CN113444895B - Alkaline metal evaporation and filtration device and method - Google Patents
Alkaline metal evaporation and filtration device and method Download PDFInfo
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- CN113444895B CN113444895B CN202010231932.2A CN202010231932A CN113444895B CN 113444895 B CN113444895 B CN 113444895B CN 202010231932 A CN202010231932 A CN 202010231932A CN 113444895 B CN113444895 B CN 113444895B
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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
-
- 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 filtering device and method, wherein the alkaline metal evaporation filtering device comprises a shell, a smelting crucible, a temperature control drip pipe and a shaping crucible, an operating cavity is formed in the shell, the smelting crucible is positioned in the operating cavity, the temperature control drip pipe is connected to an outlet at the bottom of the smelting crucible, the shaping crucible is positioned in the operating cavity and right below the temperature control drip pipe, an air pumping and charging 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, an air 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 drip pipe. The device can quantitatively process 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
The alkali metal is generally active, the directly purchased alkali metal is easy to oxidize in the packaging and preserving processes, the oxidized alkali metal can form compact membranous oxide on the upper layer of the metal liquid surface in a heating and melting state, the evaporation rate in the experiment can be influenced in the evaporation and use process, and in order to meet the requirement of the experiment on the evaporation rate of the alkali metal, the oxide needs to be removed first and then the evaporation experiment needs to be carried out.
When the alkali metal is used for removing the oxide in the prior art, the alkali metal sample is extremely easy to oxidize if not used for the first time after being treated, and the repeated treatment is needed, so that the time and the labor are wasted, and the energy and the sample are wasted.
Disclosure of Invention
The invention aims to solve the problem that alkali metal is easy to waste in repeated treatment in the prior art, and provides an alkali metal evaporation and filtration device.
Another object of the present invention is to provide an evaporation filtration method of the basic metal evaporation filtration apparatus.
The technical scheme adopted for realizing the purpose of the invention is as follows:
the alkaline metal evaporation and filtration device comprises a shell, a smelting crucible and a shaping crucible, wherein an operation cavity is formed in the shell, and the smelting crucible and the shaping crucible are positioned in the operation cavity, wherein:
a heating body is fixed outside the smelting crucible, a temperature control drip pipe is connected to an outlet at the bottom of the smelting crucible, a filtering piece is fixed in the temperature control drip pipe, an opening is formed in the top of the shaping crucible, and the shaping crucible is positioned right below the temperature control drip pipe;
the shell is provided with an air pumping and charging interface for communicating with the vacuum maintaining system or the buffer gas distribution system, the smelting crucible is provided with an air injection hole for connecting with the buffer gas pressure control system positioned outside the shell, and the smelting crucible is provided with a vacuum pumping system positioned outside the shell.
In the above technical scheme, the filter element 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 drip pipe.
In the technical scheme, the buffer gas pressure control system is provided with a vacuum gauge to adjust the buffer gas pressure in the smelting crucible.
In the above technical scheme, the gas injection hole and the vacuum pumping hole are respectively 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 drip pipe comprises a straight pipe and a temperature control assembly fixed on the outer wall of the straight pipe, and the filter element is fixed on the inner wall of the straight pipe.
In the technical scheme, the smelting crucible comprises a crucible body and a cover body detachably assembled on an opening at the top 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 of a funnel-shaped structure, and the temperature control drip pipe is connected to the opening at the bottommost end of the funnel-shaped structure.
In the above technical scheme, the shell includes the shell body and can dismantle sealed in shell cover top opening's lid, offer the hole on the lid and supply two connecting tube to wear out, wherein one connecting tube be used for connecting gas injection hole and buffer gas pneumatic control system, another connecting tube be used for connecting vacuum hole and vacuum system, be formed with on shell body or the lid the interface is inflated in the evacuation.
In another aspect of the present invention, the evaporation filtration method of the alkaline metal evaporation filtration device further comprises the following steps:
step 1, opening a shell, taking out the smelting crucible, and placing alkali metal into the smelting crucible;
step 4, starting a heating body and a temperature-control drip pipe, regulating 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 filter element in the temperature-control drip pipe, and dripping in the shaping crucible;
when alkali metal is still remained in the smelting crucible and needs to be taken again, carrying out step 7:
and 7, replacing the shaping crucible, closing the shell, communicating the vacuumizing interface with the vacuum maintaining system to vacuumize the operation cavity, communicating the vacuumizing hole with the vacuumizing system to vacuumize the smelting crucible, slowly injecting the needed buffer gas through the vacuumizing interface by the buffer gas distribution system, adjusting the pressure of the buffer gas in the smelting crucible through the buffer gas pressure control system, and continuing the steps 4 and 5.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the smelting crucible is heated by the heating body, so that alkali in the crucible is heated to be in a liquid state, oxide floats above liquid alkali metal in the heating process, liquid drops from the bottom, a small amount of oxide is filtered, and a filter piece is not easy to block.
2. The temperature of the temperature-control drip pipe is regulated to control whether liquid metal drips from the lower part of the smelting crucible, when the liquid level of the lower shaping crucible reaches the required height, the temperature-control drip part is closed to heat, so that alkali metal in the heating crucible stops dripping, and filtration is completed, thereby realizing quantitative batch evaporation and purification.
3. The alkaline metal evaporation and filtration device is carried out under the protection of buffer gas, has high safety coefficient, is convenient to operate, and can be used without special training. The alkaline metal evaporation filter device has the advantages of simple structure, low manufacturing cost and convenience for commercialization popularization and application.
Drawings
Fig. 1 is a schematic diagram showing the structure of an alkali metal evaporation filter device.
FIG. 2 is a schematic diagram showing the positional relationship between a shaping crucible and a melting crucible.
In the figure: the device comprises a shell, a pumping and inflating interface, a connecting pipeline, a heating body, a temperature control drip pipe, a shaping crucible, a gas injection hole, a smelting crucible, a filtering piece and a vacuumizing hole, wherein the shell is arranged at the bottom of the shell, the pumping and inflating interface is arranged at the bottom of the shell, the connecting pipeline is arranged at the bottom of the shell, the heating body is arranged at the bottom of the shell, the temperature control drip pipe is.
Detailed Description
The invention is described in further detail below with reference to the drawings and the specific examples. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
The alkaline metal evaporation filtering device comprises a shell 1, a smelting crucible 8, a temperature control drip pipe 5 and a shaping crucible 6, wherein an operation cavity is formed in the shell, the smelting crucible 8 is positioned in the operation cavity, the temperature control drip pipe 5 is connected to an outlet at the bottom of the smelting crucible 8, the shaping crucible 6 is positioned in the operation cavity and is positioned right below the temperature control drip pipe 5, a heating body 4 is fixedly arranged outside the smelting crucible 8, and a filtering piece 9 is fixedly arranged in the temperature control drip pipe 5.
The shell 1 is provided with an air pumping and charging interface 2 for communicating with a vacuum maintaining system or a buffer gas distribution system, the smelting crucible is provided with an air injection hole 7 for connecting with a buffer gas pressure control system positioned outside the shell, and the smelting crucible is provided with a vacuum pumping hole 10 for connecting with a vacuum pumping system positioned outside the shell.
The heating body 4 is fixed on the outer wall of the smelting crucible 8 to form an integral structure, and the integral structure is fixed in the shell 1 through a bracket, which is not shown in the bracket drawing. 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 (armoured temperature control can be adopted) heats the alkali metal in the smelting crucible 8, the alkali metal is melted, the metal oxide keeps in a solid state, the alkali metal becomes liquid, the oxide on the surface of the alkali metal floats on the upper surface of the molten pool, the melted alkali metal enters the temperature-control drip pipe 5, the temperature-control drip pipe 5 continuously heats the alkali metal in the pipe, the alkali metal keeps in 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 cavity and the pressure of buffer gas, a pressure gauge is arranged on the shell 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 the buffer gas supplied by the buffer gas pressure control system and the buffer gas distribution system can be inert gases such as argon or neon.
The temperature of the temperature-control drip pipe 5 is controlled to achieve the aim of controlling whether the liquid metal drips from the temperature-control drip pipe 5, when the liquid level in the lower shaping crucible 6 reaches the required height, the heating of the temperature-control drip pipe 5 is closed, so that the alkali metal in the smelting crucible 8 stops dripping, and the filtration is completed.
The evaporation and filtration method of the alkaline metal evaporation and filtration device comprises the following steps:
step 1, placing alkali metal in a smelting crucible 8, and communicating an air injection hole 7 with the air pressure control system;
and 4, starting the heating body 4 and the temperature-control drip pipe 5, regulating the gas pressure in the smelting crucible 8 to several hundred Pa to several kiloPa by using a buffer gas pressure control system, and dripping the alkali metal heated into a molten state into the shaping crucible 6 by using a filter element in the temperature-control drip pipe.
when alkali metal is still remained in the smelting crucible and needs to be taken again, carrying out step 7:
and 7, replacing the shaping crucible, closing the shell, communicating the vacuumizing interface with the vacuum maintaining system to vacuumize the operation cavity, communicating the vacuumizing hole with the vacuumizing system to vacuumize the smelting crucible, slowly injecting the needed buffer gas through the vacuumizing interface by the buffer gas distribution system, adjusting the pressure of the buffer gas in the smelting crucible through the buffer gas pressure control system, and continuing the steps 4 and 5.
The vacuumizing process is to prevent liquid alkali metal bubbles formed after heating, and a glass window can be arranged on the shell 1 or a flange of the shell 1 to directly observe the liquid level in the shaping crucible 6. When the temperature control drip pipe 5 is used for the first time, the temperature control drip pipe 5 is not plugged, the air pumping interface 2 is connected with the vacuum maintaining system, the operation cavity and the smelting crucible 8 are vacuumized at the same time, and when the temperature control drip pipe is used again after cooling, the air pumping interface 2 is connected with the vacuum maintaining system to vacuumize the operation cavity, the vacuumizing holes are communicated with the vacuumizing system to vacuumize the smelting crucible, the pipeline connected with the vacuumizing holes is provided with the flow rate valve, so the vacuumizing speed is relatively low, when the vacuum is pumped for the first time, the vacuumizing system connected with the vacuumizing holes can be closed, and the vacuum degree in the smelting crucible is realized through the vacuum maintaining system connected with the air pumping interface 2 and the open temperature control drip pipe.
Example 2
In order to intercept alkali metal oxide well and not be destroyed by 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 drip pipe 5, so that effective interception can be realized and blockage is not easy to occur. Furthermore, the filtering piece is a stainless steel filtering net which is of a cylindrical net structure and is attached and fixed on the inner wall of the temperature control drip pipe.
In order to control the pressure of the buffer gas in the smelting crucible 8 in a matching way, a vacuum gauge is arranged on the buffer gas pressure control system.
In order to facilitate disassembly, VCR interfaces are fixedly connected to the gas injection holes 7 and the vacuum pumping holes 10.
In order to facilitate placement of the melting crucible 8 within the housing 1, a laboratory bench is secured within the operating chamber to place the melting crucible 8. In use, the crucible is placed on a laboratory bench (not shown).
In order to make the alkali metal in the molten state flow out smoothly, the temperature-control drip pipe 5 comprises a straight pipe and a temperature control component fixed on the outer wall of the straight pipe, and the filter element is fixed in the straight pipe. The temperature control assembly can adjust the heating temperature of the temperature control drip pipe 5. The temperature control component adopts armoured temperature control.
Example 3
In order to facilitate the placement of the alkali metal block into the melting crucible 8, the melting crucible 8 comprises a crucible body and a cover body detachably assembled on the top opening of the crucible body, and the gas injection hole 7 is formed on the cover body. When in use, alkali metal to be filtered is put into the crucible body, and the crucible cover and the crucible body are sealed.
In order to ensure that the molten alkali metal is completely discharged from the crucible body, the bottom of the crucible body is of a funnel-shaped structure, and the temperature control drip pipe 5 is connected to an opening at the bottommost end of the funnel-shaped structure.
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 can be detachably sealed on the top opening of the shell cover body, two holes are formed in the cover body and are respectively provided for two connecting pipelines 3 to penetrate out, 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's 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 "under" other elements or features would then be oriented "over" the other elements or features. Thus, the exemplary term "lower" may encompass both an upper and lower orientation. The device may be otherwise positioned (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 merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. The utility model provides an alkali metal evaporation filter equipment, its characterized in that includes the shell that inside forms the operation chamber, and is located smelting crucible and the design crucible in the operation chamber, wherein:
a heating body is fixed outside the smelting crucible, a temperature control drip pipe is connected to an outlet at the bottom of the smelting crucible, a filtering piece is fixed in the temperature control drip pipe, an opening is formed in the top of the shaping crucible, and the shaping crucible is positioned right below the temperature control drip pipe;
the shell is provided with an air pumping and charging interface for communicating with a vacuum maintaining system or a buffer gas distribution system, an air injection hole is formed on the smelting crucible for connecting with a buffer gas pressure control system positioned outside the shell, and a vacuum pumping system positioned outside the shell is formed on the smelting crucible;
an evaporative filtration method comprising the steps of:
step 1, opening a shell, taking out the smelting crucible, and placing alkali metal into the smelting crucible;
step 2, placing the smelting crucible in an operation cavity, communicating an air injection hole with the air pressure control system, communicating the vacuumizing hole with the vacuumizing system, enabling the shaping crucible to be positioned under the temperature control drip pipe, and sealing the shell;
step 3, the pumping and inflating interface is connected with the vacuum maintaining system to pump vacuum of the operation cavity, meanwhile, the interior of the smelting crucible is pumped with vacuum, when the vacuum degree in the operation cavity reaches a preset value, the vacuum maintaining system is closed, and the buffer gas distribution system slowly injects the needed buffer gas through the pumping and inflating interface;
step 4, starting a heating body and a temperature-control drip pipe, regulating 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 filter element in the temperature-control drip pipe, and dripping in the shaping crucible;
step 5, stopping heating the heating body and the temperature-control drip pipe when the liquid level in the shaping crucible reaches the required height or after the alkali metal in the smelting crucible is completely treated, and when the alkali metal is still left in the smelting crucible, the alkali metal in the temperature-control drip pipe is recovered to a solid state, the temperature-control drip pipe is blocked, and the alkali metal left in the smelting crucible is for standby;
step 6, closing a buffer gas pressure control system, opening a shell after the device is cooled, and taking out the shaping crucible to obtain purified alkali metal;
when alkali metal is still remained in the smelting crucible and needs to be taken again, carrying out step 7:
and 7, replacing the shaping crucible, closing the shell, communicating the vacuumizing interface with the vacuum maintaining system to vacuumize the operation cavity, communicating the vacuumizing hole with the vacuumizing system to vacuumize the smelting crucible, slowly injecting the needed buffer gas through the vacuumizing interface by the buffer gas distribution system, adjusting the pressure of the buffer gas in the smelting crucible through the buffer gas pressure control system, and continuing the steps 4 and 5.
2. The alkaline metal evaporation filter apparatus as defined in claim 1, wherein said filter member is a stainless steel filter screen.
3. The alkaline metal evaporation and filtration device according to claim 2, wherein the stainless steel filter screen has a cylindrical net structure and is adhered and fixed on the inner wall of the temperature-control drip tube.
4. The alkaline metal evaporation and filtration device as claimed in claim 1, wherein a vacuum gauge is provided on the buffer gas pressure control system to adjust the buffer gas pressure inside the melting crucible.
5. The alkaline metal evaporation filter device according to claim 1, wherein VCR interfaces are fixedly connected to the gas injection hole and the vacuum suction hole, respectively.
6. The alkaline metal evaporation and filtration apparatus as claimed in claim 1, wherein a laboratory bench is fixed in the operation chamber to place the melting crucible.
7. The alkaline metal evaporation and filtration device as claimed in claim 1, wherein said temperature-controlled drip tube comprises a straight tube and a temperature-controlled assembly secured to an outer wall of said straight tube, said filter being secured to an inner wall of said straight tube.
8. The alkaline metal evaporation and filtration apparatus as defined in claim 1, wherein said melting crucible comprises a crucible body and a cover body detachably mounted on a top opening of said crucible body, said gas injection hole and said vacuum suction hole being formed in said cover body.
9. The alkaline metal evaporation and filtration device according to claim 8, wherein the bottom of the crucible body is in a funnel-shaped structure, and the temperature control drip pipe is connected to an opening at the bottommost end of the funnel-shaped structure.
10. The alkaline metal evaporation and filtration device according to claim 1, wherein the housing comprises a housing body and a cover body detachably sealed at an opening at the top of the housing cover body, and two connecting pipes are provided on the cover body for penetrating out, wherein one connecting pipe is used for connecting the gas injection hole and the buffer gas pressure control system, the other connecting pipe is used for connecting the vacuumizing hole and the vacuumizing system, and the vacuumizing interface is formed on the housing body or the cover body.
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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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| CN113444895A (en) | 2021-09-28 |
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