CN118028624B - In-situ on-line treatment method and device for thermal magnesium refining slag - Google Patents

In-situ on-line treatment method and device for thermal magnesium refining slag Download PDF

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CN118028624B
CN118028624B CN202410429936.XA CN202410429936A CN118028624B CN 118028624 B CN118028624 B CN 118028624B CN 202410429936 A CN202410429936 A CN 202410429936A CN 118028624 B CN118028624 B CN 118028624B
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separator
refining slag
magnesium
situ
magnesium refining
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CN118028624A (en
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高金涛
郭占成
兰茜
汪增武
李想
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B26/00Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/20Obtaining alkaline earth metals or magnesium
    • C22B26/22Obtaining magnesium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/04Working-up slag

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  • Environmental & Geological Engineering (AREA)
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  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
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Abstract

The invention belongs to the technical field of magnesium refining slag treatment, in particular to an in-situ on-line treatment method and device for hot magnesium refining slag, which can fully utilize latent heat of magnesium refining slag during discharge, realize in-situ on-line high-efficiency separation of a solid-liquid mixture of the magnesium refining slag by utilizing a separator, recycle a flux liquid phase to a coarse magnesium solvent refining process, realize high-efficiency recycling of magnesium smelting resources, and realize the in-situ on-line treatment of the hot magnesium refining slag, wherein the solid phase removal rate is more than 94%, and the purity of the flux in slag ladle is more than 98%.

Description

In-situ on-line treatment method and device for thermal magnesium refining slag
Technical Field
The invention relates to the technical field of magnesium refining slag treatment, in particular to an in-situ on-line treatment method and device for thermal magnesium refining slag.
Background
In industry, an electrolytic method and a Pidgeon method (also called a silicothermic reduction method) are often adopted to smelt and produce metal magnesium, the Pidgeon method has the advantages of short magnesium smelting process flow, low investment and low cost, magnesium steam is obtained after magnesium oxide obtained by calcining dolomite is reduced under high temperature and vacuum conditions, crude magnesium is obtained after the magnesium steam is condensed, a certain amount of oxide impurities are contained in the crude magnesium, and in order to provide a magnesium ingot product with qualified quality, the impurities are required to be removed again through refining. The impurities in the crude magnesium are removed by a flux refining method, the flux is mainly NaCl, KCl, mgCl 2 and fluoride with specific functions, most of the oxides can be wetted by NaCl and KCl, mgO and CaO can form stable complexes with MgCl 2, and the oxide impurities migrate into the flux. The metal impurities such as Na, K and the like can undergo a displacement reaction with MgCl 2, and the impurities can enter a flux, so that coarse magnesium refining is realized, the flux and the metal magnesium are layered due to huge physical property differences, and the flux becomes magnesium refining slag due to the fact that a large amount of impurities are absorbed, and is discharged from a refining furnace into a slag ladle at fixed time. Therefore, the flux plays an important role in refining coarse magnesium, the flux flows into the magnesium refining slag after refining, the magnesium refining slag cannot be stacked in open air because the flux is easy to hydrolyze and absorb moisture and cannot be buried more, meanwhile, the particle size of oxide impurities in the magnesium refining slag is small, no efficient separation technology is used for directly treating the magnesium refining slag on line in the industry at present, and a large amount of magnesium refining slag can only be piled in a storehouse. In addition, the general laboratory procedures are: firstly, the magnesium refining slag is hydrolyzed and then evaporated to extract salt flux, and the rest solid phase is prepared into related products, but the method needs a large amount of water resources, and the evaporation and crystallization process has high energy consumption and lower efficiency.
Disclosure of Invention
In order to solve the technical problems, the invention mainly aims to provide the in-situ on-line treatment method and the in-situ on-line treatment device for the hot magnesium refining slag, wherein the magnesium refining slag contains a large amount of flux components, if the flux components can be separated on line when the magnesium refining slag is discharged from a refining furnace, and the flux components are recycled to be used in the coarse magnesium refining process, so that the high-efficiency recycling of resources can be realized, the process energy consumption during coarse magnesium refining and magnesium refining slag treatment can be reduced, and the purposes of reducing carbon and reducing carbon are achieved.
In order to solve the technical problems, according to one aspect of the present invention, the following technical solutions are provided:
an in-situ on-line treatment method of hot magnesium refining slag comprises the following steps:
s1, discharging thermal magnesium refining slag generated during refining of a crude magnesium flux into a slag ladle with heating and heat preservation functions, and ensuring that the magnesium refining slag has good fluidity;
S2, starting the separator to enter a rotating state, and immersing the separator into magnesium refining slag at a certain rotating speed;
S3, adjusting the rotating speed of the separator and the depth of immersing the magnesium refining slag, enabling the solid-liquid mixture of the magnesium refining slag to continuously enter the separator, enabling the flux liquid phase to flow back into the slag ladle during the period, enabling the oxide solid phase to be intercepted in the separator, so as to realize solid-liquid separation, and discharging the oxide solid phase;
s4, repeating the step S3 until no oxide solid phase is discharged, wherein the residual liquid phase in the slag ladle is high-purity flux, and the flux can be recycled for refining the coarse magnesium flux.
As a preferable scheme of the in-situ on-line treatment method of the thermal magnesium refining slag, the invention comprises the following steps: in the step S1, the temperature of the thermal state magnesium refining slag generated during the refining of the crude magnesium flux is 710-740 ℃.
As a preferable scheme of the in-situ on-line treatment method of the thermal magnesium refining slag, the invention comprises the following steps: in the step S1, the temperature of the magnesium refining slag in the slag ladle is controlled to be 600-700 ℃.
As a preferable scheme of the in-situ on-line treatment method of the thermal magnesium refining slag, the invention comprises the following steps: in the step S3, the gravity coefficient generated when the separator rotates is 100-500 g.
As a preferable scheme of the in-situ on-line treatment method of the thermal magnesium refining slag, the invention comprises the following steps: in the step S3, the depth of the separator immersed into the magnesium refining slag is 10-15 cm.
As a preferable scheme of the in-situ on-line treatment method of the thermal magnesium refining slag, the invention comprises the following steps: in the step S3, the rotation time of the separator is 1-10 min.
In order to solve the above technical problems, according to another aspect of the present invention, the following technical solutions are provided:
an in-situ on-line treatment device for thermal magnesium refining slag, which is used for realizing the in-situ on-line treatment method for the thermal magnesium refining slag, comprises the following steps:
A support system and a separation system;
The support system consists of a support main body, a rotation and lifting main body and a horizontal cantilever; the support main body is provided with a rotating and lifting main body and a horizontal cantilever in a coupling way and is used for realizing horizontal rotation and vertical lifting of the separation system;
The separation system comprises a separator rotating connecting rod and a separator; the rotating connecting rod of the separator is connected with the horizontal cantilever to control the separator to stably rotate.
As a preferable scheme of the in-situ on-line treatment device for the thermal magnesium refining slag, the invention comprises the following steps: the separator comprises a separator main body and a separator shell, wherein the separator shell is matched and nested with the separator main body, the separator main body is removed from the separator shell after separation treatment is completed, and oxide solid phase in the separator is discharged.
The beneficial effects of the invention are as follows:
The invention provides a method and a device for in-situ on-line treatment of thermal magnesium refining slag, which can fully utilize latent heat of the magnesium refining slag during discharge, realize in-situ on-line high-efficiency separation of a solid-liquid mixture of the magnesium refining slag by utilizing a separator, and recycle a flux liquid phase to a coarse magnesium solvent refining process to realize high-efficiency recycling of magnesium smelting resources.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to the structures shown in these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of an in-situ on-line treatment process for a hot magnesium refinery slag according to the present invention;
FIG. 2 is a schematic structural diagram of an in-situ on-line treatment device for the hot magnesium refining slag;
FIG. 3 is a macro morphology, SEM image and EDS image of a sample of the in-situ on-line treatment of a hot magnesium refinery slag of example 1;
FIG. 4 is a macro morphology, SEM image and EDS image of the sample after in-situ on-line treatment of the hot magnesium refinery slag of example 4.
Wherein: 1-supporting body, 2-rotating and lifting body, 3-horizontal cantilever, 4-separator rotating connecting rod, 5-separator body, 6-separator shell.
The achievement of the objects, functional features and advantages of the present invention will be further described with reference to the accompanying drawings, in conjunction with the embodiments.
Detailed Description
The following description will be made clearly and fully with reference to the technical solutions in the embodiments, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
According to one aspect of the invention, the invention provides the following technical scheme:
as shown in FIG. 1, the in-situ on-line treatment method of the thermal magnesium refining slag comprises the following steps:
s1, discharging thermal magnesium refining slag generated during refining of a crude magnesium flux into a slag ladle with heating and heat preservation functions, and ensuring that the magnesium refining slag has good fluidity;
S2, starting the separator to enter a rotating state, and immersing the separator into magnesium refining slag at a certain rotating speed;
S3, adjusting the rotating speed of the separator and the depth of immersing the magnesium refining slag, enabling the solid-liquid mixture of the magnesium refining slag to continuously enter the separator, enabling the flux liquid phase to flow back into the slag ladle during the period, enabling the oxide solid phase to be intercepted in the separator, so as to realize solid-liquid separation, and discharging the oxide solid phase;
s4, repeating the step S3 until no oxide solid phase is discharged, wherein the residual liquid phase in the slag ladle is high-purity flux, and the flux can be recycled for refining the coarse magnesium flux.
Preferably, in the step S1, the temperature of the hot magnesium refining slag generated during the refining of the crude magnesium flux is 710 to 740 ℃.
Preferably, in the step S1, the temperature of the magnesium refining slag in the slag ladle is controlled to be 600-700 ℃.
Preferably, in the step S3, the gravity coefficient generated when the separator rotates is 100 to 500g.
Preferably, in the step S3, the separator is immersed in the magnesium refining slag to a depth of 10 to 15cm.
Preferably, in the step S3, the rotation time of the separator is 1 to 10 minutes.
According to another aspect of the invention, the invention provides the following technical scheme:
as shown in fig. 2, an in-situ on-line treatment device for thermal magnesium refining slag is configured to implement the in-situ on-line treatment method for thermal magnesium refining slag, including:
A support system and a separation system;
The support system consists of a support main body 1, a rotation and lifting main body 2 and a horizontal cantilever 3; the support main body 1 is provided with a rotation and lifting main body 2 and a horizontal cantilever 3 in a coupling way, and is used for realizing horizontal rotation and vertical lifting of the separation system;
The separation system comprises a separator rotating connecting rod 4 and a separator; the separator rotating connecting rod 4 is connected with the horizontal cantilever 3 and controls the separator to stably rotate.
Preferably, the separator comprises a separator body 5 and a separator shell 6, wherein the separator shell 6 is matched and nested with the separator body 5, the separator body 5 is removed from the separator shell 6 after separation treatment is completed, and oxide solid phase in the separator is discharged.
The technical scheme of the invention is further described below by combining specific embodiments.
The in-situ on-line treatment device for the hot magnesium refining slag is adopted in each embodiment to realize the in-situ on-line treatment of the hot magnesium refining slag.
Example 1
An in-situ on-line treatment method of hot magnesium refining slag comprises the following steps:
S1, discharging hot magnesium refining slag (components: mgO 47.5 wt%, mgF 210.3 wt%,NaCl 23.7 wt%,MgCl2 16.2 wt%,CaCl2 2.3.3 wt% and temperature: 720 ℃) generated during refining of crude magnesium flux in a certain workshop into a slag ladle with heating and heat preservation functions, controlling the temperature of the magnesium refining slag in the slag ladle to be 700 ℃, and ensuring that the magnesium refining slag has good fluidity;
S2, starting the separator to enter a rotating state, and immersing the separator into the magnesium refining slag at a low rotating speed;
S3, adjusting the rotating speed of the separator and the depth of the immersed magnesium refining slag, wherein the gravity coefficient generated when the separator rotates is 300g, the depth of the separator immersed magnesium refining slag is 10cm, so that a solid-liquid mixture of the magnesium refining slag continuously enters the separator, a flux liquid phase flows back into a slag ladle during the period, an oxide solid phase is intercepted in the separator, solid-liquid separation is realized, and the oxide solid phase is discharged after 10 minutes of separation;
s4, repeating the step S3 until no oxide solid phase is discharged, wherein the residual liquid phase in the slag ladle is high-purity flux, and the flux can be recycled for refining the coarse magnesium flux.
The solid phase collected in the separation device and the residual flux liquid phase in the slag ladle are sampled, and then the components are detected and assayed, and the macro morphology shooting and SEM-EDS analysis are carried out, so that the results are shown in figure 3. As can be seen from FIG. 3, the solid phase in the magnesium refining slag mainly consists of MgO and MgF 2 particles, the solid phase content is about 48.7%, the particle size range of the solid phase particles in the magnesium refining slag is 8-20 μm after separation by a separation device, the solid phase removal rate reaches 94.87% after in-situ on-line treatment, the residual flux liquid phase in the slag ladle consists of MgCl 2 and NaCl, and the purity of the flux in the slag ladle reaches 98.17%.
Example 2
The difference from example 1 is that the gravity coefficient generated when the separator rotates was 400g, and the depth of the separator immersed in the magnesium refining slag was 15cm.
In this embodiment, the solid phase removal rate after in-situ on-line treatment reaches 96.95%, the purity of the flux in the slag ladle reaches 98.91%, and it can be seen that the separation efficiency can be further improved by improving the gravity coefficient and the submerging depth of the separation equipment.
Example 3
The difference from example 1 is that a different hot magnesium refining slag (composition: mgO 47.3 wt%, mgF 210.5 wt%,NaCl 23.4 wt%,MgCl2 16.6 wt%,CaCl2 2.2.2. 2.2 wt%; temperature: 750 ℃ C.) was treated.
In this embodiment, the solid phase removal rate after in-situ on-line treatment is 94.39%, and the purity of the flux in the slag ladle is 98.01%.
Example 4
An in-situ on-line treatment method of hot magnesium refining slag comprises the following steps:
S1, discharging hot magnesium refining slag (component :MgO 39.6 wt%,CaO 4.2 wt%,MgF2 7.3 wt%,NaCl 28.1 wt%,MgCl2 17.8 wt%,CaCl2 3.0 wt%;, temperature: 740 ℃) generated during refining of crude magnesium flux in a certain workshop into a slag ladle with heating and heat preservation functions, controlling the temperature of the magnesium refining slag in the slag ladle to be 720 ℃, and ensuring that the magnesium refining slag has good fluidity;
S2, starting the separator to enter a rotating state, and immersing the separator into the magnesium refining slag at a low rotating speed;
S3, adjusting the rotating speed of the separator and the depth of the immersed magnesium refining slag, wherein the gravity coefficient generated when the separator rotates is 200g, the depth of the separator immersed magnesium refining slag is 15cm, so that a solid-liquid mixture of the magnesium refining slag continuously enters the separator, a flux liquid phase flows back into a slag ladle during the period, an oxide solid phase is intercepted in the separator, solid-liquid separation is realized, and the oxide solid phase is discharged after 10 minutes of separation;
s4, repeating the step S3 until no oxide solid phase is discharged, wherein the residual liquid phase in the slag ladle is high-purity flux, and the flux can be recycled for refining the coarse magnesium flux.
The solid phase collected in the separation device and the residual flux liquid phase in the slag ladle are sampled, and then the components are detected and assayed, and the macro morphology shooting and SEM-EDS analysis are carried out, so that the results are shown in figure 4. As can be seen from FIG. 4, the solid phase in the magnesium refining slag mainly consists of MgO and MgF 2 particles, the solid phase content is about 45.3%, the particle size range of the solid phase particles in the magnesium refining slag is known to be 5-30 μm after separation by a separation device, the solid phase removal rate is 95.36% after in-situ on-line treatment, the residual flux liquid phase in the slag ladle consists of MgCl 2 and NaCl, and the purity of the flux in the slag ladle is 98.42%.
Example 5
The difference from example 4 is that the gravitational coefficient generated when the separator rotates is 300g.
In this embodiment, the solid phase removal rate after in-situ on-line treatment reaches 96.18%, the purity of the flux in the slag ladle reaches 98.63%, and it can be seen that the separation efficiency can be further improved by improving the gravity coefficient.
Example 6
The difference from example 4 is that a different hot magnesium refining slag (composition :MgO 39.9 wt%,CaO 4.3 wt%,MgF2 7.1 wt%,NaCl 27.7 wt%,MgCl2 17.5 wt%,CaCl2 3.5 wt%; temperature: 740 ℃ C.) was treated; the gravitational coefficient generated when the separator was rotated was 350g.
In this embodiment, the solid phase removal rate after in-situ on-line treatment is 97.19%, and the purity of the flux in the slag ladle is 98.78%.
The invention can fully utilize the latent heat of the magnesium refining slag during discharge, realize the in-situ on-line high-efficiency separation of the solid-liquid mixture of the magnesium refining slag by using the separator, and the flux liquid phase can be recycled to the crude magnesium solvent refining process to realize the high-efficiency recycling of the magnesium smelting resources.
The foregoing description is only of the preferred embodiments of the present invention and is not intended to limit the scope of the invention, and all equivalent structural changes made by the content of the present invention or direct/indirect application in other related technical fields are included in the scope of the present invention.

Claims (8)

1. The in-situ on-line treatment method of the thermal magnesium refining slag is characterized by comprising the following steps of:
s1, discharging thermal magnesium refining slag generated during refining of a crude magnesium flux into a slag ladle with heating and heat preservation functions, and ensuring that the magnesium refining slag has good fluidity;
S2, starting the separator to enter a rotating state, and immersing the separator into magnesium refining slag at a certain rotating speed;
S3, adjusting the rotating speed of the separator and the depth of immersing the magnesium refining slag, enabling the solid-liquid mixture of the magnesium refining slag to continuously enter the separator, enabling the flux liquid phase to flow back into the slag ladle during the period, enabling the oxide solid phase to be intercepted in the separator, so as to realize solid-liquid separation, and discharging the oxide solid phase;
s4, repeating the step S3 until no oxide solid phase is discharged, wherein the residual liquid phase in the slag ladle is high-purity flux, and the flux can be recycled for refining the coarse magnesium flux;
the in-situ on-line treatment device for the thermal magnesium refining slag adopted by the in-situ on-line treatment method for the thermal magnesium refining slag comprises the following components:
A support system and a separation system;
The support system consists of a support main body, a rotation and lifting main body and a horizontal cantilever; the support main body is provided with a rotating and lifting main body and a horizontal cantilever in a coupling way and is used for realizing horizontal rotation and vertical lifting of the separation system;
The separation system comprises a separator rotating connecting rod and a separator; the rotating connecting rod of the separator is connected with the horizontal cantilever to control the separator to stably rotate.
2. The in-situ on-line treatment method for hot magnesium refining slag according to claim 1, wherein in the step S1, the temperature of the hot magnesium refining slag generated during the refining of the crude magnesium flux is 710-740 ℃.
3. The in-situ on-line treatment method of hot magnesium refining slag according to claim 1, wherein in the step S1, the temperature of the magnesium refining slag in the slag ladle is controlled to be 600-700 ℃.
4. The in-situ on-line treatment method for hot magnesium refining slag according to claim 1, wherein in the step S3, the gravity coefficient generated when the separator rotates is 100-500 g.
5. The in-situ on-line treatment method of hot magnesium refining slag according to claim 1, wherein in the step S3, the separator is immersed into the magnesium refining slag to a depth of 10-15 cm.
6. The in-situ on-line treatment method of hot magnesium refining slag according to claim 1, wherein in the step S3, the rotation time of the separator is 1-10 min.
7. An in-situ on-line treatment device for thermal magnesium refining slag, for implementing the in-situ on-line treatment method for thermal magnesium refining slag according to any one of claims 1 to 6, comprising:
A support system and a separation system;
The support system consists of a support main body, a rotation and lifting main body and a horizontal cantilever; the support main body is provided with a rotating and lifting main body and a horizontal cantilever in a coupling way and is used for realizing horizontal rotation and vertical lifting of the separation system;
The separation system comprises a separator rotating connecting rod and a separator; the rotating connecting rod of the separator is connected with the horizontal cantilever to control the separator to stably rotate.
8. The in-situ on-line treatment device for hot magnesium refining slag according to claim 7, wherein the separator comprises a separator body and a separator housing, the separator housing is nested with the separator body in a matched manner, the separator body is removed from the separator housing after the separation treatment is completed, and the oxide solid phase in the separator is discharged.
CN202410429936.XA 2024-04-10 2024-04-10 In-situ on-line treatment method and device for thermal magnesium refining slag Active CN118028624B (en)

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JP4435800B2 (en) * 2007-04-09 2010-03-24 株式会社湯沢亜鉛鍍金工業所 Hot-dip galvanizing method and robot apparatus in hot-dip galvanizing treatment
JP5638222B2 (en) * 2009-11-04 2014-12-10 株式会社アーレスティ Heat-resistant magnesium alloy for casting and method for producing alloy casting
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CN113832351A (en) * 2021-10-18 2021-12-24 北京科技大学 Method for recycling molten salt and metal aluminum by virtue of supergravity synergistic treatment of magnesium refining slag and aluminum ash

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