 7 can be started to purify the sodium-potassium alloy in the sodium-potassium alloy preparation container 1, and then the sodium-potassium alloy proportion measuring device 5 is started to measure the proportion of the sodium-potassium alloy in real time. Under the state of starting the sodium-potassium alloy purification device 7, a valve between the electromagnetic pump 8 and the sodium-potassium alloy preparation container 1 can be opened, and a valve on a branch of the sodium-potassium alloy purification device 7 is opened, so that the sodium-potassium alloy in the sodium-potassium alloy preparation container 1 can enter the sodium-potassium alloy purification device 7 to realize the purification of the sodium-potassium alloy, and the sodium-potassium alloy is guided back to the sodium-potassium alloy preparation container 1 after the purification; and in the state of measuring the ratio of the sodium-potassium alloy, opening a valve between the sodium-potassium alloy preparation container and the electromagnetic pump 8, and opening a valve on a branch of the sodium-potassium alloy ratio measuring device 5, so that the sodium-potassium alloy in the sodium-potassium alloy preparation container 1 can enter the sodium-potassium alloy ratio measuring device 5 to realize the measurement of the ratio of the sodium-potassium alloy, and guiding the sodium-potassium alloy back to the sodium-potassium alloy preparation container 1 after the ratio of the sodium-potassium alloy is measured. In other embodiments, the sodium-potassium alloy purifying device 7 and the sodium-potassium alloy ratio measuring device 5 can also be in series relationship, that is: the sodium-potassium alloy purification device 7 and the sodium-potassium alloy proportion measurement device 5 can work simultaneously.
According to the embodiment of the invention, the electromagnetic pump is arranged on the main path of the sodium-potassium alloy proportion measuring device and the sodium-potassium alloy purifying device, so that no matter the proportion measurement of the sodium-potassium alloy is started or the purification of the sodium-potassium alloy is started, the electromagnetic pump can provide driving force for the flow of the sodium-potassium alloy, and the control of the flow of the sodium-potassium alloy can be realized by adjusting the voltage of the electromagnetic pump.
In some embodiments, as shown in fig. 1, the regulating device 6 includes a sodium regulating member 61 and a potassium regulating member 62. The sodium adjusting member 61 is provided between the sodium storage device 2 and the sodium-potassium alloy preparation vessel 1, and is used for opening and closing communication between the sodium storage device 2 and the sodium-potassium alloy preparation vessel 1. Before the sodium-potassium alloy is prepared, the adjusting device can be opened, so that the sodium storage device 2 is communicated with the sodium-potassium alloy preparation container 1, and the sodium storage device 2 introduces a first set amount of sodium into the sodium-potassium alloy preparation container 1; after the sodium-potassium alloy is prepared, the actual sodium-potassium ratio of the sodium-potassium alloy is obtained through a sodium-potassium alloy ratio measuring device 5, the sodium supplement amount is determined according to the ratio, and the sodium adjusting piece 61 can control the flow from the sodium storage device 2 to the sodium-potassium alloy preparation container 1 according to the sodium supplement amount; further, a potassium adjuster 62 is provided between the potassium reservoir 3 and the sodium-potassium alloy production vessel 1 to open and close communication between the potassium reservoir 3 and the sodium-potassium alloy production vessel 1. The potassium storage device 3 introduces a second set amount of potassium into the sodium-potassium alloy preparation container 1; after the sodium-potassium alloy is prepared, the actual sodium-potassium ratio of the sodium-potassium alloy is obtained through the sodium-potassium alloy ratio measuring device 5, the potassium supplementing amount is determined according to the actual sodium-potassium ratio, and the potassium adjusting piece 62 can control the flow from the sodium storage device 2 to the sodium-potassium alloy preparation container 1 according to the potassium supplementing amount.
The adjusting device comprises the sodium adjusting piece and the potassium adjusting piece, and the sodium adjusting piece and the potassium adjusting piece can accurately control the content of sodium and potassium which are supplemented into the sodium-potassium alloy preparation container, so that the ratio of the sodium-potassium alloy can be accurately controlled in a required range, and the accuracy of the sodium-potassium ratio of the prepared sodium-potassium alloy is improved.
In some embodiments, as shown in fig. 1, the sodium adjuster 61 includes a first metering barrel 611 and a first one-way valve 612. First metering barrel 611 is communicated with sodium-potassium alloy preparation container 1, first one-way valve 612 is communicated with sodium storage device 2 and first metering barrel 611, and first one-way valve 612 is used for adjusting the volume of sodium entering first metering barrel 611 from sodium storage device 2. In the embodiment of the present invention, the needle valve is used as the first one-way valve 612 for controlling the sodium storage device 2 and the first metering barrel 611, the needle valve can bear a large pressure, the sealing performance is good, and the on-off of the pipeline between the sodium storage device 2 and the first metering barrel 611 can be accurately controlled.
Before the sodium-potassium alloy is prepared, the first one-way valve 612 and the first metering barrel 611 can be opened, so that a first set amount of sodium can be introduced into the sodium-potassium alloy preparation container in the sodium storage device 2; after the sodium-potassium alloy is prepared, the actual sodium-potassium ratio of the sodium-potassium alloy is detected by the sodium-potassium alloy ratio measuring device 5, and the conduction time of the first one-way valve 612 is controlled to control the sodium output volume of the sodium storage device 2, so that the actual sodium-potassium ratio in the sodium-potassium alloy preparation container 1 is adjusted to be consistent with the set sodium-potassium ratio.
The potassium adjuster 62 includes a second metering barrel 621 and a second one-way valve 622 in communication with the potassium reservoir. The potassium adjuster 62 is identical in structure and adjustment to the sodium adjuster 61 and will not be described in detail.
In some embodiments, as shown in FIG. 1, level gauges 9 are provided in the sodium reservoir 2 and the potassium reservoir 3. According to the embodiment of the invention, the liquid level meters 9 are arranged in the sodium storage device 2 and the potassium storage device 3, so that the liquid levels of sodium and potassium in the sodium storage device 2 and the potassium storage device 3 can be detected in real time, and the set amount of sodium and potassium can be introduced into the sodium-potassium alloy preparation container through the liquid level change value of the liquid level meters 9 before the sodium-potassium alloy is prepared, so that the accuracy of matching between the actual sodium-potassium ratio and the set sodium-potassium ratio is improved in the process of preparing the sodium-potassium alloy for the first time, and the difficulty of subsequently adjusting the sodium-potassium ratio is reduced.
In some embodiments, a liquid level meter 9 is also provided in the sodium-potassium alloy preparation vessel 1 as described in fig. 1. According to the embodiment of the invention, the liquid level meter 9 is arranged in the sodium-potassium alloy preparation container 1, so that the liquid level of the sodium-potassium alloy in the sodium-potassium alloy preparation container can be detected in real time.
Referring to fig. 1 and 2, an embodiment of the present invention further provides a manufacturing method of a manufacturing apparatus for a sodium-potassium alloy according to any one of the above embodiments, where the manufacturing method includes:
s1, starting the inert gas supply device 4, filling inert gas into the sodium-potassium alloy preparation container 1, the sodium storage device 2 and the potassium storage device 3, and leading the gas in the sodium-potassium alloy preparation container 1, the sodium storage device 2 and the potassium storage device 3 to beH in the body2The content of O is less than or equal to 50 mu L/L, and O2The content of the sodium-potassium alloy is less than or equal to 50 mu L/L, inert gas is filled into the sodium-potassium alloy preparation container 1, the sodium storage device 2 and the potassium storage device 3, so that the concentration of the inert gas in the sodium-potassium alloy preparation container 1, the sodium storage device 2 and the potassium storage device 3 is higher, and the safety of the sodium-potassium alloy preparation process is improved due to the stable chemical property of the inert gas.
And S2, opening the sodium storage device 2 and the potassium storage device 3, delivering a first set amount of sodium and a second set amount of potassium into the sodium-potassium alloy preparation container 1 according to the set proportion of the sodium-potassium content, and closing the sodium storage device 2 and the potassium storage device 3. Wherein, the measurement of the first set amount and the second set amount can be realized by liquid level meters 9 arranged on the sodium storage device 2 and the potassium storage device 3. S3, preparing the sodium-potassium alloy in the sodium-potassium alloy preparation container 1. The first set amount of sodium and the second set amount of potassium are reacted in the sodium-potassium alloy production vessel 1 under the set temperature and pressure conditions to produce the sodium-potassium alloy.
S4, conveying the sodium-potassium alloy to a sodium-potassium alloy proportion measuring device to detect the current proportion of the sodium-potassium content in the sodium-potassium alloy; according to the embodiment of the invention, the current proportion of the sodium-potassium alloy is detected according to the difference of the resonance frequencies of the sodium-potassium alloy with different proportions in the vibration loop of the component.
S5, determining the supplement amount of sodium or potassium to be supplemented according to the difference between the current proportion and the set proportion; the sodium-potassium alloy ratio measuring device in the embodiment of the invention can adopt a mode of measuring for multiple times, that is, after the first preparation, the sodium-potassium alloy can be introduced into the sodium-potassium alloy ratio measuring device for measurement, sodium and potassium are introduced into the sodium-potassium alloy preparation container through the adjusting device according to the measured ratio, and the step of measuring the total sodium-potassium ratio can be repeated until the measured sodium-potassium alloy ratio is close to the required ratio.
And S6, correspondingly opening the sodium storage device and the potassium storage device, and conveying a supplementing amount of sodium or potassium to the sodium-potassium alloy preparation container. Until the ratio of the sodium-potassium alloy measured by the sodium-potassium alloy ratio measuring device 5 meets the required ratio.
In some embodiments, after step S3 and before step S4, further comprising:
and S35, sending the sodium-potassium alloy in the sodium-potassium alloy preparation container to a sodium-potassium alloy purification device at a set flow rate. According to the embodiment of the invention, the electromagnetic pump can be used for providing driving force for the circulation of the sodium-potassium alloy, and the flow regulation of the sodium-potassium alloy is realized by regulating the voltage of the electromagnetic pump.
In some embodiments, the set flow rate is 0.1-1 m3H; that is, the sodium-potassium alloy in the sodium-potassium alloy preparation vessel is purified by feeding the sodium-potassium alloy to the sodium-potassium alloy purification apparatus at a set flow rate. Wherein the set flow rate may be 0.5m3/h。
In some embodiments, before turning on the sodium storage device 2 and the potassium storage device 3 and turning off the sodium storage device 2 and the potassium storage device 3 after delivering the first set amount of sodium and the second set amount of potassium into the sodium-potassium alloy preparation container 1 according to the set ratio of the sodium-potassium content at step S2, the method further comprises:
s21, heating the sodium-potassium alloy preparation container, the sodium storage device and the potassium storage device to 100-250 ℃. The heat source of the sodium-potassium alloy preparation equipment can be achieved by laying electric heaters on the equipment and the pipeline, and the sodium-potassium alloy preparation equipment is heated to 100-250 ℃ through the electric heaters in a heat conduction mode.
The following is an example of the preparation of about 200L of a sodium potassium alloy with a set ratio of sodium to potassium of 50% each:
1) the positive pressure argon gas replacement operation is carried out on the sodium-potassium alloy preparation equipment through the inert gas supply device 4, so that the water and oxygen content in the gas in the system is not more than 50 mu L/L.
2) By a liquid level measurement method, about 100L of sodium and potassium are respectively input into a sodium-potassium alloy preparation container from a potassium storage device and a sodium storage device container, and the sodium-potassium alloy preparation container is heated to 120 ℃ to react sodium and potassium to prepare the sodium-potassium alloy.
3) Starting the electromagnetic pump to make the sodium-potassium alloy in 0.5m3The flow rate of the flow/h is sent to a sodium-potassium alloy purification device to purify the sodium-potassium alloy.
4) After purifying for 1 hour, closing the sodium-potassium alloy purification device, starting the sodium-potassium alloy proportion measuring device, opening an inlet and outlet valve of the sodium-potassium alloy proportion measuring device, and carrying out online measurement on the sodium-potassium alloy proportion to obtain the current proportion value of the sodium-potassium alloy.
5) When the proportion of potassium in the sodium-potassium alloy is low, a small amount of potassium is supplemented through a potassium adjusting piece; or when the proportion of sodium in the sodium-potassium alloy is lower, a small amount of sodium is supplemented by the sodium adjusting piece; and purifying the sodium-potassium alloy again and measuring the current proportion of sodium and potassium of the sodium-potassium alloy until the difference range between the current proportion and the set proportion meets the requirement.
6) The sodium-potassium alloy is supplied to the user through the outlet pipe 10 of the sodium-potassium alloy preparation vessel.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention.
Claims (10)
1. A preparation equipment of sodium-potassium alloy is characterized by comprising the following components:
the sodium-potassium alloy preparation container is used for preparing sodium-potassium alloy;
the sodium storage device is connected with the sodium-potassium alloy preparation container to convey sodium to the sodium-potassium alloy preparation container;
the potassium storage device is connected with the sodium-potassium alloy preparation container to convey potassium to the sodium-potassium alloy preparation container;
an inert gas supply device which is communicated with the sodium-potassium alloy preparation container, the sodium storage device and the potassium storage device to provide inert gas;
the sodium-potassium alloy proportion measuring device is connected with the sodium-potassium alloy preparation container so as to detect the proportion of the sodium-potassium alloy in the sodium-potassium alloy preparation container;
and the adjusting device is used for adjusting the ratio of sodium and potassium conveyed to the sodium-potassium alloy preparation container.
2. The manufacturing apparatus according to claim 1, further comprising:
and the sodium-potassium alloy purification device is connected with the sodium-potassium alloy preparation container and is used for removing impurities in the sodium-potassium alloy preparation container.
3. The manufacturing apparatus according to claim 2, further comprising:
and the electromagnetic pump is connected between the sodium-potassium alloy preparation container and the sodium-potassium alloy purification device and between the sodium-potassium alloy preparation container and the sodium-potassium alloy proportion measurement device so as to drive the sodium-potassium alloy in the sodium-potassium alloy preparation container to be conveyed to the sodium-potassium alloy purification device and the sodium-potassium alloy proportion measurement device.
4. The manufacturing apparatus according to claim 1, wherein the adjusting device includes:
the sodium adjusting piece is arranged between the sodium storage device and the sodium-potassium alloy preparation container and is used for opening and closing the communication between the sodium storage device and the sodium-potassium alloy preparation container;
and the potassium adjusting piece is arranged between the potassium storage device and the sodium-potassium alloy preparation container and is used for opening and closing the communication between the potassium storage device and the sodium-potassium alloy preparation container.
5. The manufacturing apparatus of claim 4, wherein the sodium conditioner comprises:
a first metering barrel communicated with the sodium-potassium alloy preparation container;
the first one-way valve is communicated with the sodium storage device and the first metering barrel so as to adjust the volume of sodium entering the first metering barrel from the sodium storage device;
the potassium regulating member includes:
the second metering barrel is communicated with the sodium-potassium alloy preparation container;
and the second one-way valve is communicated with the potassium storage device and the second metering barrel so as to adjust the volume of potassium entering the second metering barrel from the potassium storage device.
6. The manufacturing apparatus according to claim 1, wherein level gauges are provided in the sodium storage device and the potassium storage device.
7. A method for producing a sodium-potassium alloy using the production apparatus according to any one of claims 1 to 6, comprising:
s1, opening the inert gas supply device, and filling inert gas into the sodium-potassium alloy preparation container, the sodium storage device and the potassium storage device to enable H in the gas in the sodium-potassium alloy preparation container, the sodium storage device and the potassium storage device2The content of O is less than or equal to 50 mu L/L, and O2The content of the (D) is less than or equal to 50 mu L/L;
s2, opening the sodium storage device and the potassium storage device, and closing the sodium storage device and the potassium storage device after conveying a first set amount of potassium and a second set amount of sodium into the sodium-potassium alloy preparation container according to the set proportion of the sodium-potassium content;
s3, preparing a sodium-potassium alloy in the sodium-potassium alloy preparation container;
s4, conveying the sodium-potassium alloy to the sodium-potassium alloy proportion measuring device to detect the current proportion of the sodium-potassium content in the sodium-potassium alloy;
s5, determining the supplement amount of sodium or potassium to be supplemented according to the difference value between the current proportion and the set proportion;
and S6, correspondingly opening the sodium storage device and the potassium storage device, and conveying the supplement amount of sodium or potassium to the sodium-potassium alloy preparation container.
8. The method of claim 7, further comprising, after step S3 and before step S4:
and S35, sending the sodium-potassium alloy in the sodium-potassium alloy preparation container to a sodium-potassium alloy purification device at a set flow rate, and purifying the sodium-potassium alloy for a set time.
9. The method according to claim 8, wherein the set flow rate is 0.1 to 1m3/h。
10. The method according to claim 7, further comprising, before step S2:
s21, heating the sodium-potassium alloy preparation container, the sodium storage device and the potassium storage device to 100-250 ℃.
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| CH95461A (en) * | 1913-11-05 | 1922-07-17 | Hackspill Louis | Process for preparing a sodium-potassium alloy. |
| CN101195878A (en) * | 2007-12-29 | 2008-06-11 | 中国原子能科学研究院 | Preparation method and device of sodium-potassium alloy |
| CN105369041A (en) * | 2015-12-15 | 2016-03-02 | 中国原子能科学研究院 | Sodium-potassium alloy vacuum distillation device |
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2021
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| CH95461A (en) * | 1913-11-05 | 1922-07-17 | Hackspill Louis | Process for preparing a sodium-potassium alloy. |
| CN101195878A (en) * | 2007-12-29 | 2008-06-11 | 中国原子能科学研究院 | Preparation method and device of sodium-potassium alloy |
| CN105369041A (en) * | 2015-12-15 | 2016-03-02 | 中国原子能科学研究院 | Sodium-potassium alloy vacuum distillation device |
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