CN109055996B - Method for preparing aluminum-samarium intermediate alloy by submerged cathode molten salt electrolysis - Google Patents
Method for preparing aluminum-samarium intermediate alloy by submerged cathode molten salt electrolysis Download PDFInfo
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- 150000003839 salts Chemical class 0.000 title claims abstract description 52
- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 41
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 40
- 239000000956 alloy Substances 0.000 title claims abstract description 40
- -1 aluminum-samarium Chemical compound 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 24
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 26
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910021175 SmF3 Inorganic materials 0.000 claims abstract description 25
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000002844 melting Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 239000012856 weighed raw material Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000007769 metal material Substances 0.000 abstract description 3
- 239000004411 aluminium Substances 0.000 abstract 2
- 229910052772 Samarium Inorganic materials 0.000 description 8
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 8
- 229910052761 rare earth metal Inorganic materials 0.000 description 7
- 239000000126 substance Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 150000002910 rare earth metals Chemical class 0.000 description 3
- 230000005611 electricity Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910013618 LiCl—KCl Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- 229910000612 Sm alloy Inorganic materials 0.000 description 1
- 229910001361 White metal Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- KPLQYGBQNPPQGA-UHFFFAOYSA-N cobalt samarium Chemical compound [Co].[Sm] KPLQYGBQNPPQGA-UHFFFAOYSA-N 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000009533 lab test Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000028161 membrane depolarization Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000010969 white metal Substances 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/36—Alloys obtained by cathodic reduction of all their ions
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/02—Electrodes; Connections thereof
- C25C7/025—Electrodes; Connections thereof used in cells for the electrolysis of melts
Abstract
The invention belongs to the technical field of metal materials, and particularly discloses a method for preparing an aluminum-samarium intermediate alloy by submerged cathode molten salt electrolysisThe following steps are respectively weighed: SmF3、LiF、K3AlF6、Sm2O3And an aluminum ingot, and the mass ratio of the raw materials is ensured as follows: (SmF)3+LiF):K3AlF620:80-10: 90; (2) k in the step (1)3AlF6Putting into an electrolytic cell, heating to raise the temperature until K is reached3AlF6Adding SmF after complete melting3+ LiF; to be SmF3+ LiF is completely melted, then adding aluminium ingot, after the aluminium ingot is melted, adding Sm2O3Until the mixture is melted; (3) and (4) carrying out fused salt electrolysis, wherein the prepared aluminum-samarium intermediate alloy sinks at the bottom of the electrolytic bath. The method for preparing the aluminum-samarium intermediate alloy by cathode molten salt electrolysis is environment-friendly and low in production cost, and the prepared aluminum-samarium intermediate alloy is deposited at the bottom of the molten salt and is suitable for industrial mass production and application.
Description
Technical Field
The invention belongs to the technical field of metal materials, and particularly discloses a method for preparing an aluminum-samarium intermediate alloy by submerged cathode molten salt electrolysis.
Background
The rare earth samarium is a white metal and is mainly applied to samarium-cobalt magnetic materials. At present, samarium is continuously developed to be applied in other fields, for example, the solid solubility in magnesium reaches 5.8 percent, and the performance of magnesium alloy can be improved through solid solution strengthening. In addition, samarium can obviously improve the comprehensive service performance and the corrosion resistance of the aluminum alloy, and is widely applied to the production and preparation of metal materials.
The rare earth elements have high chemical activity, are easy to burn and have serious segregation,if the rare earth metal is directly added into the alloy, the rare earth element is seriously burnt, so in order to ensure that the rare earth element can fully play a role, the rare earth element is added into the metal in the form of rare earth intermediate alloy under the normal condition. At present, the preparation method of the aluminum-samarium intermediate alloy is mainly a molten salt electrolysis method which is divided into a chloride system and a fluoride system, wherein the Sm is researched by Harbin engineering university in China3+Electrochemical behaviour in chloride (LiCl-KCl) molten salt system. But due to SmCl3Strong hygroscopicity and environmental pollution generated by electrolysis2The chloride system is gradually replaced by the fluoride electrolysis system.
In the fused salt electrolysis process, Sm3+Inclined to obtain an electron Sm on the cathode2+Is difficult to be reduced to Sm on the cathode, and Sm is2+The anode loses electrons again to form Sm3+A reduction-oxidation-reduction cycle is formed, and the electricity is consumed and accumulated in the dielectric medium, so that the current efficiency is reduced (the current efficiency refers to the effective utilization rate of direct current actually used for oxidizing and reducing a certain substance in the electrolytic process).
In order to solve the technical problems, the applicant applies a method for preparing an aluminum-samarium intermediate alloy by a liquid cathode molten salt electrolysis method (application publication number is CN104775137A) in 1 month in 2014, wherein the method is SmF3+ LiF is the molten salt system, Sm2O3Is an electrolyte, aluminum is a liquid cathode, graphite is an anode, and the cathode current density is 1-2A/cm at the temperature of 750-2Electrolysis is carried out under the conditions of (1).
The applicant finds that although the above patent solves the problem of current consumption during the electrolysis process, the produced samarium-aluminum master alloy liquid floats on the liquid surface of the molten salt. When the product is collected, researchers (or workers) need to scoop out the aluminum-samarium intermediate alloy liquid on the molten salt liquid level, then cast, and strip the molten salt after cooling for weighing and analysis, namely the method is only suitable for laboratory tests.
Disclosure of Invention
The invention aims to provide a method for preparing an aluminum-samarium intermediate alloy by cathode molten salt electrolysis, which is environment-friendly and suitable for industrial mass production.
In order to achieve the purpose, the basic scheme of the invention is as follows:
a method for preparing aluminum-samarium intermediate alloy by sinking cathode molten salt electrolysis comprises the following steps,
(1) respectively weighing the following raw materials: SmF3、LiF、K3AlF6、Sm2O3And an aluminum ingot, and the mass ratio of the raw materials is ensured as follows: (SmF)3+LiF):K3AlF6＝20:80-10:90；
(2) K in the step (1)3AlF6Putting into an electrolytic cell, heating to raise the temperature until K is reached3AlF6Adding SmF after complete melting3And LiF; to be SmF3And after LiF is completely melted, adding an aluminum ingot, and after the aluminum ingot is melted, adding Sm2O3Until the mixture is melted;
(3) and carrying out molten salt electrolysis, wherein the cathode of the molten salt electrolysis is liquid aluminum, the anode of the molten salt electrolysis is graphite, and the prepared aluminum-samarium intermediate alloy sinks at the bottom of the electrolytic bath.
The working principle and the beneficial effects of the basic scheme are as follows:
SmF of the invention3+ LiF is SmF3And LiF, in SmF according to the invention3+ LiF is the molten salt system (the molten salt system is used as the reaction medium and the electrolysis medium), Sm2O3Is an electrolyte; the invention takes liquid aluminum (which is prepared from molten aluminum ingots) with depolarization function and capable of reducing the precipitation potential of samarium as a cathode.
Due to SmF3+ LiF (especially SmF)3) Has a relatively high density of K3AlF6Is less dense, so that when prepared, SmF is first mixed3+ LiF molten salt system dissolved in K3AlF6Internal, helps to reduce SmF3The overall density of the + LiF molten salt system is reduced (or "neutralized") below that of liquid aluminum, resulting in SmF3+ LiF meltThe salt system is arranged at the upper part of the electrolytic bath, and the liquid aluminum is deposited at the bottom of the electrolytic bath.
During electrolysis, the generated aluminum-samarium intermediate alloy liquid is attached to a cathode (liquid aluminum), namely the generated aluminum-samarium intermediate alloy liquid is gradually accumulated at the bottom of an electrolytic cell, workers can take the aluminum-samarium intermediate alloy liquid out through the existing equipment, and the structure of the electrolytic cell is not required to be improved for preparing the aluminum-samarium intermediate alloy.
In addition, the invention controls SmF3+ LiF and K3AlF6In a mass ratio of (A) to (B)3AlF6Not only can reduce the density of a molten salt system to ensure that liquid aluminum sinks to the bottom of the electrolytic cell to realize the sinking of a product (aluminum-samarium intermediate alloy), but also can ensure Sm2O3The melting degree in the molten salt has small influence on the conductivity of the molten salt.
After electrolysis, compared with CN104775137A (a method for preparing the aluminum-samarium intermediate alloy by a liquid cathode molten salt electrolysis method, the current efficiency can reach more than 90 percent, and the Sm content in the aluminum-samarium alloy can reach more than 30 percent (the Sm content is the proportion of the Sm in the aluminum-samarium intermediate alloy), the Sm content and the current efficiency of the method are reduced, but the method adopted by the application does not need workers to scoop out the aluminum-samarium intermediate alloy liquid on the upper layer of the molten salt, does not need to improve the structure of an electrolytic cell for preparing the aluminum-samarium intermediate alloy, is very suitable for industrial mass production and application, and is completely different from the prior application (CN104775137A) or a plurality of theoretical researches concentrated on preparing the aluminum-samarium intermediate alloy.
The invention employs fluoride systems (SmF)3、LiF、K3AlF6) No harmful gas is produced, and the method is environment-friendly. The invention adopts the cheap and easily obtained Sm2O3As an electrolysis raw material, the production cost can be greatly saved.
Further, SmF3LiF 75:25-90:10, SmF3When the ratio of LiF is in the range of 75:25-90:10, the current efficiency and the Sm content in the product are both better.
Further, Sm2O3The content of (B) is 1-3 wt% of the total amount of the molten salt, and Sm can be ensured2O3In SmF3LiF and K3AlF6The solubility is preferred. The total amount of molten salt referred to in this application is SmF3And the sum of the LiF masses.
Further, the electrolysis temperature in the step (3) is 800-900 ℃, so that the higher current efficiency can be kept, and the volatilization of the molten salt can be reduced.
Further, the step (1) further comprises: the raw materials after weighing are respectively dried and preheated, and the raw materials are preheated, so that the raw materials can be effectively prevented from absorbing water.
Further, the drying preheating temperature of the step (1) is 200 ℃, and the drying preheating time is 2 hours. The drying temperature of 200 ℃ can achieve better drying effect and can prevent SmF3And LiF absorbs water, thereby preventing other side reactions from occurring.
Drawings
FIG. 1 is a SEM scan at low magnification of an aluminum samarium master alloy prepared in example 3 of the present invention;
fig. 2 is a SEM scanning photograph of the samaric intermediate alloy prepared in example 3 of the present invention at high magnification.
Detailed Description
The present invention will be described in further detail below by way of specific embodiments:
examples
A method for preparing an aluminum-samarium intermediate alloy by submerged cathode molten salt electrolysis comprises the following steps:
(1) respectively weighing the following raw materials: SmF3、LiF、K3AlF6、Sm2O3And the aluminum ingot ensures that the raw materials have the mass ratio: (SmF)3+LiF):K3AlF6＝20:80-10:90，SmF3:LiF＝75:25-90:10，Sm2O3The content of (C) is 1-3 wt% of the total amount of the molten salt, K3AlF6The content of the molten salt is 80-90 wt% of the total amount of the molten salt; and weighing SmF3、LiF、K3AlF6、Sm2O3And drying and preheating the aluminum ingot at 200 ℃ for 2h respectively for later use.
(2) The preheated K in the step (1)3AlF6Putting into an electrolytic cell, heating and raising the temperatureAt the temperature of 800 ℃ and 900 ℃ for K3AlF6Adding preheated SmF after complete melting3And LiF; to be SmF3After LiF is completely melted, adding preheated aluminum ingot, and after the aluminum ingot is melted, adding Sm2O3Until the mixture is melted;
(3) carrying out molten salt electrolysis: taking liquid aluminum as a cathode, graphite as an anode, cathode current of 50A and electrolysis time of 30-40min, and sinking the prepared aluminum-samarium intermediate alloy at the bottom of the electrolytic bath.
(4) And after the electrolysis is finished, taking out the aluminum samarium intermediate alloy liquid, and casting the aluminum samarium intermediate alloy liquid into a mold for stripping.
The samarium, the simple substance samarium, the Sm or the Sm simple substance are all equivalent.
According to the method, the embodiment is as follows:
examples 1 to 6 differ only in the amount of raw material charged, examples 7 to 9 differ only in the electrolysis temperature, and examples 10 to 13 differ only in Sm2O3The contents of (A) and (B) are different, and the specific input amounts, electrolysis temperatures and Sm of examples 1 to 132O3The content of (B) is shown in Table 1, wherein Sm is2O3Is Sm in2O3Ratio of the amount of the molten salt (hereinafter abbreviated as Sm)2O3Occupancy).
The electrolysis conditions (except for electrolysis temperature) for examples 1-13 were: the liquid aluminum is used as a cathode, the graphite is used as an anode, the cathode current is 50A, and the electrolysis time is 30-40 min.
TABLE 1
And (4) conclusion:
(1) examples 1 to 4 differ only in SmF3Different mass ratios of LiF, wherein the Sm content and current efficiency of example 3 were the best.
(2) Example 3 (SmF)3+LiF:K3AlF6Sm content 20:80) was example 6 (SmF)3+LiF:K3AlF610:90) twice the Sm content, but the current efficiency of example 3The ratio was 22.8 times the current efficiency of example 6, because of SmF in example 6 compared to example 33+ low LiF content, Sm2O3The solubility in a molten salt system is reduced, and the current efficiency is lower;
example 5 (SmF)3+LiF:K3AlF640:60) SmF3The + LiF content is too high, the liquid aluminum does not contact the electrolytic bath and cannot be used as a cathode for conducting electricity (the density of a molten salt system is greater than that of the liquid aluminum), so that samarium cannot be electrolyzed.
(3) As can be seen from comparison of examples 3 and 7 to 9, the increase in electrolysis temperature is effective in improving the current efficiency, but at higher temperatures, SmF3The solubility in the molten salt is increased, and the electrolyzed samarium is dissolved in the molten salt, so that the product separation is not facilitated. In addition, too high a temperature also leads to K3AlF6The volatilization of the catalyst is accelerated, the cost is increased, and the method is not favorable for industrial large-scale production and application.
(4) Sm in example 12, which is obtained by comparing example 3 with examples 10 to 132O3The content is less than 0.1 wt%, and the Sm content and the current efficiency of example 12 are far lower than those of example 3 and example 10; sm of example 132O3In the amount of > 3 wt%, but Sm content and current efficiency of example 13 were similar to those of examples 3 and 11, in general, when Sm was present2O3When the amount is 1 to 3 wt%, the content of Sm and the current efficiency are preferable.
(5) The intricately arranged white strips in fig. 1 and 2 are the prepared samarium-aluminum master alloy, and the morphology of the white strips is similar to the engraved pattern after being enlarged, and the morphology and the distribution of the strips are the same no matter how much the content of the Sm in the samarium-aluminum master alloy is.
The results of the EDS spectra measured at a, b and c in FIG. 2 are shown in Table 2 below.
TABLE 2
From table 2, it can be seen that the samarium-aluminum master alloy with higher Sm content can be successfully prepared after the cathode sinking molten salt electrolysis.
The foregoing is merely an example of the present invention and common general knowledge of known specific structures and features of the embodiments is not described herein in any greater detail. It should be noted that, for those skilled in the art, without departing from the structure of the present invention, several changes and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent.
Claims (4)
1. A method for preparing aluminum-samarium intermediate alloy by submerged cathode molten salt electrolysis is characterized by comprising the following steps of,
(1) respectively weighing the following raw materials: SmF3、LiF、K3AlF6、Sm2O3And an aluminum ingot, and the mass ratio of the raw materials is ensured as follows: (SmF)3+LiF):K3AlF6＝20:80，SmF3:LiF＝80：20；
(2) K in the step (1)3AlF6Putting into an electrolytic cell, heating to raise the temperature until K is reached3AlF6Adding SmF after complete melting3And LiF; to be SmF3And after LiF is completely melted, adding an aluminum ingot, and after the aluminum ingot is melted, adding Sm2O3Until the mixture is melted;
(3) and carrying out molten salt electrolysis at 900 ℃, wherein the cathode of the molten salt electrolysis is liquid aluminum, the anode of the molten salt electrolysis is graphite, and the prepared aluminum-samarium intermediate alloy sinks at the bottom of the electrolytic bath.
2. The method for preparing the samarium-aluminum intermediate alloy by the submerged cathode molten salt electrolysis of claim 1, wherein Sm is2O3The content of (B) is 1-3 wt% of the total amount of the molten salt.
3. A method of producing samarium-aluminum master alloy by submerged cathode molten salt electrolysis as claimed in claim 1, wherein the step (1) further comprises: drying and preheating the weighed raw materials respectively.
4. The method for preparing the samarium-aluminum intermediate alloy by using the submerged cathode molten salt electrolysis as claimed in claim 3, wherein the temperature of the drying preheating in the step (1) is 200 ℃, and the time of the drying preheating is 2 h.
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