CN115710642A - Chlorine and ammonia-containing zinc dross microwave vacuum smelting method and microwave vacuum furnace - Google Patents
Chlorine and ammonia-containing zinc dross microwave vacuum smelting method and microwave vacuum furnace Download PDFInfo
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Abstract
The invention discloses a microwave vacuum smelting method of zinc dross containing chlorine and ammonia and a microwave vacuum furnace thereof, wherein the zinc dross containing chlorine and ammonia components and metal zinc particles, carbon powder and a binder are mixed to be made into blocks or clusters, the blocks or clusters are placed in the microwave vacuum furnace, the chlorine and the ammonia are decomposed at 900 +/-50 ℃, and then the zinc is reduced and steamed at 1200-1300 ℃; removing dust from chlorine and ammonia gas, discharging by a vacuum pump, and absorbing and washing by clear water, weak alkaline water or weak acid water; condensing the zinc vapor by circulating water to obtain metal zinc liquid, and recovering the metal zinc liquid cast ingot; and returning the zinc steaming residue to a zinc system or a rotary kiln to recover valuable components. The method has the advantages of short flow, low energy consumption, less three wastes, high recovery rate, low cost and good social and economic benefits.
Description
Technical Field
The invention belongs to the field of zinc smelting and comprehensive recovery, and particularly relates to a method for recovering metal zinc from zinc dross containing chlorine and ammonia through microwave vacuum carbothermic reduction and a microwave vacuum furnace.
Background
The zinc smelting by fire method or wet method has the process of refined zinc ingot casting. In the process, after the zinc sheets are melted, the oxide skin of the original zinc and the metal zinc are separated by ammonium chloride slagging. During the slagging-off and slagging-off processes, a plurality of fine metal zinc particles are inevitably removed along with the slag, so that the zinc content of the dross reaches more than 80 percent, even more than 93 percent. The scum generally contains 2-5% of chlorine and ammonia, 0.5-1% of iron and the yield is about 50 kg/ton of zinc. 1 ten thousand tons of zinc ingots are cast to produce 500 tons of zinc dross, and according to the current production of 600 ten thousand tons of zinc per year in China, about 30 ten thousand tons of zinc dross per year are produced. In addition, similar zinc-containing dross is also generated when zinc-based alloys are processed. Therefore, how to treat the zinc dross and recover the metal zinc in the zinc dross has great significance in energy conservation and emission reduction.
At present, the treatment and comprehensive recovery of zinc dross are divided into two technologies of wet process and fire process, wherein the wet process is to dissolve dross with acid or ammonium and alkali, then purify and electrolyze to obtain zinc sheet or zinc powder or produce zinc ammonia chemical products. In the dissolving process, because the scum contains a large amount of metal zinc particles, a large amount of hydrogen is generated, and great fire hazard is caused to the safety of the environment. After dissolution, the zinc product can be obtained by purification, electrolysis and casting. Therefore, the process is long, the energy consumption is high, the waste water amount is large, and the recovery cost is high. At present pyrometallurgical recovery is at first carried out artifical screening to the dross, or washing, obtain the coarse grain or the mixed granule of thickness that mainly contain metallic zinc, pyrometallurgical founding at normal atmospheric temperature, because zinc dross can partial oxidation in slagging process, can generate one deck oxide film on granule zinc surface, influence the melting of zinc, the energy consumption is higher, also need the slagging to carry out the liquid-solid separation simultaneously, carry out artifical screening or washing in addition and not only increase labour's consumption, and dust pollution or waste water pollution are all great, therefore metallic zinc's rate of recovery is low, the waste residue waste water volume is big, recovery cost is high. If the metal zinc is directly evaporated in the electric heating vacuum furnace, the refined zinc is cast by condensation, although slagging is avoided, an oxidation layer is not generated, and the distilled zinc steam can be melted only at a high temperature of over 1200 ℃ due to the influence of the oxidation layer on the surface of zinc particles. The electric heat is slowly conducted in vacuum, the temperature of an electrode is required to be greatly higher than the temperature of materials, and the temperature of the electrode is required to be higher than 1300 ℃ when the temperature of the materials in a reaction chamber is required to reach more than 1200 ℃ in a common vacuum furnace, so that the electrode loss is large, the furnace wall around the electrode is also large in burning loss, the service life of a furnace body is short, and the maintenance and the overhaul are frequent. Therefore, the direct vacuum smelting is more difficult, and a successful example is not provided so far.
Disclosure of Invention
In order to overcome the defects of the wet method, the fire method and the pure vacuum smelting, the invention provides a method for performing carbon thermal reduction smelting by using a microwave vacuum furnace, which can be mixed with reduced carbon under the condition of not screening or washing scum with water, perform reduction smelting by using microwave radiation heating in the vacuum furnace, decompose zinc chloride and ammonium chloride to obtain metal zinc steam, condense cast ingots, simultaneously reduce zinc oxide, and recover zinc in zinc particles and zinc in scum ash. The method has the advantages of short flow, low energy consumption, less three wastes, high recovery rate, low cost and good social and economic benefits.
The technical scheme of the invention is as follows:
a microwave vacuum smelting method of zinc dross containing chlorine and ammonia comprises the following steps:
step 1: sampling and testing chemical components of the zinc dross, adding reduced carbon powder according to carbon/zinc =0.1-0.2, uniformly mixing, adding a binder according to 5-8% of the mixture, and drying in a brick shape or a pellet shape for later use; the zinc dross is dross generated when the metal zinc or zinc-based alloy is melted and is thermally fried by ammonium chloride to separate dross and metal, the total zinc content is more than or equal to 90 percent, the particle zinc is more than or equal to 70 percent, the chlorine is less than or equal to 5 percent, and the ammonia is less than or equal to 5 percent;
step 2: adding the zinc dross lumps prepared in the step (1) into a microwave vacuum furnace until the lower edges of gas guide windows of a reaction chamber and a condensation chamber are parallel, then closing a furnace door, and starting a vacuum pump to vacuumize; when the vacuum degree meets the requirement, starting microwave radiation, and when the furnace temperature reaches the required lower limit, starting circulating cooling water;
the microwave vacuum carbon thermal reduction smelting of the zinc dross is divided into two stages, wherein the first stage mainly has the task of low-temperature decomposition deamination and chlorine, and the second stage mainly carries out high-temperature carbon thermal reduction smelting;
the microwave vacuum smelting conditions of the first stage are as follows: microwave radiation frequency is 0.5-1GHz, vacuum degree is less than or equal to 600Pa, reaction chamber furnace temperature is 900 +/-50 ℃, condensation chamber furnace temperature is 500-550 ℃, and time is 1.5-2 hours;
the conditions of the microwave vacuum carbon thermal reduction smelting in the second stage are that the microwave radiation frequency is 1-10GHz, the vacuum degree is less than or equal to 600Pa, the temperature of the reaction chamber is 1200 +/-50 ℃, the temperature of the condensation chamber is 500 +/-50 ℃, the time is 3-5 hours or the vacuum degree at the smelting end point is less than or equal to 80Pa;
and step 3: the air outlet of the vacuum pump is hermetically connected with a pipeline of the waste gas washing tower, the leaching tower is subjected to negative pressure operation, and is leached by clear water or weak alkaline water with the pH =8-12 or weak acidic water with the pH =3-5, and the waste gas is discharged after reaching the standard;
and 4, step 4: after the second-stage smelting in the step 2 is finished, firstly closing the microwave radiation, closing the vacuum pump when the furnace temperature of the reaction chamber is reduced to below 600 ℃, and releasing the pressure to normal pressure by using inert gas to cast zinc ingots; and opening a furnace door of the reaction chamber to clean residues after the temperature of the reaction chamber is reduced to 300 +/-50 ℃, and cleaning the dust removal filter.
Further, the reduced carbon powder in the step 1 is one of activated carbon powder, carbon black powder or coke powder, the carbon content is more than or equal to 90%, and the particle size of the carbon powder is more than or equal to 40 meshes.
Further, the binder in step 1 is pulp.
Further, in the step 1, the brick blocks are of the size of a conventional brick, the pellet shape is that the diameter is =1-5cm, and the drying is carried out until the moisture is less than or equal to 10%.
Further, in the step 4, if the next furnace production is not performed immediately, the cooling water is stopped.
Further, in the step 4, the microwave vacuum carbon thermal reduction smelting of zinc dross containing chlorine and ammonium is completed, 0-1# refined zinc ingots are obtained, and the residues are returned to the rotary kiln for production.
The microwave vacuum smelting furnace in the step 2 comprises a reaction chamber, a condensation chamber and a dust removal filter, wherein the reaction chamber is provided with a furnace door, the reaction chamber is communicated with the condensation chamber through a liquid zinc flow port, the reaction chamber and the condensation chamber share a furnace iron shell, a heat insulation layer is arranged below the furnace iron shell, refractory bricks are laid below the heat insulation layer, a microwave radiation element is arranged below the refractory bricks of the reaction chamber, a material layer is arranged in the reaction chamber, and a reaction chamber temperature measurement pipe is arranged on the material layer; zinc liquid flowing out of a liquid zinc flow port of the reaction chamber enters a metal zinc liquid pool in the condensation chamber, and a metal zinc ingot casting port is arranged at the lower part of the metal zinc liquid pool; a metal condensation plate is arranged below a refractory brick of the condensation chamber, a condensation chamber temperature measuring pipe is arranged in the condensation chamber, the condensation chamber is connected with the dust removal filter through a vacuum exhaust pipe and an inert gas pressure relief pipe, and a vacuum gauge is arranged on the inert gas pressure relief pipe; the dust removing filter is connected with a vacuum pump through a pipeline connected with the vacuum pump.
The reaction chamber is built by silicon carbide plates or bricks below the air guide window, and a heat insulation layer between the reaction chamber and the furnace iron shell is made of diatomite bricks with the thickness of 6.5 cm; the metal condensing plate of the condensing chamber is made into a hollow water-through shape by a zinc corrosion resistant stainless steel plate or a titanium plate; the dust removal filter is made of stainless steel meshes of more than 60 meshes.
The working principle and the process characteristics of the invention are as follows:
the raw materials used in the invention do not contain other heavy metal components except that the total zinc content is more than or equal to 90 percent, the particle zinc content is more than or equal to 70 percent, the chlorine content is less than or equal to 5 percent, the ammonia content is less than or equal to 5 percent, and the iron content is about 1 percent, and the raw materials are a mixture of relatively pure metal zinc, zinc chloride and zinc oxide. By utilizing the characteristic that zinc chloride, zinc oxide, ferric oxide and ammonium chloride absorb microwave to generate heat, firstly, zinc chloride and ammonium chloride are decomposed at low temperature, and then zinc oxide is reduced by high-temperature carbon heat, wherein the ferric oxide is metal zinc and metal iron, and simultaneously a zinc oxide film on the surface of the particle zinc is damaged. Then utilizing the characteristic of vacuum to reduce melting point temperature of the material, quickly removing, decomposing and reducing the chlorine gas, ammonia gas, carbon dioxide and carbon monoxide gas produced by reaction to implement the first separation of metal material and non-metal material, and making metal zinc be evaporated into metal zinc vapour at higher temperature and separated from metal iron. The zinc vapor is condensed into liquid zinc and enters a zinc liquid pool, the non-metal gas can not be cooled into liquid and is quickly discharged by a vacuum pump, and the aim of directly smelting the refined zinc of No. 0-1 by microwave vacuum without sieving and washing is fulfilled. The first characteristic of the invention is that microwave vacuum carbon thermal reduction smelting technology must be adopted.
As is known, the propagation speed of the microwave in vacuum is the light speed, no energy loss exists in the propagation, and the microwave can penetrate into the substance to cause oscillation heating of molecules, atoms, ions and the like and catalyze chemical reactions. The microwave energy can make the material produce instantaneous high temperature inside and outside simultaneously, and has no heat transfer gradient and propagation time. The other non-microwave heating is that the heating body firstly heats, then the heating body is conducted to the surface of the substance, and then the heating body is conducted to the inside, so that the heat propagation gradient and the conduction time exist, and the space temperature is higher than the temperature in the substance. In the smelting in a pure vacuum furnace, because the space is not provided with a heat transfer medium, no matter internal heating or external heating is carried out, the heat absorption of a substance is slower, the longer time is needed, the difference between the space temperature and the internal temperature of the substance is larger, a zinc steam condensing chamber is arranged in the smelting furnace, and if the space temperature is greatly higher than the substance temperature, a lot of useless work has to be done to increase the energy consumption.
In the invention, zinc dross absorbs microwave to decompose and reduce at high temperature inside and outside the material instantly by the aid of the added reduced carbon, zinc oxide, zinc chloride, ammonium chloride and other components, and simultaneously destroys an oxide film of particle zinc, directly transfers heat energy to metal zinc, rapidly evaporates under the action of vacuum, enters a condensation chamber and is cooled into liquid zinc, and the whole process flows from a high-temperature section inside the material to a low-temperature section of the condensation chamber. Therefore, compared with other methods, the microwave vacuum carbon thermal reduction smelting of the zinc dross has the advantages of short time, high efficiency and obvious energy saving.
The second characteristic of the invention is that zinc dross microwave vacuum carbon thermal reduction smelting containing chlorine and ammonia is carried out in two sections. Because the material contains about 5 percent of zinc chloride and ammonium chloride, chlorine gas can be generated by decomposing at a lower temperature, ammonia gas is almost completely decomposed at 900 +/-50 ℃, and the decomposition temperature is also reduced under a vacuum condition. However, evaporation of metallic zinc also occurs in small amounts, and zinc chloride is generated by contact of zinc vapor with chlorine gas, and in particular, under the temperature condition of the condensation chamber, zinc chloride is not decomposed once generated, and in order to prevent secondary generation of zinc chloride, zinc chloride must be decomposed first at a relatively low temperature, and ammonium chloride must be removed. And increasing the temperature promotes carbothermic reduction of the zinc oxide and substantial evaporation of the metallic zinc. Ensuring the direct yield of the metallic zinc. Therefore, low temperature decomposition of dechlorination and ammonia in the first stage is necessary. The operation conditions of the first-stage dechlorination and the ammonia are set to be 0.5-1GHz of microwave radiation frequency, the temperature of the reaction chamber is controlled to be 900 +/-50 ℃, the vacuum degree is less than or equal to 600Pa, and the decomposition reaction time is 1.5-2 hours, so that the chlorine and the ammonia in the materials can be basically removed. At this time, carbothermic reduction of zinc oxide is still rare and metallic zinc is not largely evaporated. The second stage of operation raises the microwave radiation frequency to 1-10GHz, which raises the temperature inside the reaction chamber to about 1200 deg.c. So that the zinc oxide film on the surface of the zinc particles in the zinc oxide material can quickly undergo carbothermic reduction reaction, and the metal zinc can be greatly evaporated and can be completely evaporated after 3-5 hours. The microwave radiation heating temperature is increased along with the increase of radiation frequency, namely the heating capacity of high-frequency microwaves is greater than that of low-frequency microwaves, and the penetrating capacity of the low-frequency microwaves for substances is greatly higher than that of the high-frequency microwaves. The radiant power mainly affects the microwave radiant flux and affects the amount of microwave absorption by the material.
Through the explanation of the principle and the analysis of the characteristics, the invention is the most advanced technical process for smelting the dross containing chlorine and ammonia zinc at present, and 0-1# refined zinc products can be obtained with low energy consumption, low pollution, high efficiency and low cost.
Drawings
FIG. 1 is a schematic view of a microwave vacuum smelting furnace according to the present invention.
The labels in the figure are: 1. the device comprises a reaction chamber, 2, a condensation chamber, 3, a furnace door, 4, a furnace iron shell, 5, a heat preservation layer, 6, refractory bricks, 7, a microwave radiation element, 8, a material layer, 9, a reaction chamber temperature measuring pipe, 10, a liquid zinc flow port, 11, a metal condensation plate, 12, a metal zinc liquid pool, 13, a metal zinc ingot casting port, 14, a condensation chamber temperature measuring pipe, 15, a vacuum pumping pipe, 16, a dust removal filter, 17, a vacuum gauge, 18, an inert gas pressure relief pipe, 19 and a vacuum pump pipeline.
Detailed Description
The invention is further illustrated by the following figures and examples.
Example 1: when an enterprise founds electrolytic zinc sheets, ammonium chloride is used for stir-frying and slagging off at the temperature of about 500 ℃, zinc dross containing chlorine and ammonia is produced, dross is tested, the total zinc content is 94.3%, iron is 1.2%, chlorine is 2.8%, and ammonia is 1.53%, the dross is sieved by a 40-mesh sieve, coarse zinc particles on the sieve are obtained by 75.2%, undersize materials are obtained by 24.8%, and undersize materials are washed by water, and fine zinc particles are obtained by 10.3%; weighing 50kg of zinc dross, adding carbon black powder according to carbon/zinc =0.15, uniformly mixing, adding paper pulp according to 6% of the weight of the material, uniformly mixing to prepare 150 x 80 x 30mm bricks, and drying to obtain 7.5kg of zinc dross per brick.
Putting 40 blocks into a microwave vacuum oven; vacuumizing to about 600Pa, starting microwave radiation, wherein the microwave frequency is 1GHz, the temperature of the reaction chamber reaches 850 ℃ after 30 minutes, starting a condensation chamber to circulate cooling water, controlling the temperature of the condensation chamber to be 450-500 ℃, regulating the microwave frequency to be 0.6GHz after 60 minutes, controlling the temperature of the reaction chamber to be about 950 ℃, and regulating the cooling water to ensure that the temperature of the condensation chamber is between 500 and 550 ℃; increasing the microwave frequency of the reaction chamber to 5GHz after 90 minutes, increasing the temperature of the reaction chamber to about 1150 ℃ after 30 minutes, adjusting the microwave frequency to 10GHz, gradually increasing the temperature of the reaction chamber to about 1250 ℃ after 1.1 hour, simultaneously adjusting the circulating condensed water, and controlling the temperature of the condensation chamber to about 550 ℃; the time of low-temperature section is controlled to be 1.5 hours, and the time of high-temperature section smelting is controlled to be 2 hours.
The vacuum degree reaches about 100Pa, the microwave is closed, the temperature of the reaction chamber is gradually reduced, and the vacuumizing is stopped after the temperature reaches 600 ℃; cooling to about 550 ℃, filling nitrogen, and vacuumizing to normal pressure; after the temperature is reduced to 300 ℃, the furnace door is opened, the smelting residue is taken out, the weight reduction of the material reaches more than 90 percent, the material is sampled and tested after being crushed, the residue contains 1.5 percent of zinc, 11.3 percent of iron, trace of chlorine and ammonia, and the rest of the components are mainly residual carbon.
Example 2: the brick of example 1 was placed in a microwave vacuum oven and operated at a first stage of vacuum of 600Pa or less, a microwave frequency of 0.5GHz, a reaction chamber temperature of 850-900 deg.C, a condensing chamber temperature of 500 + -20 deg.C for 2 hours, a second stage of microwave frequency was initially adjusted to 10GHz, a reaction chamber temperature of 1250-1300 deg.C, a condensing chamber temperature of 550 + -10 deg.C for 2.5 hours. The vacuum degree at the operation end point is less than or equal to 80Pa, and the rest of the operation conditions are the same as those of the example 1. The weight of the material is reduced by 92 percent, the sampling and testing residue contains 0.53 percent of zinc, 12.1 percent of ferrum, and trace elements of chlorine and ammonia, and the quality of the metal zinc is 99.993 percent.
Example 3: some enterprises produce aluminum-containing zinc-base alloy, and zinc dross is fried with zinc chloride and ammonium chloride to obtain the alloy containing 87.5% of zinc, 1.2% of aluminum, 1.3% of iron, 5.2% of chlorine and 2.3% of ammonia. Pellets with a diameter of 1-5cm were prepared according to the formulation of example 1. 20kg of raw materials are placed in a microwave vacuum oven, the operation is carried out according to the conditions of the example 2, after the operation is finished, the weight of residues is reduced by 89.5%, the zinc content is 0.82%, the aluminum content is 10.3%, the iron content is 12.5%, the ammonia chloride content is trace, and the rest is mainly residual carbon. The distilled zinc has the mass of 99.986 percent.
Referring to fig. 1, the microwave vacuum oven comprises a reaction chamber 1, a condensation chamber 2 and a dust removal filter 16, wherein the reaction chamber 1 is provided with an oven door 3, the reaction chamber 1 is communicated with the condensation chamber 2 through a liquid zinc flow port 10, the reaction chamber 1 and the condensation chamber 2 share an iron furnace shell 4, an insulating layer 5 is arranged below the iron furnace shell 4, refractory bricks 6 are laid below the insulating layer 5, a microwave radiation element 7 is arranged below the refractory bricks 6 of the reaction chamber 1, a material layer 8 is arranged in the reaction chamber 1, and the material layer 8 is provided with a reaction chamber temperature measuring tube 9; zinc liquid flowing out of a liquid zinc flow port 10 of the reaction chamber 1 enters a metal zinc liquid pool 12 in the condensation chamber 2, and a metal zinc ingot casting port 13 is arranged at the lower part of the metal zinc liquid pool 12; a metal condensation plate 11 is arranged below a refractory brick 6 of the condensation chamber 2, a condensation chamber temperature measuring pipe 14 is arranged in the condensation chamber 2, the condensation chamber 2 is connected with a dust removal filter 16 through a vacuum exhaust pipe 15 and an inert gas pressure relief pipe 18, and a vacuum gauge 17 is arranged on the inert gas pressure relief pipe 18. The dust removing filter 16 is connected with a vacuum pump through a pipeline 19 connected with the vacuum pump.
The reaction chamber 1 is completely built by silicon carbide plates or bricks below the air guide window, and a heat insulation layer 5 between the reaction chamber 1 and the furnace iron shell 4 is a diatomite brick with the thickness of 6.5 cm; the metal condensing plate 11 of the condensing chamber 2 is made of a zinc corrosion resistant stainless steel plate or a titanium plate into a hollow water-through shape; the dust removal filter is made of stainless steel meshes of more than 60 meshes.
The invention is the most advanced technical process for smelting the dross containing chlorine and ammonia zinc at present, and can obtain 0-1# refined zinc products with low energy consumption, low pollution, high efficiency and low cost.
The above examples are merely illustrative of the present invention and the present invention is not limited thereto.
Claims (10)
1. A microwave vacuum smelting method of zinc dross containing chlorine and ammonia is characterized in that: the method comprises the following steps:
step 1: sampling and testing chemical components of the zinc dross, adding reduced carbon powder according to carbon/zinc =0.1-0.2, uniformly mixing, adding a binder according to 5-8% of the mixture, and drying in a brick shape or a pellet shape for later use; the zinc dross is dross generated when the metal zinc or zinc-based alloy is melted and is fried by ammonium chloride to separate slag and metal, the total zinc content is more than or equal to 90 percent, the particle zinc is more than or equal to 70 percent, the chlorine is less than or equal to 5 percent, and the ammonia is less than or equal to 5 percent;
and 2, step: adding the zinc dross lumps prepared in the step 1 into a microwave vacuum furnace until the lower edges of the gas guide windows of the reaction chamber and the condensation chamber are parallel, closing a furnace door, and starting a vacuum pump to vacuumize; when the vacuum degree meets the requirement, starting microwave radiation, and when the furnace temperature reaches the required lower limit, starting circulating cooling water;
the microwave vacuum carbon thermal reduction smelting of the zinc dross is divided into two stages, wherein the main task of the first stage is low-temperature decomposition deamination and chlorine, and the second stage is mainly high-temperature carbon thermal reduction smelting;
the microwave vacuum smelting conditions of the first stage are as follows: microwave radiation frequency is 0.5-1GHz, vacuum degree is less than or equal to 600Pa, reaction chamber furnace temperature is 900 +/-50 ℃, condensation chamber furnace temperature is 500-550 ℃, and time is 1.5-2 hours;
the conditions of the microwave vacuum carbon thermal reduction smelting in the second stage are that the microwave radiation frequency is 1-10GHz, the vacuum degree is less than or equal to 600Pa, the temperature of the reaction chamber is 1200 +/-50 ℃, the temperature of the condensation chamber is 500 +/-50 ℃, the time is 3-5 hours or the vacuum degree at the smelting end point is less than or equal to 80Pa;
and step 3: the air outlet of the vacuum pump is hermetically connected with a pipeline of the waste gas washing tower, the washing tower is subjected to negative pressure operation, washed by clear water or weak alkaline water with PH =8-12 or weak acidic water with PH =3-5, and discharged after reaching the standard;
and 4, step 4: after the second stage of smelting in the step 2 is finished, firstly, the microwave radiation is turned off, the vacuum pump is turned off when the furnace temperature of the reaction chamber is reduced to below 600 ℃, and the inert gas is used for releasing the pressure to normal pressure for casting the zinc ingot; and opening a furnace door of the reaction chamber to clean residues after the temperature of the reaction chamber is reduced to 300 +/-50 ℃, and cleaning a dust removal filter.
2. The microwave vacuum smelting method of zinc dross containing chlorine and ammonia according to claim 1, wherein: the reduced carbon powder in the step 1 is one of activated carbon powder, carbon black powder or coke powder, the carbon content is more than or equal to 90 percent, and the particle size of the carbon powder is more than or equal to 40 meshes.
3. The microwave vacuum smelting method of zinc dross containing chlorine and ammonia according to claim 1, wherein: the binder in the step 1 is paper pulp.
4. The microwave vacuum smelting method of zinc dross containing chlorine and ammonia according to claim 1, wherein the microwave vacuum smelting method comprises the following steps: in the step 1, the brick blocks are of the size of a conventional brick, the diameter of the pellet is =1-5cm, and the pellet is dried until the moisture is less than or equal to 10%.
5. The microwave vacuum smelting method of zinc dross containing chlorine and ammonia according to claim 1, wherein: and 4, if the next furnace is not immediately produced, stopping cooling water.
6. The microwave vacuum smelting method of zinc dross containing chlorine and ammonia according to claim 1, wherein: and 4, completing microwave vacuum carbon thermal reduction smelting of zinc dross containing chlorine and ammonium to obtain 0-1# refined zinc ingots, and returning residues to the rotary kiln for production.
7. The microwave vacuum smelting method of zinc dross containing chlorine and ammonia according to claim 1, wherein: the microwave vacuum furnace in the step 2 comprises a reaction chamber (1), a condensation chamber (2) and a dust removal filter (16), wherein the reaction chamber (1) is provided with a furnace door (3), the reaction chamber (1) and the condensation chamber (2) are communicated through a liquid zinc flow port (10), the reaction chamber (1) and the condensation chamber (2) share a furnace iron shell (4), a heat insulation layer (5) is arranged below the furnace iron shell (4), refractory bricks (6) are laid below the heat insulation layer (5), a microwave radiation element (7) is arranged below the refractory bricks (6) of the reaction chamber (1), a material layer (8) is arranged in the reaction chamber (1), and the material layer (8) is provided with a reaction chamber temperature measuring tube (9); zinc liquid flowing out of a liquid zinc flow port (10) of the reaction chamber (1) enters a metal zinc liquid pool (12) in the condensation chamber (2), and a metal zinc ingot casting port (13) is arranged at the lower part of the metal zinc liquid pool (12); a metal condensation plate (11) is arranged below a refractory brick (6) of the condensation chamber (2), a condensation chamber temperature measuring pipe (14) is arranged in the condensation chamber (2), the condensation chamber (2) is connected with a dust removal filter (16) through a vacuum exhaust pipe (15) and an inert gas pressure relief pipe (18), and a vacuum gauge (17) is arranged on the inert gas pressure relief pipe (18); the dust removal filter (16) is connected with a vacuum pump through a pipeline (19) connected with the vacuum pump.
8. The microwave vacuum furnace for the chlorine and ammonia containing zinc dross microwave vacuum smelting method of claim 7, wherein: the reaction chamber (1) is completely built by silicon carbide plates or bricks below the air guide window, and the heat insulation layer (5) between the reaction chamber and the furnace iron shell (4) is a diatomite brick with the thickness of 6.5 cm.
9. A microwave vacuum furnace for a chlorine and ammonia containing zinc dross microwave vacuum process as claimed in claim 7, wherein: the metal condensing plate (11) of the condensing chamber (2) is made into a hollow water-through shape by a zinc corrosion resistant stainless steel plate or a titanium plate.
10. The microwave vacuum furnace for the chlorine and ammonia containing zinc dross microwave vacuum smelting method of claim 7, wherein: the dust removal filter is made of stainless steel meshes of more than 60 meshes.
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| KR20110043946A (en) * | 2009-10-22 | 2011-04-28 | 고려대학교 산학협력단 | Method for recovering a metal |
| CN101705370A (en) * | 2009-11-23 | 2010-05-12 | 锡矿山闪星锑业有限责任公司 | Method for recovering valuable metal from ferro-aluminum slag and special horizontal vacuum furnace |
| CN102220480A (en) * | 2011-05-20 | 2011-10-19 | 昆明理工大学 | Method for removing fluorine and chlorine from zinc oxide smoke dust by microwave roasting |
| CN108642303A (en) * | 2018-05-29 | 2018-10-12 | 贵州宏达环保科技有限公司 | A kind of vacuum smelting method of zinc oxide ore |
| CN108754178A (en) * | 2018-07-06 | 2018-11-06 | 六盘水中联工贸实业有限公司 | A kind of smelting process of zinc sulfide concentrates |
| CN109022808A (en) * | 2018-08-24 | 2018-12-18 | 贵州省冶金化工研究所 | A kind of comprehensive recovering process of the dust of Ferrous Metallurgy containing zinc |
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