CN110863217A - Novel ionic liquid electrolyte and method for low-temperature electrolytic refining of raw aluminum by using same - Google Patents
Novel ionic liquid electrolyte and method for low-temperature electrolytic refining of raw aluminum by using same Download PDFInfo
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- CN110863217A CN110863217A CN201911246877.8A CN201911246877A CN110863217A CN 110863217 A CN110863217 A CN 110863217A CN 201911246877 A CN201911246877 A CN 201911246877A CN 110863217 A CN110863217 A CN 110863217A
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- 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
- C25C3/06—Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
- C25C3/18—Electrolytes
Abstract
A novel ionic liquid electrolyte is prepared by mixing and reacting carbonic ester or pyridine compounds with excessive anhydrous aluminum halide at room temperature under the protection of inert gas. The method for low-temperature electrolytic refining of raw aluminum by using the ionic liquid electrolyte comprises the following steps: 1) under the protection of inert gas, taking original aluminum as a working electrode, graphite or glassy carbon or platinum as a counter electrode and refined aluminum as a reference electrode, and carrying out electrolytic refining reaction in an ionic liquid electrolyte; 2) after the refining reaction is finished, the counter electrode is taken out under the protection of inert gas, washed and dried by absolute ethyl alcohol, and refined aluminum with the purity higher than 99.95 percent can be obtained through separation. The method has the advantages of easily obtained raw materials, simple and convenient process and low cost, can finish low-temperature electrolytic refining of the raw aluminum, and has lower energy consumption and higher reaction efficiency; the refining effect is better.
Description
Technical Field
The invention belongs to the field of metal smelting, and particularly relates to a novel ionic liquid electrolyte and a method for low-temperature electrolytic refining of raw aluminum by using the same.
Background
Aluminum is an important metal material, the annual output is the first in the domestic nonferrous metal industry for a long time, and the aluminum plays an important role in promoting the economic and social development. As is known, raw aluminum (commonly called aluminum ingot) obtained by industrial production is the most common aluminum product in the market, and the purity of the raw aluminum is generally about 99.5%. With the continuous improvement of the requirements of people on the quality of products, the raw aluminum is difficult to meet the application requirements in many fields. In this context, refined aluminum (also referred to as high purity aluminum internationally) having a purity of more than 99.95% is widely favored. The refined aluminum has better conductivity, ductility, reflectivity and oxidation resistance than the original aluminum, can be used for preparing advanced materials such as disk substrates, integrated circuit leads, capacitor anode foils and the like, and has wide development prospect in the leading-edge fields of electronics, communication, national defense, aerospace and the like.
At present, it is common in industry to produce refined aluminum from raw aluminum as a main raw material by a three-layer liquid electrolytic refining method or a segregation melting method. Generally, the two methods have the advantages of low cost, large yield and investment saving, but have the defects of high energy consumption (15-18 kWh/kg), high temperature (700-900 ℃) and heavy equipment corrosion. At the same time, the product gap is still large, presenting a difficult situation of starvation. These problems are mainly due to the intrinsic drawbacks of the conventional processes and are difficult to solve by means of adjustments within the technology. Therefore, the development of more efficient and green low-temperature preparation technology is the key of future work.
As early as the middle of the last century, researchers developed organic molten salt electrolytes in order to implement low temperature aluminum electrolysis processes. After decades of exploration, the substances are found to be completely composed of anions and cations, and the melting point of the substances can be as low as about room temperature, so the substances are collectively called ionic liquid. Research shows that the ionic liquid can be used as a novel green electrolyte for an aluminum refining process, has low reaction temperature (lower than 100 ℃), low energy consumption (6-9 kWh/kg), high selectivity and simple and convenient operation, and is an ideal material for replacing the traditional high-temperature molten salt system. However, the prior work mainly focuses on electrolytic refining of aluminum alloys such as aluminum copper, aluminum magnesium and the like, reports on raw aluminum are few, and ionic liquid electrolytes for low-temperature refining of raw aluminum are lacked, so that the related research is insufficient, and the development and industrial application of the technology are not facilitated.
Under the technical background, in order to further solve the problems of low-temperature electrolytic refining of the raw aluminum, research and development of an ionic liquid electrolyte system are required to be enhanced, so that main impurity elements such as iron, copper, magnesium, zinc, silicon and the like are effectively separated, the reaction efficiency and the product purity are remarkably improved, and the industrial application of the technology is promoted better.
Disclosure of Invention
The invention aims to provide a novel ionic liquid electrolyte and a preparation method thereof, and simultaneously, the ionic liquid electrolyte is used for carrying out low-temperature electrolytic refining on raw aluminum, which is another main object of the invention.
In order to realize the purpose of the invention, the following technical scheme is adopted: a novel ionic liquid electrolyte is prepared by mixing and reacting carbonic ester or pyridine compounds with excessive anhydrous aluminum halide at room temperature under the protection of inert gas.
Further, the molecular structure of the carbonate is
Wherein R is1Represents a hydrogen atom or a hydrocarbon group; r2Represents a hydrogen atom or a hydrocarbon group; r3Represents a hydrogen atom or a hydrocarbon group; r4Represents a hydrogen atom or a hydrocarbon group.
Further, the molecular structure of the pyridine compound is
Wherein R is1Represents a hydrogen atom or a hydrocarbon group; r2Represents a hydrogen atom or a hydrocarbon group; r3Represents a hydrogen atom or a hydrocarbon group; r4Represents a hydrogen atom or a hydrocarbon group; r5Represents a hydrogen atom or a hydrocarbon group.
Further, the anhydrous aluminum halide is one of anhydrous aluminum trichloride, anhydrous aluminum tribromide and anhydrous aluminum triiodide.
Further, the inert gas is one of nitrogen, argon, helium and neon with the purity higher than 99.99%, and the room temperature is 15-30 ℃.
Furthermore, the excessive anhydrous aluminum halide means that the anhydrous aluminum halide is higher in molar amount than the carbonate or pyridine compound, and the molar ratio of the carbonate or pyridine compound to the anhydrous aluminum halide is 1: 1.5-1: 2.5.
The method for low-temperature electrolytic refining of raw aluminum by using the ionic liquid electrolyte comprises the following steps:
1) under the protection of inert gas, taking original aluminum as a working electrode, graphite or glassy carbon or platinum as a counter electrode and refined aluminum as a reference electrode, and carrying out electrolytic refining reaction in an ionic liquid electrolyte;
2) after the refining reaction is finished, the counter electrode is taken out under the protection of inert gas, washed and dried by absolute ethyl alcohol, and refined aluminum with the purity higher than 99.95 percent can be obtained through separation.
Further, the purity of the refined aluminum in the step 1) is higher than 99.95%, the inert gas is one of nitrogen, argon, helium and neon with the purity higher than 99.99%, the electrolytic refining reaction adopts a potentiostatic method, the reaction temperature is 40-90 ℃, and the potential and current density of the working electrode are 0.1-0.5V and 10-30 mA/cm respectively2The reaction time is 0.5-2.5 h.
Further, the inert gas in the step 2) is one of nitrogen, argon, helium and neon with the purity higher than 99.99%.
Compared with the prior art, the invention has the following technical advantages:
1) the novel ionic liquid electrolyte adopted by the invention is generated by the reaction of carbonate or pyridine compounds and excessive anhydrous aluminum halide, related raw materials are easy to obtain, the preparation process is simple and convenient, the cost is lower, and the system has higher stability;
2) the ionic liquid electrolyte is adopted, so that low-temperature electrolytic refining of the raw aluminum can be completed, and the method has low energy consumption and high reaction efficiency;
3) the test shows that the purity of the refined aluminum product is higher than 99.95%, the current efficiency is higher than 99.5%, the contents of most impurity elements such as iron, copper, magnesium, zinc, silicon and the like in the original aluminum can be obviously reduced, and the refining effect is good.
Detailed Description
The present invention is illustrated by the following examples, but the present invention is not limited to the following examples, and all the implementations that meet the purpose described above and below are within the technical scope of the present invention.
In the invention, the synthesis process of the novel ionic liquid electrolyte is carried out at room temperature, and the temperature range of the room temperature is 15-30 ℃.
Example 1
A novel ionic liquid electrolyte is obtained by mixing and reacting ethylene carbonate and anhydrous aluminum trichloride according to a molar weight ratio of 1:2 at room temperature under the protection of argon.
The ionic liquid electrolyte is adopted to carry out low-temperature electrolytic refining on the raw aluminum, and the steps are as follows:
1) under the protection of argon, remelting aluminum ingot Al99.60 is used as a working electrode, graphite is used as a counter electrode, and refined aluminum is used as a reference electrode, and electrolytic refining reaction is carried out in an ionic liquid electrolyte. Wherein the reaction temperature is 40 ℃, and the potential and the current density of the working electrode are respectively 0.4V and 10 mA/cm2The reaction time is 2.5 h.
2) And after the refining reaction is finished, taking out the counter electrode under the protection of argon, cleaning and airing the counter electrode by using absolute ethyl alcohol, and separating to obtain the refined aluminum product.
Example 2
A novel ionic liquid electrolyte is obtained by mixing propylene carbonate and anhydrous aluminum triiodide in a molar ratio of 1:1.5 for reaction at room temperature under the protection of nitrogen.
The ionic liquid electrolyte is adopted to carry out low-temperature electrolytic refining on the raw aluminum, and the steps are as follows:
1) under the protection of nitrogen, remelting aluminum ingot Al99.50 is used as a working electrode, glassy carbon is used as a counter electrode, and refined aluminum is used as a reference electrode, and electrolytic refining reaction is carried out in an ionic liquid electrolyte. Wherein the reaction temperature is 60 ℃, and the potential and the current density of the working electrode are respectively 0.3V and 15 mA/cm2The reaction time is 2 h.
2) And after the refining reaction is finished, taking out the counter electrode under the protection of nitrogen, cleaning and airing the counter electrode by using absolute ethyl alcohol, and separating to obtain the refined aluminum product.
Example 3
A novel ionic liquid electrolyte is obtained by mixing and reacting 1, 2-butylene carbonate and anhydrous aluminum tribromide in a molar weight ratio of 1:2.5 at room temperature under the protection of neon.
The ionic liquid electrolyte is adopted to carry out low-temperature electrolytic refining on the raw aluminum, and the steps are as follows:
1) under the protection of neon gas, remelting aluminum ingot Al99.70 is used as a working electrode, platinum is used as a counter electrode, and refined aluminum is used as a reference electrode, and electrolytic refining reaction is carried out in an ionic liquid electrolyte. Wherein the reaction temperature is 70 ℃, and the potential and the current density of the working electrode are respectively 0.2V and 25 mA/cm2The reaction time is 1 h.
2) And after the refining reaction is finished, taking out the counter electrode under the protection of neon, cleaning and airing the counter electrode by using absolute ethyl alcohol, and separating to obtain the refined aluminum product.
Example 4
A novel ionic liquid electrolyte is obtained by mixing and reacting 4-propyl pyridine and anhydrous aluminum trichloride according to a molar weight ratio of 1:2.2 at room temperature under the protection of argon.
The ionic liquid electrolyte is adopted to carry out low-temperature electrolytic refining on the raw aluminum, and the steps are as follows:
1) under the protection of argon, remelting aluminum ingot Al99.50 is used as a working electrode, glassy carbon is used as a counter electrode, and refined aluminum is used as a reference electrode, and electrolytic refining reaction is carried out in an ionic liquid electrolyte. Wherein the reaction temperature is 90 ℃, and the potential and the current density of the working electrode are respectively 0.1V and 10 mA/cm2The reaction time is 1.5 h.
2) And after the refining reaction is finished, taking out the counter electrode under the protection of argon, cleaning and airing the counter electrode by using absolute ethyl alcohol, and separating to obtain the refined aluminum product.
Example 5
A novel ionic liquid electrolyte is obtained by mixing and reacting 3-ethylpyridine and anhydrous aluminum tribromide in a molar ratio of 1:2 at room temperature under the protection of helium.
The ionic liquid electrolyte is adopted to carry out low-temperature electrolytic refining on the raw aluminum, and the steps are as follows:
1) under the protection of helium, remelting aluminum ingot Al99.70 is used as a working electrode, graphite is used as a counter electrode, and refined aluminum is used as a reference electrode, and electrolytic refining reaction is carried out in an ionic liquid electrolyte. Wherein the reaction temperature is 60 ℃, and the potential and the current density of the working electrode are respectively 0.5V and 30 mA/cm2The reaction time is 1 h.
2) And after the refining reaction is finished, taking out the counter electrode under the protection of helium, cleaning and airing the counter electrode by using absolute ethyl alcohol, and separating to obtain the refined aluminum product.
Example 6
A novel ionic liquid electrolyte is obtained by mixing and reacting 3, 5-dimethylpyridine and anhydrous aluminum triiodide in a molar ratio of 1:1.8 at room temperature under the protection of nitrogen.
The ionic liquid electrolyte is adopted to carry out low-temperature electrolytic refining on the raw aluminum, and the steps are as follows:
1) under the protection of nitrogen, remelting aluminum ingot Al99.60 is used as a working electrode, platinum is used as a counter electrode, and refined aluminum is used as a reference electrode, and electrolytic refining reaction is carried out in an ionic liquid electrolyte. Wherein the reaction temperature is 50 ℃, and the potential and the current density of the working electrode are respectively 0.3V and 15 mA/cm2The reaction time is 2 h.
2) And after the refining reaction is finished, taking out the counter electrode under the protection of nitrogen, cleaning and airing the counter electrode by using absolute ethyl alcohol, and separating to obtain the refined aluminum product.
Performance testing
The performance of the refined aluminum obtained in examples 1 to 6 was tested by an X-ray spectrometer and inductively coupled plasma atomic emission spectroscopy, and the specific results are shown in table 1.
According to the test result, the quality purity of the refined aluminum obtained by the invention is higher than 99.95%, and the current efficiency is higher than 99.5%. The reaction temperature is lower than 100 ℃, the operation is simple and convenient, the energy consumption is low, and the reaction efficiency and the product purity are higher.
Claims (9)
1. A novel ionic liquid electrolyte is characterized in that: the ionic liquid electrolyte is obtained by mixing and reacting carbonic ester or pyridine compounds with excessive anhydrous aluminum halide at room temperature under the protection of inert gas.
2. A novel ionic liquid electrolyte as claimed in claim 1 wherein: the molecular structure of the carbonic ester is
Wherein R is1Represents a hydrogen atom or a hydrocarbon group; r2Represents a hydrogen atom or a hydrocarbon group; r3Represents a hydrogen atom or a hydrocarbon group; r4Represents a hydrogen atom or a hydrocarbon group.
3. A novel ionic liquid electrolyte as claimed in claim 1 wherein: the molecular structure of the pyridine compound is
Wherein R is1Represents a hydrogen atom or a hydrocarbon group; r2Represents a hydrogen atom or a hydrocarbon group; r3Represents a hydrogen atom or a hydrocarbon group; r4Represents a hydrogen atom or a hydrocarbon group; r5Represents a hydrogen atom or a hydrocarbon group.
4. A novel ionic liquid electrolyte as claimed in claim 1 wherein: the anhydrous aluminum halide is one of anhydrous aluminum trichloride, anhydrous aluminum tribromide and anhydrous aluminum triiodide.
5. A novel ionic liquid electrolyte as claimed in claim 1 wherein: the inert gas is one of nitrogen, argon, helium and neon with the purity higher than 99.99%, and the room temperature is 15-30 ℃.
6. A novel ionic liquid electrolyte as claimed in claim 1 wherein: the excessive anhydrous aluminum halide means that the molar amount of the anhydrous aluminum halide is higher than that of the carbonate or pyridine compound, and the molar ratio of the carbonate or pyridine compound to the anhydrous aluminum halide is 1: 1.5-1: 2.5.
7. A method for low-temperature electrorefining of raw aluminum using an ionic liquid electrolyte, using the ionic liquid electrolyte of any one of claims 1 to 6, comprising the steps of:
1) under the protection of inert gas, taking original aluminum as a working electrode, graphite or glassy carbon or platinum as a counter electrode and refined aluminum as a reference electrode, and carrying out electrolytic refining reaction in an ionic liquid electrolyte;
2) after the refining reaction is finished, the counter electrode is taken out under the protection of inert gas, washed and dried by absolute ethyl alcohol, and refined aluminum with the purity higher than 99.95 percent can be obtained through separation.
8. The method for low-temperature electrorefining of raw aluminum using ionic liquid electrolyte as claimed in claim 7, wherein: the purity of the refined aluminum in the step 1) is higher than 99.95%, the inert gas is one of nitrogen, argon, helium and neon with the purity higher than 99.99%, the electrolytic refining reaction adopts a potentiostatic method, the reaction temperature is 40-90 ℃, and the potential and current density of a working electrode are 0.1-0.5V and 10-30 mA/cm respectively2The reaction time is 0.5-2.5 h.
9. The method for low-temperature electrorefining of raw aluminum using ionic liquid electrolyte as claimed in claim 7, wherein: and 2) the inert gas in the step 2) is one of nitrogen, argon, helium and neon with the purity higher than 99.99%.
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| CN113913868A (en) * | 2021-10-29 | 2022-01-11 | 北京欧菲金太科技有限责任公司 | Ionic liquid electrolyte, 6N ultra-pure aluminum obtained by ionic liquid electrolyte and preparation method of ionic liquid electrolyte |
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