CN117778758A - Bismuth tellurium alloy separation method - Google Patents
Bismuth tellurium alloy separation method Download PDFInfo
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- CN117778758A CN117778758A CN202311827521.XA CN202311827521A CN117778758A CN 117778758 A CN117778758 A CN 117778758A CN 202311827521 A CN202311827521 A CN 202311827521A CN 117778758 A CN117778758 A CN 117778758A
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- tellurium
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- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 90
- 229910001215 Te alloy Inorganic materials 0.000 title claims abstract description 39
- 238000000926 separation method Methods 0.000 title claims abstract description 30
- 229910052714 tellurium Inorganic materials 0.000 claims abstract description 75
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims abstract description 74
- 238000005292 vacuum distillation Methods 0.000 claims abstract description 21
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000001257 hydrogen Substances 0.000 claims abstract description 20
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 20
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 20
- 230000003647 oxidation Effects 0.000 claims abstract description 18
- 230000009467 reduction Effects 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000010439 graphite Substances 0.000 claims abstract description 14
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000004821 distillation Methods 0.000 claims description 9
- 229910001152 Bi alloy Inorganic materials 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 description 23
- 239000002184 metal Substances 0.000 description 23
- 229910000416 bismuth oxide Inorganic materials 0.000 description 8
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000002844 melting Methods 0.000 description 6
- 230000001105 regulatory effect Effects 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 238000011144 upstream manufacturing Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000033116 oxidation-reduction process Effects 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- 229910001451 bismuth ion Inorganic materials 0.000 description 1
- UDRRLPGVCZOTQW-UHFFFAOYSA-N bismuth lead Chemical compound [Pb].[Bi] UDRRLPGVCZOTQW-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
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- 238000009854 hydrometallurgy Methods 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
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- 231100001081 no carcinogenicity Toxicity 0.000 description 1
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Abstract
The invention discloses a bismuth tellurium alloy separation method, which comprises the steps of placing bismuth tellurium alloy in a crucible for low-temperature vacuum distillation; the inside of the crucible is divided into an upper layer and a lower layer by a graphite sieve plate, the bismuth-tellurium alloy is placed on the graphite sieve plate, after the vacuum distillation is completed, the residue on the graphite sieve plate is coarse tellurium, and the aggregate at the bottom of the crucible is coarse bismuth; carrying out high-temperature vacuum distillation on the crude bismuth, collecting volatile matters to obtain pure tellurium, wherein the residue is pure bismuth; the crude tellurium is oxidized at high temperature, the oxidation mixed product is subjected to low-temperature hydrogen reduction to recover pure tellurium, and then high-temperature hydrogen reduction is performed to recover pure bismuth. The method can realize the high-efficiency separation of bismuth and tellurium, obtain more than 3N (99.9%) of metallic bismuth and more than 3N (99.9%) of pure tellurium, has simple operation, low energy consumption and high efficiency, is environment-friendly and is beneficial to industrial production.
Description
Technical Field
The invention relates to a method for separating bismuth and tellurium alloy, in particular to a method for separating 3N-level metal bismuth and pure tellurium from bismuth and tellurium alloy, belonging to the technical field of metal purification.
Background
Bismuth has a series of excellent characteristics such as high specific gravity, low melting point, volume expansion and thermal shrinkage during solidification, and the like, and particularly, the non-toxicity and non-carcinogenicity of bismuth lead the bismuth to have a plurality of special applications. Bismuth is widely applied to the fields of semiconductor refrigeration sheets, metallurgy, chemical industry, electronics, aerospace, medicine and the like.
Bismuth-based materials are widely used in the preparation of gastric drugs, semiconductors, superconductors, catalysts, cosmetics, pigments, chemical agents and other fields, and have the characteristics of industrial chain length and multi-field intersection. The project is the upstream matching industry of the bismuth industry chain, the related industries are numerous, the upstream is the industries of mining, mineral separation, equipment manufacturing, smelting and the like, and the downstream is oriented to the fields of digital, electric appliances, IT, automobiles, aviation, national defense and the like, and has remarkable driving effect on the upstream and downstream industries.
At present, bismuth and tellurium alloys with higher tellurium content can be obtained after preliminary purification of bismuth ore, wherein the tellurium content can reach 10-30%, the traditional bismuth and tellurium separation method has higher production cost and serious environmental pollution, and more three wastes are generated. For example, the prior art mainly adopts hydrometallurgy to realize the separation of bismuth-tellurium alloy: 1. acid leaching and separation: the bismuth and tellurium alloy is dissolved by hydrochloric acid, and then bismuth ions in the solution are separated out by adding the reagent, so that the purpose of separating bismuth and tellurium is achieved. 2. Alkaline leaching separation: the molten alloy is blown at a certain temperature, such as a large amount of air, to oxidize the metal tellurium in the alloy into tellurium oxide, then caustic soda is added, and the tellurium oxide floating on the upper layer of the metal is dissolved in the caustic soda, so that the purpose of bismuth and tellurium separation is achieved. The two methods use reagents such as acid, alkali and the like in the production process, so that the environment is greatly influenced, and simultaneously, more three wastes are generated, so that the production cost is high.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide the bismuth-tellurium alloy separation method, which can realize the high-efficiency separation of bismuth and tellurium by combining low-temperature vacuum, high-temperature distillation, high-temperature oxidation, step reduction and other processes to obtain more than 3N (99.9%) of metallic bismuth and more than 3N (99.9%) of pure tellurium, and has the advantages of simple operation, low energy consumption, high efficiency, environmental friendliness and contribution to industrial production.
In order to achieve the technical aim, the invention provides a bismuth tellurium alloy separation method, which comprises the following steps:
1) Placing bismuth tellurium alloy in a crucible for low-temperature vacuum distillation; the inside of the crucible is divided into an upper layer and a lower layer by a graphite sieve plate, the bismuth-tellurium alloy is placed on the graphite sieve plate, after the vacuum distillation is completed, the residue on the graphite sieve plate is coarse tellurium, and the aggregate at the bottom of the crucible is coarse bismuth;
2) Carrying out high-temperature vacuum distillation on the crude bismuth, collecting volatile matters to obtain pure tellurium, wherein the residue is pure bismuth;
3) And (3) carrying out high-temperature oxidation on the crude tellurium, carrying out low-temperature hydrogen reduction on the oxidation mixed product to recover pure tellurium, and then carrying out high-temperature hydrogen reduction on the oxidation mixed product to recover pure bismuth.
The bismuth tellurium alloy separation method provided by the invention has the key points that the high-efficiency separation of bismuth tellurium can be realized by adopting the combined technological thought of low-temperature vacuum, high-temperature distillation, high-temperature oxidation and step reduction, and the purity of the obtained metal bismuth and tellurium can reach more than 3N levels. According to the invention, the bismuth-tellurium alloy is initially separated by utilizing a special crucible, bismuth in the bismuth-tellurium alloy can be initially separated from tellurium in a molten state under a low-temperature vacuum condition by utilizing the difference of the melting temperature and the density of tellurium, molten metal bismuth is finally gathered at the bottom of the crucible through a graphite sieve plate, tellurium is reserved on the sieve plate, the bismuth-tellurium alloy can be initially separated, the bismuth content in the separated crude bismuth is 95-98%, the tellurium content is 2-5%, the tellurium content in the crude tellurium is 80-90%, and the bismuth content in the crude tellurium is 10-20%. The metal tellurium in the crude bismuth is removed by high-temperature vacuum distillation, so that the purity of the metal bismuth can be improved to 3N (99.9%), and 3N (99.9%) metal tellurium can be obtained by volatilization and recovery. The bismuth content in the crude tellurium is still relatively high, and the tellurium and the bismuth are separated according to the difference of oxidation-reduction characteristics of the tellurium and the bismuth. The crude tellurium is heated at high temperature and blown with a large amount of air to oxidize to obtain bismuth oxide and tellurium oxide mixture, and the mixed oxide is reduced step by step at different reducing temperatures to obtain pure tellurium with the concentration of more than 3N (99.9%) and metallic bismuth with the concentration of more than 3N (99.9%).
As a preferable scheme, the bismuth and tellurium alloy contains 70-90% of bismuth by mass and 10-30% of tellurium by mass. The bismuth-tellurium alloy is obtained by preliminary purification of bismuth ore, and the mass content of tellurium in the conventional bismuth-tellurium alloy reaches 10-30%, so that the bismuth-tellurium alloy separation method is satisfied.
As a preferable scheme, the aperture of the graphite sieve plate is 2-4 mm. The graphite sieve plate has a proper micropore structure, which is beneficial to the permeation separation of liquid metal bismuth.
As a preferred embodiment, the conditions of the cryogenic vacuum distillation are: the temperature is 350-450 ℃, the vacuum degree is 50-0.1 Pa, and the time is 1-3 hours. The preferred vacuum distillation conditions are favorable for separating tellurium from bismuth, if the vacuum distillation temperature is too low, bismuth is difficult to separate efficiently, and if the temperature is too high, the tellurium content of the entering bismuth is increased, and the purpose of primary separation cannot be achieved. Under the preferable vacuum distillation condition, the mass content of bismuth in the crude bismuth obtained by separation is 95-98%, and the mass content of tellurium is 2-5%; and the mass content of tellurium in the crude tellurium is 80-90%, and the mass content of bismuth is 10-20%, so that the purpose of preliminary separation is achieved. The physical characteristics of bismuth and tellurium are fully utilized in the low-temperature vacuum distillation process, and the density is 9.78g/cm based on the melting point of the metallic bismuth being 271 DEG C 3 Boiling point 1564 ℃; the melting point of the metal tellurium is 452 ℃, and the density is 6.25g/cm 3 The vacuum smelting is carried out near the melting point of bismuth-tellurium alloy, the metal bismuth with larger density is left at the lower layer, tellurium is slowly raised to the upper layer, but the temperature is not too high, preferably kept at 350-450 ℃, the high temperature under vacuum can lead to distillation volatilization of both the metal bismuth and tellurium, the distilled high-tellurium low-bismuth alloy is left on the sieve plate in a semi-solid state, and the low-melting metal bismuth is left under the sieve plate through sieve holes after being melted.
As a preferable embodiment, the conditions of the high temperature vacuum distillation are as follows: the distillation temperature is 500-600 ℃, the vacuum degree is 0.1-0.01 Pa, and the time is 4-8 hours. A small amount of tellurium in the crude bismuth can be volatilized and separated by vacuum distillation, and 99.9% of metallic bismuth and pure tellurium are respectively obtained.
As a preferable embodiment, the conditions of the high-temperature oxidation are: the temperature is 800-1000 ℃, and compressed air is used as oxidizing gas. Through the high-temperature oxidation process, the crude tellurium can be completely oxidized to obtain a mixture of tellurium oxide and bismuth oxide.
As a preferable embodiment, the conditions for the low-temperature hydrogen reduction are as follows: under the hydrogen atmosphere, the temperature is 470-550 ℃ and the time is 2-4 hours. According to the characteristics of different oxidation-reduction performances of tellurium oxide and bismuth oxide, tellurium can be reduced to liquid state preferentially by controlling reduction at low temperature, so that separation is realized. The purity of hydrogen was 3N (99.9%).
As a preferred embodiment, the conditions for high temperature hydrogen reduction are: under the hydrogen atmosphere, the temperature is 750-950 ℃ and the time is 2-4 hours. After separation by preferential reduction of tellurium oxide to tellurium, the remaining bismuth oxide is reduced to metallic bismuth at a higher reduction temperature. The purity of hydrogen was 3N (99.9%).
Compared with the prior art, the technical scheme of the invention has the beneficial technical effects that:
according to the bismuth tellurium alloy separation method provided by the invention, the technology of combining low-temperature vacuum, high-temperature distillation, high-temperature oxidation and distributed reduction can be used for realizing the efficient separation of bismuth tellurium alloy, more than 3N (99.9%) of metallic bismuth and more than 3N (99.9%) of pure tellurium are obtained, the whole separation process does not need reagents such as acid, alkali and the like, the cost is low, almost no three wastes are generated, and the influence on the environment is avoided.
Detailed Description
The following specific examples are intended to further illustrate the present invention, but not to limit the scope of the claims.
The inside of the crucible used in the following examples was divided into upper and lower layers by a graphite sieve plate having a pore diameter of 3mm.
Example 1
Adding 2kg of bismuth-tellurium alloy with 70% of bismuth content and 30% of tellurium content into a layered distillation furnace of a crucible, heating to 350 ℃, preserving heat for 3 hours under vacuum 50Pa to obtain coarse bismuth on a screen and coarse bismuth under the screen respectively, adding the coarse bismuth under the screen into the vacuum distillation furnace, regulating the temperature to 500 ℃, preserving heat for 4 hours under vacuum 0.1Pa to obtain 3N (99.9%) metal bismuth and 3N (99.9%) metal tellurium which are collected by volatilization, heating the coarse tellurium on the screen to 800 ℃ by a high-frequency test furnace after the crucible is filled with silicon carbide ink, introducing air metal for complete oxidation, controlling the average oxidation reaction speed to 1kg/h, collecting oxidation products, adding the oxidation products into a single-tube furnace, regulating the temperature to 470 ℃, introducing hydrogen for preserving heat for 2 hours, cooling, collecting 3N (99.9%) metal tellurium and 3N (99.9%) bismuth oxide, adding the bismuth oxide into a tubular atmosphere furnace again, regulating the temperature to 750 ℃, and introducing hydrogen for preserving heat for 3 hours to obtain 3N (99.9%) metal bismuth.
Bismuth purity detection equipment: inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma emission spectrometry (ICP-OES).
Example 2
Adding 2kg of bismuth-tellurium alloy with 90% of bismuth content and 10% of tellurium content into a layered distillation furnace of a crucible, heating to 450 ℃, preserving heat for 2 hours under vacuum 1Pa to obtain coarse bismuth on a screen and coarse bismuth under the screen respectively, adding the coarse bismuth under the screen into the vacuum distillation furnace, regulating the temperature to 600 ℃, preserving heat for 4 hours under vacuum 0.01Pa to obtain 3N (99.9%) metal bismuth and 3N (99.9%) metal tellurium which are collected by volatilization, heating the coarse tellurium on the screen to 1000 ℃ by a high-frequency test furnace after the crucible is filled with silicon carbide ink, introducing air until the metal is completely oxidized, controlling the average oxidation reaction speed to 1.5kg/h, collecting oxidation products, adding the oxidation products into a single-tube furnace, regulating the temperature to 550 ℃, introducing hydrogen for preserving heat for 4 hours, collecting 3N (99.9%) metal tellurium and 3N (99.9%) bismuth oxide after cooling, adding the bismuth oxide into the tubular atmosphere furnace again, regulating the temperature to 950 ℃, and introducing hydrogen for preserving heat for 4 hours to obtain 3N (99.9%) metal bismuth.
Comparative example 1
Adding 2kg of bismuth-tellurium alloy with 90% of bismuth content and 10% of tellurium content into a layered distillation furnace of a crucible, heating to 280 ℃, and carrying out vacuum 1Pa heat preservation for 2 hours to respectively obtain coarse tellurium on a screen and coarse bismuth under the screen, wherein coarse tellurium on the screen and coarse bismuth under the screen are not obtained after vacuum heat preservation is finished, the alloy is not melted, and still remains on a screen plate completely.
The foregoing description, for the convenience of the reader, has focused on a representative sample of all possible embodiments, that is presented to explain the principles of the invention and to illustrate the best mode for practicing the invention. This description is not intended to be exhaustive of all of the possible variations. Other variations or modifications not illustrated are also possible.
Claims (8)
1. A bismuth tellurium alloy separation method is characterized in that: the method comprises the following steps:
1) Placing bismuth tellurium alloy in a crucible for low-temperature vacuum distillation; the inside of the crucible is divided into an upper layer and a lower layer by a graphite sieve plate, the bismuth-tellurium alloy is placed on the graphite sieve plate, after the vacuum distillation is completed, the residue on the graphite sieve plate is coarse tellurium, and the aggregate at the bottom of the crucible is coarse bismuth;
2) Carrying out high-temperature vacuum distillation on the crude bismuth, collecting volatile matters to obtain pure tellurium, wherein the residue is pure bismuth;
3) And (3) carrying out high-temperature oxidation on the crude tellurium, carrying out low-temperature hydrogen reduction on the oxidation mixed product to recover pure tellurium, and then carrying out high-temperature hydrogen reduction on the oxidation mixed product to recover pure bismuth.
2. The method for separating bismuth and tellurium alloy according to claim 1, wherein: the bismuth-tellurium alloy contains 70-90% of bismuth by mass and 10-30% of tellurium by mass.
3. The method for separating bismuth and tellurium alloy according to claim 1, wherein: the aperture of the graphite sieve plate is 2-4 mm.
4. A bismuth tellurium alloy separation method according to any one of claims 1-3, wherein: the conditions of the low-temperature vacuum distillation are as follows: the temperature is 350-450 ℃, the vacuum degree is 50-0.1 Pa, and the time is 1-3 hours.
5. A bismuth tellurium alloy separation method according to claim 1 or 2, wherein: the conditions of the high-temperature vacuum distillation are as follows: the distillation temperature is 500-600 ℃, the vacuum degree is 0.1-0.01 Pa, and the time is 4-8 hours.
6. A bismuth tellurium alloy separation method according to claim 1 or 2, wherein: the conditions of the high-temperature oxidation are as follows: the temperature is 800-1000 ℃, and compressed air is used as oxidizing gas.
7. A bismuth tellurium alloy separation method according to claim 1 or 2, wherein: the conditions for the low temperature hydrogen reduction are: under the hydrogen atmosphere, the temperature is 470-550 ℃ and the time is 2-4 hours.
8. A bismuth tellurium alloy separation method according to claim 1 or 2, wherein: the conditions for the high temperature hydrogen reduction are: under the hydrogen atmosphere, the temperature is 750-950 ℃ and the time is 2-4 hours.
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| CN202311827521.XA CN117778758A (en) | 2023-12-28 | 2023-12-28 | Bismuth tellurium alloy separation method |
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