CN112028033B - Device and method for purifying selenium through crystallization - Google Patents
Device and method for purifying selenium through crystallization Download PDFInfo
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- CN112028033B CN112028033B CN202010877357.3A CN202010877357A CN112028033B CN 112028033 B CN112028033 B CN 112028033B CN 202010877357 A CN202010877357 A CN 202010877357A CN 112028033 B CN112028033 B CN 112028033B
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/02—Elemental selenium or tellurium
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/08—Production of homogeneous polycrystalline material with defined structure from liquids by zone-melting
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
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Abstract
The invention relates to the technical field of selenium purification, in particular to a device and a method for purifying selenium through crystallization. The device comprises a power regulating system 1, a heating system 4, a vertical crystallization reactor 5 and a temperature measuring system 7; the power regulating system 1 is connected with the heating system 4 through a lead 2; the heating system 4 is fixed in the midair through a support frame 3; the heating area of the heating system 4 is a hollow annular structure; the temperature measuring end of the temperature measuring system 7 is positioned in the heating area; the vertical crystallization reactor 5 can move up and down in the heating area of the heating system 4 through a positioning and adjusting system 6; porous filter materials are placed in the vertical crystallization reactor 5. Compared with the traditional zone melting method, the method has the advantages of shortened production period and better purification effect.
Description
Technical Field
The invention relates to the technical field of selenium purification, in particular to a device and a method for purifying selenium through crystallization.
Background
Selenium (Se) is a metal with important strategic significance in the high-tech field, is an essential trace element in organisms, and has an average abundance of about 0.05ppm in the crust. In recent years, selenium has been the focus of much scientific research in the fields of semiconductor materials and human health due to its unique semiconductor and anticancer properties.
The selenium produced in industry is a primary product, and can be purified by further refining to obtain pure selenium meeting the preparation requirements of related materials. At present, the selenium purification methods published at home and abroad mainly comprise a crude selenium redox method and H2Se thermal decomposition method, ion exchange method, zone melting method, vacuum distillation method, etc., wherein the zone melting method is widely used for purification of selenium due to its simple process. The traditional zone melting method adopts a horizontal placement mode, has obvious effect of removing impurity Cu, but for impurities such as Si, Zn, Fe, Na, Al and the like, because the distribution coefficient of the impurities and Se is close to 1, the impurities cannot be deeply removed (Su C H, Sha Y G]Journal of crystal growth 1998,187(3-4): 569-.
Disclosure of Invention
The invention aims to provide a device and a method for purifying selenium by crystallization, which can effectively remove impurities such as Si, Zn, Cu, Fe, Na, Al and the like, shorten the production period and have better purification effect compared with the traditional zone melting method.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a device for purifying selenium by crystallization, which comprises a power regulating system 1, a heating system 4, a vertical crystallization reactor 5 and a temperature measuring system 7;
the power regulating system 1 is connected with the heating system 4 through a lead 2;
the heating system 4 is fixed in the midair through a support frame 3; the heating area of the heating system 4 is a hollow annular structure;
the temperature measuring end of the temperature measuring system 7 is positioned in the heating area;
the vertical crystallization reactor 5 can move up and down in the heating area of the heating system 4 through a positioning and adjusting system 6;
porous filter materials are placed in the vertical crystallization reactor 5.
Preferably, the height of the heating area of the heating system 4 is 1-5 cm, and the diameter is 2-6 cm.
Preferably, the outer diameter of the vertical crystallization reactor 5 is smaller than the diameter of the heating zone; the length of the vertical crystallization reactor 5 is 20-60 cm.
Preferably, the positioning and adjusting system 6 comprises a supporting device and an automatic lifting device; the automatic lifting device is fixedly connected with the vertical crystallization reactor 5 and drives the vertical crystallization reactor 5 to move up and down by moving up and down on the supporting device.
Preferably, the pore diameter of the porous filtering material is 0.01-0.1 mm.
Preferably, the density of the porous filtering material is 5-6 g/cm3。
Preferably, the heating system 4 is heated by using a resistance wire or an induction coil.
The invention provides a method for purifying selenium by crystallization based on the device in the scheme, which comprises the following steps: placing a selenium material to be purified in a vertical crystallization reactor 5, then placing a porous filtering material on the selenium material to be purified, adjusting a power adjusting system 1 to enable a heating system 4 to be heated to a purification temperature, and after a temperature system 7 to be detected determines that the purification temperature is stable, placing the vertical crystallization reactor 5 filled with the selenium material and the porous filtering material in a heating area of the heating system 4; the vertical crystallization reactor 5 is driven by the positioning and adjusting system 6 to move from bottom to top, so that the top to the bottom of the vertical crystallization reactor 5 sequentially passes through the heating regions.
Preferably, the mass content of Se in the selenium material to be purified is more than 92 percent.
Preferably, the moving speed of the vertical crystallization reactor 5 is 1-10 mm/min.
The invention provides a device for purifying selenium by crystallization, which comprises a power regulating system 1, a heating system 4, a vertical crystallization reactor 5 and a temperature measuring system 7; the power regulating system 1 is connected with the heating system 4 through a lead 2; the heating system 4 is fixed in the midair through a support frame 3; the heating area of the heating system 4 is a hollow annular structure; the temperature measuring end of the temperature measuring system 7 is positioned in the heating area; the vertical crystallization reactor 5 can move up and down in the heating area of the heating system 4 through a positioning and adjusting system 6; porous filter materials are placed in the vertical crystallization reactor 5.
Compared with the traditional zone melting, the invention sets the crystallization reactor as a vertical crystallization reactor, belongs to the vertical zone melting, and places porous filtering materials in the vertical crystallization reactor 5, when in use, selenium materials to be purified are placed in the vertical crystallization reactor 5, then the porous filtering materials are placed on the selenium materials, the positioning adjusting system 6 is utilized to drive the top to the bottom of the vertical crystallization reactor 5 to pass through a heating zone in sequence, the selenium materials are melted in the heating zone, and cooling crystallization is carried out after leaving the heating zone, on one hand, the impurity removal is realized by utilizing the principle of zone melting and the difference of the solubility of the impurities between solid and liquid; on the other hand, the impurity sedimentation is realized in the melting zone by utilizing the fact that the specific gravity of some impurities is larger than that of selenium, and the impurities are concentrated at the bottom of the crystallization reactor along with the gradual downward movement of the melting zone. Meanwhile, as the selenium melt moves downwards from top to bottom in sequence, the porous filtering material moves downwards along with the melt under the action of self gravity, so that light large-particle impurities with specific gravity smaller than that of the selenium melt can be prevented from floating upwards, the separation effect of the impurities is further improved, and the impurities such as Si, Zn, Cu, Fe, Na, Al and the like are effectively removed. Compared with the traditional horizontal zone smelting, the device has better separation effect, can reduce the up-and-down movement times and shorten the production period.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for purifying selenium by crystallization according to the present invention;
wherein, the device comprises a power adjusting system 1, a lead 2, a support frame 3, a heating system 4, a vertical crystallization reactor 5, a positioning adjusting system 6 and a temperature measuring system 7.
Detailed Description
As shown in FIG. 1, the invention provides a device for purifying selenium by crystallization, which comprises a power regulating system 1, a heating system 4, a vertical crystallization reactor 5 and a temperature measuring system 7;
the power regulating system 1 is connected with the heating system 4 through a lead 2;
the heating system 4 is fixed in the midair through a support frame 3; the heating area of the heating system 4 is a hollow annular structure;
the temperature measuring end of the temperature measuring system 7 is positioned in the heating area;
the vertical crystallization reactor 5 can move up and down in the heating area of the heating system 4 through a positioning and adjusting system 6;
porous filter materials are placed in the vertical crystallization reactor 5.
The device for purifying selenium by crystallization provided by the invention comprises a power regulating system 1, wherein the power regulating system 1 is used for regulating the heating temperature of a heating system 4. The present invention has no special requirements for the structure of the power conditioning system 1, and any power conditioning system capable of adjusting the heating temperature is well known in the art.
The device for purifying selenium by crystallization provided by the invention comprises a heating system 4. In the present invention, the heating system 4 is connected to the power conditioning system 1 via a line 2. In the present invention, the heating system 4 is used for heating the vertical crystallization reactor 5 to perform zone melting.
In the present invention, the heating system 4 is fixed in the mid-air by the support frame 3. The specific position of the heating system 4 is not particularly limited in the invention, and the requirement that the bottom of the vertical crystallization reactor 5 does not contact any object when the vertical crystallization reactor moves up and down in the heating area can be met.
In the present invention, the heating zone of the heating system 4 has a hollow ring-shaped structure. In the invention, the height of the heating area of the heating system 4 is preferably 1-5 cm, and more preferably 2-4 cm; the diameter is preferably 2-6 cm, and more preferably 3-5 cm.
In the present invention, the heating system 4 is preferably heated by using a resistance wire or an induction coil.
The device for purifying selenium by crystallization provided by the invention comprises a vertical crystallization reactor 5, wherein the vertical crystallization reactor 5 can move up and down in a heating area of a heating system 4 through a positioning and adjusting system 6. In the invention, the vertical crystallization reactor 5 is used for containing selenium materials to be purified and providing a reaction place for zone melting.
In the present invention, the vertical crystallization reactor 5 is preferably tubular, the outer diameter of the vertical crystallization reactor 5 is preferably smaller than the diameter of the heating zone, and the length of the vertical crystallization reactor 5 is preferably 20 to 60cm, and more preferably 30 to 50 cm. The invention controls the outer diameter of the vertical crystallization reactor 5 to be smaller than the diameter of the heating area, can avoid the vertical crystallization reactor 5 from contacting with the heating area, and ensures that the vertical crystallization reactor 5 is heated uniformly. In the present invention, the material of the vertical crystallization reactor 5 is preferably a material resistant to a high temperature of 800 ℃, and may be, but not limited to, graphite or quartz.
As an embodiment of the present invention, the positioning adjustment system 6 includes a supporting device and an automatic lifting device; the automatic lifting device is fixedly connected with the vertical crystallization reactor 5 and drives the vertical crystallization reactor 5 to move up and down by moving up and down on the supporting device. The supporting device and the automatic lifting device are not limited in any way, and the functions can be achieved.
In the invention, a porous filtering material is placed in the vertical crystallization reactor 5, and the aperture of the porous filtering material is preferably 0.01-0.1 mm, and more preferably 0.04-0.08 mm. In the present invention, the porous filter material is preferably circular, and the diameter is preferably 0.5cm smaller than the inner diameter of the vertical crystallization reactor 5. The invention controls the aperture of the porous filter material in the range, on one hand, the selenium melt can be allowed to pass through, and on the other hand, the light large particle impurities in the selenium melt can be prevented from floating upwards, so that the light large particle impurities and the particles with larger specific weight are concentrated at the bottom of the vertical crystallization reactor 5.
The device for purifying selenium by crystallization provided by the invention comprises a temperature measuring system 7, wherein a temperature measuring end of the temperature measuring system 7 is positioned in a heating area and is used for measuring the temperature of the heating area. In the present invention, the temperature measuring end of the temperature measuring system 7 is preferably not in contact with the heating area. The temperature measuring system 7 is not limited in any way, and any temperature measuring system with a temperature measuring function known in the art may be used, and may be specifically, but not limited to, a thermocouple.
The invention provides a method for purifying selenium by crystallization based on the device in the scheme, which comprises the following steps: placing the selenium material to be purified in a vertical crystallization reactor 5, then placing a porous filtering material on the selenium material to be purified, adjusting a power adjusting system 1 to enable a heating system 4 to be heated to a purification temperature, and after a temperature system 7 to be detected determines that the purification temperature is stable, placing the vertical crystallization reactor 5 filled with the selenium material and the porous filtering material in a heating area of the heating system 4; the vertical crystallization reactor 5 is driven by the positioning and adjusting system 6 to move from bottom to top, so that the top to the bottom of the vertical crystallization reactor 5 sequentially passes through the heating regions.
In the invention, the mass content of Se in the selenium material to be purified is preferably more than 92%, and the selenium material to be purified is preferably powder or block.
In the invention, the purification temperature is preferably 260-300 ℃, and the purification temperature is controlled in the range, so that the selenium can be ensured to be molten, and the selenium has lower viscosity and better fluidity.
In the present invention, the moving speed of the vertical crystallization reactor 5 is preferably 1 to 10mm/min, and more preferably 3 to 8 mm/min. The invention controls the moving speed of the vertical crystallization reactor 5 within the range, can ensure better impurity removal effect and has lower energy consumption.
In the process that the top part and the bottom part of the vertical crystallization reactor 5 sequentially pass through the heating region, selenium materials in the vertical crystallization reactor 5 are melted when reaching the heating region, cooled and crystallized after leaving the heating region, and the impurity is removed by utilizing the solubility difference of the impurities between solid and liquid; on the other hand, after the selenium material is melted in the heating area, the impurity is settled in the melting area by utilizing the difference of the specific gravity of the impurity and the selenium, and the impurity is gradually enriched to the bottom of the crystallization reactor along with the gradual downward movement of the melting area; meanwhile, as the selenium melt moves downwards from top to bottom in sequence, the porous material moves downwards along with the melt under the action of self gravity, so that the floating of light large-particle impurities with the specific gravity smaller than that of the selenium melt can be avoided, the separation effect of the impurities is further improved, the effective removal of impurities such as Si, Zn, Cu, Fe, Na, Al and the like is realized, and finally the porous material is settled to the bottom of the vertical crystallization reactor 5.
The invention has no special requirement on the number of times of the vertical crystallization reactor 5 moving from bottom to top, and can be set according to the impurity removal effect. When the number of the downward movement times of the vertical crystallization reactor 5 is increased, the purity of the finally obtained selenium is increased.
In the process of the invention, when the vertical crystallization reactor 5 moves from bottom to top repeatedly, the porous material is always positioned at the bottom of the vertical crystallization reactor 5.
The apparatus and method for purifying selenium by crystallization provided by the present invention will be described in detail with reference to the following examples, which should not be construed as limiting the scope of the present invention.
Example 1
The adopted device is shown in figure 1, and the selenium material is purified by the following specific steps: the selenium material to be purified (Se99.1%) was placed in a vertical crystallization reactor 5 (diameter 1.6cm, height 30cm), on which a porous filter material (diameter 1.1cm, pore diameter 0.02mm, density 5.5 g/cm) was placed3) Heating system 4 (heating area diameter is 2.0cm, height is 1.0cm) is heated to 250 ℃ by adjusting power adjusting system 1, the moving speed of automatic lifting device in positioning adjusting system 6 is set to be 0.5mm/min, automatic lifting device drives vertical crystallization reactor 5 to move from bottom to top, the top to bottom of vertical crystallization reactor 5 sequentially passes through the heating area, selenium material is melted in the heating area, and after melting, porousThe material moves downwards along with the melt, when the melt leaves the heating area, the melt is cooled and crystallized, the process of moving the vertical crystallization reactor 5 from bottom to top is repeated for 5 times, and the purity of the selenium after the reaction is finished is 99.98%.
Example 2
The adopted device is shown in figure 1, and the selenium material is purified by the following specific steps: the selenium material to be purified (Se98.2%) was placed in a vertical crystallization reactor 5 (diameter 2.5cm, height 50cm), on which a porous filter material (diameter 2.0cm, pore diameter 0.07mm, density 5.7 g/cm) was placed3) The temperature of a heating system 4 (the diameter of a heating area is 3.0cm, the height of the heating area is 2.0cm) is increased to 260 ℃ by adjusting a power adjusting system 1, the moving speed of an automatic lifting device in a positioning adjusting system 6 is set to be 1mm/min, the automatic lifting device drives a vertical crystallization reactor 5 to move from bottom to top, so that the top to the bottom of the vertical crystallization reactor 5 sequentially passes through the heating area, selenium materials are melted in the heating area, the melted porous materials move downwards along with a melt, the melt is cooled and crystallized after leaving the heating area, the moving process of the vertical crystallization reactor 5 from bottom to top is repeated for 5 times, and the purity of the selenium after the reaction is 99.95%.
Example 3
The adopted device is shown in figure 1, and the selenium material is purified by the following specific steps: the selenium material to be purified (Se99.92%) was placed in a vertical crystallization reactor 5 (diameter 3.5cm, height 60cm), and a porous filter material (diameter 3cm, pore diameter 0.01mm, density 5.1 g/cm) was placed on the selenium material3) The temperature of a heating system 4 (the diameter of a heating area is 5cm, the height of the heating area is 4cm) is increased to 260 ℃ by adjusting a power adjusting system 1, the moving speed of an automatic lifting device in a positioning adjusting system 6 is set to be 1mm/min, the automatic lifting device drives a vertical crystallization reactor 5 to move from bottom to top, the top to the bottom of the vertical crystallization reactor 5 sequentially passes through the heating area, a selenium material is melted in the heating area, a melted porous material moves downwards along with a melt, the melt is cooled and crystallized after leaving the heating area, the moving process of the vertical crystallization reactor 5 from bottom to top is repeated for 5 times, and the purity of the selenium after the reaction is 99.995%.
Comparative examples 1 to 3
The difference from the examples 1 to 3 is that the vertical zone melting is changed into the horizontal zone melting, a horizontal crystallization reactor is used, a porous filtering material is not used, and the rest conditions are the same as those of the examples 1 to 3, and the result shows that the purity of the crude selenium raw material obtained by 20 times of horizontal zone melting in the example 1 is 99.8%; the purity of the crude selenium raw material obtained by 20 horizontal zone smelts in the embodiment 2 is 99.1%; the purity of the crude selenium raw material in example 3 after 20 horizontal zone smelts was 99.93%.
Comparative example 4
The difference from example 1 is that no porous filter material was used and the purity of selenium after the reaction was 99.91%.
As can be seen from the above examples and comparative examples, the purification device and method of the present invention can purify selenium materials, compared with the traditional horizontal zone melting, the device of the present invention has better separation effect, and can reduce the times of up-down movement and shorten the production period.
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 (7)
1. A method for purifying selenium by crystallization, comprising the steps of: placing the selenium material to be purified in a vertical crystallization reactor (5), then placing a porous filtering material on the selenium material to be purified, adjusting a power adjusting system (1) to enable a heating system (4) to be heated to a purification temperature, and after a temperature system (7) to be detected determines that the purification temperature is stable, placing the vertical crystallization reactor (5) filled with the selenium material and the porous filtering material in a heating area of the heating system (4); the vertical crystallization reactor (5) is driven to move from bottom to top by the positioning and adjusting system (6), so that the top to the bottom of the vertical crystallization reactor (5) sequentially passes through the heating region;
the moving speed of the vertical crystallization reactor (5) is 1-10 mm/min;
the purification temperature is 260-300 ℃;
the device for crystallizing and purifying selenium comprises a power regulating system (1), a heating system (4), a vertical crystallization reactor (5) and a temperature measuring system (7);
the power regulating system (1) is connected with the heating system (4) through a lead (2);
the heating system (4) is fixed in the mid-air through a support frame (3); the heating area of the heating system (4) is a hollow annular structure;
the temperature measuring end of the temperature measuring system (7) is positioned in the heating area;
the vertical crystallization reactor (5) can move up and down in a heating area of the heating system (4) through a positioning and adjusting system (6);
a porous filtering material is placed in the vertical crystallization reactor (5); the aperture of the porous filtering material is 0.01-0.1 mm; the density of the porous filtering material is 5-6 g/cm3。
2. The method according to claim 1, wherein the selenium material to be purified has a Se content of > 92% by mass.
3. An apparatus for use in a method for the crystalline purification of selenium as claimed in claim 1 or 2, comprising a power regulation system (1), a heating system (4), a vertical crystallization reactor (5) and a temperature measurement system (7);
the power regulating system (1) is connected with the heating system (4) through a lead (2);
the heating system (4) is fixed in the midair through a support frame (3); the heating area of the heating system (4) is a hollow annular structure;
the temperature measuring end of the temperature measuring system (7) is positioned in the heating area;
the vertical crystallization reactor (5) can move up and down in a heating area of the heating system (4) through a positioning and adjusting system (6);
the vertical crystallization reactor (5)A porous filter material is placed in the porous filter material; the aperture of the porous filtering material is 0.01-0.1 mm; the density of the porous filtering material is 5-6 g/cm3。
4. The device according to claim 3, characterized in that the heating zone of the heating system (4) has a height of 1-5 cm and a diameter of 2-6 cm.
5. The apparatus according to claim 3 or 4, characterized in that the vertical crystallization reactor (5) has an outer diameter smaller than the diameter of the heating zone; the length of the vertical crystallization reactor (5) is 20-60 cm.
6. The device according to claim 3, characterized in that said positioning adjustment system (6) comprises a support device and an automatic lifting device; the automatic lifting device is fixedly connected with the vertical crystallization reactor (5) and drives the vertical crystallization reactor (5) to move up and down by moving up and down on the supporting device.
7. The device according to claim 3, characterized in that the heating system (4) uses resistance wire heating or induction coil heating.
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