METHOD FOR REFINING BERYLLIUM BY MOLTEN SALT ELECTROLYSIS

20240254644 ยท 2024-08-01

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Cpc classification

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Abstract

The present disclosure relates to a method for refining beryllium by molten salt electrolysis, the method comprises: firstly, constructing an electrochemical system, wherein an anode chamber contains an anode molten salt electrolyte, a crude beryllium anode is inserted in the anode molten salt electrolyte, a cathode chamber contains a cathode molten salt electrolyte, a cathode is inserted in the cathode molten salt electrolyte, the anode molten salt electrolyte and the cathode molten salt electrolyte are not in contact with each other but are connected with each other via a liquid alloy at the bottom of the inside of an electrolysis cell; and applying a current for electrolysis to obtain refined solid beryllium at the cathode.

Claims

1. A method for refining beryllium by molten salt electrolysis, comprising the following steps: (1) Constructing an electrochemical system: the electrolytic cell is divided into an anode chamber and a cathode chamber, wherein the anode chamber contains an anode molten salt electrolyte, a crude beryllium anode is inserted in the anode molten salt electrolyte, the cathode chamber contains a cathode molten salt electrolyte, a cathode is inserted in the cathode molten salt electrolyte, a liquid alloy is at the bottom of the inside of the electrolytic cell: the anode molten salt electrolyte and the cathode molten salt electrolyte are not in contact with each other but are connected via the liquid alloy at the bottom of the inside of the electrolytic cell; (2) Applying a current for electrolysis, the beryllium metal in the anode is oxidized to beryllium ions, the beryllium ions from the anode are moved into the anode molten salt electrolyte, the beryllium ions in the anode molten salt electrolyte are reduced to beryllium metal at the interface between the anode molten salt electrolyte and the liquid alloy, the beryllium metal at the interface between the anode molten salt electrolyte and the liquid alloy is dissolved into the liquid alloy, meanwhile the beryllium metal in the liquid alloy is oxidized to beryllium ions at the interface between the liquid alloy and the cathode molten salt electrolyte, the beryllium ions at the interface between the liquid alloy and the cathode molten salt electrolyte are moved into the cathode molten salt electrolyte, the beryllium ions in the cathode molten salt electrolyte are reduced to beryllium metal on the cathode surface.

2. A method for refining beryllium by molten salt electrolysis according to claim 1, the cathode is a nickel, tungsten or molybdenum cathode.

3. A method for refining beryllium by molten salt electrolysis according to claim 1, the liquid alloy is an alloy comprised of beryllium and one or several of copper, silver, gold, manganese.

4. A method for refining beryllium by molten salt electrolysis according to claim 3, the liquid alloy is an alloy comprised of beryllium and copper in an atomic ratio of 28:72.

5. A method for refining beryllium by molten salt electrolysis according to claim 3, the liquid alloy is an alloy comprised of beryllium and gold in an atomic ratio of 21:79.

6. A method for refining beryllium by molten salt electrolysis according to claim 1, the anode molten salt electrolyte is a halide molten salt containing beryllium ions, preferably the anode molten salt electrolyte is a mixture of beryllium fluoride and one or several of lithium fluoride, sodium fluoride, potassium fluoride, magnesium fluoride, and calcium fluoride.

7. A method for refining beryllium by molten salt electrolysis according to claim 1, the cathode molten salt electrolyte is a halide molten salt containing beryllium ions, preferably the cathode molten salt electrolyte is a mixture of beryllium fluoride and one or several of lithium fluoride, sodium fluoride, potassium fluoride, magnesium fluoride, and calcium fluoride.

8. A method for refining beryllium by molten salt electrolysis according to claim 1, under the condition of applying a current, the density of both the anode molten salt electrolyte and the cathode molten salt electrolyte is lower than the density of the liquid alloy.

9. A method for refining beryllium by molten salt electrolysis according to claim 1, the purity of the crude beryllium in the crude beryllium anode is not lower than 90%.

10. A method for refining beryllium by molten salt electrolysis according to claim 1, the anode current density is between 0.1 A/cm.sup.2 and 1.5 A/cm.sup.2, the electrolysis temperature is between 600? C. and 1100? C.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0019] FIG. 1 is an electrolysis device diagram of the method for refining beryllium by molten salt electrolysis described in the present disclosure;

[0020] Where, 1anode; 2anode molten salt electrolyte; 3liquid alloy; 4cathode; 5cathode molten salt electrolyte; 6anode chamber; 7cathode chamber.

DETAILED DESCRIPTION OF THE EMBODIMENTS

[0021] To make the purpose, technical solutions and advantages of the present disclosure clearer, the technical solutions of the present disclosure will be described in detail below. Obviously, the described embodiments are only a part of the embodiments of the present disclosure, but are not all of the embodiments. Based on the embodiments in the present disclosure, all other implementations obtained by those of ordinary skill in the art without any creative work fall within the scope of protection of the present disclosure. Unless otherwise specified, the proportions indicated in the embodiments are mass percentages.

Embodiment 1

[0022] This embodiment provides a method for refining beryllium by molten salt electrolysis, comprising the following steps: [0023] (1) As shown in FIG. 1, a beryllium-containing alloy (21 at. % beryllium, 79 at. % gold) is added to the bottom of the inside of the electrolytic cell, it's ensured that the electrolytic cell will be divided into an anode chamber and a cathode chamber after the alloy is melted, a mixture of 30% lithium fluoride, 68% potassium fluoride and 2% beryllium fluoride is added into the anode chamber as an anode molten salt electrolyte and into the cathode chamber as a cathode molten salt electrolyte, the electrolytic cell is heated to 600? C., an anode made of crude beryllium with a purity of 90% is immersed in the anode molten salt electrolyte and a nickel cathode is immersed in the cathode molten salt electrolyte respectively. [0024] (2) Applying a current for electrolysis, the anode current density is controlled at 0.1 A/cm2, the duration of electrolysis is 24 hours, the solid beryllium metal is obtained at the cathode, and its purity is analyzed to be 99.90%.

Embodiment 2

[0025] This embodiment provides a method for refining beryllium by molten salt electrolysis, comprising the following steps: [0026] (1) As shown in FIG. 1, a beryllium-containing alloy (28 at. % beryllium, 72 at. % copper) is added to the bottom of the inside of the electrolytic cell, it's ensured that the electrolytic cell will be divided into an anode chamber and a cathode chamber after the alloy is melted. A mixture of 95% lithium fluoride and 5% beryllium fluoride is added into the anode chamber as an anode molten salt electrolyte, a mixture of 90% lithium fluoride and 10% beryllium fluoride is added into the cathode chamber as a cathode molten salt electrolyte, the electrolytic cell is heated to 900? C., an anode made of crude beryllium with a purity of 92% is immersed in the anode molten salt electrolyte and a molybdenum cathode is immersed in the cathode molten salt electrolyte respectively. [0027] (2) Applying a current for electrolysis, the anode current density is controlled at 0.2 A/cm2, the duration of electrolysis is 12 hours, the solid beryllium metal is obtained at the cathode, and after analysis its purity is analyzed to be 99.91%.

Embodiment 3

[0028] This embodiment provides a method for refining beryllium by molten salt electrolysis, comprising the following steps: [0029] (1) As shown in FIG. 1, a beryllium-containing alloy (30 at. % beryllium, 35 at. % copper, 35 at. % silver) is added to the bottom of the inside of the electrolytic cell, it's ensured that the electrolytic cell will be divided into an anode chamber and a cathode chamber after the alloy is melted, a mixture of 35% magnesium fluoride, 45% calcium fluoride, and 20% beryllium fluoride is added into the anode chamber as an anode molten salt electrolyte and into the cathode chamber as a cathode molten salt electrolyte, the electrolytic cell is heated to 1100? C., an anode made of crude beryllium with a purity of 95% is immersed in the anode molten salt electrolyte and a tungsten cathode is immersed in the cathode molten salt electrolyte respectively. [0030] (2) Applying a current for electrolysis, the anode current density is controlled at 0.5 A/cm2, the duration of electrolysis is 6 hours, the solid beryllium metal is obtained at the cathode, and its purity is analyzed to be 99.95%.

Embodiment 4

[0031] This embodiment provides a method for refining beryllium by molten salt electrolysis, comprising the following steps: [0032] (1) As shown in FIG. 1, a beryllium-containing alloy (30 at. % beryllium, 70 at. % copper) is added to the bottom of the inside of the electrolytic cell, it's ensured that the electrolytic cell will be divided into an anode chamber and a cathode chamber after the alloy is melted, a mixture of 50% potassium fluoride and 50% beryllium fluoride is added into the anode chamber as an anode molten salt electrolyte and into the cathode chamber as a cathode molten salt electrolyte, the electrolytic cell is heated to 950? C., an anode made of crude beryllium with a purity of 97% is immersed in the anode molten salt electrolyte and a tungsten cathode is immersed in the cathode molten salt electrolyte respectively. [0033] (2) Applying a current for electrolysis, the anode current density is controlled at 1 A/cm2, the duration of electrolysis is 3 hours, the solid beryllium metal is obtained at the cathode, and its purity is analyzed to be 99.96%.

Embodiment 5

[0034] This embodiment provides a method for refining beryllium by molten salt electrolysis, comprising the following steps: [0035] (1) As shown in FIG. 1, a beryllium-containing alloy (30 at. % beryllium, 70 at. % manganese) is added to the bottom of the inside of the electrolytic cell, it's ensured that the electrolytic cell will be divided into an anode chamber and a cathode chamber after the alloy is melted, a mixture of 30% lithium fluoride and 70% beryllium fluoride is added into the anode chamber as an anode molten salt electrolyte and into the cathode chamber as a cathode molten salt electrolyte, the electrolytic cell is heated to 950? C., an anode made of crude beryllium with a purity of 99% is immersed in the anode molten salt electrolyte and a tungsten cathode is immersed in the cathode molten salt electrolyte respectively. [0036] (2) Applying a current for electrolysis, the anode current density is controlled at 1.5 A/cm2, the duration of electrolysis is 2 hours, the solid beryllium metal is obtained at the cathode, and its purity is analyzed to be 99.99%.

Embodiment 6

[0037] This embodiment provides a method for refining beryllium by molten salt electrolysis, comprising the following steps: [0038] (1) As shown in FIG. 1, a beryllium-containing alloy (30 at. % beryllium, 35 at. % copper, 34% at. % silver, lat. % gold) is added to the bottom of the inside of the electrolytic cell, it's ensured that the electrolytic cell will be divided into an anode chamber and a cathode chamber after the alloy is melted, a mixture of 35% magnesium fluoride, 45% calcium fluoride, and 20% beryllium fluoride is added into the anode chamber as an anode molten salt electrolyte and into the cathode chamber as a cathode molten salt electrolyte, the electrolytic cell is heated to 1100? C., an anode made of crude beryllium with a purity of 95% is immersed in the anode molten salt electrolyte and a tungsten cathode is immersed in the cathode molten salt electrolyte respectively. [0039] (2) Applying a current for electrolysis, the anode current density is controlled at 0.5 A/cm2, the duration of electrolysis is 6 hours, the solid beryllium metal is obtained at the cathode, and its purity is analyzed to be 99.94%.

[0040] The above are only specific embodiments of the present disclosure, however, the protection scope of the present disclosure is not limited thereto, any modifications or substitutions readily apparent to those skilled in the art within the technical scope disclosed by the present disclosure should be encompassed within the scope of protection of the present disclosure. Therefore, the protection scope of the present disclosure should be subject to the protection scope of the claims.