CN113444895A - Alkaline metal evaporation and filtration device and method - Google Patents
Alkaline metal evaporation and filtration device and method Download PDFInfo
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- CN113444895A CN113444895A CN202010231932.2A CN202010231932A CN113444895A CN 113444895 A CN113444895 A CN 113444895A CN 202010231932 A CN202010231932 A CN 202010231932A CN 113444895 A CN113444895 A CN 113444895A
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- crucible
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/006—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with use of an inert protective material including the use of an inert gas
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
- C22B9/023—By filtering
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/04—Refining by applying a vacuum
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses an alkaline metal evaporation and filtration device and a method, wherein the alkaline metal evaporation and filtration device comprises a shell, a smelting crucible, a temperature control trickle tube and a shaping crucible, wherein an operation cavity is formed inside the shell, the smelting crucible is positioned in the operation cavity, the temperature control trickle tube is connected to an outlet at the bottom of the smelting crucible, the shaping crucible is positioned in the operation cavity and is positioned right below the temperature control trickle tube, a pumping and inflating interface is arranged on the shell to be communicated with a vacuum maintaining system or a buffer gas distribution system, a heating body is fixed outside the smelting crucible, a gas injection hole is fixed on the smelting crucible to be connected with a buffer gas pressure control system positioned outside the shell, and a filtering piece is fixed in the temperature control trickle tube. The device can quantitatively treat the alkali metal in batches and has high safety coefficient.
Description
Technical Field
The invention relates to the technical field of alkali metal treatment, in particular to an alkali metal evaporation and filtration device and method.
Background
Alkali metals are generally active, oxidation phenomena easily occur in the process of packaging and storing directly purchased alkali metals, oxidized alkali metals can form a dense film-shaped oxide on the upper layer of a metal liquid surface in a heating and melting state, the evaporation rate in an experiment can be influenced in the evaporation using process, and in order to meet the requirement of the experiment on the evaporation rate of the alkali metals, the oxide needs to be removed firstly and then the evaporation experiment needs to be carried out.
When the oxide is removed from the alkali metal in the prior art, the alkali metal sample is very easy to oxidize if not used at the first time after being treated, and the treatment needs to be repeated, thereby wasting time and energy and wasting energy and samples.
Disclosure of Invention
The invention aims to provide an alkali metal evaporation and filtration device aiming at the problem that alkali metal is easy to waste after repeated treatment in the prior art.
The invention also aims to provide an evaporation and filtration method of the alkali metal evaporation and filtration device.
The technical scheme adopted for realizing the purpose of the invention is as follows:
alkaline metal evaporation and filtration device, including inside formation operation chamber the shell, be located melting crucible and design crucible in the operation chamber, wherein:
a heating body is fixed outside the smelting crucible, a temperature control dripping pipe is connected to an outlet at the bottom of the smelting crucible, a filtering piece is fixed in the temperature control dripping pipe, the top of the shaping crucible is provided with an opening, and the shaping crucible is positioned under the temperature control dripping pipe;
the shell is provided with a pumping and inflating interface to communicate with the vacuum maintaining system or the buffer gas distribution system, the smelting crucible is provided with a gas injection hole to be connected with the buffer gas pressure control system positioned outside the shell, and the smelting crucible is provided with a pumping system with a pumping hole positioned outside the shell.
In the above technical scheme, the filter member is a stainless steel filter screen.
In the technical scheme, the stainless steel filter screen is of a cylindrical net structure and is attached and fixed on the inner wall of the temperature control trickling pipe.
In the technical scheme, a vacuum gauge is arranged on the buffer gas pressure control system to adjust the buffer gas pressure in the smelting crucible.
In the above technical scheme, the gas injection hole and the vacuum hole are respectively and fixedly connected with a VCR interface.
In the technical scheme, an experiment bench is fixed in the operation cavity to place the smelting crucible.
In the above technical scheme, the temperature control trickling pipe comprises a straight pipe and a temperature control assembly fixed on the outer wall of the straight pipe, and the filtering piece is fixed on the inner wall of the straight pipe.
In the above technical scheme, the melting crucible comprises a crucible body and a cover body detachably assembled on the top opening of the crucible body, and the gas injection hole and the vacuumizing hole are formed in the cover body.
In the above technical scheme, the bottom of the crucible body is funnel shaped structure, just the control by temperature change trickle flow connect in the opening part of funnel shaped structure bottom.
In the above technical solution, the housing includes a housing body and a cover body detachably sealed at an opening at the top of the housing cover body, the cover body is provided with a hole for two connecting pipes to penetrate through, one of the connecting pipes is used for connecting the gas injection hole and the buffer gas pressure control system, the other connecting pipe is used for connecting the vacuum hole and the vacuum system, and the housing body or the cover body is provided with the pumping and inflating interface.
In another aspect of the present invention, the evaporation filtration method of the alkali metal evaporation filtration device is further included, and the method comprises the following steps:
step 1, opening a shell, taking out the smelting crucible, and placing alkali metal in the smelting crucible;
step 4, starting the heating body and the temperature control trickle tube, adjusting the air pressure of buffer gas in the smelting crucible through a buffer gas air pressure control system, heating the alkali metal in a molten state in the smelting crucible, flowing through a filtering piece in the temperature control trickle tube, and dripping the alkali metal in the shaping crucible;
when alkali metal still remains in the melting crucible and needs to be taken again, the step 7 is carried out:
and 7, putting the shaped crucible back, closing the shell, communicating the pumping and inflating interface with a vacuum maintaining system to pump the operation cavity to be vacuum, communicating the pumping and vacuumizing hole with a pumping and vacuumizing system to pump the smelting crucible to be vacuum, slowly injecting the required buffer gas into the buffer gas distribution system through the pumping and inflating interface, adjusting the gas pressure of the buffer gas in the smelting crucible through the buffer gas pressure control system, and continuing to perform the steps 4 and 5.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the melting crucible is heated by the heating body, so that the alkali in the crucible is heated to be in a liquid state, in the heating process, the oxide floats above the liquid alkali, the liquid drops from the bottom, a small amount of oxide is filtered, and the filtering piece is not easy to block.
2. Through the temperature of adjustment control by temperature change trickle pipe to reach whether control liquid metal from smelting crucible below drippage purpose, set the crucible liquid level as the below and reach required height, close control by temperature change trickle part heating, make the inside alkali metal of heating crucible stop the drippage, accomplish the filtration, realize quantitative batch evaporation purification from this.
3. The alkaline metal evaporation filtering device is carried out under the protection of buffer gas, has high safety factor, is convenient to operate and can be used without special training. The alkaline metal evaporation and filtration device has the advantages of simple structure and low manufacturing cost, and is convenient for commercial popularization and application.
Drawings
Fig. 1 is a schematic structural view of an alkali metal evaporation and filtration device.
FIG. 2 is a schematic view showing the positional relationship between the shaping crucible and the melting crucible.
In the figure: 1-shell, 2-pumping and inflating interface, 3-connecting pipeline, 4-heating body, 5-temperature control trickling pipe, 6-shaping crucible, 7-gas injection hole, 8-smelting crucible, 9-filtering piece and 10-vacuumizing hole.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
Alkaline metal evaporation filter equipment, including inside shell 1 that forms the operation chamber, be located smelt the crucible 8, connect in the operation chamber smelt crucible 8 bottom export on the control by temperature change trickle pipe 5 and be located the operation intracavity just is in design crucible 6 under the control by temperature change trickle pipe 5, smelt crucible 8 external fixation and have heating member 4, control by temperature change trickle pipe 5 internal fixation has a filtration piece 9.
The shell 1 is provided with a vacuumizing and inflating interface 2 for communicating with a vacuum maintaining system or a buffer gas distribution system, the smelting crucible is provided with a gas injection hole 7 for connecting with a buffer gas pressure control system positioned outside the shell, and the smelting crucible is provided with a vacuumizing hole 10 for connecting with a vacuumizing system positioned outside the shell.
The heating body 4 is fixed on the outer wall of the melting crucible 8 and is of an integral structure, and the integral structure is fixed in the shell 1 through a support, wherein the support is not shown in the figure. The shaping crucible 6 is placed on the inner bottom surface of the shell 1, under the protection of the buffer gas, the heating body 4 (which can adopt armored temperature control) heats the alkali metal in the smelting crucible 8, the alkali metal is molten, the metal oxide keeps a solid state, the alkali metal is changed into a liquid state, the oxide on the surface of the alkali metal floats on the upper surface of a molten pool, the molten alkali metal enters the temperature control dripping pipe 5, the temperature control dripping pipe 5 continues to heat the alkali metal in the pipe, the alkali metal keeps a liquid state, the solid alkali metal oxide is filtered by the filtering piece, and the purified alkali metal liquid enters the shaping crucible 6.
In order to display the vacuum degree in the processing chamber and the pressure of the buffer gas, a pressure gauge is provided on the housing 1. The vacuum maintaining system comprises a vacuumizing pipeline communicated with the operation cavity at one end and a vacuum generator connected to the other end of the vacuumizing pipeline, and buffer gas supplied by the buffer gas pressure control system and the buffer gas distribution system can adopt inert gases such as argon or neon and the like.
The purpose of controlling whether the liquid metal drips from the temperature control dripping pipe 5 or not is achieved by controlling the temperature of the temperature control dripping pipe 5, when the liquid level in the lower fixed-type crucible 6 reaches the required height, the heating of the temperature control dripping pipe 5 is closed, so that the alkali metal in the smelting crucible 8 stops dripping, and the filtering is completed.
The evaporation and filtration method of the alkali metal evaporation and filtration device comprises the following steps:
step 1, placing alkali metal in the smelting crucible 8, and communicating a gas injection hole 7 with the gas pressure control system;
and 4, starting the heating body 4 and the temperature control trickle tube 5, adjusting the gas pressure in the smelting crucible 8 to several hundred Pa to several thousand Pa through a buffer gas pressure control system, and dripping the alkali metal which is heated to be in a molten state into the shaping crucible 6 through a filtering piece in the temperature control trickle tube.
when alkali metal still remains in the melting crucible and needs to be taken again, the step 7 is carried out:
and 7, putting the shaped crucible back, closing the shell, communicating the pumping and inflating interface with a vacuum maintaining system to pump the operation cavity to be vacuum, communicating the pumping and vacuumizing hole with a pumping and vacuumizing system to pump the smelting crucible to be vacuum, slowly injecting the required buffer gas into the buffer gas distribution system through the pumping and inflating interface, adjusting the gas pressure of the buffer gas in the smelting crucible through the buffer gas pressure control system, and continuing to perform the steps 4 and 5.
The vacuum pumping process is to prevent liquid alkali metal bubbles formed after heating, and a glass window can be arranged on the shell 1 or on a flange of the shell 1 to directly observe the liquid level in the shaping crucible 6. When the vacuum melting furnace is used for the first time, the temperature control trickle tube 5 is not blocked, the operation cavity and the melting crucible 8 are vacuumized simultaneously by connecting the vacuumizing interface 2 with the vacuum maintaining system through the vacuumizing interface 2, when the vacuum melting furnace is used after cooling, the temperature control trickle tube 5 is not blocked, so that the vacuumizing interface 2 is connected with the vacuum maintaining system to vacuumize the operation cavity, the vacuumizing hole is communicated with the vacuumizing system to vacuumize the melting crucible, the flow rate valve is assembled on a pipeline connected with the vacuumizing hole, the vacuumizing speed is relatively slow, and the vacuumizing system connected with the vacuumizing hole can be closed during the first vacuumizing, and the vacuum degree in the melting crucible is realized through the vacuum maintaining system connected with the vacuumizing interface 2 and the open temperature control trickle tube.
Example 2
In order to intercept the alkali metal oxide well and not be damaged by the alkali metal, the filter is a stainless steel filter screen 9. The stainless steel filter screen 9 is vertically fixed on the inner wall of the temperature control trickling pipe 5, can realize effective interception and is not easy to block. Furthermore, the filtering piece is a stainless steel filter screen which is of a cylindrical net structure and is attached and fixed on the inner wall of the temperature control dripping pipe.
In order to facilitate the matching control of the pressure of the buffer gas in the smelting crucible 8, a vacuum gauge is arranged on the buffer gas pressure control system.
In order to facilitate the disassembly, VCR interfaces are fixedly connected to the gas injection hole 7 and the vacuum hole 10.
In order to facilitate the placement of the melting crucible 8 in the housing 1, a laboratory bench is fixed in the operating chamber for placing the melting crucible 8. When in use, the crucible is placed on a laboratory bench (not shown).
In order to enable the alkali metal in a molten state to smoothly flow out, the temperature control dripping pipe 5 comprises a straight pipe and a temperature control assembly fixed on the outer wall of the straight pipe, and the filtering piece is fixed in the straight pipe. The temperature control component can adjust the heating temperature of the temperature control dripping pipe 5. The temperature control component adopts armor temperature control.
Example 3
In order to put the alkali metal block into the melting crucible 8 conveniently, the melting crucible 8 includes a crucible body and a lid body detachably assembled to an opening at the top of the crucible body, and the gas injection hole 7 is formed in the lid body. When the filtering crucible is used, alkali metal needing filtering is put into the crucible body, and the crucible cover and the crucible body are sealed.
In order to make the internal discharge of fused alkali metal follow crucible completely, the bottom of the crucible body is funnel shaped structure, just control by temperature change trickle tube 5 connect in the opening part of funnel shaped structure bottommost.
In order to facilitate taking and placing of the smelting crucible 8 and the shaping crucible 6, the shell 1 comprises a shell body and a cover body which is detachably sealed at the top opening of the shell cover body, two holes are formed in the cover body and are respectively penetrated by two connecting pipelines 3, one connecting pipeline 3 is used for connecting the gas injection hole 7 and the buffer gas pressure control system, the other connecting pipeline 3 is used for connecting the vacuumizing hole 10 and the vacuumizing system, and a vacuumizing interface is fixed on the shell body or the cover body.
Spatially relative terms, such as "upper," "lower," "left," "right," and the like, may be used in the embodiments for ease of description to describe one element or feature's relationship to another element or feature as illustrated in the figures. It will be understood that the spatial terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. For example, if the device in the figures is turned over, elements described as "below" other elements or features would then be oriented "above" the other elements or features. Thus, the exemplary term "lower" can encompass both an upper and a lower orientation. The device may be otherwise oriented (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.
Moreover, relational terms such as "first" and "second," and the like, may be used solely to distinguish one element from another element having the same name, without necessarily requiring or implying any actual such relationship or order between such elements.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (11)
1. Alkaline metal evaporation filter equipment, its characterized in that is including inside shell that forms the operation chamber, and be located melting crucible and design crucible in the operation intracavity, wherein:
a heating body is fixed outside the smelting crucible, a temperature control dripping pipe is connected to an outlet at the bottom of the smelting crucible, a filtering piece is fixed in the temperature control dripping pipe, the top of the shaping crucible is provided with an opening, and the shaping crucible is positioned under the temperature control dripping pipe;
the shell is provided with a pumping and inflating interface to communicate with the vacuum maintaining system or the buffer gas distribution system, the smelting crucible is provided with a gas injection hole to be connected with the buffer gas pressure control system positioned outside the shell, and the smelting crucible is provided with a pumping system with a pumping hole positioned outside the shell.
2. The alkaline metal evaporation filter of claim 1, wherein said filter element is a stainless steel filter mesh.
3. The alkaline metal evaporating and filtering device as claimed in claim 2, wherein the stainless steel filtering net is a cylindrical net structure and is attached and fixed on the inner wall of the temperature-controlled dropping flow pipe.
4. The alkaline metal evaporation and filtration apparatus as claimed in claim 1, wherein a vacuum gauge is provided on said buffer gas pressure control system to adjust the buffer gas pressure inside the melting crucible.
5. The alkaline metal evaporation filter of claim 1, wherein a VCR port is fixedly attached to each of said gas injection port and said evacuation port.
6. The alkaline metal evaporation and filtration device as claimed in claim 1, wherein a laboratory bench is fixed in the operation chamber for placing a melting crucible.
7. The alkaline metal evaporation and filtration device of claim 1, wherein said temperature-controlled trickle flow tube comprises a straight tube and a temperature-control assembly secured to an outer wall of said straight tube, said filter element being secured to an inner wall of said straight tube.
8. The alkaline metal evaporation and filtration apparatus as claimed in claim 1, wherein said melting crucible includes a crucible body and a lid body detachably fitted to a top opening of said crucible body, said gas injection hole and said evacuation hole being formed in said lid body.
9. The alkaline metal evaporation and filtration device as claimed in claim 1, wherein the bottom of the crucible body is in a funnel shape, and the temperature controlled dropping flow tube is connected to the opening at the lowermost end of the funnel shape.
10. The alkaline metal evaporation and filtration device as claimed in claim 1, wherein the housing comprises a housing body and a cover body detachably sealed to an opening at the top of the housing cover body, the cover body is provided with a hole for two connecting pipes to pass through, one of the connecting pipes is used for connecting the gas injection hole and the buffer gas pressure control system, the other connecting pipe is used for connecting the vacuum hole and the vacuum system, and the housing body or the cover body is provided with the gas pumping and filling port.
11. The evaporation filtration method of an alkaline metal evaporation filtration apparatus as set forth in any one of claims 1 to 10, comprising the steps of:
step 1, opening a shell, taking out the smelting crucible, and placing alkali metal in the smelting crucible;
step 2, placing the smelting crucible in an operation cavity, communicating a gas injection hole with the air pressure control system, communicating the vacuumizing hole with the vacuumizing system, enabling the shaping crucible to be located right below the temperature control trickle tube, and sealing the shell;
step 3, connecting the pumping and inflating interface with a vacuum maintaining system to pump the operating cavity to be vacuum, simultaneously pumping the melting crucible to be vacuum, closing the vacuum maintaining system when the vacuum degree in the operating cavity reaches a preset value, and slowly injecting the required buffer gas into the buffer gas distribution system through the pumping and inflating interface;
step 4, starting the heating body and the temperature control trickle tube, adjusting the air pressure of buffer gas in the smelting crucible through a buffer gas air pressure control system, heating the alkali metal in a molten state in the smelting crucible, flowing through a filtering piece in the temperature control trickle tube, and dripping the alkali metal in the shaping crucible;
step 5, stopping heating the heating body and the temperature control trickling pipe when the liquid level in the shaping crucible reaches the required height or after the alkali metal in the melting crucible is completely treated, recovering the alkali metal in the temperature control trickling pipe to be in a solid state when the alkali metal is remained in the melting crucible, plugging the temperature control trickling pipe, and keeping the alkali metal remained in the melting crucible for later use;
step 6, closing the buffer gas pressure control system, opening the shell after the device is cooled, and taking out the shaping crucible to obtain purified alkali metal;
when alkali metal still remains in the melting crucible and needs to be taken again, the step 7 is carried out:
and 7, putting the shaped crucible back, closing the shell, communicating the pumping and inflating interface with a vacuum maintaining system to pump the operation cavity to be vacuum, communicating the pumping and vacuumizing hole with a pumping and vacuumizing system to pump the smelting crucible to be vacuum, slowly injecting the required buffer gas into the buffer gas distribution system through the pumping and inflating interface, adjusting the gas pressure of the buffer gas in the smelting crucible through the buffer gas pressure control system, and continuing to perform the steps 4 and 5.
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| CN202010231932.2A CN113444895B (en) | 2020-03-27 | 2020-03-27 | Alkaline metal evaporation and filtration device and method |
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| CN202010231932.2A CN113444895B (en) | 2020-03-27 | 2020-03-27 | Alkaline metal evaporation and filtration device and method |
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| CN113444895B CN113444895B (en) | 2023-06-30 |
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| CN113444895B (en) | 2023-06-30 |
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