CN219430090U

CN219430090U - Vacuum reduction high-temperature reaction furnace device

Info

Publication number: CN219430090U
Application number: CN202320378939.6U
Authority: CN
Inventors: 汪大亚; 华绍广; 李书钦; 李香梅; 裴德健
Original assignee: Huawei National Engineering Research Center of High Efficient Cyclic and Utilization of Metallic Mineral Resources Co Ltd; Sinosteel Maanshan General Institute of Mining Research Co Ltd
Current assignee: Huawei National Engineering Research Center of High Efficient Cyclic and Utilization of Metallic Mineral Resources Co Ltd; Sinosteel Maanshan General Institute of Mining Research Co Ltd
Priority date: 2023-03-03
Filing date: 2023-03-03
Publication date: 2023-07-28
Anticipated expiration: 2033-03-03

Abstract

The utility model discloses a vacuum reduction high-temperature reaction furnace device, and belongs to the technical field of valuable element production or refining. The device comprises a tube furnace, wherein the tube furnace is connected with a furnace temperature controller, a water cooling cavity is connected below the tube furnace and above the tube furnace, a sublimated porcelain boat is arranged inside the tube furnace, one end of a stainless steel tee joint is connected with a reaction gas inlet, the lower end of the stainless steel tee joint is connected with a carrier gas inlet, the lower end of the stainless steel tee joint is provided with a gas outlet, the upper end of the stainless steel four joint is connected with a rotary vane vacuum pump, and a vacuum gauge is arranged on the rotary vane vacuum pump. The utility model solves the problem of complex existing technology, takes inert gas as carrier by vacuum volatilizing characteristic of Zn and Pb components in the dust of the tube furnace, introduces Zn and Pb steam into a low temperature area of a cooling cavity for liquefying and condensing, and fully separates and recovers Zn and Pb by changing the number and positions of metal collecting targets made of Al2O 3.

Description

Vacuum reduction high-temperature reaction furnace device

Technical Field

The utility model relates to the technical field of valuable element production or refining, in particular to a vacuum reduction high-temperature reaction furnace device.

Background

The electric furnace dust is a typical iron-rich dangerous waste in the metallurgical industry, and contains rich Zn and Pb resources; taking iron and steel enterprises as an example, the annual production amount of the electric furnace dust removal ash is approximately 1.5-3 ten thousand tons, and the normal production and operation activities of the enterprises are directly threatened; aiming at the electric furnace dust, the iron and steel enterprises mainly use the electric furnace dust as a raw material for extracting zinc at present, and the industrial application method is mainly a rotary kiln process and a rotary hearth furnace process.

The publication number is: chinese patent No. cn201710643213.X discloses a steelmaking dust recycling method and vacuum reduction electric furnace equipment used therefor. Mainly solves the defects of high difficulty of the existing wet process and high cost of the existing dry process. The patent uses the existing or later added iron powder in the dust as a reducing agent and a heating agent, and converts the steelmaking dust into iron-rich slag and elemental zinc ingots through oxidation-reduction reaction. Although the problems of high difficulty in wet process and high cost in dry process are solved in the above patent, the following problems still exist in actual operation and use:

1. in the prior art, zinc and lead are easily oxidized again after being reduced into steam, and the secondary refining is needed to be carried out again for obtaining metal;

2. in the prior art, the recovered metal contains more harmful elements, and impurity elements are required to be separated again in order to obtain a new product with high purity;

3. in the prior art, the ring formation of the rotary kiln and the interior of the heat exchanger of the rotary hearth furnace are easy to be blocked, so that the service life of equipment is influenced;

4. in the prior art, the rotary hearth furnace or rotary kiln process has the disadvantages of high energy consumption, high equipment investment cost, poor physical and chemical properties of products and low added value.

Disclosure of Invention

The utility model aims to provide a vacuum reduction high-temperature reaction furnace device which has the characteristics of simple process, short technical flow and high yield of valuable elements, and the whole smelting process does not generate pollution gas, so that the environment pollution is effectively improved, and the problems in the prior art are solved.

In order to achieve the above purpose, the present utility model provides the following technical solutions: the utility model provides a vacuum reduction high temperature reaction stove device, includes the tubular furnace, the tubular furnace passes through wire and outside furnace temperature controller electric connection, the below of tubular furnace is connected with quartzy material reaction tube, the both ends of quartzy material reaction tube are connected with stainless steel tee bend and stainless steel cross respectively, the intercommunication has the water-cooling chamber on the quartzy material reaction tube, the inside of quartzy material reaction tube is provided with the sublimated porcelain boat that is used for holding the sample, stainless steel tee bend's one end is connected with the reaction gas air inlet, stainless steel tee bend's lower extreme is connected with carrier gas air inlet, stainless steel cross's lower extreme is provided with the gas outlet, stainless steel cross's upper end is connected with the rotary-vane vacuum pump, be provided with the vacuum table on the rotary-vane vacuum pump.

Preferably, the tubular furnace is further provided with a temperature control system, a temperature measurement system, a reaction gas and carrier gas circulation system, a furnace body heating system, a zinc-lead recovery system and a vacuum control system.

Preferably, a base is arranged below the tube furnace, wherein installation fasteners matched with each other are arranged between the base and the quartz reaction tube, between the quartz reaction tube and the tube furnace and between the water cooling cavity and the quartz reaction tube.

Preferably, a stainless steel flange A is arranged at the joint of the quartz reaction tube and the stainless steel tee joint, a stainless steel flange B is arranged at the joint of the quartz reaction tube and the stainless steel tee joint, al2O3 tubes are respectively inserted into two ends of the quartz reaction tube, and the position of a gas outlet of the Al2O3 tube is equivalent to the position of a reactant.

Preferably, the water cooling cavity is hollow tubular with an interlayer inside, an output water pipe and an input water pipe are respectively arranged at the upper end and the lower end of the water cooling cavity, an Al2O3 metal collecting target is arranged at the center of the inside of the water cooling cavity, and the Al2O3 metal collecting target is in sealing contact with the inner wall of the quartz reaction pipe.

Preferably, the sublimation porcelain boat is positioned at a constant temperature belt position inside the quartz reaction tube.

Preferably, a temperature thermocouple is arranged in the Al2O3 pipe, and a thermocouple protection pipe is coated on the outer wall of the temperature thermocouple.

Preferably, the metal collecting target made of Al2O3 is a porous Al2O3 ceramic plate, and the number and the positions of the ceramic plates can be adjusted.

Compared with the prior art, the utility model has the following beneficial effects:

1. the vacuum reduction high-temperature reaction furnace device is essentially different from the traditional rotary kiln process and rotary hearth furnace process principle, and the zinc-lead alloy with the purity of more than 90 percent is obtained through the process of sublimation gasification-cooling solidification under the reducing roasting atmosphere and vacuum condition by depending on the characteristic of low saturated vapor pressure of zinc and lead, and compared with the traditional process, the product purity of 70-80 percent is improved by 10-20 percent.

2. According to the vacuum reduction high-temperature reaction furnace device, the carrier gas is utilized to horizontally convey reduced zinc-lead to a water cooling cavity area for cooling and solidifying, and then a plurality of layers of metal collecting targets made of Al2O3 are utilized for recycling; compared with the traditional vacuum reduction furnace, the device prolongs the residence time of cooling water in the water cooling cavity and improves the cooling effect; in addition, the corrosion of sublimated metal vapor to the inside of the quartz reaction tube can be avoided, and the service life of the quartz reaction tube is prolonged.

3. According to the vacuum reduction high-temperature reaction furnace device, the purposes of step recovery of zinc, lead and other volatile components in the tubular furnace dust are achieved by changing the reducing atmosphere, the roasting temperature and the flow of the reaction gas and the carrier gas, and the metal yield is improved by more than 20%; thereby being capable of controlling the reaction conditions more conveniently and further obtaining the reaction product with excellent physical and chemical properties.

4. According to the vacuum reduction high-temperature reaction furnace device, the positions and the number of the metal collecting targets made of Al2O3 can be adjusted, and the stay time and the cooling rate of gas in a water cooling cavity area can be effectively prolonged by adjusting the positions and the number of the metal collecting targets made of Al2O3, so that solid alloy particles with higher strength and more regular morphology are obtained.

Drawings

FIG. 1 is a schematic diagram of a method of deposition by vacuum reduction, cooling solidification according to the present utility model;

FIG. 2 is a schematic cross-sectional view of a water-cooled cavity according to the present utility model;

FIG. 3 is a plan view of a metal collecting target made of Al2O3 according to the present utility model.

In the figure: 1. a tube furnace; 2. a furnace temperature controller; 3. a quartz material reaction tube; 4. stainless steel tee joint; 5. stainless steel four-way; 6. a water cooling cavity; 7. sublimating a porcelain boat; 8. a reaction gas inlet; 9. a carrier gas inlet; 10. an air outlet; 11. a rotary vane vacuum pump; 12. a vacuum gauge; 101. installing a fastener; 31. stainless steel flange A; 32. stainless steel flange B; 33. al2O3 tube; 331. a temperature thermocouple; 332. a thermocouple protection tube; 61. al2O3 metal collecting target.

Detailed Description

The following description of the embodiments of the present utility model will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present utility model, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.

In order to solve the technical problems of low element recovery rate, low purity and poor physical and chemical properties of products commonly existing in the vacuum reduction equipment in the prior art, referring to fig. 1-3, the present embodiment provides the following technical solutions:

the vacuum reduction high-temperature reaction furnace device comprises a tubular furnace 1, wherein the tubular furnace 1 is also provided with a temperature control system, a temperature measurement system, a reaction gas and carrier gas circulation system, a furnace body heating system, a zinc-lead recovery system and a vacuum control system; a base is arranged below the tube furnace 1, wherein installation fasteners 101 matched with each other are arranged between the base and the quartz reaction tube 3, between the quartz reaction tube 3 and the tube furnace 1 and between the water cooling cavity 6 and the quartz reaction tube 3; the tube furnace 1 is electrically connected with an external furnace temperature controller 2 through a wire, a quartz material reaction tube 3 is connected below the tube furnace 1, two ends of the quartz material reaction tube 3 are respectively connected with a stainless steel tee joint 4 and a stainless steel four-way joint 5, a water cooling cavity 6 is communicated with the quartz material reaction tube 3, a sublimated porcelain boat 7 for containing samples is arranged inside the quartz material reaction tube 3, the sublimated porcelain boat 7 is positioned at a constant temperature zone position inside the quartz material reaction tube 3, one end of the stainless steel tee joint 4 is connected with a reaction gas inlet 8, the lower end of the stainless steel tee joint 4 is connected with a carrier gas inlet 9, the lower end of the stainless steel four-way joint 5 is provided with a gas outlet 10, the upper end of the stainless steel four-way joint 5 is connected with a rotary-vane vacuum pump 11, and the rotary-vane vacuum pump 11 is provided with a vacuum meter 12.

In order to reduce zinc and lead oxides in the dust of the tube furnace 1 into metallic zinc and lead, the reaction gas is usually CO or a mixed gas composed of CO and CO2, and the gas flow is 200-300 sccm; the carrier gas is used for conveying zinc and lead vapor to the position of the water cooling cavity, and inert gases such as Ar or N2 and the like which do not participate in the reaction are generally selected, wherein the gas flow is about 1.5-2 times of the gas flow of the reaction gas, namely 300-400 sccm.

A stainless steel flange A31 is arranged at the joint of the quartz reaction tube 3 and the stainless steel tee joint 4, a stainless steel flange B32 is arranged at the joint of the quartz reaction tube 3 and the stainless steel four-way joint 5, two ends of the quartz reaction tube 3 are respectively inserted with an Al2O3 tube 33, and the position of a gas outlet of the Al2O3 tube 33 is equal to the position of a reactant; the Al2O3 tube 33 is provided with a temperature thermocouple 331, and the outer wall of the temperature thermocouple 331 is covered with a thermocouple protection tube 332.

It should be noted that, the temperature thermocouple 331 may be selected according to an actual measurement range and accuracy, and when the temperature is higher than 1800 ℃, a tungsten-rhenium thermocouple is selected; when the measured temperature is 1300-1800 ℃, a type B thermocouple is selected; when the temperature is 1000-1300 ℃, an S-type thermocouple or an N-type thermocouple is generally selected; when the temperature is below 1000 ℃, a K-type thermocouple or an N-type thermocouple is generally selected.

The water cooling cavity 6 is hollow tubular with an interlayer inside, an output water pipe and an input water pipe are respectively arranged at the upper end and the lower end of the water cooling cavity 6, an Al2O3 metal collecting target 61 is arranged at the center of the inside of the water cooling cavity 6, the Al2O3 metal collecting target 61 is in sealing contact with the inner wall of the quartz reaction tube 3, the Al2O3 metal collecting target 61 is a porous Al2O3 ceramic plate, and the number and the positions of the ceramic plates can be adjusted.

Specifically, the quartz reaction tube 3 is horizontally placed into the tube furnace 1, the stainless steel tee joint 4 and the stainless steel flange A31 are sequentially installed at the end of the reaction gas inlet 8, and the sealing of the end of the carrier gas inlet 9 is realized through an O-shaped ring, a nut and a screw in the stainless steel flange A31; placing 5-10 g of electric furnace dust removal sample in the sublimation ceramic boat 7, placing the sample in a constant temperature zone area of the quartz reaction tube 3, and moving the reaction gas inlet 8 to the position right above the sample; then, a stainless steel four-way 5 and a stainless steel flange B32 are sequentially arranged at the air outlet 10 end, and the air outlet 10 end is sealed through an O-shaped ring, a nut and a screw rod in the stainless steel flange B32; finally, a nickel-chromium-nickel-silicon thermocouple for temperature measurement is installed, and the top end of the temperature thermocouple 331 is equivalent to the position of the sublimated porcelain boat 7; turning on a rotary vane vacuum pump 11, vacuumizing the reaction system, and when the number of the vacuum table 12 is-0.1 MPa and the vacuum table is kept for more than 10 minutes and no change occurs, then filling reaction gas into the system and recovering to normal pressure; repeating the steps for three times, and after the air in the system is exhausted, completing the assembly of the reaction equipment; and then the rotary vane vacuum pump 11 is started, and when the pressure in the reaction system reaches 30-100 Pa, the heating system is started. In order to fully recycle zinc and lead elements in the dust of the tubular furnace 1, adjusting the target roasting temperature to 1100 ℃; the temperature rising rate is 5 ℃/min; meanwhile, an input water pipe and an output water pipe of the water cooling cavity 6 are opened, so that the position of the water cooling cavity 6 is ensured to be in a relatively low-temperature state; according to a set heating program, after the temperature is heated to 1100 ℃, introducing a reaction gas CO, wherein the gas flow is 200sccm, and the heat preservation time is 180 minutes, so that the reactants in the sublimated porcelain boat 7 are ensured to fully react; simultaneously, introducing carrier gas Ar gas or N2 into the carrier gas inlet 9, wherein the gas flow is 300sccm, and conveying sublimated suspended particles to the position of a quenching cavity; the gaseous elemental zinc and lead are transported to the position of the water cooling cavity 6 through carrier gas, and then are cooled and solidified to form solid zinc-lead alloy; the cooled solid metal is attached to a plurality of layers of metal collecting targets 61 made of Al2O3, and the waste gas is discharged through a gas outlet 10 in the device; after the reaction is finished, firstly closing the power supply of the tube furnace 1 to cool, and simultaneously closing a carrier gas switch; keeping the components and flow of the reaction gas unchanged in the cooling process, and closing all gas switches after the temperature is reduced to be within the operable temperature range; after the furnace body of the tubular furnace 1 is cooled to room temperature, vacuum breaking operation is carried out, the quartz reaction tube 3 is opened, the sublimated porcelain boat 7 and the multilayer Al2O3 metal collecting target 61 are taken out, and finally the solid zinc, lead alloy and iron-containing tailings are obtained.

Working principle: by utilizing the vacuum volatilization characteristics of Zn and Pb components in the dust removed by the tubular furnace 1 and taking inert gas as a carrier, zn and Pb steam is introduced into a low-temperature area of the cooling cavity 6 for liquefaction and condensation, and Zn and Pb are fully separated and recovered by changing the number and positions of metal collecting targets 61 made of Al2O3, so that the metal yield and the production efficiency are greatly improved.

It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.

Although embodiments of the present utility model have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the utility model, the scope of which is defined in the appended claims and their equivalents.

Claims

1. The utility model provides a vacuum reduction high temperature reaction furnace device, includes tubular furnace (1), its characterized in that: the utility model discloses a vacuum furnace, including tubular furnace (1), quartz material reaction tube (3), water-cooling chamber (6), reaction tube (3), reaction gas air inlet (8), support gas air inlet (9), air outlet (10), vacuum pump (11), vacuum table (12) are provided with on the rotary-vane vacuum pump (11), the tubular furnace (1) is connected with outside furnace temperature controller (2) electric connection through wire, the below of tubular furnace (1) is connected with quartz material reaction tube (3), the both ends of quartz material reaction tube (3) are connected with stainless steel tee bend (4) and stainless steel cross (5) respectively, the intercommunication has water-cooling chamber (6) on quartz material reaction tube (3), the inside of quartz material reaction tube (3) is provided with and is used for holding sublimating porcelain boat (7) of sample, the one end of stainless steel tee bend (4) is connected with reaction gas air inlet (8), the lower extreme of stainless steel tee bend (4) is connected with carrier gas air inlet (9), the lower extreme of stainless steel cross (5) is provided with gas outlet (10), the upper end of stainless steel cross (5) is connected with rotary-vane vacuum pump (11).

2. The vacuum reduction high temperature reaction furnace apparatus according to claim 1, wherein: the tubular furnace (1) is also provided with a temperature control system, a temperature measurement system, a reaction gas and carrier gas circulation system, a furnace body heating system, a zinc-lead recovery system and a vacuum control system.

3. The vacuum reduction high temperature reaction furnace apparatus according to claim 1, wherein: the lower part of the tube furnace (1) is provided with a base, wherein installation fasteners (101) matched with each other are respectively arranged between the base and the quartz reaction tube (3) and between the quartz reaction tube (3) and the tube furnace (1) and between the water cooling cavity (6) and the quartz reaction tube (3).

4. The vacuum reduction high temperature reaction furnace apparatus according to claim 1, wherein: the stainless steel reaction tube is characterized in that a stainless steel flange A (31) is arranged at the joint of the quartz reaction tube (3) and the stainless steel tee joint (4), a stainless steel flange B (32) is arranged at the joint of the quartz reaction tube (3) and the stainless steel tee joint (5), al2O3 tubes (33) are respectively inserted into two ends of the quartz reaction tube (3), and the position of a gas outlet of the Al2O3 tubes (33) is equal to the position of a reactant.

5. The vacuum reduction high temperature reaction furnace apparatus according to claim 1, wherein: the water cooling cavity (6) is hollow and tubular, an interlayer is arranged in the water cooling cavity (6), an output water pipe and an input water pipe are respectively arranged at the upper end and the lower end of the water cooling cavity (6), an Al2O3 metal collecting target (61) is arranged in the center of the water cooling cavity (6), and the Al2O3 metal collecting target (61) is in sealing contact with the inner wall of the quartz reaction tube (3).

6. The vacuum reduction high temperature reaction furnace apparatus according to claim 1, wherein: the sublimation porcelain boat (7) is positioned at a constant temperature belt position inside the quartz material reaction tube (3).

7. The vacuum reduction high temperature reaction furnace apparatus according to claim 4, wherein: a temperature thermocouple (331) is arranged in the Al2O3 tube (33), and a thermocouple protection tube (332) is coated on the outer wall of the temperature thermocouple (331).

8. The vacuum reduction high temperature reaction furnace apparatus according to claim 5, wherein: the Al2O3 metal collecting target (61) is a porous Al2O3 ceramic plate, and the number and the positions of the ceramic plates can be adjusted.