阅读说明：本技术 一种分级挥发真空气化分离炉 (Vacuum gasification separation furnace for fractional volatilization ) 是由 杨斌 徐宝强 蒋文龙 刘大春 李一夫 田阳 于 2021-09-02 设计创作，主要内容包括：本发明公开一种分级挥发真空气化分离炉,属于有色金属真空冶金技术领域。本发明所述真空气化分离炉包括气化室和出料室,所述气化室包括炉壳、底部发热体、分体式侧壁发热体、气化坩埚、间壁通道、底部汇流盘、电极、一级挥发盘、二级挥发盘、三级挥发盘,一级挥发盘、二级挥发盘、三级挥发盘组合以后构成Ⅰ级冷凝区和Ⅱ级冷凝区；通过在气化坩埚与分级挥发构件间添加环径,改变高度,实现不同挥发盘上气化温度的调控。本发明设置了底部和分体式侧壁发热体,提高了蒸发坩埚内的温度。此外,炉壳及炉壳连接位置设置水冷密封结构,确保炉内的真空环境,多级挥发盘的设计实现了气化挥发物的回流和多次挥发物料的分级和循环挥发。(The invention discloses a graded volatilization vacuum gasification separation furnace, and belongs to the technical field of non-ferrous metal vacuum metallurgy. The vacuum gasification separation furnace comprises a gasification chamber and a discharge chamber, wherein the gasification chamber comprises a furnace shell, a bottom heating element, a split type side wall heating element, a gasification crucible, a dividing wall channel, a bottom confluence disc, an electrode, a first-stage volatilization disc, a second-stage volatilization disc and a third-stage volatilization disc, and the first-stage volatilization disc, the second-stage volatilization disc and the third-stage volatilization disc are combined to form a first-stage condensation zone and a second-stage condensation zone; the height is changed by adding the ring diameter between the gasification crucible and the grading volatilization component, so that the gasification temperature on different volatilization discs can be regulated and controlled. The invention is provided with the bottom and the split side wall heating body, thereby improving the temperature in the evaporation crucible. In addition, the furnace shell and the connecting position of the furnace shell are provided with water-cooling sealing structures, so that the vacuum environment in the furnace is ensured, and the design of the multi-stage volatilization disc realizes the backflow of gasified volatile matters and the grading and circulating volatilization of multiple volatile materials.)

1. The utility model provides a vacuum gasification separating furnace volatilizees in grades which characterized in that: the device comprises a gasification chamber and a discharge chamber, wherein the gasification chamber comprises a furnace shell (1), a bottom heating element (2), a split type side wall heating element (3), a gasification crucible (4), a dividing wall channel (5), a bottom confluence disc (6), an electrode (7), a primary volatilization disc (9), a secondary volatilization disc (10) and a tertiary volatilization disc (11);

the bottom heating element (2) is positioned at the bottom of the gasification chamber, the gasification crucible (4) is arranged on the bottom heating element (2), the split type side wall heating elements (3) are uniformly distributed around the gasification crucible (4), and the bottom heating element (2) and the split type side wall heating elements (3) are respectively connected with a power supply through electrodes (7); a disc-shaped primary volatilization disc (9) is arranged at the top of the gasification crucible, a plurality of air outlets are arranged around the primary volatilization disc (9), a secondary volatilization disc (10) is arranged above the primary volatilization disc (9), a I-stage condensation area is formed between the primary volatilization disc (9) and the secondary volatilization disc (10), and a plurality of openings inclined towards the gasification crucible are arranged at the bottom of the primary volatilization disc (9); top that second grade volatilizees dish (10) is equipped with tertiary the dish of volatilizing (11), second grade volatilizees dish (10) and tertiary volatilize and constitute II level condensation areas between dish (11), second grade volatilizees dish (10) top and all establishes a plurality of gas pockets tertiary volatilize dish (11) bottom all around and is equipped with a plurality of openings, the open-ended below is equipped with next door passageway (5), next door passageway (5) below is equipped with the bottom and converges dish (6), the bottom converges dish (6) and ejection of compact indoor collection crucible (8) intercommunication, the height of I level condensation area and II level condensation areas can be adjusted.

2. The staged volatilization vacuum gasification separation furnace as set forth in claim 1, wherein: the primary volatilization disc (9), the secondary volatilization disc (10) and the tertiary volatilization disc (11) are all disc-shaped, and the radiuses of the primary volatilization disc (9), the secondary volatilization disc (10) and the tertiary volatilization disc (11) are increased in sequence.

3. The vacuum evaporation and separation furnace for fractional evaporation according to any one of claims 1 to 2, wherein: the heights of the gasification crucible (4), the secondary volatilization plate (10) and the tertiary volatilization plate (11) are adjusted by the number of annular gaskets.

4. The staged volatilization vacuum gasification separation furnace as set forth in claim 3, wherein: the first-stage volatilization disc (9), the second-stage volatilization disc (10) and the third-stage volatilization disc (11) are of a double-layer structure, and cooling water is introduced into the middle.

5. The staged volatilization vacuum gasification separation furnace as set forth in claim 1, wherein: the bottom heating element (2) and the split type side wall heating element (3) are prepared from graphite materials, the split type side wall heating element (3) is composed of a plurality of graphite rods (12), and two ends of the graphite rods (12) are connected through connecting plates (13) to form a cylindrical structure.

6. The staged volatilization vacuum gasification separation furnace as set forth in claim 1, wherein: the connection between the furnace shells (1) adopts a water-cooling sealing structure, and the pressure in the furnace is less than or equal to 5 Pa.

Technical Field

The invention relates to a vacuum gasification separation furnace for fractional volatilization, belonging to the technical field of non-ferrous metal vacuum metallurgy.

Background

The principle of the vacuum gasification equipment is that after reaching the evaporation temperature under given power, metal vapor is generated and condensed on a condenser to obtain corresponding metal or alloy. The material that general vacuum gasification stove was handled is limited greatly, and specific vacuum gasification stove can only handle specific alloy material for vacuum gasification stove's use cost is higher. In recent years, a plurality of researchers develop general vacuum distillation equipment, but the vacuum distillation equipment can only realize bottom heating, so that the heating temperature cannot meet the requirement, the distillation effect is poor, and the application range is greatly limited. In addition, because the heating is not uniform, some local materials can not be heated sufficiently, and the purification efficiency is not high. The required metal elements cannot be effectively collected in the aspect of collecting materials, and are often mixed with other metal elements, so that further purification and separation are needed. Therefore, it is required to develop a vacuum gasification separation furnace which can process various high boiling point alloys and the purity of the collected products is very high.

Disclosure of Invention

In order to solve the technical problems, the invention aims to provide a novel graded volatilization vacuum gasification separation furnace, which comprises a gasification chamber and a discharge chamber, wherein the gasification chamber comprises a furnace shell 1, a bottom heating element 2, a split type side wall heating element 3, a gasification crucible 4, a partition wall channel 5, a bottom confluence disc 6, an electrode 7, a primary volatilization disc 9, a secondary volatilization disc 10 and a tertiary volatilization disc 11;

the bottom heating element 2 is positioned at the bottom of the gasification chamber, the gasification crucible 4 is arranged on the bottom heating element 2, the split type side wall heating elements 3 are uniformly distributed around the gasification crucible 4, and the bottom heating element 2 and the split type side wall heating elements 3 are respectively connected with a power supply through electrodes 7; a disc-shaped primary volatilization disc 9 is arranged at the top of the gasification crucible, a plurality of air outlets are arranged around the primary volatilization disc 9, a secondary volatilization disc 10 is arranged above the primary volatilization disc 9, a primary condensation area I is formed between the primary volatilization disc 9 and the secondary volatilization disc 10, and a plurality of openings inclined towards the gasification crucible are arranged at the bottom of the primary volatilization disc 9, so that metal vapor can conveniently flow back to the gasification crucible after being condensed; a third-stage volatilization disc 11 is arranged above the second-stage volatilization disc 10, a second-stage condensation area is formed between the second-stage volatilization disc 10 and the third-stage volatilization disc 11, a plurality of air holes are formed in the periphery of the top of the second-stage volatilization disc 10, a plurality of openings are formed in the bottom of the third-stage volatilization disc 11, a dividing wall channel 5 is arranged below each opening, a bottom convergence disc 6 is arranged below each dividing wall channel 5, the bottom convergence disc 6 is communicated with a collection crucible 8 in a discharge chamber, and the heights of the first-stage condensation area and the second-stage condensation area can be adjusted; during operation, metal vapor passes through the air holes to be cooled into liquid in the three-stage volatilization disc 11, the liquid flows into the dividing wall channel 5 from the opening by gravity, the metal liquid is converged to the bottom convergence disc 6 under the action of gravity, and finally flows into the collection crucible 8 of the discharge chamber from the opening arranged on the bottom convergence disc 6 to complete the gasification, separation and purification of the alloy, so that the separation of high-melting point components and low-melting point components in the mixed vapor can be realized.

Preferably, the primary volatilization plate 9, the secondary volatilization plate 10 and the tertiary volatilization plate 11 are all disc-shaped, and the radii of the primary volatilization plate 9, the secondary volatilization plate 10 and the tertiary volatilization plate 11 are increased in sequence.

Preferably, the gasification crucible 4, the second-stage volatilization plate 10 and the third-stage volatilization plate 11 are adjusted in height by the number of annular gaskets, so that the condensation temperature is controlled finally, and the purity of the collected metal liquid is higher by the third-stage volatilization plate 11.

Preferably, the first-stage volatilization disc 9, the second-stage volatilization disc 10 and the third-stage volatilization disc 11 are of a double-layer structure, and cooling water is introduced into the middle.

Preferably, the bottom heating element 2 and the split type side wall heating element 3 are both made of graphite materials, the split type side wall heating element 3 is composed of a plurality of graphite rods, and two ends of the plurality of graphite rods are connected through connecting plates to form a cylindrical structure.

Preferably, the connection between the furnace shells adopts a water-cooling sealing structure, and the pressure in the furnace is less than or equal to 5 Pa.

The invention has the beneficial effects that:

(1) the invention is provided with the bottom and the split side wall heating body, thereby increasing the power and the efficiency of heat transfer in the furnace, improving the temperature in the evaporation crucible (up to 2000 ℃), improving the temperature uniformity in the crucible, ensuring better vacuum distillation effect, more thorough distillation and higher purity of the collected product. Meanwhile, the split type side wall heating body is arranged into a structure with a plurality of graphite rod combinations, so that the heating power is increased, and the material is saved, so that the heating effect is better, and the disassembly, the assembly and the replacement are more convenient.

(2) The connection between the furnace shells adopts a large number of water-cooling sealing structures, so that the pressure in the furnace is ensured to be less than 5Pa, the separation efficiency is improved, and materials and components in the furnace are protected from being oxidized.

(3) The design of the multi-stage volatilization disc realizes the backflow and multiple volatilization of gasified volatile matters, improves the product quality, avoids the output of unqualified products, greatly improves the purity of the separated metal, and also designs the annular gasket, changes the height by adding the annular diameter between the gasification crucible and the graded volatilization component, and realizes the regulation and control of the gasification temperature on different volatilization discs.

Drawings

FIG. 1 is a schematic structural view of the present invention;

FIG. 2 is a cross-sectional view of the present invention;

FIG. 3 is a schematic structural view of a sidewall heater according to the present invention;

fig. 4 is a schematic structural view of a staged volatilization component according to the invention.

In the figure: 1-furnace shell; 2-bottom heating element; 3-split type side wall heating element; 4-gasifying the crucible; 5-a partition channel; 6-bottom confluence disc; 7-an electrode; 8-collecting the crucible; 9-first-stage volatilization disc; 10-a secondary volatilization plate; 11-a three-stage volatilization disc; 12-a graphite rod; 13-connecting plate.

Detailed Description

The invention is described in further detail below with reference to the figures and the embodiments, but the scope of the invention is not limited to the description.

Example 1

A new grading volatilization vacuum gasification separation furnace is shown in figure 1, and comprises a gasification chamber and a discharge chamber, wherein the gasification chamber comprises a furnace shell 1, a bottom heating element 2, a split type side wall heating element 3, a gasification crucible 4, a dividing wall channel 5, a bottom confluence disc 6, an electrode 7, a first-stage volatilization disc 9, a second-stage volatilization disc 10 and a third-stage volatilization disc 11; the bottom heating element 2 is positioned at the bottom of the gasification chamber, the gasification crucible 4 is arranged on the bottom heating element 2, the split type side wall heating elements 3 are uniformly distributed around the gasification crucible 4, and the bottom heating element 2 and the split type side wall heating elements 3 are respectively connected with a power supply through electrodes 7; a disc-shaped primary volatilization disc 9 is arranged at the top of the gasification crucible, a plurality of air outlets are arranged around the primary volatilization disc 9, a secondary volatilization disc 10 is arranged above the primary volatilization disc 9, a primary condensation area I is formed between the primary volatilization disc 9 and the secondary volatilization disc 10, and a plurality of openings inclined towards the gasification crucible are arranged at the bottom of the primary volatilization disc 9, so that metal vapor can conveniently flow back to the gasification crucible after being condensed; a third-stage volatilization disc 11 is arranged above the second-stage volatilization disc 10, a second-stage condensation area is formed between the second-stage volatilization disc 10 and the third-stage volatilization disc 11, the heights of the first-stage condensation area and the second-stage condensation area can be adjusted, a plurality of air holes are formed in the periphery of the top of the second-stage volatilization disc 10, a plurality of openings are formed in the bottom of the third-stage volatilization disc 11, a partition wall channel 5 is arranged below each opening, a bottom convergence disc 6 is arranged below each partition wall channel 5, and the bottom convergence disc 6 is communicated with a collection crucible 8 in a discharge chamber; during operation, metal vapor passes through the air holes to be cooled into liquid in the three-stage volatilization disc 11, the liquid flows into the dividing wall channel 5 from the opening by gravity, the metal liquid is converged to the bottom convergence disc 6 under the action of gravity, and finally flows into the collection crucible 8 of the discharge chamber from the opening arranged on the bottom convergence disc 6 to complete the gasification, separation and purification of the alloy, so that the separation of high-melting point components and low-melting point components in the mixed vapor can be realized.

As a preferred embodiment of this embodiment:

the primary volatilization disc 9, the secondary volatilization disc 10 and the tertiary volatilization disc 11 are all disc-shaped, and the radiuses of the primary volatilization disc 9, the secondary volatilization disc 10 and the tertiary volatilization disc 11 are sequentially increased. The first-stage volatilization disc 9, the second-stage volatilization disc 10 and the third-stage volatilization disc 11 are of a double-layer structure, and cooling water is introduced into the middle; the heights of the secondary volatilization disc 10 and the tertiary volatilization disc 11 are adjusted by the number of the annular gaskets 10, so that the control of the condensation temperature is finally realized, and the purity of the collected metal liquid is higher by the tertiary volatilization disc 11.

700kg of precious lead materials (Bi61.63%, Pb26.49%, Ag6.41%, Cu0.6011% and Sb0.0055%) are processed by the equipment. The pressure in the furnace is 5-15Pa, and the gasification temperature is 900 +/-20 ℃. Obtaining volatile matters (Bi77.55%, Pb18.67%, Ag0.0014%) through one-time vacuum gasification; and by adopting the traditional vacuum gasification equipment, under the same process conditions, the volatile matter is subjected to primary vacuum gasification, the content of silver in the volatile matter can reach 0.0018 percent after the volatile matter is subjected to secondary vacuum gasification, and the content of silver in the volatile matter is increased to 2.15 percent; therefore, the gasification efficiency can be obviously improved by the equipment.

Example 2

This embodiment bottom heat-generating body 2 and split type lateral wall heat-generating body 3 are obtained by the preparation of graphite material, and split type lateral wall heat-generating body 3 comprises 12 graphite rods 12, and every 4 stone ink stick 12 use a connecting plate 13 to connect, and the connecting plate 13 of upper and lower position sets up in turn, realizes that all graphite rods 12 connect as a whole. The bottom heating element 2 and the split type side wall heating element 3 are respectively connected with a power supply through electrodes 7. Whether can select simultaneously to open bottom heat-generating body 2 and split type lateral wall heat-generating body 3 as required in the use, split type lateral wall heat-generating body 3's structure is shown in figure 3, through split type lateral wall heat-generating body 3's design for whole gasification crucible 4 is heated more evenly, and the controllable scope of temperature is big.

In the embodiment, residual Ag-Cu-Sb alloy obtained by carrying out primary vacuum gasification on noble lead alloy obtained by smelting lead anode slime produced in a certain domestic plant in a reverberatory furnace is taken as an experimental raw material.

Table 1 shows the product composition after treatment in a conventional vacuum gasifier; table 2 shows the product composition after the treatment in the vacuum evaporation/separation furnace. The mixed steam enters a multistage condensation system, namely a stage I condensation area, the temperature of the stage I condensation area is lower than that of a gasification crucible, the melting boiling point of copper in the mixed steam is higher, and the mixed steam is liquefied and flows into the crucible; ag, Pb, Bi and the like with low boiling points enter a II-grade condensation zone, and due to further reduction of temperature, the part of mixed steam is liquefied and enters a collection chamber through a recovery channel; a more thorough vacuum gasification process is realized; comparing tables 1 and 2, the new equipment can realize the volatilization of low-melting-point components such as lead, bismuth and the like by repeating, and can greatly reduce the content of copper in volatile matters

TABLE 1 separation of the residue, volatiles major components by conventional vacuum gasification

TABLE 2 fractional volatilization vacuum gasification separation of the residue, volatiles major components