CN211311551U - Electric heating aluminum smelting device - Google Patents
Electric heating aluminum smelting device Download PDFInfo
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- CN211311551U CN211311551U CN201921541678.5U CN201921541678U CN211311551U CN 211311551 U CN211311551 U CN 211311551U CN 201921541678 U CN201921541678 U CN 201921541678U CN 211311551 U CN211311551 U CN 211311551U
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Abstract
The utility model belongs to the field of materials science, a device of electric heat aluminium smelting is related to, including following part: at least one aluminum-magnesium centrifugal separator, wherein the aluminum-magnesium centrifugal separator receives alloy liquid containing iron-containing aluminum alloy and metal magnesium which are melted into four elements of aluminum, magnesium, silicon and iron, the alloy liquid is separated into aluminum-magnesium alloy liquid and separated solid-phase metal compounds after centrifugal treatment, and the aluminum-magnesium alloy liquid is cooled to generate aluminum-magnesium alloy blocks; and the aluminum-magnesium continuous distillation separation furnace receives the aluminum-magnesium alloy blocks produced by the aluminum-magnesium centrifugal separator, re-melts and distills the aluminum-magnesium alloy blocks to separate the aluminum liquid and magnesium vapor, and the magnesium vapor is condensed to generate condensed magnesium. The utility model discloses a metal magnesium adopts the physical method to separate out aluminium, silicon and iron as the extractant, realizes melting each other aluminium and magnesium, gets rid of out alloy liquid with iron, silicon, then the aluminium-magnesium carries out the distillation separation.
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Technical Field
The utility model belongs to the field of materials science, a device of purification aluminium is related to, concretely relates to device of electric heat aluminum smelting.
Background
Aluminum is an important metal, widely used, and second only to steel. At present, all the metallic aluminum all over the world is produced by adopting an electrolytic aluminum process. However, there are several important and difficult drawbacks to the electrolytic aluminum process. This has led to a constant search for electrically heated aluminium production processes to replace electrolytic aluminium. Electrothermal aluminum production has advantages over electrolytic aluminum in several ways, at least the potential advantages that are expected: (1) the first is the difference in mineral origin: about 250 more of the minerals containing aluminum, 100 of which, i.e., 40%, are silicates, i.e., in most cases, the aluminum-containing minerals are aluminosilicates. The electric heating method can use the aluminum-silicon ore and is very wide in the nature. The electrolytic aluminum needs aluminum-containing minerals with extremely high purity, namely bauxite with high aluminum-silicon ratio, such as minerals with the aluminum-silicon ratio of 5-12, the suitable minerals are extremely limited, and the common gibbsite, diaspore, boehmite and the like are limited, so the spatial distribution of the mineral resources suitable for the electrolytic aluminum is uneven. The global crude aluminum yield is about 6000-7000 million tons per year, wherein about 51-55%, namely about 3600 million tons are produced in China, and the bauxite resource in China only accounts for 2.7% of the world. If China does not import bauxite or alumina, the high-quality bauxite suitable for electrolytic aluminum in China will be depleted in 7 years. The global bauxite mineralization zone is mainly distributed in africa, oceania, south america and south east asia. From the national distribution, bauxite is mainly distributed in Guinea, Australia, Brazil, jamaica, Vietnam, Indonesia and other countries. Imported bauxite is almost always required in major primary aluminum producing countries in the world, such as china, north america, europe, etc. That is, the major industrial countries in the world, most of the east asia, western europe, eastern europe of the former soviet union, north america, etc., located at the higher latitudes of the northern hemisphere, lack bauxite suitable for electrolytic aluminum. (2) Secondly, the pollution emission in the production process: the whole process of electrolytic aluminum production is seriously polluted. The electrolytic aluminum production process is firstly the production of alumina and secondly the electrolysis process. The two major links generate a large amount of red mud, fluoride smoke dust, fluoride gas, cyanide and other multiple pollutions caused by cathode overhaul slag, and some pollutants are extremely toxic and cause serious harm to the ecological environment and human health. The electric heating method is adopted to produce aluminum, pollution which is difficult to control is almost avoided, and oxide dust in the ore smelting furnace has no chemical toxicity and can be easily controlled. The whole production process has no treatment circulation of acid-base waste liquid, and the whole environmental protection level is much better. (3) The third is the difference in energy consumption level: in the whole process of the existing aluminum electrolysis, the process power consumption of the electrolysis link is approximately at the energy consumption level of 13000kwh per ton of aluminum, but about 1.92 tons of aluminum oxide are needed per ton of aluminum, and the energy consumption of the aluminum oxide preparation link is about 20-60GJ in terms of the energy consumption per ton of aluminum. If an electrothermal method is adopted to obtain the aluminum-silicon alloy, the energy consumption of each ton of alloy is mainly the process power consumption, under the condition of comprehensive recovery, only 12000kwh is needed approximately, and not too much energy consumption in the raw material preparation process is needed, or the energy consumption in the raw material preparation link is far lower than that in the alumina link. (4) The difference of the productivity of the equipment is large: the electric heating aluminum smelting has compact equipment, the power and the productivity of single equipment are much larger, the voltage reaches hundreds of volts, and the voltage of an electrolytic bath is only single digit. The quantity of aluminium produced by each large electrolytic cell is only hundreds of tons per year, and the aluminium smelting by the large submerged arc furnace electric heating method can reach ten thousand tons. This is because, on the one hand, the electrolysis reaction is carried out only in a plane, whereas the electrothermal process is carried out in the entire volume. Also the overall energy efficiency of the electrolysis process is not high, whereas the electric heating law is much higher. From the perspective of the reactor, an aluminum electrolysis plant often has hundreds of electrolytic cells connected in series for operation, and the requirements for power stability, operation management and maintenance are much higher. The electric heating method has the advantages of large reactor capacity, less required equipment and much more flexible production management. (5) Adaptability to use of renewable energy sources: electrolytic aluminum can only use the electricity produced by traditional fossil energy sources. In the production process of electrolytic aluminum, the electrochemical reaction of an electrolytic cell must be continuously carried out, once power failure occurs, serious production accidents of the electrolytic cell can be caused, production is stopped, and the electrolytic cell needs to be thoroughly repaired again for recovery, so that the cost is high, and the construction period of months is delayed. Therefore, the electrolytic aluminum can not be used as renewable energy sources such as wind power, photovoltaic, photo-thermal, water and electricity and the like as a power consumer to prevent power supply fluctuation, and only can use the power generated by traditional fossil energy sources such as coal, gas, fuel oil and the like, so that the global carbon emission reduction effort cannot be implemented in the electrolytic aluminum industry. (6) The treatment of silicon element utilizes: in nature, aluminum and silicon minerals are combined together, and in the two-step process of electrolytic aluminum smelting, aluminum-silicon oxides are forcibly separated under the action of an aqueous solution, then a large amount of heat energy is consumed to dry water in aluminum oxide, and the aluminum oxide is sent into an electrolytic cell to obtain electrolytic aluminum. However, about 70% of the final applications of the electrolytic aluminum require subsequent re-distribution of industrial silicon as an alloying element, which results in huge waste. Particularly, as high-grade bauxite is gradually consumed, more bauxite with lower aluminum-silicon ratio, such as 3-6 aluminum-silicon ratio, needs more silicon oxide to be removed, and therefore, the process is complicated and the cost is increased. The electrothermal method directly reduces aluminum and silicon into alloy, does not need to consume great strength to separate the aluminum and the silicon in an oxide state, does not need to dry moisture, and does not need to be specially added with industrial silicon in the later stage to improve the silicon content. Obviously, the electric heating method is more reasonable in the aspect of treating the associated silicon element. (7) The electric heating method has great cost advantage: the production cost of electrolytic aluminum is high. In the production cost of the electrolytic aluminum, the electric energy accounts for about 40%, and what is more important is the purchase cost of the aluminum oxide, wherein the aluminum oxide consumption per ton of the electrolytic aluminum is generally 1.92 tons, and the purchase cost of the aluminum oxide accounts for 40% of the selling price of the electrolytic aluminum, so that the cost of the electrolytic aluminum is high. And the cost of the electrothermal method is reduced by about 30 percent compared with the ton aluminum cost of the electrolytic method when a plant is built under the same condition.
With the increasing global aluminum consumption, the social inventory of metal aluminum and aluminum alloy is also increasing, which means that the recycled waste aluminum accumulated in the industrial process will become the main source of metal aluminum in the future, that is, the recycled aluminum replaces the original aluminum and becomes the main source of aluminum. But the recovered waste aluminum often contains excessive iron, for example, the iron content is more than 1.5 percent and even higher, which affects the quality of the regenerated aluminum, and the iron content is often diluted by adding several times of pure electrolytic aluminum, so that the iron content is reduced to an acceptable level, which means that the low cost and low energy consumption of the regenerated aluminum are also diluted by the electrolytic aluminum, and as the regenerated aluminum becomes a main stream in the future, society does not have a lot of electrolytic aluminum for dilution, so the accumulation of iron gradually climbs along with the circulation number, and the aluminum alloy is degraded. At present, manganese is added for deironing, an electromagnetic field is used for assisting filtration, and the like, so that good effects are not achieved. Therefore, the development of iron removal technology after melting the recovered scrap aluminum is urgent.
High quality bauxite suitable for electrolytic aluminum is not abundant in china storage. But there are more low-quality aluminum-containing solid wastes, typically high-alumina fly ash, high-alumina coal gangue, bauxite tailings, etc. For example, in the midwest region of inner Mongolia in China and the central north region of Shanxi province, the aluminum content in coal is high, the aluminum-silicon ratio in the coal ash after coal combustion is high, and may even be more than 1, and the aluminum content in the rest coal gangue is also high. In a part of bauxite production areas which are few in northern China, low-quality bauxite tailings, such as bauxite tailings with an aluminum-silicon ratio of 1.5-3, are abandoned and accumulated in a large amount due to being lower than the purchasing standard of downstream alumina enterprises, and the total reserved amount of the low-order bauxite resources is still large, so that a good utilization method is not provided at present.
At one time, the university of Datang electric power group union Qinghua builds a research institution of high-alumina coal in the inner Mongolia Erdos Dayue industrial park, and builds an industrial production line for extracting alumina by leaching high-alumina fly ash, but if the silicon oxide and the like in the low-order resource are removed, the pollution emission and energy consumption level are higher than those of the existing whole electrolytic aluminum process, and the low-order resource has no value in the aspects of economy and environmental protection. Later, the production lines and the technical lines thereof are not popularized and are finally disassembled by self.
The world has been concerned with direct smelting of metallic aluminium from bauxite using an electro-thermal process using carbon as a reductant for over a century. After extensive research and accumulation, several facts and conclusions can be confirmed: (1) direct reduction of aluminum by carbon is difficult. On the one hand, very high temperatures of about 2000-. Due to the temperature rise, a large amount of aluminum is volatilized into furnace gas instead of remaining in a hearth. If vacuum melting is adopted, the condition that a large amount of aluminum is volatilized exists. (2) It is easier to achieve the synergistic reduction of aluminum-silicon oxide than the reduction of pure aluminum to obtain aluminum-silicon alloy, and if the preferential reduction of iron oxide is available, the generated aluminum and silicon metals are directly dissolved with iron, which is more favorable. In general, such aluminum-silicon alloys can be reduced theoretically as long as the aluminum content does not exceed 72%. It is further advantageous if the aluminium silicon contains a certain amount of iron, for example 5-10%. (3) In many domestic iron alloy enterprises, the reduction of aluminum-containing alloys such as aluminum-silicon alloy or aluminum-silicon-iron alloy is tried by using a submerged arc furnace, and the aluminum content of less than 35 percent is easy to realize. If the alumina content of the charge stock is high, exceeding 40%, even at a ratio of 50-60% in the alloy, refractory carbides, such as silicon carbide, are particularly likely to be produced, leading to a rise in the hearth, and forced production to stop. (4) In the industrial silicon production process, the problem that the furnace bottom rises due to the generation of silicon carbide also exists, and the process is well controlled by means of process regulation, furnace bottom rotation and the like. (5) Smelting high aluminum-containing aluminum silicon or aluminum silicon iron alloy belongs to a variety difficult to smelt, and needs grinding, ball making and drying of raw materials, elaborate process control and production operation, wherein a furnace type generally suggests larger power density, furnace bottom density, more concentrated heat supply, faster temperature rise of furnace burden, and parameter optimization in the aspects of polar center circle and hearth height-diameter ratio.
In summary, some electrothermal aluminum-silicon alloy production lines with a Soviet Union period, such as Neibe's factory, which can achieve stable commercial production for decades, have 8 ore furnaces above 16500KVA for relevant production, the aluminum content of the product is about 50-60%, and the power consumption is at the level of 12000-.
In the 21 st century, the Shanghai Deng Dynasty aluminum industry company in China introduced Ukrainian expert team mastering former Soviet Union technology, and after years of research, stable commercial production is realized on the same 16500KVA AC ore-smelting furnace, the aluminum content of the product is about 50-60%, the silicon content is more than 30%, the iron content is less than 10%, and the product is identified by Henan province and is listed as an international talent cooperation demonstration project by the state foreign expert bureau.
However, in the former soviet union, ukraine, or the unique home in china, the stable production of the aluminum industry for electricity logging still cannot be used as the aluminum alloy of the metal structure. It is generally required to reduce the content of iron to below 1% and the content of silicon to below 13% to make it possible to produce casting alloy which can be used as structural material in aluminium alloy, otherwise it can only be used as compound deoxidizer in ferrous metallurgy process, and it is aluminium which is cheaper than metal aluminium in chemical function. Tests for removing iron and reducing silicon of such high aluminum alloys have been carried out, such as adding manganese to remove iron by filtration, and diluting the high aluminum alloys to silicon content of about 10% by using multiple times of electrolytic aluminum, which in turn causes that the electrothermal smelting aluminum-silicon alloy can not exist independently from the electrolytic aluminum, and the advantage of low price of raw materials is also eroded by the high cost of multiple times of electrolytic aluminum.
Therefore, even though the process and equipment technology for smelting the aluminum-silicon alloy by electric heating are carefully mastered, the aluminum-silicon-iron alloy with high aluminum content containing about 60 percent of aluminum can be produced, but the aluminum, the silicon and the iron cannot be thoroughly separated to obtain structural metal aluminum, so the process technology has no strong competitiveness in commerce and cannot replace the existing aluminum electrolysis process.
US2829961, US2974032, US4099959, US4213599 disclose that thermal reduction of alumina directly with carbon as a reducing agent is difficult to obtain metallic aluminum, and stepwise reduction of aluminum can be achieved by forming aluminum carbide as an intermediate reducing agent.
US patent US7704443 describes heating a molten material with a sidewall electrode plus a top electrode to obtain aluminum vapor. US7819937 proposes the recovery of an aluminium-containing product in the gas phase by means of a feeding device.
Richard J Fruehan in US6849101 proposes the carbothermic production of aluminum intermediate carbides from furnace gases by porous charcoal absorption, and the metallic aluminum is obtained by reaction with aluminum and alumina in the gas phase.
U.S. aluminum corporation, U.S. patent No. 200980150004.5, filed in china, proposed the use of temperature reduction to precipitate aluminum carbide and aluminum metal.
Chinese patent 200610051148.3 filed by the chinese aluminium industry proposes that the ore furnace directly produces sendust with 38% aluminium and 23% iron as a deoxidizer, but the difference between the aluminium and iron contents is too small to separate out aluminium similar to that used in structural materials.
Chinese patent application 201710874459.8 proposes the use of manganese addition to remove iron from recycled aluminium magnesium silicon alloys and then to purify the aluminium alloy liquor by removing iron containing precipitates through a ceramic foam filter screen.
Chinese patent No. 98113973.6, and 201210242147.2, propose distillation purification devices for magnesium, but all are batch-type production, and the product is single high-purity magnesium metal.
SUMMERY OF THE UTILITY MODEL
According to prior art's not enough more than, the utility model provides an electric heat aluminum smelting's device adopts metal magnesium as the extractant, adopts the physics method to isolate aluminium, silicon and iron, utilizes the unlimited characteristic of mutually dissolving of molten magnesium liquid to the aluminium liquid state of metal, selectively dissolves into metal magnesium with aluminium, and iron, silicon realize mutually melting aluminium and magnesium in the characteristic of the almost undissolved of molten metal magnesium liquid, get rid of out alloy liquid with iron, silicon, then the almag distills the separation.
The utility model relates to an electric heating aluminum smelting device, which is characterized in that the device comprises the following parts:
at least one aluminum-magnesium centrifugal separator, wherein the aluminum-magnesium centrifugal separator receives alloy liquid containing iron-containing aluminum alloy and metal magnesium which are melted into four elements of aluminum, magnesium, silicon and iron, the alloy liquid is separated into aluminum-magnesium alloy liquid and separated solid-phase metal compounds after centrifugal treatment, and the aluminum-magnesium alloy liquid is cooled to generate aluminum-magnesium alloy blocks;
and the aluminum-magnesium continuous distillation separation furnace receives the aluminum-magnesium alloy blocks produced by the aluminum-magnesium centrifugal separator, re-melts and distills the aluminum-magnesium alloy blocks to separate the aluminum liquid and magnesium vapor, and the magnesium vapor is condensed to generate condensed magnesium.
In the utility model, the iron-containing aluminum alloy is 1-20% of iron containing, 40-72% of aluminum containing, 5-50% of silicon containing electrothermal aluminum-silicon alloy and aluminum-silicon-iron alloy which are produced by reduction smelting in a submerged arc furnace, and the used raw materials are natural minerals containing aluminum, silicon and iron and energy industrial wastes, including low-order bauxite, bauxite tailings, aluminum-containing fly ash, coal gangue, kaolin and the like; the iron-containing aluminum alloy can also be recovered waste aluminum containing 1.5-10% of iron.
Wherein, the preferred scheme is as follows:
the aluminum-magnesium centrifugal separator is provided with a space enclosed by a centrifugal machine fixed cylinder wall and a centrifugal machine fixed cylinder protective cover plate, a detachable centrifugal rotating drum is arranged in the space, the centrifugal rotating drum comprises a centrifugal rotating drum bottom plate, a centrifugal rotating drum outer drum wall, a centrifugal rotating drum inner drum wall and a centrifugal rotating drum top plate, the same circle center of the outer cylinder wall of the centrifugal rotary drum and the inner cylinder wall of the centrifugal rotary drum is arranged between the bottom plate of the centrifugal rotary drum and the top plate of the centrifugal rotary drum, an annular liquid receiving groove of the centrifugal rotary drum is arranged between the outer cylinder wall and the inner cylinder wall of the centrifugal rotary drum in an annular manner, the inner space enclosed by the inner wall of the centrifugal drum is an inner cavity of the centrifugal drum, a centrifugal drum liquid injection channel leading to the inner cavity of the centrifugal drum is arranged between the protective cover plate of the centrifugal fixed drum and the top plate of the centrifugal drum, and a plurality of liquid throwing holes are uniformly formed in the inner wall of the centrifugal drum. The centrifugal drum of the aluminum-magnesium centrifugal separator is made of carbon steel, heat-resistant steel and the like, and the inner drum wall of the centrifugal drum can bear the aluminum-magnesium alloy liquid which is in direct contact with 500-1000 ℃. The centrifugal rotating speed of the aluminum-magnesium centrifugal separator is 30-5000 revolutions, and the generated centrifugal acceleration is 10-1000 times of the gravity acceleration.
The aluminum-magnesium continuous distillation separation furnace comprises an aluminum-magnesium alloy remelting furnace, a magnesium distillation tower, an aluminum liquid heat preservation furnace, a magnesium condenser, a crystallized magnesium storage chamber, a total vacuum pipeline and a vacuum pump; the magnesium-aluminum alloy remelting furnace is communicated with a top feeding hole of the magnesium distillation tower through a vacuum liquid suction pipe, a bottom discharging hole of the magnesium distillation tower is communicated to the aluminum liquid heat preservation furnace through an aluminum liquid downstream pipe, the top of the magnesium distillation tower is further communicated with a top feeding hole of a magnesium condenser through a magnesium steam pipe, a bottom discharging hole of the magnesium condenser is communicated with a crystallized magnesium storage chamber, and the top of the magnesium condenser is further communicated with a total vacuum pipeline and a vacuum pump.
The utility model discloses in, almag remelting furnace and magnesium distillation tower adopt resistance, induction heating, perhaps gas, hot-blast non-contact indirect heating, and the heating temperature of almag remelting furnace is 500 and gives other heat with sand 900 ℃, and the heating temperature of magnesium distillation tower is 700 and gives other heat with sand 1200 ℃, and the vacuum of magnesium distillation tower is absolute pressure 0.1-1000 Pa. An aluminum liquid column with the height of 3.5-5 m can be contained in the magnesium distillation tower and the aluminum liquid downstream pipe, so that the aluminum liquid column in the magnesium distillation tower is sealed under the local atmospheric pressure. Similarly, a device for blowing argon can be arranged at the bottom of the magnesium distillation tower and in the aluminum liquid concurrent flow pipe, so that immersed argon blowing stirring or jet stirring of the aluminum liquid column is realized.
The magnesium distillation tower is characterized in that a plurality of layers of distillation tower trays are vertically arranged in the inner cavity space of the magnesium distillation tower, an aluminum magnesium liquid flow receiving area is arranged on one side of the top of each distillation tower tray, an aluminum magnesium liquid falling hole is formed in the other side of the top of each distillation tower tray, a baffle is arranged around the outer edge of the top of each distillation tower tray, and a circuitous aluminum magnesium liquid flow channel formed by a flow channel cofferdam is arranged between each aluminum magnesium liquid flow receiving area and each aluminum magnesium liquid falling hole.
The shell of the magnesium distillation tower is of a double-layer steel structure and comprises an outer shell and an inner shell, an interlayer between the outer shell and the inner shell is subjected to vacuum treatment, and a fireproof heat insulation layer is built on the inner wall of the inner shell. The interlayer is a vacuumized pressure buffering area, and the shell is a pressure-bearing steel shell bearing the pressure difference between atmospheric pressure and the interlayer.
The magnesium condenser is internally provided with a cooling cavity, the top of the cooling cavity is respectively communicated with a magnesium steam pipe, a total vacuum pipeline and a vacuum pump, the bottom of the cooling cavity is communicated with a crystallized magnesium storage chamber, the cooling cavity is externally wrapped with a cooling device, a spiral magnesium scraper is arranged in the cooling cavity, a magnesium vapor baffle is further arranged at the top of the cooling cavity, and the magnesium vapor baffle is positioned between two connectors of the cooling cavity, the magnesium steam pipe, the total vacuum pipeline and the vacuum pump.
The cooling device comprises a negative pressure spray vaporization chamber, a vaporization negative pressure suction pipe and a vacuum pump, wherein the vaporization negative pressure suction pipe and the vacuum pump are connected with the negative pressure spray vaporization chamber, and a plurality of atomization water nozzles are arranged in the negative pressure spray vaporization chamber.
And a crystalline magnesium locking upper valve is arranged between the magnesium condenser and the crystalline magnesium storage chamber, and a crystalline magnesium locking lower valve is arranged at a discharge opening of the crystalline magnesium storage chamber.
The crystallized magnesium storage chamber is respectively communicated with a vacuum pumping pipeline and a vacuum breaking inflation pipeline.
And the height of the aluminum liquid concurrent flow pipe is calculated by dividing the local atmospheric pressure by the standard atmospheric pressure and multiplying by 4.5 m.
The utility model discloses a concrete technology is shown in figure 1, with an electric heating method reduction technology totally different with current mainstream high-quality bauxite-aluminium oxide-electrolytic aluminum, with low order bauxite, the bauxite tailing, fly ash, ubiquitous aluminium silicon resources such as gangue or the solid useless of aluminium-containing are low-priced raw materials, smelt the aluminium-silicon-iron alloy of high aluminium in airtight submerged arc ore electric stove through thermal reduction method, then further adopt molten liquid metal magnesium as solvent, the extractant, dissolve out aluminium selectivity from the aluminium-silicon-iron alloy, and effectively separate out iron, silicon from aluminium-magnesium alloy liquid, adopt the condensation method, or the liquation method, and the method that condensation and liquation combine, and adopt the hypergravity centrifugation method that is much higher than natural gravity separation efficiency, make more aluminium elements enter into final trade mark aluminium alloy. Meanwhile, the byproduct ferrosilicon slag is used as a reducing agent for thermal reduction of magnesium metal, so that better comprehensive utilization is achieved. In the process, an aluminum extraction metallurgical chemical process with participation of an aqueous solution and an aluminum smelting process with fluoride are not available, so that the aluminum smelting process has no aqueous solution, fluoride treatment and possible pollution risk;
replacing a plane reactor of an electrolytic cell with a three-dimensional reactor of an ore-smelting electric furnace to enlarge the capacity of a reduction reactor for single aluminum extraction metallurgy; the aluminum smelting reactor and the production process thereof can be free from the influence of power failure or power fluctuation, and the aluminum smelting production line can be used for seasonal production stop and can adjust power load in summer power utilization peak period, and the aluminum smelting production line has stronger adaptability to power fluctuation compared with an electrolytic cell.
The device and the method for realizing effective separation of aluminum and magnesium through distillation are developed, and are particularly suitable for large-scale industrialized and continuous production process.
With the gradual accumulation of the stock of the scrap aluminum in society, the proportion of the regenerated aluminum is higher and higher, but the scrap aluminum with higher iron content is difficult to remove iron, so that great limitation is brought to the use of the scrap aluminum, iron is removed by adding magnesium, and then aluminum and magnesium are separated from each other by continuous distillation, so that a wide prospect is created for the use of the scrap aluminum with high iron content, the use of degradation is not needed any more, and much fresh electrolytic aluminum is not needed to be used for diluting and reducing iron; magnesium element contained in the waste aluminum is better recycled. The waste magnesium often contains certain aluminum element, and better aluminum recovery is obtained by evaporation separation after aluminum and magnesium are mutually melted. In the past, after waste magnesium is directly distilled, residues contain a certain amount of aluminum and other metal elements, are adhered to the inner wall of a distiller, have no fluidity and are difficult to remove. Magnesium refining, no longer adopts a chemical refining method that fluorine chlorine salt pollutes the environment, but physical distillation, has good environmental effect,
in the general silicothermic reduction process of magnesium, metal impurities such as Al, Si, Fe and the like are difficult to remove due to chemical refining, so that a high-temperature and high-vacuum enhanced extraction method cannot be used, and the production capacity of equipment, the recovery rate of magnesium elements and the utilization rate of ferrosilicon are always low. The method is adopted to directly mix the crystallized crude magnesium with the aluminum alloy for synergistic purification, so that a high-temperature and high-vacuum strengthening means and process can be adopted, the yield, the magnesium element yield and the silicon element utilization rate are obviously improved, the follow-up possibility of removing impurities through refining is avoided, silicon and iron elements enter filter residues due to follow-up condensation and centrifugal separation, and aluminum elements enter aluminum liquid to be removed;
magnesium distillation is a high-energy-consumption process, one ton of magnesium is distilled and volatilized in the industry, even in a continuous production process, 15-20GJ energy is often needed, the cost is saved by adopting gas to indirectly heat, the firepower and the electric power are converted by the gas in many times, and the energy conversion efficiency is only 30-42%; magnesium distillation, wherein a device and a process similar to multi-effect evaporation are adopted, and distilled magnesium vapor is used as a heat source to indirectly heat new aluminum-magnesium alloy liquid or magnesium liquid to volatilize and purify the magnesium alloy liquid or the magnesium liquid, which is equivalent to one time of metal magnesium distillation energy consumption, and multiple times of magnesium distillation effect is generated, so that the energy-saving effect is more remarkable.
The specific process principle of the present invention can refer to the following explanations:
the desired electrothermal aluminum-smelting reaction is to make the mineral containing alumina contact with carbonaceous reducing agent, even deeply mix and pelletize, then send it into electrothermal metallurgical equipment such as ore-smelting furnace, and use electric arc high-temperature heating to hopefully produce carbon-reduced alumina reaction and obtain metallic aluminum.
The following reactions, which one wishes, do not actually occur.
Al2O3+3C＝2Al+3CO
This reaction requires extremely high temperatures, and the theoretical temperature for starting the reduction is up to 2000-2100 ℃ according to the theory of chemical thermodynamics.
ΔG0＝325660+3.75TlgT-1.5507T
The starting reduction temperature was calculated to be around the absolute temperature of 2295K, i.e., 2022 ℃ according to the above formula. The chemical thermodynamics international commercial software Factsage7.3, widely accepted by the metallurgical industry, calculates the free energy of reaction as follows, starting to produce aluminum metal at about 2053 deg.C.
TABLE 1 Standard free energy of reduction of alumina by carbon
| Temperature (degree centigrade) | Delta G0(J) |
| 1400.00 | 364910.5 |
| 1500.00 | 307004.8 |
| 1600.00 | 249307.9 |
| 1700.00 | 191812.4 |
| 1800.00 | 134511.4 |
| 1900.00 | 77398.9 |
| 2000.00 | 20468.9 |
| 2053.87 | -10122.7 |
| 2100.00 | -33911.1 |
| 2200.00 | -85180.4 |
Even at such high temperatures, however, the reduction does not result in metallic aluminum, but primarily aluminum carbide. That is, the following reaction actually occurs in a large amount.
2Al2O3+9C＝Al4C3+6CO
At high temperature, aluminum carbide and aluminum oxide are dissolved in a large amount and the generated metal aluminum is dissolved, so that the product is difficult to obtain metal pure aluminum. Meanwhile, at the high temperature of above 2000 ℃, along with the escape of CO gas in the furnace gas, a large amount of aluminum is volatilized, and the aluminum is escaped and lost in the form of aluminum vapor.
If the mineral used is a composite oxide of aluminium and silicon, or if silicon oxide is reduced synergistically with aluminium oxide, the carbothermic reduction reaction is much more advantageous.
Carbon reduction of silicon oxide, a chemical reaction represented by the following formula, is one of the main reactions for producing ferrosilicon, industrial silicon, and other silicon-based alloys.
SiO2+2C＝Si+2CO
In fact, the reduction of silicon also involves the reaction of carbides as intermediate products. The following formula
SiO2+3C＝SiC+2CO
However, the presence of carbides leads to a further reaction to reduce the semimetallic silicon.
2SiC+SiO2＝3Si+2CO
The intermediate product aluminum carbide in the aluminum reduction process can also reduce silicon oxide, so that aluminum and silicon are synergistically reduced as shown in the following reaction formula. The molar ratio of the produced aluminum to the silicon is 8:3, the mass fraction of the produced aluminum is 72 percent of the aluminum, and the reason why the aluminum content cannot exceed 72 percent theoretically when the aluminum-silicon alloy is prepared by electrothermal reduction is generally considered by the industry.
2Al4C3+3SiO2＝8Al+3Si+6CO
In addition to the formation of silicon carbide, aluminum carbide as an intermediate product, the reaction of alumina with carbon may also form carbon oxides.
4Al2O3+Al4C3＝3Al4O4C
During the whole process of carbon reduction of aluminum silicon oxide, gaseous products such as intermediate valence state silicon oxide, aluminum oxide and the like are also generated. Shown in the following reaction formula
SiO2+C＝SiO↑+CO↑
Al2O3+2C＝Al2O↑+2CO↑
During the rising process, if the hearth is deeper, the low-valence gas oxides continue to react, so that the aluminum-silicon alloy is obtained. This requires that the reactor be designed to be relatively deep so that there is sufficient residence and reaction time for the gaseous intermediate.
The aluminum carbide is destroyed due to the existence of silicon, particularly silicon and carbon elements in the same family, and the silicon has greater activity to combine with other elements such as aluminum and the like and occupy the position which is originally carbon, so that aluminum-silicon alloy is generated in a large amount instead of aluminum carbide. After the silicon and the aluminum are mutually dissolved, the activity of the aluminum is reduced, and the reaction for preparing the aluminum by reduction is carried out to a greater extent.
In general, the theoretical and practical conclusions regarding electric furnace smelting of aluminum-silicon alloys indicate the following suggestions: (1) the smelting of aluminum-silicon alloy or aluminum-silicon-iron alloy by the submerged arc furnace is industrially feasible, and pure aluminum can not be obtained by an electrothermal method; (2) aluminum-silicon-containing cheap resources in nature or energy industry are adopted, if the aluminum-silicon ratio is 1.3-1.6, an alloy containing 50-60% of aluminum can be obtained by smelting, and if the alloy contains 5-10% of iron, the smelting difficulty is easier than that of the aluminum-silicon alloy containing iron and less than 1.5%; (3) before the minerals are put into the furnace, the minerals and the carbonaceous reducing agent are ground into powder, then the powder is pelletized by using a binder under certain pressure, and the pellets which are dried into certain strength are put into the furnace so as to keep certain strength in the furnace and enable the CO gas of the reduction product to escape from a gap out of a hearth. The pellet pressing strength is too low, and the pellets are easily crushed in the furnace, resulting in blocking of gas passages. The pellet pressing strength is too high, the pellets are too compact, gas cannot escape from the pellets in the reduction process, and further reduction is also hindered. (4) The reducing agent can be selected from a plurality of reducing agents, such as bituminous coal, has certain volatile components, and the pellets become a porous structure after being heated, so that the reaction gas can escape. Other carbonaceous reducing agents, such as biomass carbon, petroleum coke, semi coke, anthracite, have also been suggested, but in general, porous carbonaceous reducing agents are preferred; (5) the amount of the carbonaceous reducing agent is slightly lower than the theoretical amount, for example, 94 percent is good, so that the probability of generating carbide can be reduced; (6) high-alumina fly ash, coal gangue, low-order bauxite and tailings thereof, kaolin and the like are all suitable low-cost aluminum-silicon mineral resources. In northern Shanxi jin such as Touger flag of Thysaucklo and inner Mongolia Ordos, a large amount of high-aluminum coal resources are available, the aluminum-silicon ratio can reach 1 or more, and coal gangue and coal ash of coal-fired power plants are also high-aluminum. In addition, in bauxite production areas such as Shanxi, Henan and Guangxi in south China, a large amount of low-order bauxite or bauxite tailings with the aluminum-silicon ratio lower than 3 are abandoned due to the fact that the low-order bauxite or bauxite tailings do not meet the purchasing standard of an alumina plant used for electrolytic aluminum, and are good mineral resources of the electrothermal aluminum-silicon alloy through mixing; (7) if the feed contains higher calcium oxide, then the charging conditions are not favorable. The melting point of the furnace charge is reduced due to the calcium oxide, so that the furnace charge is melted prematurely, and the reduction process of aluminum and silicon is influenced. When part of high-sulfur coal is combusted in a boiler combustion chamber, in order to reduce the burden of subsequent flue gas desulfurization, certain lime is often mixed for combustion, so that the lime content in the fly ash of a power plant is higher than the ash content of the original fuel coal, which is a negative factor; (8) from the perspective of subsequent extraction of metallic aluminum, the higher the aluminum content, the better the aluminum content, and the lower the iron content, but the difficulty of smelting in a submerged arc furnace can be generally achieved at the better levels of 55-63% of aluminum, 30-36% of silicon, 2-10% of iron, and a small amount of titanium, which are generally considered together with iron; (9) the smooth operation of the submerged arc furnace is influenced, and besides whether the alloy liquid can smoothly flow out, the risk of furnace bottom rising is also caused. The alloy liquid is not easy to flow out, the density of the alloy liquid is very small, the density is almost in the order of 2500kg/M3, and even the density is lower than that of ores and carbides, which is different from other common iron alloys, so that the alloy liquid in a hearth floats above furnace burden, the tapping is difficult, the current does not pass through the hearth, the hearth is relatively cold, refractory carbides such as silicon carbide and the like are generated to be deposited and rise on the hearth, the production is very short, the hearth has to be stopped for overhaul, even hard hearth carbides which are difficult to remove need to be exploded, and the production process can only maintain dozens of days; (10) the produced aluminum-silicon alloy and aluminum-silicon-iron alloy still contain certain carbides, unreacted alumina-silicon oxide and the like, are mixed in the alloy liquid and need to be refined and removed. The refining method is preferably chemical refining, a small amount of halide is used as a refining agent for removal, a physical method, such as a supergravity centrifugal method, can also be considered, and the environmental pollution in the halide using process is reduced; (11) some attempts have been made to reduce the initial temperature of the reduction reaction by carbothermic reduction of alumina under vacuum, but the effect is not satisfactory because the vacuum lowers the temperature at which the reduction reaction starts, but also lowers the boiling point of metallic aluminum, resulting in a large amount of volatilization of metallic aluminum generated under vacuum; (12) from the perspective of electric furnace equipment, the alloy is suitable for electro-thermal smelting of aluminum-silicon alloy, and is approximately similar to refractory high-silicon alloy such as industrial silicon, for example, silicon-calcium alloy. It is a better practice to rotate the furnace shell to counteract or delay furnace bottom rising for industrial silicon. If the campaign period caused by the rising of the furnace bottom can be prolonged to 10-12 months, the whole production process can realize better commercial operation; (13) the temperatures of the reaction zone and the furnace bottom must be high, and the time for heating the furnace charge to the reaction temperature is short, namely, the temperature is high, 2200 ℃ is needed, and the heating speed is high, so that the retention time is reduced in a temperature area which is easy to generate carbide as far as possible; (14) the general submerged arc furnace for smelting Al-Si alloy needs a deeper hearth, a smaller pole center circle diameter and a larger specific power per unit area of the furnace bottom, such as 450-. (15) The power of the electric furnace is more than 16500KVA, which is the general proposal given by the leading organization in the world in the field of former Soviet Union and Ukrainian, and the power intensity of the area of the furnace bottom and the power intensity of the volume of the furnace hearth are both larger above the power; (16) in theory, the direct-current submerged arc furnace is a good choice, and particularly, the bottom anode is used, so that the temperature of the furnace bottom is high, and the furnace bottom is not easy to expand. However, the bottom anode is expensive and easily damaged, resulting in a too short campaign and an insufficient reliability of the electric furnace. The alternating current submerged arc furnace is still the main furnace at present. (17) It has been proposed to add a false bottom made of a perforated refractory material so that once the liquid ferrosilicon is produced, it flows rapidly from the false bottom to the bottom, avoiding the formation of carbides by contact with carbonaceous reducing agents, and at the same time, preventing the aluminium-silicon alloy produced from floating above the charge and causing difficulty in tapping.
Attempts and practices for electroheat aluminum refining began approximately in the 1880 s and numerous studies and practices were conducted in the uk, france, germany, the united states, canada, china, the former soviet union, and later ukraina. But finally, the commercialization is realized by the first Nienbo and other factories of the former Soviet Union and the subsequent Ukrainian metallurgy world.
In addition, the process is adopted in Germany before the end of the second war, namely the third empire, not only can the aluminum-silicon alloy be produced, but also the structural aluminum alloy can be finally obtained, and the process is named as the Beck process, but the provided data is not sufficient.
Despite the great efforts made by the western scientific and industrial sectors, it has not been completely commercialized nor has it been possible to create any impact on the production of primary aluminum monopolized by electrolytic aluminum. For this reason, it may be that: the western scientific and technological industrialization system follows a strict stepwise amplification path of laboratory bench test-pilot test-industrial trial production, so that scientists engaged in research must smoothly realize the stable output of electrothermal aluminum-silicon alloy, particularly aluminum-silicon containing more than 50 percent, in a small laboratory scale, and then accept the trial production of larger electric furnaces in the industry. However, the remarkable point of electrothermal aluminum-silicon alloy is that, because of the requirement of extremely high crucible temperature and rapid temperature rise process, the power density of the furnace bottom of a small electric furnace cannot meet the temperature and the temperature rise speed, even a few thousand KVA electric furnaces cannot meet the requirement, and as suggested by the former Soviet Union experts, a 16500KVA electric furnace is the lower limit of the power of equipment capable of stably producing. As the procussive Soviet Union and the crushing Germany before the end of the second war execute the military or quasi-military war regime, the so-called 'market economic law' or 'equipment and scale progressive amplification' chemical metallurgy economic law is not strictly followed, so that the conventional progressive amplification process can be overcome, and the trial production is directly carried out by adopting an industrial large-scale electric furnace, thereby obtaining 'unexpected' success. Of course, this is only a reasonable guess.
Aluminum-silicon alloy or sendust alloy containing a high aluminum content, such as aluminum 50 to 65%, iron and titanium 1.5 to 10%, and silicon in the balance approximately 30 to 38%, which is periodically discharged from a submerged arc furnace, is called primary aluminum-silicon alloy, primary alloy, coarse alloy, intermediate alloy, etc., and if cast aluminum alloy or wrought aluminum alloy containing silicon and iron even lower is not extracted, only as a deoxidizer for steel or a reducing agent for hot magnesium, which is of low economic value, it does not produce the desired industrial raw aluminum for the aluminum industry mainly including structural materials.
The initial refining or treatment method is to reduce the iron content in the primary alloy as much as possible, for example, about 1.5% or even lower, remove the mixed carbides and oxides by simple chemical refining of the liquid alloy, then remove the iron by adding manganese, and dilute the liquid alloy with electrolytic aluminum after the iron reduction to reduce the silicon content from 30-38% to 10-13%, that is, the silicon content of eutectic aluminum-silicon alloy or hypoeutectic, which means that 3-4 times of high-quality and high-price electrolytic aluminum liquid is used to dilute one time of the primary aluminum-silicon alloy, which is not cost-effective, so that some cost advantages obtained by the electrothermal method are diluted by 3-4 times of electrolytic aluminum, and the cost advantages are offset. FIG. 2 is a phase diagram of Al-Si binary alloy, and it can be seen that Si in general Al alloy should not exceed 13%, otherwise it becomes hypereutectic alloy, and the application range is limited.
The difficulty in smelting low-iron aluminum-silicon alloy is high. The iron content contributes to the reduction of aluminum and silicon. The alloy containing 20-30% of aluminum, 30-40% of silicon and 20-30% of iron as a deoxidizer has no two difficulties in smelting compared with the conventional silicon alloy.
In order to produce low-iron alloys, the selection of raw materials must be careful, the low-iron raw materials are used, the electrodes are expensive carbon self-baking electrodes, and the pre-baking electrodes cannot be used, and the electrodes are self-sintered in a steel shell by using electrode paste, so the cost is low, but certain iron content is brought into the product, so the electrode cannot be used. Once the iron content is higher than 1.5%, the method for removing iron by adding manganese and diluting and reducing silicon by pure aluminum cannot be implemented. This solution is obviously not applicable as a subsequent operation in submerged arc furnace smelting.
It is feasible to select a metal Me which has stronger dissolving capacity to aluminum but has low solubility to silicon and iron elements, so that a selective dissolving method can be adopted, the Al-Me binary alloy is formed by common refining impurity removal methods of non-ferrous metals such as liquation, condensation and the like, the ferrosilicon in the Al-Me binary alloy is separated into by-products, and then a method is adopted, for example, distillation separation of Al and Me metals is realized by utilizing different vapor pressures. This selective dissolution, or physical "extraction" of the molten metal, requires two steps to complete. In the first step, dissolution is followed by solid-liquid separation. And secondly, distilling and separating. The Me metals can be selected from the common metals such as lead, mercury, zinc, magnesium and the like, and have the separable characteristics to a certain extent. Lead and mercury as poisonous heavy metals have adverse effects on human health and environment, and are not good choices. More preferably, zinc and magnesium are used. Zinc is a common metal and is reasonably useful. However, the advantages of magnesium are more obvious compared with zinc. The main body is as follows: (1) the mass of the aluminum-silicon alloy treated by zinc is about 3-4 times that of the aluminum-silicon alloy, and the mass of magnesium is only about 1 time. The reason is that the zinc has larger atomic weight and density, and the mass multiple is larger in terms of atomic number proportion and volume, so that the amount of zinc which needs to be used and circulated is larger; (2) the price of zinc is much higher than that of magnesium. In the last 20 years, with the great development of the magnesium industry, particularly the new magnesium producing country with 86% of the global magnesium production in China, the price of magnesium is always at the same level as that of aluminum loitering, and is even lower than the zinc price. This is advantageous when magnesium is used as the "extractant". (3) The capability of magnesium for removing iron and silicon in the aluminum-silicon alloy is superior to that of zinc. Zinc does not remove the silicon element bound in aluminum at higher temperatures, and magnesium is much more effective. (4) The ferrosilicon solid-phase educt removed from the aluminum-silicon alloy carries a certain aluminum content, and is an excellent reducing agent for magnesium metal smelting by a hot method, which means that the hot method aluminum smelting and the hot method magnesium smelting can form a coupling production relation, and the closed-loop coupling not only brings the progress and upgrade of the aluminum industry, but also has a huge promotion effect on the magnesium industry, and can form the aluminum-magnesium win-win co-production. In contrast, zinc is adopted to extract aluminum, so that zinc is only a simple metal for circulation, and the influence on the existing zinc smelting industry is avoided. (5) The adoption of magnesium as an extractant means that a large-scale light alloy combined factory forms a good interaction between aluminum and magnesium industrial plates. The reducing agent is evolved from ferrosilicon into ferrosilicon, and the reducing capability of aluminum is stronger than that of silicon, so that the energy consumption, material consumption and production period of magnesium smelting are greatly improved compared with the simple use of ferrosilicon. In addition, the existing magnesium chemical refining is omitted, the coarse crystallized magnesium is used as an extracting agent to extract pure aluminum, the purity of magnesium steam which is originally forbidden in the magnesium smelting link does not need to be more concerned, the high-temperature high-vacuum process can be adopted to strengthen rapid smelting, the magnesium smelting period is shortened, even if the magnesium contains higher silicon, aluminum and iron, the content is not enough, and the impurity elements of silicon, aluminum and iron become useful products in the subsequent aluminum-silicon-magnesium mutual melting stage.
Magnesium is a preferred molten metal for dissolving aluminum because of its special properties; the liquid state can be infinitely miscible with aluminum, as shown in the aluminum magnesium binary alloy state diagram of fig. 3, but hardly dissolves iron and silicon. FIG. 4 shows that the soluble iron content of Mg-based alloy solution is very low, and in general non-ferrous metal industry, it can be considered as a good metal with low iron. FIG. 5 shows the solubility of silicon in magnesium, but the content of soluble silicon element in magnesium is also low due to the formation of Mg2Si compound, and particularly, as the temperature is lowered, silicon element precipitates with magnesium to form a compound. But magnesium and aluminum can be infinitely mutually dissolved in liquid state, the eutectic interval is large, the eutectic temperature is as low as about 480 ℃, and is reduced by nearly 200 ℃ compared with the melting temperature of aluminum and magnesium of pure metal, which means that soluble iron and silicon in the eutectic are further and thoroughly removed.
The process of dissolving aluminum by magnesium and separating the aluminum from the ferrosilicon can adopt a condensation method or a liquation method. From the perspective of energy utilization, the temperature of the hot ferro-silicon-aluminum alloy liquid discharged from the ore-smelting furnace is as high as 1300-. Drying and preheating crude magnesium or waste magnesium, or firstly melting, or carefully mixing with aluminum-silicon-iron liquid, and then cooling to a certain temperature above 480 ℃ of the liquidus of aluminum and magnesium at the lowest. The addition of magnesium is preferably 0.5-2 times of the Al-Si-Fe alloy liquid, and the more the magnesium content is, the more thoroughly the purification and iron removal and silicon reduction are. After cooling and condensation, only relatively pure aluminum-magnesium alloy liquid is kept in a liquid state, and the iron element and aluminum are combined into complex aluminum-iron metal compounds and aluminum-silicon-iron metal compounds, which are more typical to FeAl3, which means that iron will combine with about 1.5 times of metal aluminum, as shown in an aluminum-iron binary state diagram shown in FIG. 6. Most of silicon element is combined with magnesium to form Mg2Si, the melting point is higher than 1000 ℃, so that solid-phase precipitate is mainly FeAl3 and Mg2Si, the density of the former is larger than that of the aluminum-magnesium alloy liquid, and the density of magnesium silicide is not obviously different from that of the aluminum-magnesium alloy liquid. Figure 7 shows that at 550 c for the almgsi ternary alloy, magnesium combines with silicon to form magnesium silicide, while almag forms the liquid alloy.
The method for separating the silicon-aluminum alloy liquid from the solid-phase precipitate dispersed in the silicon-aluminum alloy liquid has various methods, and common solid-liquid separation methods have certain effects. Such as gravity settling, vacuum filtration, pressure filtration, and spiral electrothermal crystallizers on inclined planes used in the nonferrous metal tin industry. But the most effective solid-liquid separation belongs to the super-gravity centrifugal separation. The centrifugal separation of solid and liquid can be carried out by centrifugal sedimentation or centrifugal filtration. Centrifugal filtration is suitable for the aluminum-magnesium alloy liquid and a large proportion of solid-phase precipitates in the aluminum-magnesium alloy liquid. Compared with natural gravity sedimentation, centrifugal separation has the advantages that centrifugal force borne by solid phase particles can be many times of gravity, and the effect of strengthened separation is achieved. The separation factor is generally defined as the ratio of the centrifugal force to the gravity of solid phase particles, and can be calculated by simple formula in engineering, as shown in the following formula
Where Fc represents the multiple of centrifugal force to gravity, dimensionless. r is the centrifuge radius in meters. ω is angular velocity, dimensionless. N is the rotation speed, unit rpm, revolutions per minute.
In the pyrometallurgical industry, the almag liquid centrifugation in the utility model, or in the centrifugal casting of other ferrous alloys or non-ferrous alloys, if centrifuge rotational speed 1000rpm, that is to say the rotational speed 1000 revolutions per minute, rotary drum diameter 1 meter, separation factor is 556 so, that is to say, the centrifugal force is up to 556 times of gravity.
Compared with a horizontal cantilever centrifugal machine and a horizontal riding wheel type centrifugal machine, the vertical centrifugal machine can adopt a larger centrifugal radius, and is more favorable. The centrifugation process can be completed within 10-20 minutes generally, but the cooling and condensation in the early stage and the finishing process in the later stage are time-consuming, and in order to improve the utilization rate of the centrifuge, a centrifuge is adopted to match a plurality of centrifugal rotating drum modes. The centrifugal rotary drum is of a concentric double-rotary drum structure, a core cavity at the innermost layer is used for containing ferrosilicon-magnesium quaternary alloy liquid, then the steel rotary drum is made to contact with hot alloy liquid and absorb heat, so that the alloy liquid is cooled quickly and generates a condensation effect, after the heat is absorbed and dissipated outwards by the rotary drum for a period of time, the temperature is close to a set separation temperature, for example, 530 ℃, then the whole centrifugal rotary drum is placed into a centrifugal machine and locked, then the centrifugal machine is started, so that the ferrosilicon and magnesium silicide combined with solid-phase ferrosilicon are thrown out from a liquid throwing hole, and the solid-phase ferrosilicon and magnesium silicide are used as filter residues and are left in the inner drum. It should be noted that the liquid throwing holes on the inner wall of the centrifugal drum are not used for solid-liquid separation, are really used for solid-liquid separation, are in a network structure formed by the bridging action of crystals among precipitated solid-phase substances, and filter the aluminum magnesium alloy liquid. The liquid throwing hole in the macro scale is only a channel for liquid alloy to flow out, and is not a filter medium, and the filter medium which really plays a role is a micro crystal structure combined by separated solid phases.
Through the processes of cooling, condensation and centrifugal separation, most of iron and silicon elements exist in filter residue in a solid phase form, and the filtrate is relatively pure aluminum-magnesium large-proportion alloy liquid, the melting point of the alloy liquid is low, and the lowest melting point is below 480 ℃. The separation of the aluminium and magnesium is subsequently achieved by distillation. The lower the temperature of the condensation, the lower the iron and silicon content in the al-mg alloy liquid, but in industrial production, the temperatures of condensation and centrifugal separation are set according to the actual product requirements, and do not need to be close to the solidification line of al-mg, and as shown in the separation process shown in fig. 8, the iron and silicon content in the liquid phase gradually decreases to a very low level in the al-mg alloy liquid phase as the temperature decreases.
The vapor pressure of the metal increases with increasing temperature. The vapor pressure of the metal can be calculated from the following equation.
lg p＝AT-1+B lg T+CT+D
Where P is the vapor pressure Pa, T is the absolute temperature, and A, B, C, D is a constant. Vapor pressure of aluminum and magnesium
lg pAl＝-16380/T-1.01g T+14.445
lg pMg＝-7550/T-1.41lg T+14.915
Referring to tables 2 to 4, the vapor pressure of aluminum magnesium was calculated as follows. As can be seen, magnesium is a volatile metal and has a vapor pressure 5-8 orders of magnitude greater than that of aluminum. This shows that distillation can be used to separate the al from the mg more thoroughly. That is to say, magnesium volatilizes and escapes from the alloy molten pool under the condition that the aluminum-magnesium alloy liquid is heated at high temperature, magnesium vapor is cooled in another condensation space and condensed into liquid or solid, and the liquid or solid is separated from the residual aluminum liquid in the original molten pool.
TABLE 2 vapor pressure comparison of magnesium and aluminum and multiples thereof
| Temperature in centigrade | Absolute temperature | Mg vapor pressure (Pa) | Al vapor pressure (Pa) | Multiple of |
| 650 | 923 | 3.58E+02 | 5.41E-07 | 6.62E+08 |
| 700 | 973 | 8.75E+02 | 4.19E-06 | 2.09E+08 |
| 750 | 1023 | 1.95E+03 | 2.65E-05 | 7.37E+07 |
| 800 | 1073 | 4.03E+03 | 1.41E-04 | 2.86E+07 |
| 850 | 1123 | 7.78E+03 | 6.43E-04 | 1.21E+07 |
| 900 | 1173 | 1.42E+04 | 2.58E-03 | 5.49E+06 |
| 950 | 1223 | 2.45E+04 | 9.21E-03 | 2.66E+06 |
| 1000 | 1273 | 4.04E+04 | 2.97E-02 | 1.36E+06 |
| 1050 | 1323 | 6.41E+04 | 8.76E-02 | 7.32E+05 |
| 1100 | 1373 | 9.82E+04 | 2.38E-01 | 4.12E+05 |
TABLE 3 vapor pressure of metallic magnesium and various impurity elements
Saturated vapor pressure of metal magnesium and each impurity element at different temperatures
TABLE 4 lower limit of the content of main impurity elements in magnesium which can be achieved by distillation
The lowest content of each impurity element in the metal magnesium can be achieved by distillation at different temperatures
The vapor pressure of the binary alloy liquid composed of aluminum and magnesium was lower than that of the pure metal, not only due to the decrease in concentration but also due to the interaction between the aluminum and magnesium alloys, forming a negative difference in activity coefficient, so that the vapor pressure of each of the aluminum and magnesium was accelerated and decreased in a nonlinear degree, and the activity coefficient values shown in table 5 were obtained.
TABLE 5 activity coefficients of Al-Mg Components (temperature: 800 ℃ C.)
| NAl | 1.00 | 0.9 | 0.8 | 0.7 | 0.6 | 0.5 | 0.4 | 0.3 | 0.2 | 0.1 | 0.0 |
| γAl | 1.000 | 0.971 | 0.900 | 0.817 | 0.732 | 0.658 | 0.599 | 0.555 | 0.530 | 0.522 | 0.526 |
| γMg | 0.168 | 0.301 | 0.464 | 0.623 | 0.763 | 0.871 | 0.942 | 0.982 | 0.997 | 1.000 | 1.000 |
The density ratio of al to mg in the gas phase can be calculated according to the following formula, where N is the mole fraction, P is the vapor pressure, and M is the molar mass.
From the above formula, it is estimated that, at 1000 ℃, even if the magnesium content in the al-mg alloy liquid is reduced to 1 wt.%, the activity coefficient of magnesium is reduced to 0.168, because the vapor pressure of magnesium is still 136 ten thousand times that of aluminum at this temperature, the instantaneous magnesium quality in the gas phase is still as high as 2000 times that of aluminum, which means that the content of aluminum in the instantaneous gas phase is still less than 0.05%, which indicates that purer metallic magnesium can be obtained from the condensed gas phase product, so that the al and the mg can be separated more thoroughly.
The metal evaporation rate per unit area can be calculated by the following formula
Where ω is the evaporation rate, g/cm2/hr；
A coagulation coefficient α, maximum 1, typically a fraction less than 1;
pPavapor pressure in Pa;
m, molar mass.
The calculated evaporation rate of pure magnesium is shown in table 6 below. The actual evaporation rate is less than this theoretical value. During the evaporation of the aluminum-magnesium alloy liquid, the vapor pressure of magnesium is reduced in a nonlinear acceleration manner with the decreasing concentration of magnesium, so that the actual evaporation rate is less than 1% of the theoretical value of pure metal, for example, in the aluminum-magnesium alloy liquid containing 1 wt% of magnesium, the vapor pressure of magnesium is only about 1/600 of pure metal, and the evaporation rate is also reduced sharply. The evaporation rate can be accelerated by increasing the evaporation area, raising the temperature and improving the vacuum degree, and the production efficiency is ensured. In addition, the metal evaporation has a critical pressure, and the vacuum degree lower than the critical pressure, the evaporation rate reaches the maximum value at the temperature, the vacuum degree is continuously increased, and the propagation rate is not increased, as shown in fig. 9, the vacuum degree in the industrial production is not required to be lower than the critical pressure too much.
TABLE 6 evaporation Rate of magnesium metal at different temperatures
| Temperature (. degree.C.) | 500 | 600 | 700 | 800 | 900 | 1000 |
| Evaporation rate (g cm)-2·h-1) | 1.68 | 17.5 | 110 | 484 | 1620 | 4450 |
In the vapor phase from the evaporation, the aluminum content in the condensate varies depending on the temperature of evaporation. If higher purity of magnesium is sought for distillation, lower temperatures are required, with correspondingly lower evaporation rates but lower yields. In industrial mass production, the aluminum content of distilled magnesium will be high if the evaporation rate is required to be high to maintain the output of the equipment. If the magnesium is recycled as an extractant, the use of the aluminum is not influenced by the aluminum. If sold as a by-product, it cannot be regarded as pure magnesium or high-purity magnesium, and is suitable as an aluminum-containing magnesium alloy, such as an aluminum-containing magnesium alloy of AZ series, which is an alloy product in a wide range of applications.
In the residual aluminum liquid, when the magnesium content is reduced to a relatively low level, for example, 0.2%, the rate of continuous distillation is greatly reduced, and simultaneously, the evaporation amount of aluminum is relatively increased. To this concentration, three approaches are advisable: one is to introduce argon into the aluminum liquid at the bottom of the distillation tank to continue distillation, and distill more magnesium out by using the bubble volume of argon blowing until the content of the magnesium is ultra-low; secondly, stopping distillation, after the residual aluminum liquid flows out, removing magnesium in the residual aluminum liquid or replacing the residual aluminum liquid with aluminum by adopting a chemical refining method, for example, introducing chlorine, aluminum chloride, sodium fluoroaluminate and the like, and oxidizing magnesium into molten salt through mutual replacement of aluminum and magnesium. And thirdly, a certain aluminum content is reserved, so that the distillation raffinate is used as an aluminum alloy containing magnesium, or an aluminum alloy containing silicon and magnesium, and is also a commonly used aluminum alloy type.
Although the separation of Al-Mg alloy is better achieved by distillation, the practice of distillation of small amounts of Mg is currently limited to batch equipment and processes, such as waste Mg recovery, high purity Mg preparation, and distillation recovery of excess Mg in the production of titanium sponge, in a sealed crucible that can be heated, solid or liquid Mg is placed in the crucible, and the Mg is evaporated into a condensing chamber or zone by continuous heating and vacuum pumping, and then condensed into pure Mg that is collected. The whole process has no flow of molten metal, so the evaporation area is very small, and is inevitable intermittent production, the distillation is finished, the vacuum is broken, the crystallized pure magnesium is taken out for subsequent treatment, the production rhythm is discontinuous, the efficiency is low, the equipment temperature reduction caused by breaking the vacuum and recovering the vacuum brings the reduction of energy efficiency, and the continuous flow separation of two kinds of molten metal to be separated is avoided, so the requirement of large-scale production is difficult to meet.
The filter residue left in the centrifugal filtration is mainly composed of almost all iron elements, most silicon elements, a certain amount of aluminum elements combined by iron, a certain amount of magnesium elements combined by silicon and the like, and can be called ferrosilicon filter residue. The main phases comprise FeAl3 metal compound, Mg2Si, FeSiAl, crystalline Si and the like. The ferrosilicon filter residue is most suitable for being used as a reducing agent for smelting magnesium by a hot method, or can be used as a compound deoxidizer in the steel industry. If the magnesium in the steel composite deoxidizer is not needed by customers, the magnesium is distilled and recovered in vacuum to obtain the ferro-silico-aluminum, and even the ferro-aluminum content needs to be remelted to increase the content of the ferro-aluminum so as to ensure that the density and the composition meet the requirements of steel users.
The reducing agent for smelting magnesium by a hot method replaces the commonly used #75 ferrosilicon, is suitable for a horizontal tank reduction process of a Pidgeon method, even a vertical tank process, a resistance internal heat process and an electric arc melting reduction process, and has stronger reducing capability than the ferrosilicon. The concrete advantages are that: (1) the reducing agent carries magnesium, namely Mg2Si, and can be separated out only by physical distillation under high-temperature vacuum; (2) the reducing agent contains aluminum, so that the reduction rate, the reduction energy consumption, the ferrosilicon excess, the reduction temperature, the reduction vacuum degree and the like of magnesium smelting are superior to those of pure ferrosilicon; (3) the iron content in the reducing agent is far lower than the 25% level in the #75 ferrosilicon, and various reduction indexes are further improved; (4) the crude magnesium does not need to be refined and is directly transported to an aluminum smelting workshop for remelting, so that the refining cost is reduced; (5) the conventional crude magnesium fluoride is refined, the pollution is heavy, and the great risk of strict control and limitation in the aspects of environmental laws and regulations is faced; (6) the dedusting ash of the electric heating aluminum smelting contains aluminum silicon metal powder which can be used as a magnesium smelting reducing agent; the contained MgO and CaO, namely dolomite magnesium ore micro powder, is returned to a magnesium plant to be used as a magnesium smelting raw material, so that the economy of magnesium smelting is further improved; (7) the most important reduction process can adopt a high-temperature and high-speed reduction process, the excessive contents of aluminum, silicon and iron impurities in the crude magnesium are not considered, the metal impurities cannot be removed by the original fluoride chemical refining, the aluminum and magnesium coproduction and the metal impurities are all available products, the quality maintenance is not required to be carried out at a low speed, and the production efficiency can be improved by 50-100%.
The solid reduction of the silicothermic process for smelting magnesium has the original smelting period of 12 hours, and adopts a smelting mode of 'medium temperature, medium vacuum and low speed' to protect the product quality and prevent the over standard of silicon, aluminum and iron elements in a magnesium ingot. The utility model discloses in, adopt vacuum distillation to purify magnesium, preceding magnesium ingot need mutually melt with ferro-silicon-aluminum alloy, and all metallic impurity in the magnesium all obtains recycle. The event the utility model discloses the aluminium magnesium heat method coproduction that realizes has broken through the low-speed mode of pijiang method magnesium smelting, adopts the process reinforcement three high modes of "high temperature high vacuum high speed", and energy consumption reduction, material consumption reduction, reduction time shorten, the cost of labor, coal gas cost all reduce to some extent, and productivity increase, investment reduce simultaneously. The whole process flow of the electric heating aluminum smelting and metal magnesium coproduction is shown in figure 10.
Drawings
FIG. 1 is a schematic representation of an overall process for electroheating aluminum production;
FIG. 2 is a state diagram of an aluminum-silicon binary alloy;
FIG. 3 is a state diagram of an Al-Mg binary alloy;
FIG. 4 is a graph of the solubility of iron in a magnesium-based alloy;
FIG. 5 is a state diagram of a magnesium-silicon binary alloy;
FIG. 6 is a state diagram of an Fe-Al binary alloy;
FIG. 7 is a state diagram of an Al-Mg-Si ternary alloy;
FIG. 8 shows the effect of iron and silicon removal in liquid phase condensation and centrifugal separation;
FIG. 9 is a critical vacuum for metal distillation speed;
FIG. 10 is a schematic view of a thermal aluminum magnesium co-production process;
FIG. 11 is a diagram of a centrifugal separation and distillation separation process arrangement;
FIG. 12 is a schematic view of an apparatus of an aluminum magnesium centrifugal separator;
FIG. 13 is a schematic view of the process of the centrifugal separation of aluminum and magnesium;
FIG. 14 shows the measurement of iron and silicon removal by centrifugal separation;
FIG. 15 is a schematic view of an apparatus of a continuous distillation separation furnace for aluminum and magnesium in example 1;
FIG. 16 is a schematic diagram of a distillation tray arrangement;
FIG. 17 is a schematic view of a vertical stacking of distillation trays;
FIG. 18 is the internal heating type double shell distillation furnace body in example 3;
FIG. 19 is a schematic view showing the apparatus of the continuous distillation separation furnace for aluminum and magnesium in example 3;
in the figure: 301. an aluminum-magnesium centrifugal separator 302, a centrifuge fixing cylinder wall 303, a centrifuge fixing cylinder protective cover plate 310, a centrifuge drum 311, a centrifuge drum bottom plate 312, a centrifuge drum outer cylinder wall 313, a centrifuge drum inner cylinder wall 314, a centrifuge drum top plate 317, a centrifuge drum inner cavity 318, a centrifuge drum annular liquid receiving groove 319, a centrifuge drum liquid injection channel 320, a liquid throwing hole 330, an original aluminum-silicon-iron-magnesium quaternary alloy liquid 340, an aluminum-magnesium alloy filtrate 350, a silicon iron filter residue 601, a regenerative heating furnace 602, a regenerative body and air channel 611, an aluminum-magnesium alloy remelting furnace 612, an aluminum-magnesium alloy block 613, an aluminum-magnesium alloy liquid 614, a vacuum liquid absorbing pipe 621, a magnesium distillation tower 622, a distillation tower tray 623, an aluminum liquid down-flow pipe 624, a pure aluminum liquid 625, an aluminum liquid holding furnace 626, an aluminum liquid dosing pump 630, a negative pressure spray vaporizing chamber 633, an atomizing water nozzle 634, a vaporizing negative pressure suction pipe and vacuum pump 641, a spiral magnesium scraper 642, a magnesium vapor baffle 643, a crystallized magnesium locking upper valve 645, a crystallized magnesium locking lower valve 646, a crystallized magnesium storage chamber 650, a total vacuum pipeline and vacuum pump 651, pure magnesium liquid 652, a magnesium liquid quantitative pump 653, a magnesium remelting furnace 661, a vacuum pumping pipeline 662, a vacuum breaking inflation pipeline 701, an outer shell 702, a hot flue gas inlet 703, a flue gas outlet 720, a refractory heat insulation layer 721, an inner shell 722, a hot flue gas pipeline distillation tray 763, an interlayer vacuum pipeline 802, an aluminum magnesium liquid junction area 803, an aluminum magnesium liquid falling hole 804, a fence 805, a flow channel cofferdam 806, an aluminum magnesium liquid flow channel 807, an aluminum magnesium liquid returning flow direction tray 821, a k-stage distillation tray 822, a k-stage distillation junction area 823, a k-stage distillation falling hole 828, A liquid receiving position 831 of a kth-stage distillation tray, a kth + 1-stage distillation tray 832, a flow receiving area 833 of a kth + 1-stage distillation tray, a dropping hole 838 of a kth + 1-stage distillation tray, a liquid receiving position 848 of a kth + 1-stage distillation tray, a liquid receiving position P1 of a kth + 2-stage distillation tray, a working vacuum pressure P2 of the double-shell distillation furnace and a sandwich buffer pressure of the double-shell distillation furnace.
Detailed Description
The present invention will be further described with reference to the following examples and accompanying drawings.
Example 1:
high-alumina fly ash and bauxite tailings are proportioned to achieve the aluminum-silicon ratio of 1.5, stoichiometric bituminous coal is added as a carbonaceous reducing agent, aluminum, silicon and iron oxide in ash content brought by the bituminous coal are counted, the mixture is fully mixed and ground, pulp waste liquid is used as a binder, a pressing ball is kneaded and dried to prepare a furnace charge with certain strength, the furnace charge is added into a 16500KVA modified alternating current ore furnace, the aluminum-silicon-iron alloy liquid is prepared through electrothermal reduction, the liquid outlet temperature is about 1500 ℃, certain carbide and unreduced oxide are mixed, and mixed with mixed halogen salt for refining, so that the initial aluminum-silicon-iron alloy containing 10 percent of iron, 30 percent of silicon and 60 percent of aluminum is obtained. The power consumption of each ton of the ferro-silicon-aluminum ternary alloy is 13000 kwh.
And (3) carrying out mutual melting on the ternary alloy liquid and the collected crude magnesium: preheating and drying crude magnesium in an aluminum-magnesium mutual smelting furnace, adding a small amount of ternary alloy liquid in batches, stirring and standing, after a period of time, completely mixing, and slowly heating to 1000 ℃, wherein the amount of the ternary alloy liquid is 1000kg, the amount of the crude magnesium is 1200 kg. The overall flow is shown in fig. 11.
Fig. 12 is an arrangement of equipment and connections for the centrifugation stage, and fig. 13 is a fragmented display of the centrifugation process. The mixed aluminum-silicon-iron-magnesium quaternary alloy liquid is added into the inner cavity 317 of the centrifugal drum through the liquid injection channel 319 of the centrifugal drum, and at the moment, the centrifugal drum 310 is positioned at a liquid injection station and is not positioned on the aluminum-magnesium centrifugal separator 301. The top plate 314 of the centrifugal rotary drum is covered, and inert gas is filled for protection, so that the original aluminum-silicon-iron-magnesium quaternary alloy liquid 330 in the inner cavity 317 of the centrifugal rotary drum is not contacted with the outside, and magnesium is protected from being oxidized by air. The inner wall 313 of the centrifugal drum and the bottom plate 311 of the centrifugal drum absorb the heat of the quaternary alloy liquid to increase the temperature, the centrifugal drum is kept standing for a period of time, the whole centrifugal drum 310 is lifted up when the temperature is uniform and reaches a predetermined temperature, for example, 530 ℃, and is arranged inside the fixed drum wall 302 of the centrifuge, and the fixed drum is covered with the protective cover plate 303 of the fixed drum of the centrifuge for fixation. Then the aluminium magnesium centrifuge 301 is started to rotate at a speed of 1000 rpm.
The diameter of the inner cavity 317 of the centrifugal rotary drum 310 is 1 meter, the height of the inner wall 313 of the centrifugal rotary drum is 700mm, the total volume is about 540 liters, 700 kilograms of the original Al-Si-Fe-Mg quaternary alloy liquid 330 is injected at one time, and a certain free space is left. The liquid throwing holes 320 are through holes, the holes are in a circular truncated cone shape from inside to outside, the diameter of the innermost side of each hole is 6mm, the diameter of the outermost side of each hole is 8mm, the holes are evenly distributed on the inner cylinder wall 313 of the centrifugal rotary drum, and the total area of the holes occupies 10-15% of the outer surface area of the inner cylinder wall 313 of the centrifugal rotary drum.
The aluminum-magnesium centrifugal separator 301 rotates to perform solid-liquid separation operation, the solid-phase particles separated from the original aluminum-silicon-iron-magnesium quaternary alloy liquid 330 comprise almost all iron and silicon elements, part of the aluminum and magnesium elements combined with iron and silicon, and the rest is low-iron low-silicon aluminum-magnesium alloy liquid, under the action of centrifugal force, the aluminum-magnesium alloy liquid is thrown out from the gap of the solid-phase particles and moves away from the rotating center, passes through the liquid throwing hole 320 to reach the centrifugal drum annular liquid receiving groove 318, continuously jets out and collides with the centrifugal drum outer cylinder wall 312, is cooled and condensed after contacting with the centrifugal drum outer cylinder wall 312, and is adhered to the centrifugal drum outer cylinder wall 312, and at the moment, the aluminum-magnesium alloy filtrate 340 is stored in the centrifugal drum annular liquid receiving groove 318 and is physically separated from the ferrosilicon filter residue 350 staying in the inner cavity 317 of the centrifugal drum.
The original Al-Si-Fe-Mg quaternary alloy liquid 330 is sampled and analyzed before cooling and condensation, the iron content is 4.55 percent, the silicon content is 13.64 percent, and the sample analysis from the Al-Mg alloy filtrate 340 after centrifugal separation operation shows that the iron content is 0.01 percent and the silicon content is 0.24 percent, which shows that the aluminum element in the original Al-Si-Fe is completely separated from the silicon and the iron. The total metering result is that the original aluminum-silicon-iron-magnesium quaternary alloy liquid 330 accounts for 2200kg, after centrifugal separation, the aluminum-magnesium alloy filtrate 340 accounts for 1150kg, the rest is the ferrosilicon filter residue 350, and a little oxidation loss of magnesium and aluminum is also counted in the ferrosilicon filter residue 350.
Through centrifugal separation, 600kg of aluminum element, 460kg of the aluminum element enters the aluminum-magnesium alloy filtrate 340, and the rest is in the ferrosilicon filter residue 350, so that the extraction rate of aluminum reaches 76.7%.
After the obtained aluminum-magnesium alloy filtrate 340 is condensed, 41% of aluminum, 58.7% of magnesium, 0.24% of silicon and only 0.01% of iron are contained, and the results of removing iron and reducing silicon are shown in fig. 14. This large proportion of aluminum-magnesium alloy has four uses even without distillation separation. The aluminum-magnesium alloy with large proportion is very brittle, is not like common metal, is more similar to the characteristics of ceramics, is particularly easy to mechanically crush and grind into fine powder, while the common aluminum alloy or the magnesium alloy is very sticky and is not easy to process into fine powder when being mechanically processed into powder, so that the aluminum-magnesium alloy has better service performance in certain occasions needing the aluminum-magnesium powder, such as the fields of military industry, civil fireworks and crackers and the like, if further specific requirements on the proportion of the aluminum and the magnesium are provided, certain aluminum or magnesium can be added after remelting, or corresponding components of aluminum-magnesium alloy filtrate 340 are preset when the magnesium is added in the early period, and the massive and flaky aluminum-magnesium alloy can be sold to enterprises for manufacturing the aluminum-magnesium alloy powder.
The more common and thorough practice suitable for large industrial scale is to use a continuous distillation furnace to realize the complete finishing separation of aluminum and magnesium for the concretions of the aluminum-magnesium alloy filtrate 340.
The protective cover plate 303 of the centrifuge fixing barrel of the aluminum magnesium centrifuge 301 is opened, the whole centrifuge bowl 310 is taken out from the centrifuge fixing barrel wall 302 and moved to the cleaning station of the centrifuge bowl 310, so that the aluminum magnesium centrifuge 301 is emptied for the next alloy liquid to be separated and the centrifuge bowl 310 contained therein. And opening the top plate 314 of the centrifugal drum, and manually taking out the concretions of the aluminum-magnesium alloy filtrate 340 in the annular liquid receiving groove 318 of the centrifugal drum or ejecting the concretions by a mechanical tool for distillation separation. Meanwhile, the residual ferrosilicon filter residue 350 in the inner cavity 317 of the centrifugal drum is manually taken out or ejected by a mechanical tool to be used as a byproduct, a composite deoxidizer for steel production and a reducing agent for smelting magnesium by a hot method, or the ferrosilicon filter residue is subjected to proper component adjustment before the application.
The solidification product of the al-mg alloy filtrate 340 as the main product enters a distillation separation link, as shown in fig. 15. The solidified block or sheet of the al-mg alloy filtrate 340 is put into an al-mg alloy remelting furnace 611 as an al-mg alloy block 612 in the distillation step, and at this time, a certain amount of al-mg alloy liquid 613 is already retained in the al-mg alloy remelting furnace 611, and as a continuous production process, a certain amount of melted al-mg alloy liquid 613 is always retained in the crucible of the al-mg alloy remelting furnace 611, and the newly added al-mg alloy block 612 is melted in the existing al-mg alloy liquid 613. In this embodiment, the al-mg alloy remelting furnace 611 is placed in the regenerative heating furnace 601, and the regenerative heating furnace 601 is switched to use the heat accumulator and the air channel 602, so as to ensure high energy efficiency of gas heating.
The almag liquid 613 contained in the almag remelting furnace 611 is sucked into the magnesium distillation tower 621 through a vacuum suction pipe 614, naturally flows downwards from the top or middle upper part of the magnesium distillation tower 621, falls down through repeated baffling, and is laid on the multistage distillation tray 622 to form a thin layer of the almag liquid, magnesium evaporation occurs due to heating, and enters a gas phase, and magnesium vapor leaves the magnesium distillation tower 621 from the magnesium vapor pipe 630 under the vacuum suction effect and enters the magnesium condenser 631 to be condensed into a liquid or solid state. In this embodiment, the magnesium distillation tower 621 is placed in the regenerative heating furnace 601, the magnesium distillation tower 621 is made of heat-resistant steel, the outer wall is heated by flame or hot air, the temperature is maintained at 1000 ℃, the internal vacuum degree is 0.1-133Pa, and the vacuum system forms continuous suction force on the magnesium distillation tower 621 through the total vacuum pipeline and the vacuum pump 650, and the magnesium condenser 631 and the magnesium vapor pipe 630 which are connected in series.
The distillation tray 622 of fig. 16 is a disk-shaped device for evaporation of the almag liquid, and a plurality of distillation trays are vertically stacked in the magnesium distillation tower 621 for the almag liquid 613 to flow and lay down on it layer by layer for evaporation, and so that the residual liquid can continue to flow downward. On each distillation tray 622, the periphery is a fence 804 with the height of 30-60mm, one side of the distillation tray 622 is provided with an aluminum magnesium liquid junction area 802, the other side is provided with an aluminum magnesium liquid falling hole 803, an aluminum magnesium alloy liquid 613 flowing down from the upper distillation tray 622 falls into the aluminum magnesium liquid junction area 802, then flows along an aluminum magnesium liquid channel 806 restrained by a channel cofferdam 805 in a zigzag mode in the direction indicated by the aluminum magnesium liquid retracing flow direction 807 until the aluminum magnesium liquid is fully paved and passes through the surface of the whole distillation tray 622, and finally flows from the aluminum magnesium liquid falling hole 803 on the other side to the lower distillation tray 622.
Each distillation tray 622 is arranged opposite to the aluminum magnesium liquid falling hole 803 of the next distillation tray 622, as shown in fig. 17, a k-th distillation tray 821 is positioned above a k + 1-th distillation tray 831, an aluminum magnesium alloy liquid 613 firstly falls to a k + 1-th distillation tray junction area 822 according to the position indicated by a k-th distillation tray junction position 828, then flows through all flow channels of the k-th distillation tray 821, finally falls to the k + 1-th distillation tray junction area 832 from the k-th distillation tray junction area 823, and gradually flows through the flow channels of the current layer from the k + 1-th distillation tray junction area 832 as indicated by the k + 1-th distillation tray junction position 838, and finally flows downwards from the k + 1-th distillation tray junction area 833 as indicated by a k + 2-th distillation tray junction position 848 in the figure. The distillation tray 622 may be made of graphite, ceramic, or composite material, such as a structure with a heat-resistant steel surface plated with a carbide or nitride coating resistant to corrosion by high-temperature molten aluminum or molten magnesium.
While the aluminum-magnesium alloy liquid 613 flows through each distillation tray 622, magnesium vapor is continuously heated and evaporated and leaves the aluminum-magnesium alloy liquid 613, so that the magnesium concentration in the aluminum-magnesium alloy liquid 613 is continuously reduced, the magnesium concentration is already low or even close to zero after reaching the distillation tray 622 on the lowest layer, and the residual pure aluminum liquid 624 flows into an aluminum liquid holding furnace 625 through an aluminum liquid downstream pipe 623, wherein the aluminum liquid holding furnace 625 is communicated with the atmosphere and is in a normal pressure state. The height of the pure aluminum liquid 621 in the aluminum liquid downstream pipe 623 and the magnesium distillation tower 621 should be about 3.5-5 m, so that the aluminum liquid column can help to maintain the vacuum in the magnesium distillation tower 621, i.e., the liquid column is sealed. In low-altitude plain areas, the air pressure is higher, the liquid column height is about 4.5 meters, and in high-altitude plateau areas, the air pressure is lower, and the liquid column height is only 4 meters. The pure aluminum liquid 624 contained in the aluminum liquid holding furnace 625 can be directly refined and alloyed in situ, or can be directly removed by using a device such as an aluminum liquid quantitative pump 626 or a vacuum ladle, and the liquid state is transported to the next link for further downstream processing. In this embodiment, the magnesium distillation tower 621 has an inner diameter of 700mm and an inner height of 4 m, and is made of heat-resistant steel, the diameter of the built-in distillation tray 622 is slightly smaller than that of the magnesium distillation tower 621, 35 layers of distillation trays 622 are provided in total, the total evaporation area is 11 square meters, and about 150kg of magnesium can be distilled per hour.
As for the flow rate control of the vacuum pipette 614, the flow rate is generally determined by a method of theoretical design in advance and correction by industrial trial production. The vacuum suction pipe 614 is provided with an openable and closable control mechanism capable of controlling the amount of liquid flowing. The size of the open and close valve on the vacuum pipette 614 can be determined by several attempts at a given distillation temperature and vacuum level. And through setting the flow from large to small or from small to large, sampling and analyzing the magnesium-containing proportion in the pure aluminum liquid 624 flowing out from the tail end of the aluminum liquid downstream pipe 623, wherein if the magnesium content exceeds a set value, the set flow is too large, and the adjustment is required to be reduced.
In the regenerative heating furnace 601, a plurality of magnesium distillation columns 621 may be provided to operate simultaneously. In this embodiment, in order to reduce the cost of distillation energy, a gas heat accumulating type combustion heating is adopted, that is, for the magnesium distillation tower 621, the gas heat accumulating type combustion heating is an external heating type, and non-contact isolated heating must be adopted. Therefore, the magnesium distillation tower 621 is subjected to the pressure with the pressure difference of the inside and the outside being close to one atmospheric pressure, and is subjected to the action of high temperature of about 1000 ℃, the magnesium distillation tower 621 is generally made into a cylindrical shape, the diameter is not suitable to be large, for example, the diameter of 700 plus 1000mm, if the diameter is too large, a thickened heat-resistant steel shell is required, the manufacturing cost is high, and the heat transfer resistance is also larger, so that the arrangement mode that a plurality of magnesium distillation towers 621 are arranged in parallel in one heat accumulating type heating furnace 601 is preferably adopted.
The evaporated magnesium vapor enters the magnesium condenser 631 through the magnesium vapor pipe 630, and the remaining non-condensable gases bypass a magnesium vapor baffle 642 and enter the bulk vacuum line and vacuum pump 650. The magnesium condenser 631 shell is a device keeping low temperature, which can adopt water cooling, in order to save water and better control temperature, a negative pressure spray vaporization chamber 632 is adopted, one or more spray water nozzles 633 are arranged in the negative pressure spray vaporization chamber, when the temperature of the magnesium condenser 631 needs to be reduced, the spray water nozzles 633 are opened to spray water mist to the negative pressure spray vaporization chamber 632, the negative pressure spray vaporization chamber 632 is connected with a vaporization negative pressure suction pipe and a vacuum pump 634, the inside is negative pressure or vacuum, so that the water and the water mist in the negative pressure state below one atmospheric pressure are vaporized, the vaporization temperature is lower than 100 ℃, the vacuum degree is set so that the water vaporization temperature is lower than 70 ℃, scaling is avoided, the water vaporization absorbs a large amount of heat, the temperature of the magnesium condenser 631 shell is reduced, and the metal magnesium vapor can be. The magnesium vapor is condensed into solid crystals on the inner wall of the magnesium condenser 631, and the solid crystals are accumulated more and more, and in order to maintain continuous production, a spiral magnesium scraper 641 is arranged in the middle of the magnesium condenser 631, similar to a rotary spiral scraper, and the crystallized magnesium condensed on the wall is scraped by a spiral cutter head to become magnesium powder or powdery crystals, and the magnesium powder falls below the magnesium condenser 631, and is periodically opened through a crystallized magnesium locking upper valve 643 to drop the magnesium powder into a crystallized magnesium storage chamber 646, and the crystallized magnesium storage chamber 646 is communicated with the atmosphere through a crystallized magnesium locking lower valve 645. Before the crystalline magnesium locking lower valve 645 is opened, the crystalline magnesium locking upper valve 643 is strictly locked, the crystalline magnesium storage chamber 646 is filled with inert gas, generally argon or nitrogen, through the vacuum-breaking gas-filling pipeline 662, so that the internal pressure of the crystalline magnesium storage chamber 646 is balanced with the external atmospheric pressure, and then the crystalline magnesium locking lower valve 645 is opened, so that magnesium fragments stored in the crystalline magnesium storage chamber 646 fall down. If the recycling is realized, the magnesium fragments are directly collected and returned to the most front end of the ferro-silicon-aluminum ternary alloy liquid mutual melting link. If the crystallized magnesium chips are to be remelted for sale as a commodity or further processed further, the magnesium chips in the crystallized magnesium storage chamber 646 fall through the opened crystallized magnesium lock down valve 645 into a magnesium remelting furnace 653, are heated to be remelted into pure magnesium liquid 651, and are removed by a device such as a molten magnesium injection dosing pump 652 or the ingot is directly withdrawn. After the crystallized magnesium storage chamber 646 is emptied, the lower locking valve 645 is closed in time, the crystallized magnesium storage chamber 646 is vacuumized through the vacuum pumping pipeline 661 to reach the same vacuum degree as the magnesium condenser 631, so that the upper locking valve 643 for crystallized magnesium is opened to receive a new batch of scraped crystallized magnesium powder.
In this embodiment, the components of the final pure aluminum liquid 624 are mixed and used according to 6061 aluminum alloy and other silicon-containing casting aluminum alloys.
Example 2:
the components of the recovered mixed waste aluminum after melting are 3.5% of iron, 7.6% of silicon and 2.3% of magnesium, and the components can not be separated in advance by a mechanical method. The method adopts the recovered waste magnesium to carry out mutual melting, centrifugal filtration for iron removal and distillation separation, thereby realizing the synergistic impurity removal and regeneration of the aluminum and the magnesium.
The waste magnesium contains 10.1 percent of aluminum, 0.2 percent of iron and 0.5 percent of silicon, which are added according to 50 percent of the amount of the waste aluminum, and the waste magnesium is melted in an induction furnace or a gas heating furnace to form aluminum-magnesium-silicon-iron quaternary alloy liquid, and then the aluminum-magnesium-silicon-iron quaternary alloy liquid enters a centrifugal rotary drum for separation.
Because the proportion of solid phase precipitates which are possibly formed is less, after the original Al-Si-Fe-Mg quaternary alloy liquid 330 is injected into the centrifugal rotating drum 310, a certain amount of the ferrosilicon filter residues 350 which are centrifugally filtered in the previous batches are added, and the cooling effect is realized.
After centrifugal filtration, most of the iron in the original Al-Si-Fe-Mg quaternary alloy liquid 330 enters the ferrosilicon filter residue 350, and the silicon is reduced to a great extent. The distilled pure aluminum liquid 624 contains less than 0.3% of iron and about 2% of silicon, meets the component requirements of most cast aluminum alloys, and is recycled as the cast aluminum alloy by adding certain alloy elements.
Meanwhile, the distilled and condensed pure magnesium solution 651 is also purified, the aluminum content is less than 0.2 percent, and the method is suitable for preparing common magnesium alloy.
The impurity removal and regeneration of the waste aluminum and the waste magnesium are realized, and the economic value and the application field are greatly improved compared with the prior art.
Example 3:
the magnesium distillation tower 621 adopted in the embodiment 1 is externally heated, and the inside is vacuum to realize the evaporation separation of magnesium, because the shell of the magnesium distillation tower 621 needs to bear high temperature and high pressure, the diameter of the magnesium distillation tower 621 cannot be too large, and often cannot exceed 1 meter, so the volume is smaller, and in addition, from the pressure bearing angle, the magnesium distillation tower is preferably cylindrical, and the possible other shapes are limited.
In this embodiment, a magnesium distillation tower 621 suitable for large-scale production, i.e., a double-shell internal heating type distillation furnace, is used. As shown in fig. 18 and 19. FIG. 18 shows the double shell internal heat distillation furnace itself, and FIG. 19 shows the whole connection relationship.
The housing 701 is made of a common steel plate, and can be a flat or curved steel plate which is thickened or provided with reinforcing ribs and reinforcing supports, or a cylinder structure suitable for pressure resistance. The inner shell 721 is made of a common steel plate and is formed in a rectangular parallelepiped shape surrounded by common planes. The inner shell 721 is provided with a refractory heat insulating layer 720 therein, which is made of masonry heat insulating material and refractory material, and the innermost layer of refractory material is made of aluminum-magnesium or graphite so as not to react with magnesium vapor in vacuum. And (3) sealing a gap between the outer shell 701 and the inner shell 721, vacuumizing to enable the interlayer buffer pressure P2 of the double-shell distillation furnace to be consistent with or close to the working vacuum pressure P1 of the double-shell distillation furnace in the inner shell 721, and ensuring the vacuum degree in the interlayer by using an interlayer vacuum pipeline 763. The heating device is placed inside the refractory heat insulating layer 720 by means of resistance heating or radiant heat pipe heating. The hot flue gas duct distillation tray 722 can be composed of a plurality of stacked hot flue gas ducts which are closely arranged or ribs are welded, the type of the heating pipes which are tightly combined with the distillation tray 722 is shown in fig. 18 and fig. 19, or the resistance heating pipes and the hot flue gas ducts which are thermally radiated are additionally and independently arranged inside the refractory heat insulation layer 720, the heat is transferred to the aluminum-magnesium alloy liquid flowing on the distillation tray 722 of the hot flue gas duct by means of radiation heat, and the structure and the function of the distillation tray 722 of the hot flue gas duct are the same as those of the distillation tray 622 in the embodiment 1. In the embodiment, the gas radiation heat pipe is adopted for heating so as to save energy cost, the gas radiation heat pipe is a hollow heat-resistant steel or ceramic pipe, hot gas and smoke are circulated inside the gas radiation heat pipe, the temperature can reach 900-.
By adopting the double-shell internal heating type distillation furnace, the respective 'division' of the work is realized by being equivalent to a double-shell furnace shell: the outer shell 701 bears pressure, the inner shell 721 is heated, the heated inner furnace shell does not bear pressure, and the pressure-bearing outer shell 701 is not heated, so that large-scale production is easily realized, for example, the area of a hot flue gas pipeline distillation tower plate 722 can reach the evaporation area of 3X3 square meters or 5X5 square meters, if tens of layers of hot flue gas pipeline distillation tower plates 722 are provided, the total evaporation area can reach hundreds of square meters, the amount of magnesium evaporated in each hour reaches more than several tons, and large-scale production is realized.
Example 4:
the solid ferrosilicon residue 350 obtained by centrifugal filtration has various directions of use as a by-product. If the magnesium in the steel is not distilled and separated, the steel can be used as a magnesium-smelting reducing agent and a steel composite deoxidizer. The magnesium reducing agent used in the hot smelting is the most preferable scheme. The whole material realizes closed loop circulation.
The ferrosilicon filter residue 350 is transported to a hot-process magnesium smelting workshop, is mixed with dolomite calcined dolomite and then is pressed into balls, enters a horizontal tank or a vertical tank for smelting magnesium by a Pidgeon process, and is heated in vacuum, different from the common ferrosilicon, Mg2Si in a reducing agent is decomposed at high temperature in vacuum, and magnesium vapor is released to be condensed. Then the residual aluminum and silicon are subjected to reduction reaction with MgO in the calcined dolomite in sequence and slag-forming reaction with CaO in the calcined dolomite.
Because of the participation of aluminum, the utilization rate of a reducing agent, the utilization rate of calcined dolomite, the reduction temperature and the vacuum degree, the service life of a reduction tank, the yield of unit time, the yield of unit equipment and the energy consumption of fuel gas are optimized and improved to a greater extent than those of the common #75 silicon iron, and because the obtained crude magnesium does not need to be refined, the final capacity of furnace burden and the reducing agent can be squeezed out by adopting high-temperature high vacuum, so that the metallic impurities of silicon, aluminum, iron and calcium of the crystallized crude magnesium are improved, and the yield of the alloy is increased for the crude magnesium which is subsequently fused with the aluminum-silicon-iron ternary alloy liquid. Among them, calcium, which is more active, is easily substituted with a desired metal element in both magnesium and aluminum.
If the ferrosilicon filter residue 350 is required to be made into ferrosilicon or ferrosilico-aluminum strictly meeting the grade requirement, distilling and demagging can be carried out in a closed electric arc furnace or an induction furnace, vacuum breaking is carried out, condensed magnesium is taken out, waste steel and ferrosilicon are added to adjust components until the components meet the grade requirement, or an aluminothermic method is adopted, materials containing ferric oxide and silicon oxide are added to consume aluminum elements in the materials, the iron and the silicon are reduced to be alloyed, the alloy meeting the grade is obtained, and the byproduct high-aluminum slag is used as a raw material required by the refractory material industry and the like.
Claims (8)
1. An electric heating aluminum smelting device is characterized by comprising the following parts:
at least one aluminium magnesium centrifuge (301); the aluminum-magnesium centrifugal separator (301) is provided with a space enclosed by a centrifuge fixing barrel wall (302) and a centrifuge fixing barrel protection cover plate (303), a detachable centrifugal drum (310) is arranged in the space, the centrifugal drum (310) comprises a centrifugal drum bottom plate (311), a centrifugal drum outer barrel wall (312), a centrifugal drum inner barrel wall (313) and a centrifugal drum top plate (314), the centrifugal drum outer barrel wall (312) and the centrifugal drum inner barrel wall (313) are arranged between the centrifugal drum bottom plate (311) and the centrifugal drum top plate (314) in the same circle center, an annular centrifugal drum liquid receiving groove (318) in annular arrangement is formed between the centrifugal drum outer barrel wall (312) and the centrifugal drum inner barrel wall (313), an internal space enclosed by the centrifugal drum inner barrel wall (313) is a centrifugal drum inner cavity (317), and a centrifugal drum inner cavity (317) is formed between the centrifuge fixing barrel protection cover plate (303) and the centrifugal drum top plate (314) The liquid injection channel (319) of the centrifugal rotating drum is characterized in that a plurality of liquid throwing holes (320) are uniformly formed in the inner wall (313) of the centrifugal rotating drum;
at least one aluminum-magnesium continuous distillation separation furnace; the aluminum-magnesium continuous distillation separation furnace comprises an aluminum-magnesium alloy remelting furnace (611), a magnesium distillation tower (621), an aluminum liquid heat preservation furnace (625), a magnesium condenser (631), a crystallized magnesium storage chamber (646), a total vacuum pipeline and a vacuum pump (650); the aluminum magnesium alloy remelting furnace (611) is communicated with a top feeding hole of the magnesium distillation tower (621) through a vacuum liquid suction pipe, a bottom discharging hole of the magnesium distillation tower (621) is communicated to an aluminum liquid heat preservation furnace (625) through an aluminum liquid forward flow pipe (623), the top of the magnesium distillation tower (621) is further communicated with a top feeding hole of a magnesium condenser (631) through a magnesium steam pipe (630), the bottom discharging hole of the magnesium condenser (631) is communicated with a crystallized magnesium storage chamber (646), and the top of the magnesium condenser (631) is further communicated with a total vacuum pipeline and a vacuum pump (650).
2. An electric aluminum smelting apparatus according to claim 1, wherein: a plurality of layers of distillation trays (622) are vertically arranged in the inner cavity space of the magnesium distillation tower (621), one side of the top of each distillation tray (622) is provided with an aluminum magnesium liquid flow receiving area (802), the other side of each distillation tray is provided with an aluminum magnesium liquid falling hole (803), the outer edge of the top of each distillation tray (622) is surrounded by a baffle (804), and a circuitous aluminum magnesium liquid flow channel (806) formed by a flow channel cofferdam (805) is arranged between the aluminum magnesium liquid flow receiving area (802) and the aluminum magnesium liquid falling hole (803).
3. An electric aluminum smelting apparatus according to claim 1 or 2, wherein: the shell of the magnesium distillation tower (621) adopts a double-layer steel structure and comprises an outer shell (701) and an inner shell (702), an interlayer between the outer shell (701) and the inner shell (702) is subjected to vacuum treatment, and a fireproof heat insulation layer (720) is built on the inner wall of the inner shell (702).
4. An electric aluminum smelting apparatus according to claim 1, wherein: magnesium condenser (631) inside has a cooling cavity, the top of cooling cavity communicates magnesium steam pipe (630) and total vacuum pipe and vacuum pump (650) respectively, and bottom intercommunication crystallized magnesium apotheca (646), the outside parcel of cooling cavity is provided with the heat sink, be provided with the spiral in the cooling cavity and scrape magnesium ware (641), the top still is provided with magnesium vapour baffle (642) in the cooling cavity, magnesium vapour baffle (642) are located between two connectors of cooling cavity and magnesium steam pipe (630) and total vacuum pipe and vacuum pump (650).
5. An electric aluminum smelting apparatus according to claim 4, wherein: the cooling device comprises a negative pressure spray vaporization chamber (632), a vaporization negative pressure suction pipe and a vacuum pump (634) which are connected with the negative pressure spray vaporization chamber (632), and a plurality of atomization water nozzles (633) are arranged in the negative pressure spray vaporization chamber (632).
6. An electric aluminum smelting apparatus according to claim 1 or 4, wherein: a crystallized magnesium locking upper valve (643) is arranged between the magnesium condenser (631) and the crystallized magnesium storage chamber (646), and a crystallized magnesium locking lower valve (645) is arranged at a discharge opening of the crystallized magnesium storage chamber (646).
7. An electric aluminum smelting apparatus according to claim 1, wherein: the crystallized magnesium storage chamber (646) is respectively communicated with a vacuum pumping pipeline (661) and a vacuum breaking inflation pipeline (662).
8. An electric aluminum smelting apparatus according to claim 1, wherein: and the height of the aluminum liquid concurrent flow pipe (623) is calculated by dividing local atmospheric pressure by standard atmospheric pressure and multiplying by 4.5 m.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921541678.5U CN211311551U (en) | 2019-09-17 | 2019-09-17 | Electric heating aluminum smelting device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921541678.5U CN211311551U (en) | 2019-09-17 | 2019-09-17 | Electric heating aluminum smelting device |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113621823A (en) * | 2021-08-13 | 2021-11-09 | 西安交通大学 | Method and device for preparing high-purity metal or alloy by efficient distillation |
| CN115283593A (en) * | 2022-08-18 | 2022-11-04 | 重庆新钰立金属科技有限公司 | Forming method of aluminum forging of generator oil tank frame |
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2019
- 2019-09-17 CN CN201921541678.5U patent/CN211311551U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113621823A (en) * | 2021-08-13 | 2021-11-09 | 西安交通大学 | Method and device for preparing high-purity metal or alloy by efficient distillation |
| CN115283593A (en) * | 2022-08-18 | 2022-11-04 | 重庆新钰立金属科技有限公司 | Forming method of aluminum forging of generator oil tank frame |
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