CN106801234B - The preparation method of aluminium lithium intermediate alloy - Google Patents
The preparation method of aluminium lithium intermediate alloy Download PDFInfo
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- CN106801234B CN106801234B CN201710034150.8A CN201710034150A CN106801234B CN 106801234 B CN106801234 B CN 106801234B CN 201710034150 A CN201710034150 A CN 201710034150A CN 106801234 B CN106801234 B CN 106801234B
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Abstract
The invention discloses a kind of preparation method of aluminium lithium intermediate alloy, comprising steps of A, by the furnace charge that opens comprising LiCl being placed in electrolytic cell and carrying out opening furnace, opens furnace charge melting and obtain electrolyte；B, electrolysis unit is switched into electrolysis system；C, solid aluminium is placed on the electrolytic anode of electrolysis unit and is immersed in electrolyte with electrolytic anode；D, the electrolysis power of electrolysis unit is opened, solid aluminium is fused into liquid aluminium and is settled down on the cathode conductive plate of bottom of electrolytic tank, and connect to form liquid cathode with cathode conductive plate；E, LiCl is added according to electrolytic condition timing, LiCl is electrolysed and forms liquid aluminium lithium alloy with one step alloying of liquid aluminium；F, by liquid aluminium lithium alloy timing discharging and ingot bar molding, aluminium lithium intermediate alloy is obtained.Preparation method according to the present invention is carried out based on large scale electrolytic cell；Meanwhile the preparation method fully relies on electrolysis self-heating and realizes temperature control, no external heat is suitable for industrial amplification production.
Description
Technical field
The invention belongs to field of alloy preparation technology, in particular, being related to a kind of aluminium based on industrial large scale electrolytic cell
The preparation method of lithium intermediate alloy.
Background technique
With the development of high-performance aerospace aircraft, to the lightweight of its internal component, more stringent requirements are proposed.
Aluminium alloy is most widely used one kind non-ferrous metal structural material in industry, and Li is the most light metal of nature, density
Only 0.534g/cm3, into aluminium alloy be added 1wt% Li, can make alloy density reduce by 3%, elasticity modulus improve 6%, and
And alloy has ageing strengthening effect, therefore adds Li in aluminium alloy and caused more and more to pay close attention to.Aluminium lithium alloy is excellent
The characteristics such as good low-density, high specific strength, high specific stiffness make it become the primary structure of the aerospace flight vehicle of a new generation
Material.
Li chemical activity is very high, in the form of pure metal Li when Melting of Al-li Alloy, can bring very to production and keeping
It is big difficult, and Li is added in the form of aluminium lithium intermediate alloy, then well solve this problem.The preparation of aluminium lithium intermediate alloy
Mainly there is the method for producing aluminium lithium intermediate alloy at present to the method for mixing and fused salt electrolysis process mostly to the method for mixing, but the technique is made
Valence cost, lithium burn out rate and due to aluminium and lithium density and different melting points greatly caused by the unequal aspect of alloying component restriction.
And fused salt electrolysis process is improved on the basis of traditional electrolyte legal system lithium, a step DIRECT ALLOYING, reduces the oxidation of metal
Loss, and technology stability is good.
It mainly includes solid state cathode method and liquid cathode method that fused salt electrolysis process, which prepares aluminium lithium intermediate alloy,.Solid state cathode method is
Using solid Al as cathode, LiCl-KCl is electrolyte, 440 DEG C~500 DEG C of electrolysis temperature, utilizes Li+After cathodic discharge, Li+To
Aluminium lithium alloy is diffuseed to form in solid Al.Liquid cathode method is using liquid Al as cathode, and LiCl-LiF is electrolyte, with LiCl or
Li2CO3For raw material, electrolysis temperature is 680 DEG C or so, and maximum current efficiency is up to 66.1%.But above-mentioned preparation method is used at present
Shi Jun is based on the lab scale of laboratory, and all external heats provide heat, the technique of technique and industrial large scale electrolytic cell
Difference is larger, can not be applied in industrial amplification production.
Summary of the invention
To solve the above-mentioned problems of the prior art, the present invention provides a kind of preparation method of aluminium lithium intermediate alloy,
The preparation method is carried out based on large scale electrolytic cell, which fully relies on electrolysis self-heating and realize temperature control, without outer
Heating is suitable for industrial amplification production close to industrialization electrolysis process.
In order to achieve the above object of the invention, present invention employs the following technical solutions:
A kind of preparation method of aluminium lithium intermediate alloy, comprising steps of A, furnace charge will be opened be placed in the electrolytic cell of electrolysis unit,
The electrolysis unit is carried out using starting the arc heating to open furnace, it is described to open furnace charge melting acquisition electrolyte；The furnace charge that opens includes
LiCl；B, after wait open furnace, the electrolysis unit is switched into electrolysis system；C, solid aluminium is placed in the electrolysis unit
On electrolytic anode, and immersed in the electrolyte together with the electrolytic anode；D, the electrolysis power of the electrolysis unit is opened,
The solid aluminium fusing generates liquid aluminium and is settled down on the cathode conductive plate of the bottom of electrolytic tank, and conductive with the cathode
Plate connects to form liquid cathode；E, LiCl is added into the electrolytic cell according to electrolytic condition timing, the LiCl is given birth to by electrolysis
At lithium metal, the lithium metal and the one step alloying of liquid aluminium form liquid aluminium lithium alloy；F, the liquid aluminium lithium is closed
Golden timing discharging and ingot bar molding, obtain aluminium lithium intermediate alloy.
Further, in the step B, the Faradaic current for controlling the electrolysis unit is 5000A~7000A, electric current
Density is 2.5A/cm2~3A/cm2, electrolysis temperature is 690 DEG C~720 DEG C.
Further, the furnace charge that opens further includes eutectic auxiliary material；It is opened in furnace charge described, the quality percentage of the LiCl
Number is at least 50%.
Further, the eutectic auxiliary material is KCl.
Further, in the step A, open the specific method of furnace to the electrolysis unit comprising steps of by institute
The tip for opening arc electrode for stating electrolysis unit is in contact with the graphite protection block on the cathode conductive plate, and prevents from described opening arc
Electrode is in contact with the cathode conductive plate；Furnace charge will be opened described in part to be placed in the electrolytic cell；Open alternating current steady voltage plug
Furnace charge is opened described in heating, makes described to open furnace charge and become liquid completely；Using molten salt electrolyte conductive heater, gradually to the electrolysis
Supplement opens furnace charge in slot, obtains the electrolyte, and the electrolyte is made to reach electrolysis aequum.
Further, the electrolysis aequum, which refers to, immerses the rear holding electricity in the electrolyte for the electrolytic anode
Solve the dosage when spacing between the bottom end and the cathode conductive plate of anode is at least 5cm.
It further, include: logical by the specific method that the electrolysis unit switches to electrolysis system in the step B
The electrode lifting device for crossing the electrolysis unit increases the arc electrode that opens, to open arc electricity described in electrolytic anode replacement
Pole.
Further, the material of the electrolytic anode is graphite, and the material of the cathode conductive plate is molybdenum or tungsten.
Further, the upper end of the electrolytic anode is in the form of a column, and lower end is in platform-like, and the width of the lower end is greater than upper
The width at end；Wherein, the platform of the lower end of the electrolytic anode has through-hole, so that after solid aluminium fusing generates liquid aluminium
It is settled down on the cathode conductive plate through the through-hole.
Further, in the step C, before the solid aluminium is placed on the electrolytic anode of the electrolysis unit,
The pre-heat treatment is carried out to the solid aluminium.
The present invention obtains the aluminium lithium that can be applied to large scale electrolytic cell by rationally designing the parameters such as Faradaic current, temperature
The preparation method of intermediate alloy, the preparation method are a kind of industrialized electrolysis process, are suitable for industrial amplification production；Meanwhile
The preparation method fully relies on electrolysis self-heating and realizes temperature control, is not necessarily to external heat, overcomes small through laboratory in the prior art
Try the problem of technological parameter obtained can not be suitable for the large scale electrolytic cell of industrial amplification production.
Detailed description of the invention
What is carried out in conjunction with the accompanying drawings is described below, the description of the embodiment of the present invention and other aspects, features and advantages
It will become clearer, in attached drawing:
Fig. 1 is the step flow chart of the preparation method of aluminium lithium intermediate alloy according to the present invention；
Fig. 2 is the structural schematic diagram of the electrolysis unit of embodiment according to the present invention；
Fig. 3 is the structural schematic diagram for opening arc electrode of embodiment according to the present invention；
Fig. 4 is the structural schematic diagram of the electrolytic anode of embodiment according to the present invention.
Specific embodiment
Hereinafter, with reference to the accompanying drawings to detailed description of the present invention embodiment.However, it is possible to come in many different forms real
The present invention is applied, and the present invention should not be construed as limited to the specific embodiment illustrated here.On the contrary, providing these implementations
Example is in order to explain the principle of the present invention and its practical application, to make others skilled in the art it will be appreciated that the present invention
Various embodiments and be suitable for the various modifications of specific intended application.In the accompanying drawings, for the sake of clarity, element can be exaggerated
Shape and size, and identical label will be used to indicate the same or similar element always.
Fig. 1 is the step flow chart of the preparation method of the aluminium lithium intermediate alloy of embodiment according to the present invention.
Referring in particular to Fig. 1, the preparation method of aluminium lithium intermediate alloy according to the present invention includes the following steps:
Step S1, furnace charge will be opened to be placed in the electrolytic cell of electrolysis unit, electrolysis unit is opened using starting the arc heating
Furnace opens furnace charge melting and obtains electrolyte.
Specifically, opening furnace charge includes LiCl, certainly, in order to obtained when opening furnace it is lower open furnace temperature, reduce energy consumption,
It is preferred that opening in furnace charge further includes the eutectic auxiliary material such as KCl；When opening in furnace charge includes eutectic auxiliary material, the wherein quality hundred of LiCl
Score is not less than 50%, and KCl is preferably mixed acquisition according to mass ratio with LiCl for 1:1 in the present embodiment and opens furnace charge.
The structural schematic diagram for the electrolysis unit that the preparation method of the present embodiment is based on is as shown in Figure 2.The electrolysis unit packet
The electrolytic cell 11 of the square shape of a masonry is included, the bottom of electrolytic cell 11 is inserted with cathode conductive plate 12, sets on cathode conductive plate 12
It is equipped with graphite protection block 121, electrode lifting device 13 is provided with by electrolytic cell 11, the mechanical arm 131 of the electrode lifting device 13,
Mechanical arm 131 opens arc electrode (not shown) or electrolytic anode (not shown) for hanging to set.As shown in figure 3, opening arc electricity
The great tip 151 for having a wedge shape or taper, when using opening arc electrode and carrying out opening furnace, the tip 151 is towards in electrolytic cell 11
Portion；As shown in figure 4, electrolytic anode has the lower end 162 of connected columnar upper end 161 and platform-like, electrolytic anode is being utilized
When being electrolysed, the upper end 161 is connected with the end of extension 131, and towards inside electrolytic cell 11, lower end 162 has for lower end 162
There are several through-hole (not shown)s towards inside electrolytic cell 11, in this way, the electrolytic anode can be in subsequent load bearing solid aluminium
During, so that the liquid aluminium that fusing obtains is settled down to the bottom of electrolytic cell 11 via these through-holes.
In the present embodiment, the material of electrolytic anode is preferably graphite, and the material of cathode conductive plate 12 is preferably molybdenum, certainly
It is also possible to such as tungsten conduction and metal material resistant to high temperature.
In the present embodiment, electrolysis unit is carried out referring to following method opening furnace operation: (1) arc electrode will be opened and is hung at machine
The end of tool arm 131, and so that the tip for opening arc electrode 151 is in contact with graphite protection block 121, and prevent from opening arc electrode and cathode
Conductive plate 12 is in contact；(2) furnace charge will be partially opened to be placed in electrolytic cell 11；(3) it opens alternating current steady voltage plug heating and opens furnace charge, make
Open furnace charge becomes liquid completely；(4) raising of arc electrode will be opened by electrode lifting device 13, will be added using molten salt electrolyte conduction
Heat, gradually into electrolytic cell 11, supplement opens furnace charge, obtains electrolyte, and electrolyte is made to reach electrolysis aequum.
It is worth noting that electrolysis aequum described herein, which refers to, immerses rear holding electrolysis in electrolyte for electrolytic anode
Spacing between the bottom end and cathode conductive plate of anode is at least dosage when 5cm, and this spacing is also referred to as pole span.
In the present embodiment, in Starting-up process, total addition 140kg opens furnace charge.
Step S2, after wait open furnace, electrolysis unit is switched into electrolysis system.
Specifically, arc electrode will be opened by the electrode lifting device of electrolysis unit to increase, and opened with electrolytic anode replacement
Arc electrode, meanwhile, graphite protection block 121 is removed together.
Step S3, solid aluminium is placed on electrolytic anode, and is immersed in electrolyte together with electrolytic anode.
Electrolyte temperature is higher when Given this, and bumping occurs when contacting solid aluminium in it in order to prevent, preferably to solid aluminium
It is placed it on electrolytic anode again after carrying out the pre-heat treatment.
In the present embodiment, the dosage of solid aluminium is 10kg.
Step S4, the electrolysis power of electrolysis unit is opened, solid aluminium fusing generates liquid aluminium and is settled down to cathode conductive plate
On, and connect to form liquid cathode with cathode conductive plate.
The Faradaic current for controlling electrolysis unit is 5000A~7000A, current density 2.5A/cm2~3A/cm2, electrolysis temperature
Degree is 690 DEG C~720 DEG C；In the present embodiment, preferably adjusting Faradaic current first is 7000A, so that the furnace temperature of electrolysis unit
It is rapidly heated to 700 DEG C, rear to reduce Faradaic current and be maintained at 5000A, holding current density is 2.5A/cm2, control electrolysis temperature
Degree is 700 DEG C ± 10 DEG C.
Step S5, LiCl is added into electrolytic cell according to electrolytic condition timing, LiCl is by electrolytically generated lithium metal, lithium metal
Liquid aluminium lithium alloy is formed with one step alloying of liquid aluminium.
In the present embodiment, 7kg LiCl is added according to electrolytic condition determination per hour.
It during adding LiCl, is preferably slowly added, to prevent the tail gas that generates in electrolytic process from will add
LiCl takes away, and causes loss of material.
Step S6, by liquid aluminium lithium alloy timing discharging and ingot bar forms, and obtains aluminium lithium intermediate alloy.
Before discharging, to prevent quenching from causing, liquid aluminium lithium alloy solidifies or electrolyte is precipitated, preferably can be by electrolysis unit
Furnace temperature rise to 720 DEG C or more, then discharging container is placed in electrolyte after being kept the temperature contain liquid aluminium lithium alloy carry out
Discharging finally carries out an ingot bar molding to the liquid aluminium lithium alloy after discharging, on the one hand ensure that nothing in liquid aluminium lithium alloy
It cools down and carries electrolyte secretly, while the aluminium lithium intermediate alloy obtained being avoided the bad phenomenon of block layering occur.
While carrying out the discharging of liquid aluminium lithium alloy, inevitably entrainment portions electrolyte, this partial electrolyte
In cooling procedure, inorganic salts can be generated to be attached on the surface of aluminium lithium intermediate alloy, the strong absorptive of LiCl draws in order to prevent
The alloy surface moisture absorption is played, after obtaining aluminium lithium intermediate alloy, mechanical grinding preferably is carried out to its surface, and be sealed.
Preferably, when carrying out the discharging of liquid aluminium lithium alloy from cathode conductive plate, preferred remainder liquid aluminium lithium
Alloy guarantees the gold of next manufacturing cycle electrolysis initial stage generation using the liquid cathode as electrolysis initial stage in next manufacturing cycle
Belong to lithium and directly generate liquid aluminium lithium alloy in bottom of electrolytic tank, without floating to bath surface.
It is worth noting that the relative amount of lithium depends mainly between discharging time in the aluminium lithium intermediate alloy finally obtained
Every discharging time interval is longer, and the relative amount of lithium is higher in the aluminium lithium intermediate alloy of acquisition.
In the present embodiment, discharging in every three hours is primary, and 10kg solid aluminium is added after discharging and is continuously prepared.To for 24 hours
The preparation process of (discharging 8 times altogether) carries out average computation, produces aluminium lithium intermediate alloy 85.4kg altogether, and current efficiency is about 55%,
Lithium yield is about 81%.
It takes the aluminium lithium intermediate alloy surface of the above-mentioned acquisition that wherein discharges three times to carry out mechanical grinding, clears up surface fused salt, take
After the dissolution of fritter sample, constituent analysis is carried out by Atomic Emission Spectrometer AES (abbreviation ICP), the results are shown in Table 1 for analysis.
Table 1 discharge three times acquisition aluminium lithium intermediate alloy constituent analysis comparison (wt%)
From table 1 it follows that being closed among the aluminium lithium obtained according to the preparation method of the aluminium lithium intermediate alloy of the present embodiment
The mass percent of Li is 15%~21% in gold, simultaneously as the composition and purity of furnace charge are opened, wherein can also coexist a small amount of
Other impurities element.
Although the present invention has shown and described referring to specific embodiment, it should be appreciated by those skilled in the art that:
In the case where not departing from the spirit and scope of the present invention being defined by the claims and their equivalents, can carry out herein form and
Various change in details.
Claims (9)
1. a kind of preparation method of aluminium lithium intermediate alloy, the preparation method is a kind of industrialization suitable for industrial amplification production
Electrolysis process；Characterized in that it comprises the following steps:
A, furnace charge will be opened to be placed in the electrolytic cell of electrolysis unit, the electrolysis unit is carried out using starting the arc heating to open furnace, institute
It states and opens furnace charge melting acquisition electrolyte；The furnace charge that opens includes LiCl；
B, after wait open furnace, the electrolysis unit is switched into electrolysis system；The Faradaic current for controlling the electrolysis unit is
5000A~7000A, current density 2.5A/cm2~3A/cm2, electrolysis temperature is 690 DEG C~720 DEG C；
C, solid aluminium is placed on the electrolytic anode of the electrolysis unit, and immerses the electrolyte together with the electrolytic anode
In；
D, the electrolysis power of the electrolysis unit is opened, the solid aluminium fusing generates liquid aluminium and is settled down to the cell bottom
On the cathode conductive plate in portion, and it connect to form liquid cathode with the cathode conductive plate；
E, LiCl is added into the electrolytic cell according to electrolytic condition timing, the LiCl is by electrolytically generated lithium metal, the gold
Belong to lithium and the one step alloying of liquid aluminium forms liquid aluminium lithium alloy；
F, by the liquid aluminium lithium alloy timing discharging and ingot bar molding, aluminium lithium intermediate alloy is obtained.
2. preparation method according to claim 1, which is characterized in that the furnace charge that opens further includes eutectic auxiliary material；Institute
It states and opens in furnace charge, the mass percent of the LiCl is at least 50%.
3. preparation method according to claim 2, which is characterized in that the eutectic auxiliary material is KCl.
4. preparation method according to claim 1 to 3, which is characterized in that in the step A, filled to the electrolysis
Set the specific method for carrying out opening furnace comprising steps of
The tip for opening arc electrode of the electrolysis unit is in contact with the graphite protection block on the cathode conductive plate, and is prevented
The arc electrode that opens is in contact with the cathode conductive plate；
Furnace charge will be opened described in part to be placed in the electrolytic cell；
It opens and opens furnace charge described in alternating current steady voltage plug heating, make described to open furnace charge and become liquid completely；
Using molten salt electrolyte conductive heater, gradually into the electrolytic cell, supplement opens furnace charge, obtains the electrolyte, and make institute
It states electrolyte and reaches electrolysis aequum.
5. the preparation method according to claim 4, which is characterized in that the electrolysis aequum refers to the electrolytic anode
When the spacing between the bottom end and the cathode conductive plate of the electrolytic anode being kept to be at least 5cm after immersing in the electrolyte
Dosage.
6. the preparation method according to claim 4, which is characterized in that in the step B, the electrolysis unit is switched
Specific method to electrolysis system includes:
The arc electrode that opens is increased by the electrode lifting device of the electrolysis unit, to be opened described in electrolytic anode replacement
Arc electrode.
7. preparation method according to claim 1, which is characterized in that the material of the electrolytic anode is graphite, the yin
The material of pole conductive plate is molybdenum or tungsten.
8. preparation method according to claim 1, which is characterized in that the upper end of the electrolytic anode is in the form of a column, and lower end is in
Platform-like, and the width of the lower end is greater than the width of upper end；Wherein, the platform of the lower end of the electrolytic anode has through-hole,
So that the solid aluminium fusing is settled down on the cathode conductive plate after generating liquid aluminium through the through-hole.
9. preparation method according to claim 1, which is characterized in that in the step C, the solid aluminium is placed in institute
Before stating on the electrolytic anode of electrolysis unit, the pre-heat treatment is carried out to the solid aluminium.
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| CN1004497B (en) * | 1986-12-30 | 1989-06-14 | 冶金工业部包头稀土研究院 | Mfr. of al-li intermediate-alloy |
| RO115890B1 (en) * | 1996-11-11 | 2000-07-28 | Sc Inst De Metale Neferoase Si | PROCESS FOR PREPARING Al -Li PRE-ALLOY |
| CN102212843A (en) * | 2011-05-25 | 2011-10-12 | 中国科学院青海盐湖研究所 | Start-up method for preparing metal and alloys through molten salt electrolysis |
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