CN102706144A - Fractional condensation vacuum furnace - Google Patents

Fractional condensation vacuum furnace Download PDF

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Publication number
CN102706144A
CN102706144A CN2012101648169A CN201210164816A CN102706144A CN 102706144 A CN102706144 A CN 102706144A CN 2012101648169 A CN2012101648169 A CN 2012101648169A CN 201210164816 A CN201210164816 A CN 201210164816A CN 102706144 A CN102706144 A CN 102706144A
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China
Prior art keywords
condenser
condensate pans
crucible
temperature
vacuum
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CN2012101648169A
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Chinese (zh)
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熊利芝
何则强
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Jishou University
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Jishou University
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Priority to CN2012101648169A priority Critical patent/CN102706144A/en
Publication of CN102706144A publication Critical patent/CN102706144A/en
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The invention discloses a fractional condensation vacuum furnace, which is a metallurgy vacuum device for directly extracting and obtaining high-quality metal from ores. The fractional condensation vacuum furnace comprises a furnace cover 1, a cooling water outlet 2, a condenser 3, a furnace body 4, a thermocouple 5, a heat shield 6, a cooling water inlet 7, a crucible 8, a heating body 9, a water-cooling electrode 10, a furnace bottom 11, condensing discs 12, a vacuum pump port 13 and the like. The condenser 3 is directly connected with the crucible 8, is formed by overlapping a plurality of condensing discs and has a certain sealing performance; in the reaction process, the condenser temperature declines from high to low gradually. The substance reacts and evaporates in the crucible, and then enters the condenser, and diffuses from bottom to top along the condenser; because saturation vapor pressure of each substance is different, the substance condenses are separated on different condensing discs; and the product quality is improved drastically. The vacuum furnace uses residual heat to improve energy efficiency, thus improving product quality.

Description

A kind of fractional condensaion vacuum drying oven
Technical field
Vacuum metallurgy equipment.
Background technology
The condenser of classical vacuum equipment generally adopts the mode of water-cooled, and directly by the water condenser condensation, the total condensation of this favourable product improved productive rate after products obtained therefrom distilled from raw material.But in condensation process, except the condensation of purpose product, also have the impurity substances of quite a few also to be condensed, cause product quality to reduce, the entrained heat of the steam that distills simultaneously also fails to make full use of.In order to improve the quality of products, improve efficiency, shortened process; Also meet simultaneously the requirement of building a resource-conserving and environment-friendly society, the condenser of the vacuum drying oven of classics is improved and transforms, adopt fractional condenser; To from crucible, evaporate the gas that through a gradually cold fractional condenser; Utilize the difference of each material saturated vapour pressure under different temperatures in the steam, different material will be in the different parts condensation of condenser, thereby realizes the separation of material.
Summary of the invention
The design's purpose is a kind of also vacuum drying oven of refining purpose product that directly from mineral, refines of design; Comprise that water-cooling system, gas charging system, fractional condensaion vacuum furnace body, temperature control and detection system and vacuum obtain and detection system is formed, the fractional condensaion vacuum furnace body comprises that bell 1, coolant outlet 2, condenser 3, shaft 4, thermocouple 5, heat shield 6, cooling water inlet 7, graphite crucible 8, graphite heater 9, water cooled electrode 10, furnace bottom 11, condensate pans 12, vavuum pump interface 13 etc. partly form.Thermocouple detects the temperature at furnace bottom, condenser bottom and top respectively, with the control reaction temperature, detects condenser temperature.Condenser is formed by stacking and has certain sealing as food steamer many condensate pans.The bottom-up continuous reduction of the temperature of condensate pans in the condenser in experimentation.Leave the aperture of two meniscus shapeds on each condensate pans in the condenser, be beneficial to gas and pass through, the cryosurface of condensate pans is coniform for standing upside down; Increase the area of cryosurface like this; Help the abundant condensation of material, simultaneously, if material is liquid during condensation on condensate pans; Material will will help the collection of product along the face of handstand circular cone toward dirty and accumulate droplet and drip in the next condensate pans; Crucible closely links to each other with condenser, makes the steam that product produces through distillation from crucible directly get into condenser by crucible, and constantly upwards spreads through different condensate pans along condenser.Because each vapour pressure and saturated vapour pressure under different temperatures are different, each material will be on different condensate pans condensation and separating.
In smelting process, raw material is contained in the crucible, through water cooled electrode the electric current in the external world is guided in the vacuum drying oven on the graphite heater base; Cause placing the graphite heater heating on the heater base, the crucible temperature at heater center rises rapidly, because the heater periphery is provided with the multilayer insulation cover; Therefore the temperature in the crucible is the highest part of temperature in the whole vacuum drying oven; Be reaction center, the steam that the crucible internal reaction produces, steam gets into different parts condensation in the fractional condenser.When reaction temperature during at 1000 ~ 1250 ℃, the condenser overhead temperature is at 45 ~ 50 ℃, 650 ~ 850 ℃ of bottom condensate pans temperature, and the condenser overhead temperature is few with general water-cooled condenser temperature difference, has guaranteed that each hot volatile materials is than total condensation; The temperature of condenser bottom is higher, shows that the bottom-up temperature of condenser constantly reduces, and helps the different parts condensation of various materials of different nature at condenser, reaches the purpose of separation.In whole process, vacuumize with vavuum pump, the good airproof performance of this vacuum drying oven, vacuum can reach 5Pa.Vacuum drying oven with the design directly extracts and refined metals zinc from smithsonite and smithsonite, obtains metallic zinc purity and reaches 99.995%, also obtains the byproduct and the impurity lead of purer cadmium metal simultaneously.
The design possesses following characteristics: 1) along with the rising of reaction temperature; The temperature at condensate pans top is between 45 ~ 50 ℃; Be more or less the same with the condensation temperature of general water-cooled condenser, the hot volatile substance that can guarantee from crucible, to evaporate in condenser than total condensation; The rate of recovery of product increases; Other impurity substances also is able to condensation, helps further handling or directly obtaining purer accessory substance; Prevent flying away of hot volatile materials; Hot volatile matter content is very low in the gas behind condenser, helps the further recycling to tail gas.2) along with the rising of reaction temperature, the temperature of bottom cold dish constantly raises.3) temperature of condensate pans is much higher than the temperature of top condensate pans, the i.e. bottom-up continuous reduction of the temperature of each condensate pans in the condenser bottom in the experimentation.This constantly reduces steam temperature in the diffusion process bottom-up along condenser; When dropping to uniform temperature, wherein some material is in hypersaturated state, beginning condensation on condensate pans; The material that is condensed simultaneously also can evaporate; On condensate pans, have the condensation and the evaporation of material so simultaneously, and the two is in the dynamic process, condensate pans in this process be cooling medium be again evaporimeter; Along with the continuous condensation and the evaporation of material, help the removal of impurity in the product and the raising of product quality.The steam that from crucible, evaporates material is in the process of suitable condensate pans through condensation, the continuous removal of impurities of evaporation; Make product quality improve greatly; Simultaneously in this process, do not increase energy consumption and just make full use of waste heat, make efficiency improve, added value of product increases.4) device structure is simple, and requirement on machining accuracy is not high, and cost is low.5) easy to operate, each experiment finishes, as long as open bell successively; Take off condensate pans at different levels, never obtain different material on the condensate pans, then take out crucible; Can the reaction residues in the crucible be taken out,, can install equipment by opposite order if begin new experiment.
Description of drawings
Fig. 1 is a fractional condensaion vacuum drying oven furnace binding sketch map, and 1 is bell, the 2nd among the figure, coolant outlet, the 3rd, and condenser, the 4th, shaft, the 5th, thermocouple, the 6th, heat shield, the 7th, cooling water inlet, the 8th, graphite crucible, the 9th, graphite heater, water 10 are cold electrodes, the 11st, furnace bottom, the 12nd, condensate pans, the 13rd, vavuum pump interface.
The specific embodiment
Below in conjunction with accompanying drawing this equipment is described in further detail:
This experimental facilities is suitable for refining and the more volatile material of refining in the mineral, obtains high quality of products, like zinc oxide ore.Present embodiment comprises that water-cooling system, gas charging system, fractional condensaion vacuum furnace body, temperature control and detection system and vacuum obtain and detection system is formed, and fractional condensaion vacuum furnace body (see figure 1) comprises that bell 1, coolant outlet 2, condenser 3, shaft 4, thermocouple 5, heat shield 6, cooling water inlet 7, graphite crucible 8, graphite heater 9, water cooled electrode 10, furnace bottom 11, condensate pans 12, vavuum pump interface 13 etc. partly form.
It is following that the fractional condensaion vacuum drying oven extracts grading purification product step:
As shown in Figure 1, open bell 1, take out condensate pans 12 successively, raw material is put into graphite crucible 8; Install condensate pans 12 successively, build bell 1, open cooling water and be evacuated to about system pressure 5Pa, stove begins heat temperature raising; According to the experiment needs, be chosen under the suitable temperature, through gas charging system regulating system pressure; Be warming up to temperature requiredly, product produces and evaporation in the reaction center graphite crucible, and steam gets into fractional condenser 3 condensations; Steam is bottom-up continuous diffusion in condenser, because each vapour pressure and the saturated vapour pressure under different temperatures are different, each material will condensation on different condensate pans.The insulation certain hour, outage, fast cooling stops vavuum pump, closes cooling water, blow-on.Take out condensate pans successively, from different condensate pans, take off different products, take out slag in the crucible.
Adopt the fractional condensaion vacuum drying oven, make full use of waste heat, obtain high purity product, improve efficiency, promote product quality, shortened process reduces production costs.

Claims (1)

1. fractional condensaion vacuum drying oven; It is characterized in that: it is obtained by water-cooling system, gas charging system, fractional condensaion vacuum furnace body, temperature control and detection system and vacuum and detection system is formed, and the fractional condensaion vacuum furnace body comprises that bell 1, coolant outlet 2, condenser 3, shaft 4, thermocouple 5, heat shield 6, cooling water inlet 7, graphite crucible 8, graphite heater 9, water cooled electrode 10, furnace bottom 11, condensate pans 12, vavuum pump interface 13 etc. partly form; Thermocouple detects the temperature at furnace bottom, condenser bottom and top respectively, with the control reaction temperature, detects condenser temperature; Condenser is formed by stacking and has certain sealing as food steamer many condensate pans; The bottom-up continuous reduction of the temperature of condensate pans in the condenser in experimentation; Leave the aperture of two meniscus shapeds on each condensate pans in the condenser, be beneficial to gas and pass through, the cryosurface of condensate pans is coniform for standing upside down; Increase the area of cryosurface like this; Help the abundant condensation of material, simultaneously, if material is liquid during condensation on condensate pans; Material will will help the collection of product along the face of handstand circular cone toward dirty and accumulate droplet and drip in the next condensate pans; Crucible closely links to each other with condenser, makes the steam that product produces through distillation from crucible directly get into condenser by crucible, and constantly upwards spreads through different condensate pans along condenser; Because each vapour pressure and saturated vapour pressure under different temperatures are different, each material will be on different condensate pans condensation and separating.
CN2012101648169A 2012-05-25 2012-05-25 Fractional condensation vacuum furnace Pending CN102706144A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107217145A (en) * 2016-12-09 2017-09-29 郴州万墨环保科技有限公司 A kind of method that copper anode mud vacuum reduction takes off lead antimony bismuth selen-tellurjum arsenic
CN109082542A (en) * 2018-02-24 2018-12-25 虔东稀土集团股份有限公司 A method of it preparing the vacuum drying oven of high pure metal ytterbium and its prepares high pure metal ytterbium
CN111979425A (en) * 2020-07-24 2020-11-24 广东先导稀材股份有限公司 Refining device for high-purity metal
CN113444893A (en) * 2020-03-27 2021-09-28 核工业理化工程研究院 Height-adjustable vacuum multilayer evaporation device and evaporation method
CN113604667A (en) * 2021-07-26 2021-11-05 重庆赛迪热工环保工程技术有限公司 Multi-metal vapor vacuum step condensation method and system
CN114191835A (en) * 2021-12-28 2022-03-18 中国原子能科学研究院 Molecular distillation device and purification system for removing radioactive impurities in alloy
CN115449648A (en) * 2022-08-30 2022-12-09 昆明理工大学 Calcined dolomite vacuum carbothermic reduction magnesium smelting equipment and method

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JP2005097648A (en) * 2003-09-22 2005-04-14 Mitsui Mining & Smelting Co Ltd Method for recovering magnesium-based alloy waste material
JP2006283192A (en) * 2006-07-12 2006-10-19 Dowa Mining Co Ltd High-purity indium
CN1927701A (en) * 2006-09-29 2007-03-14 先导(清远)稀有金属化工有限公司 Producing device of high-purity selenium and producing process
CN2880850Y (en) * 2005-10-18 2007-03-21 昆明理工大学 Vacuum furnace of extracting aluminium directly from aluminium ore
DE102006056482A1 (en) * 2006-11-30 2008-06-05 Deutsche Solar Ag Apparatus and method for processing non-ferrous metals
CN101935767A (en) * 2010-09-26 2011-01-05 山西龙港高纯材料有限公司 Method for preparing high-purity arsenic
CN101956083A (en) * 2010-10-29 2011-01-26 曲智 Process method and equipment for smelting magnesium by using magnesite with one-step method

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005097648A (en) * 2003-09-22 2005-04-14 Mitsui Mining & Smelting Co Ltd Method for recovering magnesium-based alloy waste material
CN2880850Y (en) * 2005-10-18 2007-03-21 昆明理工大学 Vacuum furnace of extracting aluminium directly from aluminium ore
JP2006283192A (en) * 2006-07-12 2006-10-19 Dowa Mining Co Ltd High-purity indium
CN1927701A (en) * 2006-09-29 2007-03-14 先导(清远)稀有金属化工有限公司 Producing device of high-purity selenium and producing process
DE102006056482A1 (en) * 2006-11-30 2008-06-05 Deutsche Solar Ag Apparatus and method for processing non-ferrous metals
CN101935767A (en) * 2010-09-26 2011-01-05 山西龙港高纯材料有限公司 Method for preparing high-purity arsenic
CN101956083A (en) * 2010-10-29 2011-01-26 曲智 Process method and equipment for smelting magnesium by using magnesite with one-step method

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107217145A (en) * 2016-12-09 2017-09-29 郴州万墨环保科技有限公司 A kind of method that copper anode mud vacuum reduction takes off lead antimony bismuth selen-tellurjum arsenic
CN109082542A (en) * 2018-02-24 2018-12-25 虔东稀土集团股份有限公司 A method of it preparing the vacuum drying oven of high pure metal ytterbium and its prepares high pure metal ytterbium
CN109082542B (en) * 2018-02-24 2019-05-07 虔东稀土集团股份有限公司 A method of it preparing the vacuum drying oven of high pure metal ytterbium and its prepares high pure metal ytterbium
CN113444893A (en) * 2020-03-27 2021-09-28 核工业理化工程研究院 Height-adjustable vacuum multilayer evaporation device and evaporation method
CN111979425A (en) * 2020-07-24 2020-11-24 广东先导稀材股份有限公司 Refining device for high-purity metal
CN113604667A (en) * 2021-07-26 2021-11-05 重庆赛迪热工环保工程技术有限公司 Multi-metal vapor vacuum step condensation method and system
CN114191835A (en) * 2021-12-28 2022-03-18 中国原子能科学研究院 Molecular distillation device and purification system for removing radioactive impurities in alloy
CN114191835B (en) * 2021-12-28 2022-12-13 中国原子能科学研究院 Molecular distillation device and purification system for removing radioactive impurities in alloy
CN115449648A (en) * 2022-08-30 2022-12-09 昆明理工大学 Calcined dolomite vacuum carbothermic reduction magnesium smelting equipment and method
WO2024045562A1 (en) * 2022-08-30 2024-03-07 昆明理工大学 Apparatus and method for magnesium production by means of vacuum carbothermic reduction of calcined dolomite

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Application publication date: 20121003