WO2023165540A1 - 一种连续分离二元共晶合金的竖式真空螺旋结晶设备及方法 - Google Patents

一种连续分离二元共晶合金的竖式真空螺旋结晶设备及方法 Download PDF

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WO2023165540A1
WO2023165540A1 PCT/CN2023/079160 CN2023079160W WO2023165540A1 WO 2023165540 A1 WO2023165540 A1 WO 2023165540A1 CN 2023079160 W CN2023079160 W CN 2023079160W WO 2023165540 A1 WO2023165540 A1 WO 2023165540A1
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vertical
furnace body
vacuum
discharge
inner cylinder
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PCT/CN2023/079160
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English (en)
French (fr)
Inventor
李一夫
张环
杨连峰
周生安
杨斌
陈秀敏
刘大春
徐宝强
田阳
蒋文龙
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昆明理工大学
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Priority to JP2023534072A priority Critical patent/JP2024512853A/ja
Publication of WO2023165540A1 publication Critical patent/WO2023165540A1/zh

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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
    • 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
    • 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
    • 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

Definitions

  • the invention relates to a vertical vacuum spiral crystallization device and method for continuously separating binary eutectic alloys, belonging to the technical field of nonferrous metal pyrometallurgy.
  • the crystallization separation method uses the difference in the solubility of impurities in the solid main metal and the liquid main metal to realize the separation of impurities. It belongs to metal-metal heterogeneous phase separation, and has the advantages of energy saving, low-temperature operation, and high-purity products can be separated.
  • the electrothermal continuous crystallizer invented in the 1970s in my country based on the crystallization separation method is one of the most important equipment in the tin smelting process, and its main function is to remove lead from crude tin.
  • the traditional electrothermal continuous crystallizer has low degree of automation, high water consumption, and poor working environment for workers. For decades, Chinese scientists and technicians have continued to transform it.
  • an electric heating spiral crystallizer device which mainly provides an electric heating spiral crystallizer with reasonable temperature ratio of each heating section, high stand-alone production capacity, and low water consumption in the production process.
  • an electrothermal spiral crystallizer for processing crude tin is disclosed. The purpose is to improve the use of electrothermal heating in the soldering process to reduce the environmental pollution caused by diesel combustion and improve the comfort of workers' working environment.
  • the present invention provides a vertical vacuum spiral crystallization device and method for continuous separation of binary eutectic alloys.
  • the processing object of this equipment and method is binary alloys containing any composition of eutectic phase point.
  • the equipment is easy to operate, low in strength, and no "three wastes" are produced in the processing process, which guarantees the direct recovery rate of metals to the greatest extent.
  • the working environment is good and the process is safe. controllable.
  • the present invention is realized through the following technical solutions.
  • a vertical vacuum spiral crystallization device for continuous separation of binary eutectic alloys including 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 includes a melting pot 2, a feeding pipe 3 and a feeding switch 4, the rotating system includes a rotating blade 9, a rotating shaft 10 and a motor 14, the vacuum system includes a vacuum pump 15 and a series of valves; the discharging system includes a discharging Pipe I11, discharge switch I12, baffle 17, discharge pipe II18, discharge Switch II 19, melt pot 13 and crystal pot 20;
  • the working temperature of the melting pot 2 is 300-1000°C.
  • the inside of the melting pot 2 is provided with the inlet end of the feeding pipe 3 immersed in the melt of the raw material 1, and the outlet end of the feeding pipe 3 passes through the feeding switch 4 and the vertical
  • the top of the vertical furnace body is sealed and connected, and the top of the vertical furnace body is provided with a motor 14.
  • the motor 14 is connected with the rotating shaft 10 sealed and inserted into the cylinder 8 of the vertical furnace body.
  • the rotating blade 9 is arranged on the rotating shaft 10. Vacuum the vertical furnace body to a vacuum pump 15 with a vacuum degree of 1 to 100 Pa.
  • a crystal melting zone with an inclination angle of 3° to 7° (long as 30 to 50 cm, and a width of 15 to 100 cm), the crystal melting zone is provided with baffles 17 arranged in dislocation distribution, the outer wall of the inner cylinder 8 is provided with a heating system and a circulating water cooling system, and the bottom of the crystal melting zone is provided with a temperature zone of 350 -800°C heating system, the crystal melting zone is connected to the discharge zone, the bottom of the discharge zone is equipped with a discharge pipe II18 and a discharge switch II19, the bottom of the discharge pipe II18 is equipped with a crystal pot 20, and the discharge area is equipped with a heating system, the bottom of the inner cylinder 8 is provided with a discharge pipe I11, and the discharge pipe I11 communicates with the melt pot 13 at the bottom through the discharge switch I12, and the top of the vertical furnace body is provided with an observation port 16 of the observation system.
  • the processing capacity of the vertical vacuum spiral crystallization equipment is 100-500 kg/day.
  • the heating system includes a heating element 5 and a heat insulating layer 6, the heating element 5 is a resistance wire, and the heat insulating layer 6 is an alumina refractory brick.
  • the circulating water cooling system includes a circulating water machine and a circulating water pipe 7 .
  • the inner cylinder 8 passes through the heating system of each section and the circulating water cooling system from top to bottom to form a heating area with a controllable temperature gradient that gradually decreases.
  • the top is a high temperature section
  • the bottom is a low temperature section.
  • the temperature of the high temperature section is 200-800°C
  • the temperature of the low temperature section is 100-650°C.
  • the rotation speed of the motor 14 is 0-50 rpm; the diameter of the inner tube 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 tube 8 is 5-20 mm.
  • the power of the vacuum pump 15 is a direct-coupled two-stage rotary vane vacuum pump, and the pumping rate is 15-25 L/s.
  • a vertical vacuum spiral crystallization method for continuous separation of binary eutectic alloys the specific steps of which include: continuously injecting binary eutectic alloy raw materials from a melting pot 2 into an inner cylinder 8 by using a siphon under vacuum conditions, and the inner cylinder 8 exists Temperature gradient, under the rotation of the motor 14, the crystals are continuously precipitated and driven to the top of the inner cylinder 8, and flow into the crystal melting zone, where the crystals are melted again through the baffle, and then released through the discharge switch II, and the discharge switch I is regularly opened Drain the melt.
  • the binary eutectic alloy raw material includes tin-lead alloy, tin-bismuth alloy, lead-bismuth alloy or tin-aluminum alloy gold.
  • the object of this equipment and method is binary eutectic alloy containing any composition of eutectic phase point.
  • the universality of raw materials is high, the equipment is easy to operate, low in strength, and there is no "three wastes" in the treatment process, which guarantees the maximum protection of the metal. Direct recovery rate, good working environment, safe and controllable process.
  • the vertical type of this equipment can further use gravity to accelerate the counterflow of the melt, which is more conducive to improving the purity of the crystal.
  • this equipment adds a vacuum system, which avoids the problem of metal oxidation on the one hand and improves the direct recovery rate of metals; on the other hand, the heat loss is reduced under the vacuum system and energy efficiency is improved.
  • Fig. 1 is a schematic diagram of the device structure of the present invention
  • Fig. 2 is a schematic diagram of the distribution of baffles in the present invention.
  • the vertical vacuum spiral crystallization equipment for continuous separation of binary eutectic alloys includes a vertical furnace body, a feeding system, a heating system, a circulating water cooling system, a rotating system, a vacuum system, and a discharge systems and observation systems;
  • the feeding system includes melting pot 2, feeding pipe 3 and feeding switch 4, the rotating system includes rotating blade 9, rotating shaft 10 and motor 14, the vacuum system includes vacuum pump 15 and a series of valves; the discharging system includes discharging pipe I11 , discharge switch I12, baffle plate 17, discharge pipe II18, discharge switch II19, melt pot 13 and crystal pot 20;
  • the working temperature of the melting pot 2 is 300-1000°C.
  • the inside of the melting pot 2 is provided with the inlet end of the feeding pipe 3 immersed in the melt of the raw material 1, and the outlet end of the feeding pipe 3 passes through the feeding switch 4 and the vertical
  • the top of the vertical furnace body is sealed and connected, and the top of the vertical furnace body is provided with a motor 14.
  • the motor 14 is connected with the rotating shaft 10 sealed and inserted into the cylinder 8 of the vertical furnace body.
  • the rotating blade 9 is arranged on the rotating shaft 10.
  • the baffle plate 17 of dislocation distribution is arranged on the crystal melting zone
  • the heating system and the circulating water cooling system are arranged on the outer wall of the inner cylinder 8
  • the bottom of the body melting zone is provided with a temperature range of 350-800 °C.
  • the crystal melting area communicates with the discharge area
  • the bottom of the discharge area is provided with a discharge pipe II18 and a discharge switch II19
  • the bottom of the discharge pipe II18 is provided with a crystal pot 20
  • a heating system is provided on the discharge area
  • the inner cylinder 8 There is a discharge pipe I11 at the bottom, and the discharge pipe I11 communicates with the melt pot 13 at the bottom through the discharge switch I12, and the observation port 16 of the observation system is provided on the top of the vertical furnace body.
  • the processing capacity of vertical vacuum spiral crystallization equipment is 100-500 kg/day;
  • the heating system includes heating element 5 and heat insulation layer 6, heating element 5 is resistance wire, and heat insulation layer 6 is alumina refractory brick;
  • circulating water cooling system Including the circulating water machine and the circulating water pipe 7;
  • the inner cylinder 8 passes through the heating system and the circulating water cooling system of each section from top to bottom to form a heating area with a controllable temperature gradient gradually decreasing.
  • the top is a high temperature section
  • the bottom is a low temperature section, and the high temperature
  • the temperature of the section is 200-800°C, and the temperature of the low temperature section is 100-650°C;
  • the rotating speed of the motor 14 is 0-50 rpm; the inner cylinder 8 has a diameter of 15 cm and a height of 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-coupled two-stage rotary vane vacuum pump, and the pumping rate is 15-25 L/s.
  • the vertical vacuum spiral crystallization method for continuously separating binary eutectic alloys the specific steps include:
  • the vertical vacuum spiral crystallization equipment for continuous separation of binary eutectic alloys is used.
  • the direct recovery rate of metal tin is increased by 5%, and the energy efficiency is increased by 8%.
  • the vertical vacuum spiral crystallization equipment for continuous separation of binary eutectic alloys includes a vertical furnace body, a feeding system, a heating system, a circulating water cooling system, a rotating system, a vacuum system, and a discharge systems and observation systems;
  • the feeding system includes melting pot 2, feeding pipe 3 and feeding switch 4, the rotating system includes rotating blade 9, rotating shaft 10 and motor 14, the vacuum system includes vacuum pump 15 and a series of valves; the discharging system includes discharging pipe I11 , discharge switch I12, baffle plate 17, discharge pipe II18, discharge switch II19, melt pot 13 and crystal pot 20;
  • the working temperature of the melting pot 2 is 300-1000°C.
  • the inside of the melting pot 2 is provided with the inlet end of the feeding pipe 3 immersed in the melt of the raw material 1, and the outlet end of the feeding pipe 3 passes through the feeding switch 4 and the vertical
  • the top of the vertical furnace body is sealed and connected, and the top of the vertical furnace body is provided with a motor 14.
  • the motor 14 is connected with the rotating shaft 10 sealed and inserted into the cylinder 8 of the vertical furnace body.
  • the rotating blade 9 is arranged on the rotating shaft 10.
  • the vertical furnace body is evacuated to a vacuum pump 15 with a vacuum degree of 1 to 100 Pa.
  • the top of the vertical furnace body and the inside of the inner cylinder 8 are 1 to 2 mm apart from a crystal melting zone (50 cm long and 50 cm wide) with an inclination angle of 7°. 100cm), the crystal melting zone is provided with baffles 17 arranged in dislocation distribution, the outer wall of the inner cylinder 8 is provided with a heating system and a circulating water cooling system, and the bottom of the crystal melting zone is provided with a heating system with a temperature range of 350-800°C.
  • the crystal melting zone communicates with the discharge zone, the bottom of the discharge zone is provided with a discharge pipe II18 and a discharge switch II19, the bottom of the discharge pipe II18 is provided with a crystal pot 20, the discharge area is provided with a heating system, and the bottom of the inner cylinder 8 is provided with There is a discharge pipe I11, and the discharge pipe I11 communicates with the melt pot 13 at the bottom through the discharge switch I12, and the top of the vertical furnace body is provided with an observation port 16 of the observation system.
  • the processing capacity of vertical vacuum spiral crystallization equipment is 100-500 kg/day;
  • the heating system includes heating element 5 and heat insulation layer 6, heating element 5 is resistance wire, and heat insulation layer 6 is alumina refractory brick;
  • circulating water cooling system Including the circulating water machine and the circulating water pipe 7;
  • the inner cylinder 8 passes through the heating system and the circulating water cooling system of each section from top to bottom to form a heating area with a controllable temperature gradient gradually decreasing.
  • the top is a high temperature section
  • the bottom is a low temperature section, and the high temperature
  • the temperature of the section is 200-800°C, and the temperature of the low temperature section is 100-650°C;
  • the rotating speed of the motor 14 is 0-50 rpm; the inner tube 8 has a diameter of 100 cm and a height of 5 m; the distance between the outer edge of the rotating blade 9 and the inner tube 8 is 20 mm.
  • the power of the vacuum pump 15 is a direct-coupled two-stage rotary vane vacuum pump, and the pumping rate is 15-25 L/s.
  • the vertical vacuum spiral crystallization method for continuous separation of binary eutectic alloys the specific steps include include:
  • the vertical vacuum spiral crystallization equipment for continuous separation of binary eutectic alloys is used.
  • the direct recovery rate of metal tin is increased by 4%, and the energy efficiency is increased by 15%.
  • the vertical vacuum spiral crystallization equipment for continuous separation of binary eutectic alloys includes a vertical furnace body, a feeding system, a heating system, a circulating water cooling system, a rotating system, a vacuum system, and a discharge systems and observation systems;
  • the feeding system includes melting pot 2, feeding pipe 3 and feeding switch 4, the rotating system includes rotating blade 9, rotating shaft 10 and motor 14, the vacuum system includes vacuum pump 15 and a series of valves; the discharging system includes discharging pipe I11 , discharge switch I12, baffle plate 17, discharge pipe II18, discharge switch II19, melt pot 13 and crystal pot 20;
  • the working temperature of the melting pot 2 is 300-1000°C.
  • the inside of the melting pot 2 is provided with the inlet end of the feeding pipe 3 immersed in the melt of the raw material 1, and the outlet end of the feeding pipe 3 passes through the feeding switch 4 and the vertical
  • the top of the vertical furnace body is sealed and connected, and the top of the vertical furnace body is provided with a motor 14.
  • the motor 14 is connected with the rotating shaft 10 sealed and inserted into the cylinder 8 of the vertical furnace body.
  • the rotating blade 9 is arranged on the rotating shaft 10.
  • the vertical furnace body is evacuated to a vacuum pump 15 with a vacuum degree of 1 to 100 Pa.
  • the top of the vertical furnace body and the inside of the inner cylinder 8 are 1 to 2 mm apart from a crystal melting zone (40 cm long and 40 cm wide) with an inclination angle of 6°. 80cm), the crystal melting zone is provided with baffles 17 arranged in dislocation distribution, the outer wall of the inner cylinder 8 is provided with a heating system and a circulating water cooling system, and the bottom of the crystal melting zone is provided with a heating system with a temperature range of 350-800°C.
  • the crystal melting area is connected to the discharge area, and the bottom of the discharge area is equipped with a discharge Pipe II18 and discharge switch II19, the bottom of discharge pipe II18 is provided with crystal pot 20, the discharge area is provided with a heating system, the bottom of inner cylinder 8 is provided with discharge pipe I11, and discharge pipe I11 passes through discharge switch I12 and the bottom
  • the melting pot 13 is connected, and the top of the vertical furnace body is provided with an observation port 16 of the observation system.
  • the processing capacity of vertical vacuum spiral crystallization equipment is 100-500 kg/day;
  • the heating system includes heating element 5 and heat insulation layer 6, heating element 5 is resistance wire, and heat insulation layer 6 is alumina refractory brick;
  • circulating water cooling system Including the circulating water machine and the circulating water pipe 7;
  • the inner cylinder 8 passes through the heating system and the circulating water cooling system of each section from top to bottom to form a heating area with a controllable temperature gradient gradually decreasing.
  • the top is a high temperature section
  • the bottom is a low temperature section, and the high temperature
  • the temperature of the section is 200-800°C, and the temperature of the low temperature section is 100-650°C;
  • the rotating speed of the motor 14 is 0-50 rpm; the inner tube 8 has a diameter of 80 cm and a height of 4 m; the distance between the outer edge of the rotating blade 9 and the inner tube 8 is 15 mm.
  • the power of the vacuum pump 15 is a direct-coupled two-stage rotary vane vacuum pump, and the pumping rate is 15-25 L/s.
  • the vertical vacuum spiral crystallization method for continuously separating binary eutectic alloys the specific steps include:
  • the vertical vacuum spiral crystallization equipment for continuous separation of binary eutectic alloys is used.
  • the direct recovery rate of metal aluminum is increased by 21%, and the energy efficiency is increased by 27%.
  • the vertical vacuum spiral crystallization equipment for continuous separation of binary eutectic alloys includes a vertical furnace body, a feeding system, a heating system, a circulating water cooling system, a rotating system, a vacuum system, and a discharge systems and observation systems;
  • the feeding system includes melting pot 2, feeding pipe 3 and feeding switch 4, and the rotating system includes rotating Blade 9, rotating shaft 10 and motor 14, the vacuum system consists of vacuum pump 15 and a series of valves; the discharge system includes discharge pipe I11, discharge switch I12, baffle plate 17, discharge pipe II18, discharge switch II19, melt pot 13 and crystal pot 20;
  • the working temperature of the melting pot 2 is 300-1000°C.
  • the inside of the melting pot 2 is provided with the inlet end of the feeding pipe 3 immersed in the melt of the raw material 1, and the outlet end of the feeding pipe 3 passes through the feeding switch 4 and the vertical
  • the top of the vertical furnace body is sealed and connected, and the top of the vertical furnace body is provided with a motor 14.
  • the motor 14 is connected with the rotating shaft 10 sealed and inserted into the cylinder 8 of the vertical furnace body.
  • the rotating blade 9 is arranged on the rotating shaft 10.
  • the vertical furnace body is evacuated to a vacuum pump 15 with a vacuum degree of 1 to 100 Pa.
  • the top of the vertical furnace body and the inside of the inner cylinder 8 are 1 to 2 mm apart from a crystal melting zone (45 cm long and 45 cm wide) with an inclination angle of 6°. 85cm), the crystal melting zone is provided with baffles 17 arranged in dislocation distribution, the outer wall of the inner cylinder 8 is provided with a heating system and a circulating water cooling system, and the bottom of the crystal melting zone is provided with a heating system with a temperature range of 350-800°C.
  • the crystal melting zone communicates with the discharge zone, the bottom of the discharge zone is provided with a discharge pipe II18 and a discharge switch II19, the bottom of the discharge pipe II18 is provided with a crystal pot 20, the discharge area is provided with a heating system, and the bottom of the inner cylinder 8 is provided with There is a discharge pipe I11, and the discharge pipe I11 communicates with the melt pot 13 at the bottom through the discharge switch I12, and the top of the vertical furnace body is provided with an observation port 16 of the observation system.
  • the processing capacity of vertical vacuum spiral crystallization equipment is 100-500 kg/day;
  • the heating system includes heating element 5 and heat insulation layer 6, heating element 5 is resistance wire, and heat insulation layer 6 is alumina refractory brick;
  • circulating water cooling system Including the circulating water machine and the circulating water pipe 7;
  • the inner cylinder 8 passes through the heating system and the circulating water cooling system of each section from top to bottom to form a heating area with a controllable temperature gradient gradually decreasing.
  • the top is a high temperature section
  • the bottom is a low temperature section, and the high temperature
  • the temperature of the section is 200-800°C, and the temperature of the low temperature section is 100-650°C;
  • the rotating speed of the motor 14 is 0-50 rpm; the diameter of the inner cylinder 8 is 65cm, and the height is 4m; the distance between the outer edge of the rotating blade 9 and the inner cylinder 8 is 18mm.
  • the power of the vacuum pump 15 is a direct-coupled two-stage rotary vane vacuum pump, and the pumping rate is 15-25 L/s.
  • the vertical vacuum spiral crystallization method for continuously separating binary eutectic alloys the specific steps include:
  • the vertical vacuum spiral crystallization equipment for continuous separation of binary eutectic alloys is used.
  • the metal plumbous yield is increased by 18%, and the energy efficiency is increased by 22%.

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Abstract

一种连续分离二元共晶合金的竖式真空螺旋结晶设备及方法，该设备包括竖式炉体、进料系统、加热系统、循环水冷却系统、转动系统、真空系统、出料系统及观测系统。竖式炉体利用重力加快熔体的逆流，有利于提高晶体的纯度。本设备和方法处理对象为含有共晶相点任意成分的二元合金，设备操作方便、处理过程无"三废"产生，作业环境好，过程安全可控。

Description

一种连续分离二元共晶合金的竖式真空螺旋结晶设备及方法 技术领域
本发明涉及一种连续分离二元共晶合金的竖式真空螺旋结晶设备及方法，属于有色金属火法冶炼技术领域。
背景技术
结晶分离法是利用杂质在固态主体金属和液态主体金属中溶解度的差异来实现杂质分离，属于金属-金属系异相分离，具有节能、低温操作、可分离出高纯产品等优点。我国20世纪70年代根据结晶分离法发明的电热连续结晶机是锡冶炼过程中最重要的装备之一，主要作用是实现粗锡中铅的脱除。但传统的电热连续结晶机自动化程度低、耗水量高，工人作业环境差。几十年来，我国科技人员持续对其进行了改造工作。在公开号为CN205662564U的专利中公开了一种电热螺旋结晶机的设备，主要是提供一种各加热段温度配比合理、单机产能高、生产过程中耗水量低的电热螺旋结晶机。在公开号为CN 206069975U的专利中公开了一种处理粗锡的电热式螺旋结晶机，目的是改进放焊锡过程中采用电热式加热降低柴油燃烧对环境的污染，提高工人作业环境舒适度。
发明内容
针对上述现有技术存在的问题及不足，本发明提供一种连续分离二元共晶合金的竖式真空螺旋结晶设备及方法。本设备和方法处理对象对含有共晶相点任意成分的二元合金，设备操作方便、强度低，处理过程无“三废”产生，最大限度保障了金属的直收率，作业环境好，过程安全可控。本发明通过以下技术方案实现。
一种连续分离二元共晶合金的竖式真空螺旋结晶设备，包括竖式炉体、进料系统、加热系统、循环水冷却系统、转动系统、真空系统、出料系统及观测系统；
所述进料系统包括熔料锅2、进料管3和进料开关4，转动系统包括旋转叶片9、转轴10和电机14，真空系统包括真空泵15和系列阀门组成；出料系统包括出料管Ⅰ11、出料开关Ⅰ12、挡板17、出料管Ⅱ18、出料 开关Ⅱ19、熔体锅13和晶体锅20；
进料系统中熔料锅2工作温度为300～1000℃，熔料锅2内部设有浸没在原料1熔体的进料管3入口端，进料管3出口端通过进料开关4与竖式炉体顶部密封相通，竖式炉体顶部设有电机14，电机14与密封插入到竖式炉体内筒8的转轴10连接，转轴10上设有旋转叶片9，竖式炉体顶部设有将竖式炉体抽真空至真空度为1～100Pa的真空泵15，竖式炉体顶部与内筒8内侧相距1～2mm处设有倾斜角度为3°～7°的晶体熔化区(长为30～50cm，宽为15～100cm)，晶体熔化区上设有错位分布布置的挡板17，内筒8外壁上设有加热系统和循环水冷却系统，晶体熔化区底部设有温度区域为350-800℃的加热系统，晶体熔化区与出料区相通，出料区底部设有出料管Ⅱ18和出料开关Ⅱ19，出料管Ⅱ18底部设有晶体锅20，出料区上设有加热系统，内筒8底部设有出料管Ⅰ11，出料管Ⅰ11通过出料开关Ⅰ12与底部的熔体锅13连通，竖式炉体顶部设有观测系统的观测口16。
所述竖式真空螺旋结晶设备处理量为100～500公斤/天。
所述加热系统包括发热体5和隔热层6，发热体5为电阻丝，隔热层6为氧化铝耐火砖。
所述循环水冷却系统包括循环水机和循环水管7。
所述内筒8从上至下通过每段的加热系统和循环水冷却系统依次形成可控温度梯度逐渐降低的加热区域，顶部为高温段，底部为低温段，高温段温度为200-800℃，低温段温度为100-650℃。
所述电机14转速为0～50转/分钟；内筒8直径为15～100cm，高为2～5m；旋转叶片9外边缘与内筒8间距为5～20mm。
所述真空泵15功率为直联式双级旋片真空泵，抽气速率为15～25L/s。
一种连续分离二元共晶合金的竖式真空螺旋结晶方法，其具体步骤包括：真空条件下将二元共晶合金原料从熔料锅2利用虹吸持续注入内筒8中，内筒8存在温度梯度，在电机14的转动下，晶体不断析出被传动至内筒8顶部，流入到晶体熔化区，晶体经挡板处再次熔化，再经出料开关Ⅱ放出，同时定期打开出料开关Ⅰ将熔体放出。
所述二元共晶合金原料包括锡铅合金、锡铋合金、铅铋合金或锡铝合 金。
本发明的有益效果是：
本设备和方法处理对象对含有共晶相点任意成分的二元共晶合金，原料的普适性较高，设备操作方便、强度低，处理过程无“三废”产生，最大限度保障了金属的直收率，作业环境好，过程安全可控。
相较于传统的结晶机槽体倾斜横向放置，本设备采用竖式可进一步利用重力加快熔体的逆流，更有利于提高晶体的纯度。同时，本设备增加了真空系统，一方面避免了金属氧化的问题，提高了金属的直收率；另一方面，真空系统下减少了热量散失，提高了能源效率。
附图说明
图1是本发明设备结构示意图；
图2是本发明挡板分布示意图。
图中：1-原料；2-熔料锅；3-进料管；4-进料开关；5-发热体；6-隔热层；7-循环水管；8-内筒；9-旋转叶片；10-转轴；11-出料管Ⅰ；12-出料开关Ⅰ；13-熔体锅；14-电机；15-真空泵；16-观测口；17-挡板；18-出料管Ⅱ；19-出料开关Ⅱ；20-晶体锅。
具体实施方式
下面结合附图和具体实施方式，对本发明作进一步说明。
实施例1
如图1和2所示，该连续分离二元共晶合金的竖式真空螺旋结晶设备，包括竖式炉体、进料系统、加热系统、循环水冷却系统、转动系统、真空系统、出料系统及观测系统；
进料系统包括熔料锅2、进料管3和进料开关4，转动系统包括旋转叶片9、转轴10和电机14，真空系统包括真空泵15和系列阀门组成；出料系统包括出料管Ⅰ11、出料开关Ⅰ12、挡板17、出料管Ⅱ18、出料开关Ⅱ19、熔体锅13和晶体锅20；
进料系统中熔料锅2工作温度为300～1000℃，熔料锅2内部设有浸没在原料1熔体的进料管3入口端，进料管3出口端通过进料开关4与竖式炉体顶部密封相通，竖式炉体顶部设有电机14，电机14与密封插入到竖式炉体内筒8的转轴10连接，转轴10上设有旋转叶片9，竖式炉体顶 部设有将竖式炉体抽真空至真空度为1～100Pa的真空泵15，竖式炉体顶部与内筒8内侧相距1～2mm处设有倾斜角度为3°的晶体熔化区(长为30cm，宽为15cm)，晶体熔化区上设有错位分布布置的挡板17，内筒8外壁上设有加热系统和循环水冷却系统，体熔化区底部设有温度区域为350-800℃的加热系统，晶体熔化区与出料区相通，出料区底部设有出料管Ⅱ18和出料开关Ⅱ19，出料管Ⅱ18底部设有晶体锅20，出料区上设有加热系统，内筒8底部设有出料管Ⅰ11，出料管Ⅰ11通过出料开关Ⅰ12与底部的熔体锅13连通，竖式炉体顶部设有观测系统的观测口16。
其中竖式真空螺旋结晶设备处理量为100～500公斤/天；加热系统包括发热体5和隔热层6，发热体5为电阻丝，隔热层6为氧化铝耐火砖；循环水冷却系统包括循环水机和循环水管7；内筒8从上至下通过每段的加热系统和循环水冷却系统依次形成可控温度梯度逐渐降低的加热区域，顶部为高温段，底部为低温段，高温段温度为200-800℃，低温段温度为100-650℃；
电机14转速为0～50转/分钟；内筒8直径为15cm，高为2m；旋转叶片9外边缘与内筒8间距为5mm。
真空泵15功率为直联式双级旋片真空泵，抽气速率为15～25L/s。
该连续分离二元共晶合金的竖式真空螺旋结晶方法，其具体步骤包括：
(1)将100公斤锡铅二元合金(成分：Sn90％、Pb10％)在工作温度为500℃的熔料锅2中熔化，关闭进料开关4、出料开关Ⅰ12和出料开关Ⅱ19，启动真空泵15，使竖式炉体内压力低于100Pa，并设置内筒8顶部温度232℃，低部温度183℃，启动加热系统；
(2)待竖式炉体温度梯度稳定后，打开进料管开关4，同时启动电机14，以3转/分钟的速度运行；
(3)通过观测口16查看晶体情况，晶体熔化区温度设为350℃，不定期打开出料开关，将熔体和晶体放出，最终得到含铅38.4％的焊锡和含锡99.6％的精锡产品。
本实施例中采用该连续分离二元共晶合金的竖式真空螺旋结晶设备，与传统电热结晶机相比，金属锡的直收率提高了5％，能源效率提高了8％。
实施例2
如图1和2所示，该连续分离二元共晶合金的竖式真空螺旋结晶设备，包括竖式炉体、进料系统、加热系统、循环水冷却系统、转动系统、真空系统、出料系统及观测系统；
进料系统包括熔料锅2、进料管3和进料开关4，转动系统包括旋转叶片9、转轴10和电机14，真空系统包括真空泵15和系列阀门组成；出料系统包括出料管Ⅰ11、出料开关Ⅰ12、挡板17、出料管Ⅱ18、出料开关Ⅱ19、熔体锅13和晶体锅20；
进料系统中熔料锅2工作温度为300～1000℃，熔料锅2内部设有浸没在原料1熔体的进料管3入口端，进料管3出口端通过进料开关4与竖式炉体顶部密封相通，竖式炉体顶部设有电机14，电机14与密封插入到竖式炉体内筒8的转轴10连接，转轴10上设有旋转叶片9，竖式炉体顶部设有将竖式炉体抽真空至真空度为1～100Pa的真空泵15，竖式炉体顶部与内筒8内侧相距1～2mm处设有倾斜角度为7°的晶体熔化区(长为50cm，宽为100cm)，晶体熔化区上设有错位分布布置的挡板17，内筒8外壁上设有加热系统和循环水冷却系统，晶体熔化区底部设有温度区域为350-800℃的加热系统，晶体熔化区与出料区相通，出料区底部设有出料管Ⅱ18和出料开关Ⅱ19，出料管Ⅱ18底部设有晶体锅20，出料区上设有加热系统，内筒8底部设有出料管Ⅰ11，出料管Ⅰ11通过出料开关Ⅰ12与底部的熔体锅13连通，竖式炉体顶部设有观测系统的观测口16。
其中竖式真空螺旋结晶设备处理量为100～500公斤/天；加热系统包括发热体5和隔热层6，发热体5为电阻丝，隔热层6为氧化铝耐火砖；循环水冷却系统包括循环水机和循环水管7；内筒8从上至下通过每段的加热系统和循环水冷却系统依次形成可控温度梯度逐渐降低的加热区域，顶部为高温段，底部为低温段，高温段温度为200-800℃，低温段温度为100-650℃；
电机14转速为0～50转/分钟；内筒8直径为100cm，高为5m；旋转叶片9外边缘与内筒8间距为20mm。
真空泵15功率为直联式双级旋片真空泵，抽气速率为15～25L/s。
该连续分离二元共晶合金的竖式真空螺旋结晶方法，其具体步骤包 括：
(1)将500公斤锡铅二元合金(成分：Sn95％、Pb5％)在工作温度为300℃的熔料锅2中熔化，关闭进料开关4、出料开关Ⅰ12和出料开关Ⅱ19，启动真空泵15，使竖式炉体内压力低于100Pa，并设置内筒8顶部温度232℃，低部温度183℃，启动加热系统；
(2)待竖式炉体温度梯度稳定后，打开进料管开关4，同时启动电机14，以2转/分钟的速度运行；
(3)通过观测口16查看晶体情况，晶体熔化区温度设为350℃，不定期打开出料开关，将熔体和晶体放出，最终得到含铅37.8％的焊锡和含锡99.9％的精锡产品。
本实施例中采用该连续分离二元共晶合金的竖式真空螺旋结晶设备，与传统电热结晶机相比，金属锡的直收率提高了4％，能源效率提高了15％。
实施例3
如图1和2所示，该连续分离二元共晶合金的竖式真空螺旋结晶设备，包括竖式炉体、进料系统、加热系统、循环水冷却系统、转动系统、真空系统、出料系统及观测系统；
进料系统包括熔料锅2、进料管3和进料开关4，转动系统包括旋转叶片9、转轴10和电机14，真空系统包括真空泵15和系列阀门组成；出料系统包括出料管Ⅰ11、出料开关Ⅰ12、挡板17、出料管Ⅱ18、出料开关Ⅱ19、熔体锅13和晶体锅20；
进料系统中熔料锅2工作温度为300～1000℃，熔料锅2内部设有浸没在原料1熔体的进料管3入口端，进料管3出口端通过进料开关4与竖式炉体顶部密封相通，竖式炉体顶部设有电机14，电机14与密封插入到竖式炉体内筒8的转轴10连接，转轴10上设有旋转叶片9，竖式炉体顶部设有将竖式炉体抽真空至真空度为1～100Pa的真空泵15，竖式炉体顶部与内筒8内侧相距1～2mm处设有倾斜角度为6°的晶体熔化区(长为40cm，宽为80cm)，晶体熔化区上设有错位分布布置的挡板17，内筒8外壁上设有加热系统和循环水冷却系统，晶体熔化区底部设有温度区域为350-800℃的加热系统，晶体熔化区与出料区相通，出料区底部设有出料 管Ⅱ18和出料开关Ⅱ19，出料管Ⅱ18底部设有晶体锅20，出料区上设有加热系统，内筒8底部设有出料管Ⅰ11，出料管Ⅰ11通过出料开关Ⅰ12与底部的熔体锅13连通，竖式炉体顶部设有观测系统的观测口16。
其中竖式真空螺旋结晶设备处理量为100～500公斤/天；加热系统包括发热体5和隔热层6，发热体5为电阻丝，隔热层6为氧化铝耐火砖；循环水冷却系统包括循环水机和循环水管7；内筒8从上至下通过每段的加热系统和循环水冷却系统依次形成可控温度梯度逐渐降低的加热区域，顶部为高温段，底部为低温段，高温段温度为200-800℃，低温段温度为100-650℃；
电机14转速为0～50转/分钟；内筒8直径为80cm，高为4m；旋转叶片9外边缘与内筒8间距为15mm。
真空泵15功率为直联式双级旋片真空泵，抽气速率为15～25L/s。
该连续分离二元共晶合金的竖式真空螺旋结晶方法，其具体步骤包括：
(1)将500公斤锡铝二元合金(成分：Sn20％、Al80％)在工作温度为1000℃的熔料锅2中熔化，关闭进料开关4、出料开关Ⅰ12和出料开关Ⅱ19，启动真空泵15，使竖式炉体内压力低于100Pa，并设置内筒8顶部温度232℃，低部温度183℃，启动加热系统；
(2)待竖式炉体温度梯度稳定后，打开进料管开关4，同时启动电机14，以2转/分钟的速度运行；
(3)通过观测口16查看晶体情况，晶体熔化区温度设为800℃，不定期打开出料开关，将熔体和晶体放出，最终得到含锡85％的粗锡和含铝99％的粗铝。
本实施例中采用该连续分离二元共晶合金的竖式真空螺旋结晶设备，与电解法相比，金属铝的直收率分别提高了21％，能源效率提高了27％。
实施例4
如图1和2所示，该连续分离二元共晶合金的竖式真空螺旋结晶设备，包括竖式炉体、进料系统、加热系统、循环水冷却系统、转动系统、真空系统、出料系统及观测系统；
进料系统包括熔料锅2、进料管3和进料开关4，转动系统包括旋转 叶片9、转轴10和电机14，真空系统包括真空泵15和系列阀门组成；出料系统包括出料管Ⅰ11、出料开关Ⅰ12、挡板17、出料管Ⅱ18、出料开关Ⅱ19、熔体锅13和晶体锅20；
进料系统中熔料锅2工作温度为300～1000℃，熔料锅2内部设有浸没在原料1熔体的进料管3入口端，进料管3出口端通过进料开关4与竖式炉体顶部密封相通，竖式炉体顶部设有电机14，电机14与密封插入到竖式炉体内筒8的转轴10连接，转轴10上设有旋转叶片9，竖式炉体顶部设有将竖式炉体抽真空至真空度为1～100Pa的真空泵15，竖式炉体顶部与内筒8内侧相距1～2mm处设有倾斜角度为6°的晶体熔化区(长为45cm，宽为85cm)，晶体熔化区上设有错位分布布置的挡板17，内筒8外壁上设有加热系统和循环水冷却系统，晶体熔化区底部设有温度区域为350-800℃的加热系统，晶体熔化区与出料区相通，出料区底部设有出料管Ⅱ18和出料开关Ⅱ19，出料管Ⅱ18底部设有晶体锅20，出料区上设有加热系统，内筒8底部设有出料管Ⅰ11，出料管Ⅰ11通过出料开关Ⅰ12与底部的熔体锅13连通，竖式炉体顶部设有观测系统的观测口16。
其中竖式真空螺旋结晶设备处理量为100～500公斤/天；加热系统包括发热体5和隔热层6，发热体5为电阻丝，隔热层6为氧化铝耐火砖；循环水冷却系统包括循环水机和循环水管7；内筒8从上至下通过每段的加热系统和循环水冷却系统依次形成可控温度梯度逐渐降低的加热区域，顶部为高温段，底部为低温段，高温段温度为200-800℃，低温段温度为100-650℃；
电机14转速为0～50转/分钟；内筒8直径为65cm，高为4m；旋转叶片9外边缘与内筒8间距为18mm。
真空泵15功率为直联式双级旋片真空泵，抽气速率为15～25L/s。
该连续分离二元共晶合金的竖式真空螺旋结晶方法，其具体步骤包括：
(1)将200公斤铅铋二元合金(成分：Pb62.5％，Bi37.5％)在工作温度为400℃的熔料锅2中熔化，关闭进料开关4、出料开关Ⅰ12和出料开关Ⅱ19，启动真空泵15，使竖式炉体内压力低于100Pa，并设置内筒8顶部温度232℃，低部温度183℃，启动加热系统；
(2)待竖式炉体温度梯度稳定后，打开进料管开关4，同时启动电机14，以2转/分钟的速度运行；
(3)通过观测口16查看晶体情况，晶体熔化区温度设为400℃，不定期打开出料开关，将熔体和晶体放出，最终得到含铋77％的粗铋和含铅98.7％的粗铅。
本实施例中采用该连续分离二元共晶合金的竖式真空螺旋结晶设备，与电解法相比，金属铅直收率提高了18％，能源效率提高了22％。
以上结合附图对本发明的具体实施方式作了详细说明，但是本发明并不限于上述实施方式，在本领域普通技术人员所具备的知识范围内，还可以在不脱离本发明宗旨的前提下作出各种变化。

Claims (9)

  1. 一种连续分离二元共晶合金的竖式真空螺旋结晶设备，其特征在于：包括竖式炉体、进料系统、加热系统、循环水冷却系统、转动系统、真空系统、出料系统及观测系统；
    所述进料系统包括熔料锅(2)、进料管(3)和进料开关(4)，转动系统包括旋转叶片(9)、转轴(10)和电机(14)，真空系统包括真空泵(15)和系列阀门组成；出料系统包括出料管Ⅰ(11)、出料开关Ⅰ(12)、挡板(17)、出料管Ⅱ(18)、出料开关Ⅱ(19)、熔体锅(13)和晶体锅(20)；
    所述进料系统中所述熔料锅(2)工作温度为300～1000℃，所述熔料锅(2)内部设有浸没在原料(1)熔体的所述进料管(3)入口端，所述进料管(3)出口端通过所述进料开关(4)与竖式炉体顶部密封相通，竖式炉体顶部设有所述电机(14)，所述电机(14)与密封插入到竖式炉体内筒(8)的所述转轴(10)连接，所述转轴(10)上设有所述旋转叶片(9)，所述竖式炉体顶部设有将所述竖式炉体抽真空至真空度为1～100Pa的所述真空泵(15)，所述竖式炉体顶部与所述内筒(8)内侧相距1～2mm处设有倾斜角度为3°～7°的晶体熔化区，晶体熔化区长为30～50cm，宽为15～100cm，晶体熔化区上设有错位分布布置的所述挡板(17)，所述内筒(8)外壁上设有加热系统和循环水冷却系统，晶体熔化区底部设有温度区域为350-800℃的加热系统，晶体熔化区与出料区相通，出料区底部设有所述出料管Ⅱ(18)和所述出料开关Ⅱ(19)，所述出料管Ⅱ(18)底部设有所述晶体锅(20)，出料区上设有加热系统，所述内筒(8)底部设有所述出料管Ⅰ(11)，所述出料管Ⅰ(11)通过所述出料开关Ⅰ(12)与底部的所述熔体锅(13)连通，竖式炉体顶部设有观测系统的观测口(16)。
  2. 根据权利要求1所述的连续分离二元共晶合金的竖式真空螺旋结晶设备，其特征在于：所述竖式真空螺旋结晶设备处理量为100～500公斤/天。
  3. 根据权利要求1所述的连续分离二元共晶合金的竖式真空螺旋结晶设备，其特征在于：所述加热系统包括发热体(5)和隔热层(6)，所述 发热体(5)为电阻丝，所述隔热层(6)为氧化铝耐火砖。
  4. 根据权利要求1所述的连续分离二元共晶合金的竖式真空螺旋结晶设备，其特征在于：所述循环水冷却系统包括循环水机和循环水管(7)。
  5. 根据权利要求1所述的连续分离二元共晶合金的竖式真空螺旋结晶设备，其特征在于：所述内筒(8)从上至下通过每段的加热系统和循环水冷却系统依次形成可控温度梯度逐渐降低的加热区域，顶部为高温段，底部为低温段，高温段温度为200-800℃，低温段温度为100-650℃。
  6. 根据权利要求1所述的连续分离二元共晶合金的竖式真空螺旋结晶设备，其特征在于：所述电机(14)转速为0～50转/分钟；所述内筒(8)直径为15～100cm，高为2～5m；所述旋转叶片(9)外边缘与所述内筒(8)间距为5～20mm。
  7. 根据权利要求1所述的连续分离二元共晶合金的竖式真空螺旋结晶设备，其特征在于：所述真空泵(15)为直联式双级旋片真空泵，抽气速率为15～25L/s。
  8. 一种连续分离二元共晶合金的竖式真空螺旋结晶方法，其特征在于具体步骤包括：真空条件下将二元共晶合金原料从熔料锅(2)利用虹吸持续注入内筒(8)中，内筒(8)存在温度梯度，在电机(14)的转动下，晶体不断析出被传动至内筒(8)顶部，流入到晶体熔化区，晶体经挡板处再次熔化，再经出料开关Ⅱ放出，同时定期打开出料开关Ⅰ将熔体放出。
  9. 根据权利要求8所述的连续分离二元共晶合金的竖式真空螺旋结晶方法，其特征在于：所述二元共晶合金原料包括锡铅合金、锡铋合金、铅铋合金或锡铝合金。
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