CN117512345A - Vacuum distillation furnace and method for preparing high-purity copper - Google Patents
Vacuum distillation furnace and method for preparing high-purity copper Download PDFInfo
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- CN117512345A CN117512345A CN202410002720.5A CN202410002720A CN117512345A CN 117512345 A CN117512345 A CN 117512345A CN 202410002720 A CN202410002720 A CN 202410002720A CN 117512345 A CN117512345 A CN 117512345A
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 65
- 239000010949 copper Substances 0.000 title claims abstract description 65
- 238000005292 vacuum distillation Methods 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000001704 evaporation Methods 0.000 claims abstract description 88
- 230000008020 evaporation Effects 0.000 claims abstract description 70
- 238000010438 heat treatment Methods 0.000 claims abstract description 58
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 51
- 239000011651 chromium Substances 0.000 claims abstract description 51
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000012535 impurity Substances 0.000 claims abstract description 40
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 238000009833 condensation Methods 0.000 claims abstract description 19
- 230000005494 condensation Effects 0.000 claims abstract description 19
- 239000002893 slag Substances 0.000 claims abstract description 6
- 230000007246 mechanism Effects 0.000 claims description 40
- 239000002245 particle Substances 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 230000008018 melting Effects 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 6
- 230000009467 reduction Effects 0.000 claims description 6
- 239000000956 alloy Substances 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 20
- 238000005265 energy consumption Methods 0.000 abstract description 9
- 238000009856 non-ferrous metallurgy Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 14
- 238000004821 distillation Methods 0.000 description 9
- 238000000926 separation method Methods 0.000 description 9
- 238000009835 boiling Methods 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 238000000746 purification Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 150000002739 metals Chemical class 0.000 description 4
- 229910001338 liquidmetal Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- 238000005204 segregation Methods 0.000 description 3
- 238000011282 treatment Methods 0.000 description 3
- 238000009423 ventilation Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000005349 anion exchange Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 238000004857 zone melting Methods 0.000 description 2
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000009749 continuous casting Methods 0.000 description 1
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000005674 electromagnetic induction Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
- C22B15/00—Obtaining copper
- C22B15/0026—Pyrometallurgy
- C22B15/006—Pyrometallurgy working up of molten copper, e.g. 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
- 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
Abstract
The invention belongs to the technical field of nonferrous metallurgy, and particularly discloses a vacuum distillation furnace and a method for preparing high-purity copper. The vacuum distillation furnace comprises an evaporation furnace, a condensing furnace and an air flue, wherein the upper part and the bottom part of the evaporation furnace body of the evaporation furnace are provided with a feed inlet and a slag discharge port, the evaporation furnace body is provided with a heating unit, and the top end of the evaporation furnace body is provided with a top cover; the top end of a condensing furnace body of the condensing furnace is provided with a vacuum tube, the upper part and/or the middle part of the condensing furnace body are/is provided with a plurality of chromium plates at intervals from top to bottom, and the condensing furnace body is sequentially provided with a side heating structure, a condensing plate and a condensing collecting plate at intervals below the bottom chromium plate; the top of the evaporation furnace body is provided with an air outlet, the condensation furnace body is provided with an air inlet above the top chromium plate, and the air passage is communicated with the air outlet of the evaporation furnace and the air inlet of the condensation furnace. The method comprises the steps of raw material heating, air passage control, steam impurity removal and high-purity copper collection. The invention has the characteristics of compact structure, low energy consumption, high rectification efficiency, good impurity removal effect and high purity of rectification products.
Description
Technical Field
The invention relates to the technical field of nonferrous metallurgy, in particular to a vacuum distillation furnace with compact structure, low energy consumption, high rectification efficiency, good impurity removal effect and high purity of a rectification product and a method for preparing high-purity copper.
Background
The high-purity copper is widely applied to the technical fields of tips such as electronics, communication, superconductivity, aerospace and the like with low resistivity and high electromagnetic property, and good effect is obtained.
At present, the high-purity copper technology mainly comprises methods of electrolytic refining, electron beam melting, directional solidification, anion exchange, zone melting and the like. Wherein, the electrolytic refining is effective for almost all impurities except oxygen, and has strict requirements on electrolyte; the electron beam melting is mainly effective for impurity elements with higher saturated vapor pressure than copper, such as Ag, se, te, S, bi, pb and the like, and has limited effect on other elements; the anion exchange method is to remove impurity ions in the copper solution by ion exchange, and then evaporate the solution to obtain high-purity CuCl 2 And the high-purity copper is obtained by reduction, the process flow is complex, and large-scale copper ingot blanks are difficult to produce in batches; zone melting main needleThe effect of impurities with the segregation coefficient far from 1 is obvious, the effect of removing impurities with the segregation coefficient close to 1 is limited, and the purification efficiency is low; the directional solidification is mainly used for copper continuous casting and single crystal preparation, but for metal and non-metal impurities with partial segregation coefficient close to 1, the purification needs to be carried out through multiple times of directional purification, the production cost can be obviously increased, and a large environmental protection pressure is caused.
Vacuum distillation is a common metallurgical method for smelting, refining, purifying and other treatments by mainly utilizing the boiling point difference and the saturation vapor pressure difference of different metals under the condition of reduced pressure. The existing vacuum distillation furnace is mostly in a single-hearth form, the metal at the bottom is heated, and the temperature difference of the area is controlled in the vertical direction to obtain liquid metals with different boiling points, because the liquid metals need to be distilled in a vacuum state, and cooling and furnace opening operations are needed during feeding and discharging, the liquid metals cannot continuously treat materials, the treatment efficiency is low, the energy consumption is high, the impurity elements with the boiling points close to copper are difficult to remove, and the purification effect is not obvious. Therefore, in the prior art, a chromium volatilization orifice plate is arranged between a condensing disc and an evaporating chamber of a furnace chamber, and through holes on the orifice plate, when high-temperature steam flows, the flow rate is increased due to the narrowing of a gas channel, so that the mist release amount per unit time is increased to reduce the particle size of particles; meanwhile, the chromium pore plate and Fe, si, mn, al, cl and other impurity elements are subjected to chemical reaction at high temperature, and the reaction product is adsorbed on the pore plate to remove impurities so as to improve the purity, but the problems of low treatment efficiency and high energy consumption, which are caused by incapability of continuously treating materials, still exist.
Aiming at the problem that a single-hearth vacuum distillation furnace cannot realize large-batch metal distillation, in the prior art, a horizontal structure is adopted to connect a distillation chamber and a condensation chamber side by side to form a double-hearth structure, graphite electrodes are arranged in the distillation chamber and the condensation chamber for heating, then a steam channel is arranged between the distillation chamber and the condensation chamber, and a ceramic mesh plate is arranged in the steam channel, so that a certain temperature gradient is formed in the steam channel to improve the purity of a product; however, the graphite electrode heating limits the application range because the materials in a molten state can only be added and taken out, and the high-temperature steam is condensed only through the condensing wall in the condensing chamber, so that the condensing efficiency is low, and the separation of various metals cannot be realized. Therefore, in the prior art, the evaporation furnace and the condensing furnace are separated to form a double-hearth structure, and the middle parts of the evaporation furnace and the condensing furnace are connected through the air passages with different forms, so that the energy consumption can be reduced, and the air passages with different structural forms can also shunt substances with different boiling points, thereby realizing high-efficiency separation and rectification; the condensing furnace adopts a multi-stage condensing chamber design at the upper part of the side heating so as to enlarge the temperature gradient change, thereby different metals can be condensed and collected in the corresponding condensing chamber so as to realize the separation, collection and purification of various metals. However, because the structure of the air passage is fixed, the air passage with a corresponding structure can be selected for installation and use only before the furnace is opened, and the opening size of the air passage can not be flexibly adjusted and the closing can not be realized according to the requirements in the vacuum distillation process, so that the dynamic high-efficiency distillation can not be realized, the air passage can not be closed, and the evaporation furnace and the condensing furnace are difficult to thoroughly isolate, so that the real continuous high-temperature distillation can not be realized; and the fixed structure of the air passage makes it necessary to prepare a plurality of air passages, which increases the cost and the management difficulty. In addition, because the air flue communicates the middle part of evaporating furnace and condensing furnace for the high temperature steam in the evaporating furnace not only needs guide structure and extra heating structure just can flow into the passageway, and steam still gathers in the evaporating furnace top in a large number easily moreover, thereby has increased the complexity of structure and has caused the energy consumption to increase.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the vacuum distillation furnace with compact structure, low energy consumption, high rectification efficiency, good impurity removal effect and high purity of rectification products, and also provides a method for preparing high-purity copper based on the vacuum distillation furnace.
The vacuum distillation furnace is realized by the following steps: the evaporator comprises an evaporator body, a condensing furnace and an air flue, wherein the evaporator body comprises an evaporator body, a feeding hole and a slag discharging hole which can be communicated with the inside and the outside are respectively arranged at the upper part and the bottom of the evaporator body, a heating unit is arranged at the side part, the upper part and/or the bottom of the evaporator body, and a top cover is detachably arranged at the top end of the evaporator body;
the condensing furnace comprises a condensing furnace body, a vacuum tube communicated with a vacuum system is arranged at the top end of the condensing furnace body, a plurality of transverse chromium plates are arranged at intervals from top to bottom at the upper part and/or the middle part of the condensing furnace body, and a side heating structure, a condensing plate and a condensing collecting plate are sequentially arranged below the bottom chromium plate at intervals;
the top of the evaporation furnace body is provided with an air outlet, the condensation furnace body is provided with an air inlet above the top chromium plate, and the air passage is communicated with the air outlet of the evaporation furnace and the air inlet of the condensation furnace.
Further, an opening and closing mechanism capable of controlling opening and closing is further arranged in the air passage, and a baffle plate which inclines in the condensing furnace body and extends upwards is further arranged in the air inlet of the condensing furnace body.
Further, the bottom and the side parts of the baffle are sealed with the inner wall of the condensing furnace body, and an opening with the sectional area smaller than the sectional area of the air passage is reserved between the top end of the baffle and the top wall of the condensing furnace body.
Further, the opening and closing mechanism is a double door type rotary structure with left and right halves, and the opening and closing mechanism rotates to open and close to one side of the condensing furnace.
Further, each chromium plate in the condensing furnace body is arranged in a staggered way from top to bottom, and a plurality of through holes are formed in the chromium plate at intervals.
Furthermore, at least two layers of condensing plates are alternately arranged below the side heating structure in the condensing furnace body from top to bottom, and a condensing system is arranged on the outer wall of the condensing plate in the condensing furnace body.
Furthermore, the top ends of all the chromium plates in the condensing furnace body do not exceed the furnace chamber central line of the condensing furnace body, and the top ends of all the condensing plates in the condensing furnace body exceed the furnace chamber central line of the condensing furnace body.
The method for preparing high-purity copper based on the vacuum distillation furnace is realized by the following steps: the method comprises the steps of raw material heating, air passage control, steam impurity removal and high-purity copper collection, and comprises the following specific contents:
A. heating raw materials: adding copper raw materials into an evaporation furnace through a charging hole, then opening an opening and closing mechanism to communicate the evaporation furnace with a condensing furnace, controlling a vacuum system to carry out integral vacuumizing through a vacuum tube, opening a heating unit to heat the copper raw materials after the integral vacuumizing is finished, and controlling the temperature rising rate to melt the copper raw materials;
B. airway control: in the process of melting and heating the copper raw material, closing the opening and closing mechanism to isolate the evaporation furnace from the condensing furnace, continuously controlling the vacuum system to vacuumize the condensing furnace to a preset vacuum degree, stopping, and then adjusting the opening width of the opening and closing mechanism according to the requirement after steam starts to be generated in the evaporation furnace to enable the steam in the evaporation furnace to flow into the condensing furnace;
C. removing impurities by steam: introducing steam into a condensing furnace and sinking along with the temperature reduction, wherein the steam contacts a chromium plate in the sinking process, impurity elements in the steam react with chromium at high temperature chemically to be condensed on the upper surface of the chromium plate, and continuously sinking steam is heated for the second time when reaching a side heating structure, and the steam part is evaporated upwards and condensed on the lower surface of the chromium plate;
D. collecting high-purity copper: after the time of chemical reaction and secondary heating of the steam in the condensing furnace reaches the preset duration, the side heating structure is closed, the steam is continuously cooled and sunk, most of the steam is condensed on the condensing plate to obtain high-purity copper powder, and the rest of gas is condensed on the condensing collecting plate to obtain high-purity copper particles.
Further, the copper raw material is electrolytic cathode copper, copper-rich alloy, copper-rich secondary resource and/or regenerated copper, the vacuum degree in the evaporation furnace and/or the condensing furnace is 0.1-100 Pa, the vacuum distillation temperature in the evaporation furnace is 1100-1800 ℃, the vacuum distillation time is 0.5-3 h, and the vacuum distillation heating rate is 5-20 ℃/min.
Further, in the steam impurity removal step, after the time of introducing the steam into the condensing furnace reaches a preset time, the opening and closing mechanism is closed to enable the steam in the condensing furnace to independently finish impurity removal and condensation until the time reaches the preset time; or continuously opening the opening and closing mechanism to enable the steam generated by the evaporation furnace to continuously enter the condensing furnace and remove impurities and collect high-purity copper.
The beneficial effects of the invention are as follows:
1. according to the invention, the air outlet at the top of the evaporation furnace is communicated with the air inlet above the chromium plate at the top layer of the condensing furnace through the air passage, so that high-temperature steam generated by the evaporation furnace flows along with gravity and naturally flows into the condensing furnace, the high-temperature steam is prevented from being accumulated at the top end of the evaporation furnace, a heating guide structure for steam flow can be reduced or even eliminated, the energy consumption is reduced, and the structure is simplified; and the top of the evaporation furnace and the top of the condensing furnace are communicated by the air passage, so that the temperature gradient required by vapor separation, reaction and condensation can be formed. Meanwhile, the vacuum system at the upper part of the condensing furnace can control the steam pressure to form a pressure gradient, and the heating unit of the evaporating furnace and the side heating structure of the condensing furnace are combined to form a system with controllable temperature gradient and pressure gradient, so that the reaction path of steam flow is controlled together, and the rectification efficiency and the purity of rectification products can be effectively improved.
2. According to the difference that the melting point of copper is 1083 ℃ and the melting point of chromium is 1907 ℃, and by utilizing the characteristic that impurity elements Al, cd, bi, ga, K, mg, zn, pb, ga, fe, ni, si, au, cl and the like in high-temperature steam can chemically react with chromium at high temperature in the volatilization process (according to the relationship of saturated vapor pressure, most of the impurity elements are in a gaseous state in a given distillation temperature range and have larger activation energy, and can chemically react with chromium at high temperature); by arranging the multi-layer chromium plate structure in the condensing furnace, high-temperature steam can smoothly pass through, the contact area can be increased and the temperature gradient can be improved by the multi-layer structure, so that impurity elements fully react with the chromium plate for many times and are condensed on the upper surface of the chromium plate, and the separation of the impurity elements and copper is realized; meanwhile, the side heating structure is arranged below the bottom chromium plate, so that the reaction capacity of impurity elements can be enhanced by improving the steam temperature of the lower chromium plate, the phenomenon that the impurity elements react inadequately and are brought into a final distillation product due to the fact that the temperature is too low is avoided, and when the steam in the condensing furnace is reduced to the side heating structure along with the temperature reduction, the steam is heated to the required temperature by the side heating structure and is partially transpired upwards and partially condensed on the lower surface of the chromium plate, so that the separation effect is further improved.
3. According to the invention, the upward inclined baffle is arranged in the air inlet of the condensing furnace body, so that the baffle and the top of the condensing furnace body form a necking ventilation channel to form a Laval nozzle effect, the volume of gas flowing through the baffle is reduced, the pressure is increased, and the gas is compressed and released, so that when volatile matters pass through the necking ventilation channel, high-boiling matters are condensed and separated, and flow back to the evaporating furnace under the guidance of the inclined baffle, the separation effect of volatile matters collected in the condensing furnace and residues of the evaporating furnace is better, and the baffle structure can achieve the effect of controlling the rectification time and the reflux speed by controlling the opening size and the length of the air channel.
4. The invention sets up the opening and closing mechanism that can rotate left and right in the air flue: when the opening and closing mechanism is closed, the evaporating furnace and the condensing furnace can be made into two independent operation spaces, so that the evaporating temperature gradient and the pressure gradient can be stably controlled, the feeding of the evaporating furnace can be realized, and the vacuum degree of the condensing furnace is not influenced so as to realize continuous high-temperature distillation; when the opening and closing mechanism is opened, the evaporating furnace and the condensing furnace are communicated to form a steam channel. When the opening and closing mechanism is completely opened, the air passage is a common parallel air passage, and when one quarter of the air passage is opened left and right, namely the middle opening air passage is half of the air passage, a narrow throat structure with large front and rear openings and contracted middle can be formed; the evaporation furnace disclosed by the invention has the advantages that the high-temperature steam exists and forms air pressure difference with the condensing furnace, the steam flows to the condensing furnace from the evaporation furnace through the air passage, the steam can be compressed at the narrow throat to form high-speed compressed gas, and the high-speed compressed gas is rapidly expanded to form higher-flow-rate gas after passing through the narrow throat, so that a Laval nozzle effect is formed, the rapid cooling and cooling of the volatile matters in the condensing furnace are realized, the pressure difference of the evaporation furnace at the narrow throat of the air passage is improved, and the outflow speed of the steam is accelerated; meanwhile, the left and right opening and closing structures enable two sides of the narrow throat to be of slope structures, gas reaches maximum pressure at the narrow throat and is compressed and released heat, so that high-boiling-point substances are facilitated to be condensed and separated and flow back to the evaporation furnace, low-boiling-point substances flow to the condensation furnace quickly through the narrow throat to achieve a shunting effect, and finally the effect of dynamic efficient rectification is formed. And the opening and closing mechanism increases the pressure difference between the evaporating furnace and the condensing furnace, so that high-boiling-point substances in the evaporating furnace are not easy to volatilize, and low-boiling-point substances quickly condense in the condensing furnace after passing through the air passage, thereby realizing more accurate and effective separation of alloy materials with smaller boiling point differences.
5. According to the invention, the opening and closing mechanism and the baffle are arranged in the air passage at the same time, when one fourth of the opening and closing mechanism is opened up and down, the two-stage Laval nozzle effect can be formed by the opening and closing mechanism and the baffle structure, and the dynamic efficient rectifying effect is further improved.
6. According to the invention, the condensing plate and the condensing collecting plate are sequentially arranged below the side heating structure of the condensing furnace, and the condensing system is further arranged on the side wall of the condensing furnace where the condensing plate is positioned, so that the temperature of the high-temperature steam can be quickly reduced after the high-temperature steam fully reacts with the chromium plate, copper steam is quickly condensed into copper powder particles and is mostly condensed on the condensing plate, and the rest of the copper steam is condensed on the condensing collecting plate to obtain high-purity copper powder and particles, so that the condensing efficiency is improved, the mutual fusion of copper melt particles in the steam can be reduced, and the particle size of the copper powder is effectively reduced.
In conclusion, the invention has the characteristics of compact structure, low energy consumption, high rectification efficiency, good impurity removal effect and high purity of rectification products.
Drawings
FIG. 1 is a schematic view of a vacuum distillation furnace according to the present invention;
FIG. 2 is a cross-sectional view taken along A-A of FIG. 1;
FIG. 3 is a B-B cross-sectional view of FIG. 1;
FIG. 4 is a schematic diagram of the connection between the evaporator and the condenser of the present invention;
FIG. 5 is a second schematic diagram of the connection between the evaporator and the condenser of the present invention;
in the figure: the device comprises a 1-evaporation furnace, a 11-evaporation furnace body, a 12-charging hole, a 13-slag discharging hole, a 14-top cover, a 15-charging hole end cover, a 16-slag discharging hole end cover, a 2-condensing furnace, a 21-condensing furnace body, a 22-vacuum tube, a 23-chromium plate, a 24-side heating structure, a 25-condensing plate, a 26-condensing collecting plate, a 27-condensing system, a 3-air passage, a 31-opening and closing mechanism, a 32-baffle plate, a 33-opening, a 4-furnace shell and 5-refractory bricks.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
As shown in fig. 1, 2 and 3, the vacuum distillation furnace comprises an evaporation furnace 1, a condensation furnace 2 and an air flue 3, wherein the evaporation furnace 1 comprises an evaporation furnace body 11, a charging port 12 and a slag discharging port 13 which can be communicated with the inside and the outside are respectively arranged at the upper part and the bottom of the evaporation furnace body 11, a heating unit is arranged at the side part, the upper part and/or the bottom of the evaporation furnace body 11, and a top cover 14 is detachably arranged at the top end of the evaporation furnace body 11;
the condensing furnace 2 comprises a condensing furnace body 21, a vacuum tube 22 communicated with a vacuum system is arranged at the top end of the condensing furnace body 21, a plurality of transverse chromium plates 23 are arranged at intervals from top to bottom at the upper part and/or the middle part of the condensing furnace body 21, and a side heating structure 24, a condensing plate 25 and a condensing collecting plate 26 are sequentially arranged below the bottom chromium plate 23 at intervals of the condensing furnace body 21;
the top of the evaporation furnace body 11 is provided with an air outlet, the condensation furnace body 21 is provided with an air inlet above the top chromium plate 23, and the air channel 3 is communicated with the air outlet of the evaporation furnace 1 and the air inlet of the condensation furnace 2.
The air flue 3 is also internally provided with an opening and closing mechanism 31 capable of controlling opening and closing, and the air inlet of the condensing furnace body 21 is internally provided with a baffle plate 32 which inclines towards the inside of the condensing furnace body 21 and extends upwards.
The bottom and the side parts of the baffle plate 32 are sealed with the inner wall of the condensing furnace body 21, and an opening 33 with the sectional area smaller than the sectional area of the air passage 3 is reserved between the top end of the baffle plate 32 and the top wall of the condensing furnace body 21.
The opening and closing mechanism 31 is a two-door type rotary structure with left and right halves, and the opening and closing mechanism 31 is rotated to open and close to one side of the condensing furnace 2.
Each chromium plate 23 in the condensing furnace body 21 is staggered from top to bottom, and a plurality of through holes are formed in the chromium plates 23 at intervals.
At least two layers of condensing plates 25 are alternately arranged below the side heating structure 24 in the condensing furnace body 21 from top to bottom, and a condensing system 27 is arranged on the outer wall of the condensing plate 25 in the condensing furnace body 21.
The lower part of the condensing furnace body 21 is provided with a condensing cavity with transverse dimensions larger than the middle part and the upper part of the condensing furnace body 21, the side heating structure 24 is arranged at the top end of the condensing cavity, the condensing plate 25 is arranged in the cooling cavity, the condensing system 27 is arranged on the side wall of the condensing cavity, and the condensing collecting plate 26 is arranged at the bottom end of the cooling cavity.
The top ends of the chromium plates 23 in the condensing furnace body 21 do not exceed the furnace chamber central line of the condensing furnace body 21, and the top ends of the condensing plates 25 in the condensing furnace body 21 exceed the furnace chamber central line of the condensing furnace body 21.
The heating unit is an electromagnetic induction heating body or a resistance wire arranged on the side part of the evaporation furnace body 11.
As shown in fig. 4 and 5, the condensing furnace 2 communicates with one or more evaporating furnaces 1 through a gas passage 3.
As shown in fig. 1, 2 and 3, the method for preparing high-purity copper based on a vacuum distillation furnace comprises the steps of raw material heating, air passage control, steam impurity removal and high-purity copper collection, and comprises the following specific contents:
A. heating raw materials: adding copper raw materials into the evaporation furnace 1 through a charging hole 12, then opening an opening and closing mechanism 31 to communicate the evaporation furnace 1 with a condensing furnace 2, controlling a vacuum system to carry out integral vacuumizing through a vacuum tube 22, and opening a heating unit to heat the copper raw materials after the integral vacuumizing is finished, and controlling the temperature rising rate to melt the copper raw materials;
B. airway control: in the process of melting and heating the copper raw material, closing the opening and closing mechanism 31 to isolate the evaporation furnace 1 from the condensing furnace 2, continuously controlling the vacuum system to vacuumize the condensing furnace 2 to a preset vacuum degree, stopping, and then after starting to generate steam in the evaporation furnace 1, adjusting the opening width of the opening and closing mechanism 31 according to the requirement to enable the steam in the evaporation furnace 1 to flow into the condensing furnace 2;
C. removing impurities by steam: the steam is introduced into the condensing furnace 2 and is sunk along with the temperature reduction, the steam contacts the chromium plate 23 in the sinking process, the impurity elements in the steam are chemically reacted with chromium at high temperature to be condensed on the upper surface of the chromium plate 23, the steam which is continuously sunk is heated for the second time when reaching the side heating structure 24, and the steam part is evaporated upwards and is condensed on the lower surface of the chromium plate 23;
D. collecting high-purity copper: after the chemical reaction and secondary heating time of the steam in the condensing furnace 2 reaches the preset duration, the side heating structure 24 is closed, the steam is continuously cooled and sunk, most of the steam is condensed on the condensing plate 25 to obtain high-purity copper powder, and the rest of the gas is condensed on the condensing collecting plate 26 to obtain high-purity copper particles.
The copper raw material is electrolytic cathode copper, copper-rich alloy, copper-rich secondary resource and/or regenerated copper, the vacuum degree in the evaporation furnace 1 and/or the condensing furnace 2 is 0.1-100 Pa, the vacuum distillation temperature in the evaporation furnace 1 is 1100-1800 ℃, the vacuum distillation time is 0.5-3 h, and the vacuum distillation heating rate is 5-20 ℃/min.
In the steps of airway control, steam impurity removal and high-purity copper collection, the vacuum degree value in the condensing furnace 2 is smaller than the vacuum degree value in the evaporating furnace 1; preferably, the vacuum degree in the condensing furnace 2 is 0.1 to 60Pa, and the vacuum degree in the evaporating furnace 1 is 10 to 100Pa.
In the steam impurity removal step, after the time of introducing the steam into the condensing furnace 2 reaches a preset time period, the opening and closing mechanism 31 is closed to independently finish impurity removal and condensation of the steam in the condensing furnace 2 until the preset time period is reached; or continuously opening the opening and closing mechanism 31 to enable the steam generated by the evaporation furnace 1 to continuously enter the condensing furnace 2 and remove impurities and collect high-purity copper.
In the high purity copper collection step, the side heating structure 24 is turned off while the condensing system 27 on the side wall is turned on.
The grain diameter of the high-purity copper particles is 1-100 mu m.
Example 1
As shown in fig. 1, 2 and 3, the electrolytic cathode copper is subjected to vacuum distillation by using the vacuum distillation furnace of the present invention to prepare high-purity copper particles, and the specific process is as follows:
s100: the electrolytic cathode copper is added into the evaporation furnace 1 through the feed inlet 12, then the opening and closing mechanism 31 is opened to communicate the evaporation furnace 1 with the condensing furnace 2, the vacuum system is controlled to be vacuumized to 50Pa wholly through the vacuum tube 22, the heating unit is opened to heat the electrolytic cathode copper after the completion, the heating rate is controlled to be 5-20 ℃/min, and the temperature is raised to 1100-1800 ℃ to melt the electrolytic cathode copper.
S200: in the process of melting and heating electrolytic cathode copper in the evaporation furnace 1, the opening and closing mechanism 31 in the air passage 3 is closed to isolate the evaporation furnace 1 from the condensing furnace 2, then the vacuum system is continuously controlled to vacuumize the condensing furnace 2 to 10Pa, then the vacuum system is stopped, and after the evaporation furnace 1 starts to generate steam, the opening width of the opening and closing mechanism 31 is adjusted according to the requirement, so that the steam in the evaporation furnace 1 flows into the condensing furnace 2. The opening and closing mechanism 31 and the top of the evaporation furnace 1 form a necking-shaped ventilation channel, a Laval nozzle effect can be formed, the volume of steam flowing into the opening and closing mechanism is reduced, the pressure is increased, when volatile matters pass through the air channel 3, the gas reaches the maximum pressure at the narrow throat, the gas is compressed and releases heat, high-boiling matters are condensed and separated and flow back to the evaporation furnace 1, and the separation effect of the volatile matters collected in the condensation chamber and residues in the evaporation chamber is better. The gas then enters the condensing furnace 2 and after a period of steam passes, the opening and closing mechanism 31 may be closed to achieve optimal control of the gas. The opening and closing mechanism 31 may be opened so that high-temperature steam can be continuously treated.
S300: the steam is introduced into the condensing furnace 2 and sinks along with the temperature reduction, the steam contacts the chromium plate 23 in the sinking process, impurity elements such as Fe, si, mn, al, cl and Si, S, O, N, C in the steam react with chromium at high temperature to be condensed on the upper surface of the chromium plate 23, the steam which continues to sink reaches the side heating structure 24 and heats up again, and part of the steam is transpired upwards and partially condensed on the lower surface of the chromium plate 23.
S400: after the chemical reaction and secondary heating time of the steam in the condensing furnace 2 reaches the preset time, the side heating structure 24 is closed, and meanwhile, the condensing system 27 on the side wall of the condensing furnace 2 is opened, so that the steam is quickly cooled and sunk, most of the steam is condensed on the condensing plate 25 to obtain high-purity copper powder, and the rest of the steam is condensed on the condensing collecting plate 26 to obtain high-purity copper particles.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions easily contemplated by those skilled in the art within the technical scope of the present invention should be included in the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.
Claims (10)
1. The utility model provides a vacuum distillation stove, includes evaporation furnace (1), condensing furnace (2), air flue (3), evaporation furnace (1) is including evaporation furnace body (11), upper portion and the bottom of evaporation furnace body (11) set up respectively can communicate inside and outside charge door (12), slag discharging mouth (13), the lateral part, upper portion and/or the bottom of evaporation furnace body (11) are provided with heating unit, top detachable of evaporation furnace body (11) is provided with top cap (14);
the condensing furnace is characterized in that the condensing furnace (2) comprises a condensing furnace body (21), a vacuum tube (22) communicated with a vacuum system is arranged at the top end of the condensing furnace body (21), a plurality of transverse chromium plates (23) are arranged at intervals from top to bottom at the upper part and/or the middle part of the condensing furnace body (21), and a side heating structure (24), a condensing plate (25) and a condensing collecting plate (26) are sequentially arranged below the bottom chromium plate (23) at intervals in the condensing furnace body (21);
the top of evaporation furnace body (11) is provided with the gas outlet, condensation furnace body (21) is provided with the air inlet in top chromium board (23), air flue (3) intercommunication evaporation furnace (1) gas outlet and condensation furnace (2) air inlet.
2. Vacuum distillation furnace according to claim 1, characterized in that an opening and closing mechanism (31) capable of controlling opening and closing is further arranged in the air passage (3), and a baffle plate (32) which is inclined towards the inside of the condensing furnace body (21) and extends upwards is further arranged in the air inlet of the condensing furnace body (21).
3. Vacuum distillation furnace according to claim 2, characterized in that the bottom and sides of the baffle plate (32) are sealed with the inner wall of the condensing furnace body (21), and an opening (33) with a cross-sectional area smaller than the cross-sectional area of the air passage (3) is left between the top end of the baffle plate (32) and the top wall of the condensing furnace body (21).
4. The vacuum distillation furnace according to claim 2, wherein the opening and closing mechanism (31) is a double door type rotary structure of left and right halves, and the opening and closing mechanism (31) is rotated to open and close to one side of the condensing furnace (2).
5. Vacuum distillation furnace according to claim 2, 3 or 4, characterized in that the chromium plates (23) in the condensing furnace body (21) are staggered from top to bottom, and a plurality of through holes are arranged on the chromium plates (23) at intervals.
6. Vacuum distillation furnace according to claim 5, characterized in that at least two layers of condensing plates (25) are alternately arranged below the side heating structure (24) in the condensing furnace body (21), and the condensing system (27) is arranged on the outer wall of the condensing plate (25) of the condensing furnace body (21).
7. The vacuum distillation furnace according to claim 6, wherein the top ends of the chromium plates (23) in the condensing furnace body (21) do not exceed the furnace chamber center line of the condensing furnace body (21), and the top ends of the condensing plates (25) in the condensing furnace body (21) exceed the furnace chamber center line of the condensing furnace body (21).
8. A method for preparing high-purity copper based on the vacuum distillation furnace of any one of claims 2 to 7, which is characterized by comprising the steps of raw material heating, air passage control, steam impurity removal and high-purity copper collection, and comprises the following specific contents:
A. heating raw materials: adding copper raw materials into an evaporation furnace (1) through a feed port (12), then opening an opening and closing mechanism (31) to communicate the evaporation furnace (1) with a condensing furnace (2), controlling a vacuum system to carry out integral vacuumizing through a vacuum tube (22), opening a heating unit to heat the copper raw materials after the integral vacuumizing is completed, and controlling the temperature rising rate to melt the copper raw materials;
B. airway control: in the process of melting and heating copper raw materials, the opening and closing mechanism (31) is closed to isolate the evaporation furnace (1) from the condensing furnace (2), then the vacuum system is continuously controlled to vacuumize the condensing furnace (2) to a preset vacuum degree, then the vacuum system is stopped, after steam starts to be generated in the evaporation furnace (1), the opening width of the opening and closing mechanism (31) is adjusted according to the requirement, and the steam in the evaporation furnace (1) flows into the condensing furnace (2);
C. removing impurities by steam: introducing steam into a condensing furnace (2) and sinking along with the temperature reduction, wherein the steam contacts a chromium plate (23) in the sinking process, impurity elements in the steam react with chromium at high temperature chemically to be condensed on the upper surface of the chromium plate (23), continuously sinking steam reaches a side heating structure (24) and heats up again, and a steam part is evaporated upwards and is condensed on the lower surface of the chromium plate (23);
D. collecting high-purity copper: after the time of chemical reaction and secondary heating of the steam in the condensing furnace (2) reaches a preset duration, the side heating structure (24) is closed, the steam is continuously cooled and sunk, most of the steam is condensed on the condensing plate (25) to obtain high-purity copper powder, and the rest of the gas is condensed on the condensing collecting plate (26) to obtain high-purity copper particles.
9. The method for preparing high-purity copper by using the vacuum distillation furnace according to claim 8, wherein the copper raw material is electrolytic cathode copper, copper-rich alloy, copper-rich secondary resource and/or reclaimed copper, the vacuum degree in the evaporation furnace (1) and/or the condensation furnace (2) is 0.1-100 Pa, the vacuum distillation temperature in the evaporation furnace (1) is 1100-1800 ℃, the vacuum distillation time is 0.5-3 h, and the vacuum distillation heating rate is 5-20 ℃/min.
10. The method for preparing high-purity copper by using the vacuum distillation furnace according to claim 8 or 9, wherein in the steam impurity removal step, after the time of introducing steam into the condensing furnace (2) reaches a preset time period, the opening and closing mechanism (31) is closed to enable the steam in the condensing furnace (2) to independently complete impurity removal and condensation until the preset time period is reached; or continuously opening the opening and closing mechanism (31) to enable the steam generated by the evaporation furnace (1) to continuously enter the condensing furnace (2) and remove impurities and collect high-purity copper.
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