CN114574714A - Vertical vacuum spiral crystallization equipment and method for continuously separating binary eutectic alloy - Google Patents
Vertical vacuum spiral crystallization equipment and method for continuously separating binary eutectic alloy Download PDFInfo
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- CN114574714A CN114574714A CN202210206692.XA CN202210206692A CN114574714A CN 114574714 A CN114574714 A CN 114574714A CN 202210206692 A CN202210206692 A CN 202210206692A CN 114574714 A CN114574714 A CN 114574714A
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- 238000002425 crystallisation Methods 0.000 title claims abstract description 38
- 239000006023 eutectic alloy Substances 0.000 title claims abstract description 34
- 230000008025 crystallization Effects 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title abstract description 19
- 238000007599 discharging Methods 0.000 claims abstract description 97
- 238000010438 heat treatment Methods 0.000 claims abstract description 61
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000001816 cooling Methods 0.000 claims abstract description 24
- 238000002844 melting Methods 0.000 claims description 59
- 230000008018 melting Effects 0.000 claims description 58
- 239000013078 crystal Substances 0.000 claims description 54
- 239000000155 melt Substances 0.000 claims description 19
- 238000009413 insulation Methods 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 12
- 238000007789 sealing Methods 0.000 claims description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 239000011449 brick Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 229910001152 Bi alloy Inorganic materials 0.000 claims description 4
- YVIMHTIMVIIXBQ-UHFFFAOYSA-N [SnH3][Al] Chemical compound [SnH3][Al] YVIMHTIMVIIXBQ-UHFFFAOYSA-N 0.000 claims description 4
- 229910000838 Al alloy Inorganic materials 0.000 claims description 2
- JWVAUCBYEDDGAD-UHFFFAOYSA-N bismuth tin Chemical compound [Sn].[Bi] JWVAUCBYEDDGAD-UHFFFAOYSA-N 0.000 claims description 2
- 229910001174 tin-lead alloy Inorganic materials 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 13
- 239000002184 metal Substances 0.000 abstract description 13
- 229910002056 binary alloy Inorganic materials 0.000 abstract description 6
- 238000003723 Smelting Methods 0.000 abstract description 3
- 230000005496 eutectics Effects 0.000 abstract description 3
- -1 ferrous metals Chemical class 0.000 abstract description 2
- 101100298225 Caenorhabditis elegans pot-2 gene Proteins 0.000 description 20
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 13
- 238000005485 electric heating Methods 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052797 bismuth Inorganic materials 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052745 lead Inorganic materials 0.000 description 2
- LQBJWKCYZGMFEV-UHFFFAOYSA-N lead tin Chemical compound [Sn].[Pb] LQBJWKCYZGMFEV-UHFFFAOYSA-N 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 229910001128 Sn alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000009853 pyrometallurgy Methods 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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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
- C22B25/00—Obtaining tin
- C22B25/08—Refining
-
- 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
- C22B13/00—Obtaining lead
- C22B13/06—Refining
- C22B13/10—Separating metals from lead by crystallising, e.g. by Pattison process
-
- 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
- C22B21/00—Obtaining aluminium
- C22B21/06—Obtaining aluminium refining
- C22B21/068—Obtaining aluminium refining handling in vacuum
-
- 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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/06—Obtaining bismuth
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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
- C22B9/04—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
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Abstract
The invention relates to vertical vacuum spiral crystallization equipment and a method for continuously separating binary eutectic alloy, belonging to the technical field of pyrometallurgical smelting of non-ferrous metals. The vertical vacuum spiral crystallization equipment for continuously separating the binary eutectic alloy comprises a vertical furnace body, a feeding system, a heating system, a circulating water cooling system, a rotating system, a vacuum system, a discharging system and an observation system. The equipment and the method for treating the binary alloy containing any eutectic phase point have the advantages of convenient operation of the equipment, low strength, no three wastes generated in the treatment process, guarantee of the direct yield of the metal to the maximum extent, good operation environment and safe and controllable process.
Description
Technical Field
The invention relates to vertical vacuum spiral crystallization equipment and a method for continuously separating binary eutectic alloy, belonging to the technical field of pyrometallurgical smelting of non-ferrous metals.
Background
The crystallization separation method realizes impurity separation by utilizing the solubility difference of impurities in solid main metal and liquid main metal, belongs to metal-metal series heterogeneous separation, and has the advantages of energy conservation, low-temperature operation, capability of separating out high-purity products and the like. The electrothermal continuous crystallizer invented in 70 s of 20 th century in China according to a crystallization separation method is one of the most important devices in the tin smelting process, and mainly plays a role in removing lead in crude tin. However, the traditional electric heating continuous crystallizer has low automation degree, high water consumption and poor working environment for workers. For decades, the science and technology personnel in China continuously carry out the transformation work on the Chinese medical science and technology personnel. The patent with publication number CN 205662564U discloses an electric heating spiral crystallizer, which mainly provides an electric heating spiral crystallizer with reasonable temperature proportion of each heating section, high single machine productivity and low water consumption in the production process. The patent with publication number CN 206069975U discloses an electrothermal spiral crystallizer for treating crude tin, aiming at improving the pollution of diesel oil combustion to the environment and improving the comfort of the working environment of workers by adopting electrothermal heating in the solder placing process.
The processing objects of the spiral crystallizer are all crude tin materials, and the processing objects are single. At present, the spiral crystallizer is not applied in the field of pyrometallurgy of nonferrous metals, and a patent with the publication number of CN 111172394A discloses equipment and a method for separating, purifying and recovering aluminum-tin alloy by vacuum continuous crystallization.
Disclosure of Invention
Aiming at the problems and the defects in the prior art, the invention provides vertical vacuum spiral crystallization equipment and a method for continuously separating binary eutectic alloy. The equipment and the method for treating the binary alloy containing any eutectic phase point have the advantages of convenient operation of the equipment, low strength, no three wastes generated in the treatment process, guarantee of the direct yield of the metal to the maximum extent, good operation environment and safe and controllable process. The invention is realized by the following technical scheme.
A vertical vacuum spiral crystallization device for continuously separating binary eutectic alloy comprises a vertical furnace body, a feeding system, a heating system, a circulating water cooling system, a rotating system, a vacuum system, a discharging system and an observation system;
the feeding system comprises a melting pot 2, a feeding pipe 3 and a feeding switch 4, the rotating system comprises a rotating blade 9, a rotating shaft 10 and a motor 14, and the vacuum system comprises a vacuum pump 15 and a series of valves; the discharging system comprises a discharging pipe I11, a discharging switch I12, a baffle 17, a discharging pipe II 18, a discharging switch II 19, a melt pot 13 and a crystal pot 20;
the working temperature of a melting pot 2 in a feeding system is 300-1000 ℃, the inlet end of a feeding pipe 3 immersed in a raw material 1 melt is arranged in the melting pot 2, the outlet end of the feeding pipe 3 is communicated with the top of a vertical furnace body in a sealing way through a feeding switch 4, the top of the vertical furnace body is provided with a motor 14, the motor 14 is connected with a rotating shaft 10 which is inserted into an inner cylinder 8 of the vertical furnace body in a sealing way, a rotating blade 9 is arranged on the rotating shaft 10, the top of the vertical furnace body is provided with a vacuum pump 15 for vacuumizing the vertical furnace body to the vacuum degree of 1-100 Pa, a crystal melting zone (the length is 30-50 cm, the width is 15-100 cm) with the inclination angle of 3-7 degrees is arranged at the position 1-2 mm away from the inner side of the inner cylinder 8, baffles 17 which are distributed in a staggered way are arranged on the crystal melting zone, the outer wall of the inner cylinder 8 is provided with a heating system and a circulating water cooling system, and a heating system with the temperature zone of 350-800 ℃ is arranged at the bottom of the crystal melting zone, the crystal melting area is communicated with the discharging area, a discharging pipe II 18 and a discharging switch II 19 are arranged at the bottom of the discharging area, a crystal pot 20 is arranged at the bottom of the discharging pipe II 18, a heating system is arranged on the discharging area, a discharging pipe I11 is arranged at the bottom of the inner barrel 8, the discharging pipe I11 is communicated with a melt pot 13 at the bottom through a discharging switch I12, and an observation port 16 of an observation system is arranged at the top of the vertical furnace body.
The treatment capacity of the vertical vacuum spiral crystallization equipment is 100-500 kg/day.
The heating system comprises a heating body 5 and a heat insulation layer 6, wherein the heating body 5 is a resistance wire, and the heat insulation layer 6 is an alumina refractory brick.
The circulating water cooling system comprises a circulating water machine and a circulating water pipe 7.
The inner cylinder 8 sequentially forms a heating area with controllable temperature gradient gradually reduced through the heating system and the circulating water cooling system of each section from top to bottom, the top is a high-temperature section, the bottom is a low-temperature section, the temperature of the high-temperature section is 800 ℃ for minus one year, and the temperature of the low-temperature section is 650 ℃ for minus one year.
The rotating speed of the motor 14 is 0-50 revolutions per minute; the diameter of the inner cylinder 8 is 15-100 cm, and the height is 2-5 m; the distance between the outer edge of the rotating blade 9 and the inner cylinder 8 is 5-20 mm.
The power of the vacuum pump 15 is a direct-connected double-stage rotary vane vacuum pump, and the air pumping speed is 15-25L/s.
A vertical vacuum spiral crystallization method for continuously separating binary eutectic alloy comprises the following specific steps: the binary eutectic alloy raw material is continuously injected into the inner cylinder 8 from the melting pot 2 under the vacuum condition by siphoning, the inner cylinder 8 has temperature gradient, crystals are continuously separated out under the rotation of the motor 14, are transmitted to the top of the inner cylinder 8 and flow into a crystal melting area, the crystals are remelted through a baffle and are discharged through a discharge switch II, and meanwhile, the discharge switch I is periodically opened to discharge the melt.
The binary eutectic alloy raw material comprises a tin-lead alloy, a tin-bismuth alloy, a lead-bismuth alloy or a tin-aluminum alloy.
The invention has the beneficial effects that:
the equipment and the method for treating the binary eutectic alloy containing any eutectic phase point have the advantages of higher universality of raw materials, convenient equipment operation, low strength, no three wastes in the treatment process, capability of ensuring the direct yield of metal to the maximum extent, good operating environment and safe and controllable process.
Compared with the traditional crystallizer with the groove body obliquely and transversely arranged, the vertical crystallizer can further utilize gravity to accelerate the countercurrent of the melt, and is more favorable for improving the purity of the crystal. Meanwhile, a vacuum system is added in the equipment, so that the problem of metal oxidation is avoided, and the direct recovery rate of metal is improved; on the other hand, heat loss is reduced under a vacuum system, and energy efficiency is improved.
Drawings
FIG. 1 is a schematic diagram of the apparatus of the present invention;
FIG. 2 is a schematic view of the baffle distribution of the present invention.
In the figure: 1-raw material; 2-melting material pot; 3-feeding pipe; 4-a feed switch; 5-a heating element; 6-a heat insulation layer; 7-a circulating water pipe; 8-barrel liner; 9-rotating blades; 10-a rotating shaft; 11-a discharge pipe I; 12-a discharge switch I; 13-melt pan; 14-a motor; 15-a vacuum pump; 16-observation port; 17-a baffle; 18-discharge pipe II; 19-discharge switch ii; 20-crystal pan.
Detailed Description
The invention is further described with reference to the following drawings and detailed description.
Example 1
As shown in figures 1 and 2, the vertical vacuum spiral crystallization equipment for continuously separating binary eutectic alloys comprises a vertical furnace body, a feeding system, a heating system, a circulating water cooling system, a rotating system, a vacuum system, a discharging system and an observation system;
the feeding system comprises a melting pot 2, a feeding pipe 3 and a feeding switch 4, the rotating system comprises a rotating blade 9, a rotating shaft 10 and a motor 14, and the vacuum system comprises a vacuum pump 15 and a series of valves; the discharging system comprises a discharging pipe I11, a discharging switch I12, a baffle 17, a discharging pipe II 18, a discharging switch II 19, a melt pot 13 and a crystal pot 20;
the working temperature of a melting pot 2 in a feeding system is 300-1000 ℃, the inlet end of a feeding pipe 3 immersed in a raw material 1 melt is arranged in the melting pot 2, the outlet end of the feeding pipe 3 is communicated with the top of a vertical furnace body in a sealing way through a feeding switch 4, the top of the vertical furnace body is provided with a motor 14, the motor 14 is connected with a rotating shaft 10 which is inserted into an inner cylinder 8 of the vertical furnace body in a sealing way, a rotating blade 9 is arranged on the rotating shaft 10, the top of the vertical furnace body is provided with a vacuum pump 15 which vacuumizes the vertical furnace body to the vacuum degree of 1-100 Pa, a crystal melting zone (the length is 30cm, the width is 15 cm) with the inclination angle of 3 degrees is arranged at the position 1-2 mm away from the inner side of the inner cylinder 8, a baffle 17 which is distributed in a staggered way is arranged on the crystal melting zone, a heating system and a circulating water cooling system are arranged on the outer wall of the inner cylinder 8, and a heating system with the temperature zone of 350-800 ℃ is arranged at the bottom of the crystal melting zone, the crystal melting area is communicated with the discharging area, a discharging pipe II 18 and a discharging switch II 19 are arranged at the bottom of the discharging area, a crystal pot 20 is arranged at the bottom of the discharging pipe II 18, a heating system is arranged on the discharging area, a discharging pipe I11 is arranged at the bottom of the inner barrel 8, the discharging pipe I11 is communicated with a melt pot 13 at the bottom through a discharging switch I12, and an observation port 16 of an observation system is arranged at the top of the vertical furnace body.
Wherein the treatment capacity of the vertical vacuum spiral crystallization equipment is 100-500 kg/day; the heating system comprises a heating body 5 and a heat insulation layer 6, wherein the heating body 5 is a resistance wire, and the heat insulation layer 6 is an alumina refractory brick; the circulating water cooling system comprises a circulating water machine and a circulating water pipe 7; the inner cylinder 8 sequentially forms heating areas with controllable temperature gradient gradually reduced through the heating system and the circulating water cooling system of each section from top to bottom, the top is a high-temperature section, the bottom is a low-temperature section, the temperature of the high-temperature section is 800 ℃ plus one year, and the temperature of the low-temperature section is 650 ℃ plus one year;
the rotating speed of the motor 14 is 0-50 revolutions per minute; the diameter of the inner cylinder 8 is 15cm, and the height is 2 m; the distance between the outer edge of the rotating blade 9 and the inner cylinder 8 is 5 mm.
The power of the vacuum pump 15 is a direct-connected double-stage rotary vane vacuum pump, and the air pumping speed is 15-25L/s.
The vertical vacuum spiral crystallization method for continuously separating the binary eutectic alloy comprises the following specific steps:
(1) melting 100 kg of tin-lead binary alloy (components: Sn90% and Pb 10%) in a melting pot 2 with the working temperature of 500 ℃, closing a feeding switch 4, a discharging switch I12 and a discharging switch II 19, starting a vacuum pump 15 to ensure that the pressure in a vertical furnace body is lower than 100Pa, setting the top temperature of an inner cylinder 8 to be 232 ℃ and the lower temperature to be 183 ℃, and starting a heating system;
(2) after the temperature gradient of the vertical furnace body is stable, opening a feed pipe switch 4, and simultaneously starting a motor 14 to operate at the speed of 3 revolutions per minute;
(3) checking the crystal condition through the observation port 16, setting the temperature of the crystal melting zone at 350 ℃, opening the discharging switch irregularly, discharging the melt and the crystal, and finally obtaining the soldering tin containing 38.4 percent of lead and the refined tin product containing 99.6 percent of tin.
Compared with the traditional electric heating crystallizer, the vertical vacuum spiral crystallization equipment for continuously separating the binary eutectic alloy improves the direct recovery rate of the metallic tin by 5 percent and improves the energy efficiency by 8 percent.
Example 2
As shown in fig. 1 and 2, the vertical vacuum spiral crystallization device for continuously separating binary eutectic alloy comprises a vertical furnace body, a feeding system, a heating system, a circulating water cooling system, a rotating system, a vacuum system, a discharging system and an observation system;
the feeding system comprises a melting pot 2, a feeding pipe 3 and a feeding switch 4, the rotating system comprises a rotating blade 9, a rotating shaft 10 and a motor 14, and the vacuum system comprises a vacuum pump 15 and a series of valves; the discharging system comprises a discharging pipe I11, a discharging switch I12, a baffle 17, a discharging pipe II 18, a discharging switch II 19, a melt pot 13 and a crystal pot 20;
the working temperature of a melting pot 2 in a feeding system is 300-1000 ℃, the inlet end of a feeding pipe 3 immersed in a raw material 1 melt is arranged in the melting pot 2, the outlet end of the feeding pipe 3 is communicated with the top of a vertical furnace body in a sealing way through a feeding switch 4, the top of the vertical furnace body is provided with a motor 14, the motor 14 is connected with a rotating shaft 10 which is inserted into an inner cylinder 8 of the vertical furnace body in a sealing way, a rotating blade 9 is arranged on the rotating shaft 10, the top of the vertical furnace body is provided with a vacuum pump 15 which vacuumizes the vertical furnace body to the vacuum degree of 1-100 Pa, a crystal melting zone (the length is 50cm, the width is 100 cm) with the inclination angle of 7 degrees is arranged at the position 1-2 mm away from the inner side of the inner cylinder 8, baffles 17 which are distributed in a staggered way are arranged on the crystal melting zone, a heating system and a circulating water cooling system are arranged on the outer wall of the inner cylinder 8, and a heating system with the temperature of 350-800 ℃ is arranged at the bottom of the crystal melting zone, the crystal melting area is communicated with the discharging area, a discharging pipe II 18 and a discharging switch II 19 are arranged at the bottom of the discharging area, a crystal pot 20 is arranged at the bottom of the discharging pipe II 18, a heating system is arranged on the discharging area, a discharging pipe I11 is arranged at the bottom of the inner barrel 8, the discharging pipe I11 is communicated with a melt pot 13 at the bottom through a discharging switch I12, and an observation port 16 of an observation system is arranged at the top of the vertical furnace body.
Wherein the treatment capacity of the vertical vacuum spiral crystallization equipment is 100-500 kg/day; the heating system comprises a heating body 5 and a heat insulation layer 6, wherein the heating body 5 is a resistance wire, and the heat insulation layer 6 is an alumina refractory brick; the circulating water cooling system comprises a circulating water machine and a circulating water pipe 7; the inner cylinder 8 sequentially forms heating areas with controllable temperature gradient gradually reduced through the heating system and the circulating water cooling system of each section from top to bottom, the top is a high-temperature section, the bottom is a low-temperature section, the temperature of the high-temperature section is 800 ℃ plus one year, and the temperature of the low-temperature section is 650 ℃ plus one year;
the rotating speed of the motor 14 is 0-50 revolutions per minute; the diameter of the inner cylinder 8 is 100cm, and the height is 5 m; the distance between the outer edge of the rotating blade 9 and the inner cylinder 8 is 20 mm.
The power of the vacuum pump 15 is a direct-connected two-stage rotary vane vacuum pump, and the air extraction speed is 15-25L/s.
The vertical vacuum spiral crystallization method for continuously separating the binary eutectic alloy comprises the following specific steps:
(1) melting 500 kg of tin-lead binary alloy (components: Sn95% and Pb 5%) in a melting pot 2 with the working temperature of 300 ℃, closing a feeding switch 4, a discharging switch I12 and a discharging switch II 19, starting a vacuum pump 15 to ensure that the pressure in a vertical furnace body is lower than 100Pa, setting the top temperature of an inner cylinder 8 to 232 ℃, the lower temperature to 183 ℃, and starting a heating system;
(2) after the temperature gradient of the vertical furnace body is stable, opening a feed pipe switch 4, and simultaneously starting a motor 14 to operate at the speed of 2 revolutions per minute;
(3) checking the crystal condition through an observation port 16, setting the temperature of a crystal melting zone at 350 ℃, opening a discharging switch irregularly, discharging the melt and the crystal, and finally obtaining the solder containing 37.8 percent of lead and the refined tin product containing 99.9 percent of tin.
Compared with the traditional electric heating crystallizer, the vertical vacuum spiral crystallization equipment for continuously separating the binary eutectic alloy in the embodiment has the advantages that the direct yield of the metallic tin is improved by 4 percent, and the energy efficiency is improved by 15 percent.
Example 3
As shown in fig. 1 and 2, the vertical vacuum spiral crystallization device for continuously separating binary eutectic alloy comprises a vertical furnace body, a feeding system, a heating system, a circulating water cooling system, a rotating system, a vacuum system, a discharging system and an observation system;
the feeding system comprises a melting pot 2, a feeding pipe 3 and a feeding switch 4, the rotating system comprises a rotating blade 9, a rotating shaft 10 and a motor 14, and the vacuum system comprises a vacuum pump 15 and a series of valves; the discharging system comprises a discharging pipe I11, a discharging switch I12, a baffle 17, a discharging pipe II 18, a discharging switch II 19, a melt pot 13 and a crystal pot 20;
in the feeding system, the working temperature of a melting pot 2 is 300-1000 ℃, an inlet end of a feeding pipe 3 immersed in a melt of a raw material 1 is arranged in the melting pot 2, an outlet end of the feeding pipe 3 is communicated with the top of a vertical furnace body in a sealing way through a feeding switch 4, a motor 14 is arranged at the top of the vertical furnace body, the motor 14 is connected with a rotating shaft 10 which is inserted into an inner cylinder 8 of the vertical furnace body in a sealing way, a rotating blade 9 is arranged on the rotating shaft 10, a vacuum pump 15 which vacuumizes the vertical furnace body to the vacuum degree of 1-100 Pa is arranged at the top of the vertical furnace body, a crystal melting zone (40 cm long and 80cm wide) with the inclination angle of 6 degrees is arranged at the position of 1-2 mm away from the inner side of the inner cylinder 8 at the top of the vertical furnace body, baffles 17 which are distributed and arranged are arranged on the crystal melting zone, a heating system and a circulating water cooling system are arranged on the outer wall of the inner cylinder 8, a heating system with the temperature zone of 350-800 ℃ is arranged at the bottom of the crystal melting zone, the crystal melting area is communicated with the discharging area, a discharging pipe II 18 and a discharging switch II 19 are arranged at the bottom of the discharging area, a crystal pot 20 is arranged at the bottom of the discharging pipe II 18, a heating system is arranged on the discharging area, a discharging pipe I11 is arranged at the bottom of the inner barrel 8, the discharging pipe I11 is communicated with a melt pot 13 at the bottom through a discharging switch I12, and an observation port 16 of an observation system is arranged at the top of the vertical furnace body.
Wherein the treatment capacity of the vertical vacuum spiral crystallization equipment is 100-500 kg/day; the heating system comprises a heating body 5 and a heat insulation layer 6, wherein the heating body 5 is a resistance wire, and the heat insulation layer 6 is an alumina refractory brick; the circulating water cooling system comprises a circulating water machine and a circulating water pipe 7; the inner cylinder 8 sequentially forms heating areas with controllable temperature gradient gradually reduced through the heating system and the circulating water cooling system of each section from top to bottom, the top is a high-temperature section, the bottom is a low-temperature section, the temperature of the high-temperature section is 800 ℃ plus one year, and the temperature of the low-temperature section is 650 ℃ plus one year;
the rotating speed of the motor 14 is 0-50 revolutions per minute; the diameter of the inner cylinder 8 is 80cm, and the height is 4 m; the outer edge of the rotating blade 9 is spaced from the inner cylinder 8 by 15 mm.
The power of the vacuum pump 15 is a direct-connected double-stage rotary vane vacuum pump, and the air pumping speed is 15-25L/s.
The vertical vacuum spiral crystallization method for continuously separating the binary eutectic alloy comprises the following specific steps:
(1) melting 500 kg of tin-aluminum binary alloy (components: Sn20% and Al 80%) in a melting pot 2 with the working temperature of 1000 ℃, closing a feeding switch 4, a discharging switch I12 and a discharging switch II 19, starting a vacuum pump 15 to ensure that the pressure in a vertical furnace body is lower than 100Pa, setting the top temperature of an inner cylinder 8 to 232 ℃, the lower temperature to 183 ℃, and starting a heating system;
(2) after the temperature gradient of the vertical furnace body is stable, opening a feed pipe switch 4, and simultaneously starting a motor 14 to operate at the speed of 2 revolutions per minute;
(3) checking the crystal condition through an observation port 16, setting the temperature of a crystal melting zone at 800 ℃, opening a discharging switch irregularly, discharging the melt and the crystal, and finally obtaining crude tin containing 85% of tin and crude aluminum containing 99% of aluminum.
Compared with an electrolytic method, the vertical vacuum spiral crystallization device for continuously separating the binary eutectic alloy in the embodiment has the advantages that the direct recovery rate of metal aluminum is respectively improved by 21%, and the energy efficiency is improved by 27%.
Example 4
As shown in fig. 1 and 2, the vertical vacuum spiral crystallization device for continuously separating binary eutectic alloy comprises a vertical furnace body, a feeding system, a heating system, a circulating water cooling system, a rotating system, a vacuum system, a discharging system and an observation system;
the feeding system comprises a melting pot 2, a feeding pipe 3 and a feeding switch 4, the rotating system comprises a rotating blade 9, a rotating shaft 10 and a motor 14, and the vacuum system comprises a vacuum pump 15 and a series of valves; the discharging system comprises a discharging pipe I11, a discharging switch I12, a baffle 17, a discharging pipe II 18, a discharging switch II 19, a melt pot 13 and a crystal pot 20;
the working temperature of a melting pot 2 in a feeding system is 300-1000 ℃, the inlet end of a feeding pipe 3 immersed in a raw material 1 melt is arranged in the melting pot 2, the outlet end of the feeding pipe 3 is communicated with the top of a vertical furnace body in a sealing way through a feeding switch 4, the top of the vertical furnace body is provided with a motor 14, the motor 14 is connected with a rotating shaft 10 which is inserted into an inner cylinder 8 of the vertical furnace body in a sealing way, a rotating blade 9 is arranged on the rotating shaft 10, the top of the vertical furnace body is provided with a vacuum pump 15 which vacuumizes the vertical furnace body to the vacuum degree of 1-100 Pa, a crystal melting zone with the inclination angle of 6 degrees (the length is 45cm and the width is 85 cm) is arranged at the position 1-2 mm away from the inner side of the inner cylinder 8 at the top of the vertical furnace body, a baffle 17 which is distributed in a staggered way is arranged on the crystal melting zone, a heating system and a circulating water cooling system are arranged on the outer wall of the inner cylinder 8, a heating system with the temperature zone of 350-800 ℃ is arranged at the bottom of the crystal melting zone, the crystal melting area is communicated with the discharging area, a discharging pipe II 18 and a discharging switch II 19 are arranged at the bottom of the discharging area, a crystal pot 20 is arranged at the bottom of the discharging pipe II 18, a heating system is arranged on the discharging area, a discharging pipe I11 is arranged at the bottom of the inner barrel 8, the discharging pipe I11 is communicated with a melt pot 13 at the bottom through a discharging switch I12, and an observation port 16 of an observation system is arranged at the top of the vertical furnace body.
Wherein the treatment capacity of the vertical vacuum spiral crystallization equipment is 100-500 kg/day; the heating system comprises a heating body 5 and a heat insulation layer 6, wherein the heating body 5 is a resistance wire, and the heat insulation layer 6 is an alumina refractory brick; the circulating water cooling system comprises a circulating water machine and a circulating water pipe 7; the inner cylinder 8 sequentially forms heating areas with controllable temperature gradient gradually reduced through the heating system and the circulating water cooling system of each section from top to bottom, the top is a high-temperature section, the bottom is a low-temperature section, the temperature of the high-temperature section is 800 ℃ plus one year, and the temperature of the low-temperature section is 650 ℃ plus one year;
the rotating speed of the motor 14 is 0-50 revolutions per minute; the diameter of the inner cylinder 8 is 65cm, and the height is 4 m; the distance between the outer edge of the rotating blade 9 and the inner cylinder 8 is 18 mm.
The power of the vacuum pump 15 is a direct-connected two-stage rotary vane vacuum pump, and the air extraction speed is 15-25L/s.
The vertical vacuum spiral crystallization method for continuously separating the binary eutectic alloy comprises the following specific steps:
(1) melting 200 kg of lead-bismuth binary alloy (the components are Pb62.5 percent and Bi37.5 percent) in a melting pot 2 with the working temperature of 400 ℃, closing a feeding switch 4, a discharging switch I12 and a discharging switch II 19, starting a vacuum pump 15 to ensure that the pressure in a vertical furnace body is lower than 100Pa, setting the top temperature of an inner cylinder 8 to be 232 ℃ and the lower temperature to be 183 ℃, and starting a heating system;
(2) after the temperature gradient of the vertical furnace body is stable, opening a feed pipe switch 4, and simultaneously starting a motor 14 to operate at the speed of 2 revolutions per minute;
(3) checking the crystal condition through an observation port 16, setting the temperature of a crystal melting zone at 400 ℃, and opening a discharging switch irregularly to discharge the melt and the crystal to finally obtain crude bismuth containing 77% of bismuth and crude lead containing 98.7% of lead.
Compared with an electrolytic method, the vertical vacuum spiral crystallization device for continuously separating the binary eutectic alloy in the embodiment has the advantages that the vertical metal yield is improved by 18%, and the energy efficiency is improved by 22%.
While the present invention has been described in detail with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, and various changes can be made without departing from the spirit and scope of the present invention.
Claims (9)
1. A vertical vacuum spiral crystallization device for continuously separating binary eutectic alloy is characterized in that: comprises a vertical furnace body, a feeding system, a heating system, a circulating water cooling system, a rotating system, a vacuum system, a discharging system and an observation system;
the feeding system comprises a melting pot (2), a feeding pipe (3) and a feeding switch (4), the rotating system comprises a rotating blade (9), a rotating shaft (10) and a motor (14), and the vacuum system comprises a vacuum pump (15) and a series of valves; the discharging system comprises a discharging pipe I (11), a discharging switch I (12), a baffle plate (17), a discharging pipe II (18), a discharging switch II (19), a melt pot (13) and a crystal pot (20);
the working temperature of a melting material pot (2) in the feeding system is 300-1000 ℃, the inlet end of a feeding pipe (3) immersed in a raw material (1) melt is arranged in the melting material pot (2), the outlet end of the feeding pipe (3) is communicated with the top of a vertical furnace body in a sealing way through a feeding switch (4), a motor (14) is arranged at the top of the vertical furnace body, the motor (14) is connected with a rotating shaft (10) which is inserted into an inner cylinder (8) of the vertical furnace body in a sealing way, a rotating blade (9) is arranged on the rotating shaft (10), a vacuum pump (15) for vacuumizing the vertical furnace body to the vacuum degree of 1-100 Pa is arranged at the top of the vertical furnace body, a crystal melting area with the inclination angle of 3-7 degrees is arranged at a position 1-2 mm away from the top of the vertical furnace body and the inner side of the inner cylinder (8), the length of the crystal melting area is 30-50 cm and the width is 15-100 cm, a baffle plate (17) which is arranged in a staggered way is arranged on the crystal melting area, and a heating system and a circulating system are arranged on the outer wall of the inner cylinder (8), the bottom of the crystal melting zone is provided with a heating system with a temperature zone of 350-.
2. The vertical vacuum spiral crystallization apparatus for continuously separating a binary eutectic alloy according to claim 1, wherein: the treatment capacity of the vertical vacuum spiral crystallization equipment is 100-500 kg/day.
3. The vertical vacuum spiral crystallization apparatus for continuously separating a binary eutectic alloy according to claim 1, wherein: the heating system comprises a heating body (5) and a heat insulation layer (6), wherein the heating body (5) is a resistance wire, and the heat insulation layer (6) is an alumina refractory brick.
4. The vertical vacuum spiral crystallization apparatus for continuously separating a binary eutectic alloy according to claim 1, wherein: the circulating water cooling system comprises a circulating water machine and a circulating water pipe (7).
5. The vertical vacuum spiral crystallization apparatus for continuously separating a binary eutectic alloy according to claim 1, wherein: the inner cylinder (8) sequentially forms a heating area with controllable temperature gradient gradually reduced through the heating system and the circulating water cooling system of each section from top to bottom, the top is a high-temperature section, the bottom is a low-temperature section, the temperature of the high-temperature section is 800 ℃ plus materials, and the temperature of the low-temperature section is 650 ℃ plus materials.
6. The vertical vacuum spiral crystallization apparatus for continuously separating a binary eutectic alloy according to claim 1, wherein: the rotating speed of the motor (14) is 0-50 revolutions per minute; the diameter of the inner cylinder (8) is 15-100 cm, and the height is 2-5 m; the distance between the outer edge of the rotating blade (9) and the inner cylinder (8) is 5-20 mm.
7. The vertical vacuum spiral crystallization apparatus for continuously separating a binary eutectic alloy according to claim 1, wherein: the vacuum pump (15) is a direct-connected two-stage rotary vane vacuum pump, and the air suction speed is 15-25L/s.
8. A vertical vacuum spiral crystallization method for continuously separating binary eutectic alloy is characterized by comprising the following specific steps: the binary eutectic alloy raw material is continuously injected into the inner cylinder (8) from the melting pot (2) by siphoning under the vacuum condition, the inner cylinder (8) has temperature gradient, crystals are continuously separated out under the rotation of the motor (14), are transmitted to the top of the inner cylinder (8), flow into the crystal melting area, are remelted through the baffle, are discharged through the discharge switch II, and simultaneously, the discharge switch I is periodically opened to discharge the melt.
9. The vertical vacuum spiral crystallization method for continuously separating binary eutectic alloys according to claim 8, wherein: the binary eutectic alloy raw material comprises a tin-lead alloy, a tin-bismuth alloy, a lead-bismuth alloy or a tin-aluminum alloy.
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| CN202210206692.XA CN114574714B (en) | 2022-03-04 | 2022-03-04 | Vertical vacuum spiral crystallization equipment and method for continuously separating binary eutectic alloy |
| PCT/CN2023/079160 WO2023165540A1 (en) | 2022-03-04 | 2023-03-02 | Vertical vacuum spiral crystallization apparatus and method for continuously separating binary eutectic alloy |
| JP2023534072A JP2024512853A (en) | 2022-03-04 | 2023-03-02 | Vertical vacuum spiral crystallization device and method for continuous separation of binary eutectic alloys |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN203609918U (en) * | 2013-12-03 | 2014-05-28 | 姜向前 | Vertical continuous cooling crystallizer |
| US20180044761A1 (en) * | 2015-03-10 | 2018-02-15 | Honeywell International Inc. | Method of purifying and casting materials |
| CN111172394A (en) * | 2019-09-02 | 2020-05-19 | 昆明理工大学 | Equipment and method for separating, purifying and recovering aluminum-tin alloy through vacuum continuous crystallization |
| CN212881137U (en) * | 2020-07-20 | 2021-04-06 | 烟台盛华液晶材料有限公司 | Vertical wall-scraping type continuous crystallization device |
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| DE3317537A1 (en) * | 1983-05-11 | 1984-11-15 | Schering AG, 1000 Berlin und 4709 Bergkamen | CRYSTALIZATION SEPARATOR AND METHOD FOR SEPARATING MIXTURES |
| CN85107356A (en) * | 1985-09-26 | 1986-09-03 | 云南锡业公司 | The method of tin refinement deleading, bismuth and device |
| KR100722416B1 (en) * | 2005-11-08 | 2007-05-29 | 이군희 | Crystallizer of tin and tin alloys and method thereof |
| CN113318479A (en) * | 2021-06-04 | 2021-08-31 | 北京化工大学 | Continuous multi-stage countercurrent separation and purification device |
| CN114574714B (en) * | 2022-03-04 | 2023-05-23 | 昆明理工大学 | Vertical vacuum spiral crystallization equipment and method for continuously separating binary eutectic alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN203609918U (en) * | 2013-12-03 | 2014-05-28 | 姜向前 | Vertical continuous cooling crystallizer |
| US20180044761A1 (en) * | 2015-03-10 | 2018-02-15 | Honeywell International Inc. | Method of purifying and casting materials |
| CN111172394A (en) * | 2019-09-02 | 2020-05-19 | 昆明理工大学 | Equipment and method for separating, purifying and recovering aluminum-tin alloy through vacuum continuous crystallization |
| CN212881137U (en) * | 2020-07-20 | 2021-04-06 | 烟台盛华液晶材料有限公司 | Vertical wall-scraping type continuous crystallization device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2023165540A1 (en) * | 2022-03-04 | 2023-09-07 | 昆明理工大学 | Vertical vacuum spiral crystallization apparatus and method for continuously separating binary eutectic alloy |
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