CN115491509A - Vacuum purification method for multi-stage extraction of refined bismuth - Google Patents
Vacuum purification method for multi-stage extraction of refined bismuth Download PDFInfo
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- CN115491509A CN115491509A CN202211055904.5A CN202211055904A CN115491509A CN 115491509 A CN115491509 A CN 115491509A CN 202211055904 A CN202211055904 A CN 202211055904A CN 115491509 A CN115491509 A CN 115491509A
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- China
- Prior art keywords
- stage
- bismuth
- vacuum
- temperature
- purification method
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 34
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000000746 purification Methods 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000000605 extraction Methods 0.000 title claims abstract description 11
- 229910001152 Bi alloy Inorganic materials 0.000 claims abstract description 26
- 239000007788 liquid Substances 0.000 claims abstract description 15
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052709 silver Inorganic materials 0.000 claims abstract description 13
- 239000004332 silver Substances 0.000 claims abstract description 13
- 238000002844 melting Methods 0.000 claims abstract description 8
- 230000008018 melting Effects 0.000 claims abstract description 8
- 238000003723 Smelting Methods 0.000 claims description 19
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 13
- 238000012546 transfer Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract 1
- 238000004321 preservation Methods 0.000 description 16
- 238000007670 refining Methods 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/04—Refining by applying a vacuum
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/06—Obtaining bismuth
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides a vacuum purification method for multi-stage extraction of refined bismuth, which comprises the steps of taking silver-containing crude bismuth alloy as a raw material, firstly melting the silver-containing crude bismuth alloy into a liquid state, extruding the liquid crude bismuth alloy into a vacuum furnace for three-time purification, and obtaining refined bismuth with the bismuth content higher than 99.997% and the recovery rate higher than 86%.
Description
Technical Field
The invention relates to the field of vacuum purification methods for multi-stage extraction of refined bismuth, in particular to a vacuum purification method for multi-stage extraction of refined bismuth.
Background
The common bismuth slag treatment process at present mainly comprises a wet-fire combined smelting process and a fire smelting process. Crude bismuth produced by bismuth ore reduction smelting, precipitation smelting and mixed smelting contains a lot of impurities, and even bismuth-rich concentrate with high bismuth content still cannot meet the requirements of users after smelting. The impurity components of the crude bismuth are mainly copper, lead, silver, arsenic, antimony, tellurium, tin and the like, and the impurities have great influence on the properties of the bismuth and cannot be directly applied, so that further refining is required. The crude bismuth refining method mainly comprises fire refining and electrolytic refining. At present, the mainstream crude bismuth refining method in the world is fire refining. The main advantages of fire refining are high production capacity, low selectivity to raw materials and capability of refining crude bismuth with various component contents. But the quantity of fire refining slag is large, the quantity of retained valuable metals is large, the occupied capital is large, and the production cost is high, so the invention provides a vacuum purification method for extracting refined bismuth in multiple sections, which reduces the production cost and improves the purity and the yield of the refined bismuth.
Disclosure of Invention
In view of the above, the present invention provides a vacuum purification method for multi-stage extraction of refined bismuth, which solves the above problems.
The technical scheme of the invention is realized as follows:
a vacuum purification method for multi-stage extraction of refined bismuth comprises the following steps:
(1) Melting the silver-containing crude bismuth alloy into liquid through a smelting furnace, and enabling the liquid to flow into a transfer box to prepare liquid silver crude bismuth alloy;
(2) And extruding the liquid silver crude bismuth alloy into a vacuum furnace for purification to obtain a finished product.
Further, in the step (1), the temperature of the smelting furnace is 1400-1600 ℃.
Further, in the step (2), the purification method using the vacuum furnace is divided into three stages, wherein the vacuum degree of the first stage is 4-7pa, the temperature is 500-700 ℃, the vacuum degree of the second stage is 15-20pa, the temperature is 800-900 ℃, the vacuum degree of the third stage is 28-30pa, and the temperature is 1200-1300 ℃.
Furthermore, the heat preservation time of the first stage is 1-1.5h, the heat preservation time of the second stage is 1-2h, and the heat preservation time of the third stage is 3-3.5h.
Further, in the step (1), the bismuth content in the silver crude bismuth alloy is 80-90%.
Further, the vacuum degree of the first stage is 5pa, the temperature is 600 ℃, the heat preservation time is 75min, the vacuum degree of the second stage is 18pa, the temperature is 850 ℃, the heat preservation time of the second stage is 1.5h, the vacuum degree of the third stage is 29pa, the temperature is 1250 ℃, and the heat preservation time is 3.5h.
Compared with the prior art, the invention has the following beneficial effects:
the method takes the silver crude bismuth alloy as a raw material, melts the silver-containing crude bismuth alloy into liquid through a smelting furnace, purifies the liquid silver crude bismuth alloy for three times, accelerates the smelting rate by adjusting the factors of the vacuum degree, the reaction temperature and the reaction time of a vacuum furnace, avoids the phenomena of furnace setting and the like of reaction materials, and has the direct yield of refined bismuth up to 88.97 percent and the purity of refined bismuth up to 99.997 percent.
Detailed Description
In order to better understand the technical content of the invention, specific examples are provided below to further illustrate the invention.
The experimental methods used in the examples of the present invention are all conventional methods unless otherwise specified.
The materials, reagents and the like used in the examples of the present invention can be obtained commercially without specific description.
The purity of bismuth was checked with reference to GBT915-2010 with direct yield = actual yield/theoretical yield × 100%
Example 1
(1) Melting the silver-containing crude bismuth alloy into liquid state by a smelting furnace, and enabling the liquid state to flow into a transfer box, wherein the temperature of the smelting furnace is 1400 ℃ to prepare the liquid silver crude bismuth alloy;
(2) Extruding the liquid silver crude bismuth alloy into a vacuum furnace for purification, wherein the purification method by using the vacuum furnace is divided into three stages, the vacuum degree of the first stage is 4pa, the temperature is 500 ℃, the heat preservation time of the first stage is 1h, the vacuum degree of the second stage is 15pa, the temperature is 800 ℃, the heat preservation time of the second stage is 1h, the vacuum degree of the third stage is 28pa, the temperature is 1200 ℃, and the heat preservation time of the third stage is 3h.
The purity of bismuth in the finished product is 99.997 percent, and the direct yield is 87.67 percent.
Example 2
(1) Melting the silver-containing crude bismuth alloy into liquid state by a smelting furnace, and enabling the liquid state to flow into a transfer box, wherein the temperature of the smelting furnace is 1600 ℃ to prepare the liquid silver crude bismuth alloy;
(2) Extruding the liquid silver crude bismuth alloy into a vacuum furnace for purification, wherein the purification method by using the vacuum furnace is divided into three stages, the vacuum degree of the first stage is 7pa, the temperature is 700 ℃, the heat preservation time of the first stage is 1.5h, the vacuum degree of the second stage is 20pa, the temperature is 900 ℃, the heat preservation time of the second stage is 2h, the vacuum degree of the third stage is 30pa, the temperature is 1300 ℃, and the heat preservation time of the third stage is 3.5h.
The purity of bismuth in the finished product is 99.997%, and the direct yield is 85.67%.
Example 3
(1) Melting the silver-containing crude bismuth alloy into liquid state by a smelting furnace, and enabling the liquid state to flow into a transfer box, wherein the temperature of the smelting furnace is 1500 ℃ to prepare the liquid silver crude bismuth alloy;
(2) Extruding the liquid silver crude bismuth alloy into a vacuum furnace for purification, wherein the purification method by using the vacuum furnace is divided into three stages, the first stage is at a vacuum degree of 5pa and a temperature of 600 ℃, the heat preservation time is 75min, the second stage is at a vacuum degree of 18pa and a temperature of 850 ℃, the second stage is at a heat preservation time of 1.5h, the third stage is at a vacuum degree of 29pa and a temperature of 1250 ℃, and the heat preservation time is 3.5h.
The purity of bismuth in the finished product is 99.997%, and the direct yield is 88.97%.
Comparative example 1
(1) Melting the silver-containing crude bismuth alloy into liquid state by a smelting furnace, and enabling the liquid state to flow into a transfer box, wherein the temperature of the smelting furnace is 1500 ℃ to prepare the liquid silver crude bismuth alloy;
(2) And extruding the liquid silver crude bismuth alloy into a vacuum furnace for purification, wherein the vacuum degree of the vacuum furnace is 20pa, the temperature is 1250 ℃, and the heat preservation time is 3.5h.
The purity of bismuth in the finished product is 93.67 percent, and the yield is 70.13 percent.
Comparative example 1 changes the reaction mode of the vacuum furnace, which results in the reduction of the reaction rate of the materials, incomplete removal of impurities in the silver crude bismuth alloy and the reduction of the quality of finished products.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. A vacuum purification method for multi-stage extraction of refined bismuth is characterized by comprising the following steps:
(1) Melting the silver-containing crude bismuth alloy into liquid through a smelting furnace, and enabling the liquid to flow into a transfer box to prepare liquid silver crude bismuth alloy;
(2) And extruding the liquid silver crude bismuth alloy into a vacuum furnace for purification to obtain a finished product.
2. The multi-stage vacuum purification method of refined bismuth according to claim 1, wherein in the step (1), the temperature of the melting furnace is 1400 to 1600 ℃.
3. The vacuum purification method for multistage extraction of refined bismuth as claimed in claim 1, wherein in the step (2), the purification method using a vacuum furnace is divided into three stages, the first stage having a vacuum degree of 4-7pa at a temperature of 500-700 ℃, the second stage having a vacuum degree of 15-20pa at a temperature of 800-900 ℃, and the third stage having a vacuum degree of 28-30pa at a temperature of 1200-1300 ℃.
4. The vacuum purification method for multi-stage extraction of refined bismuth as claimed in claim 3, wherein the first stage is performed for 1-1.5h, the second stage is performed for 1-2h, and the third stage is performed for 3-3.5h.
5. The vacuum purification method for multi-stage extraction of refined bismuth as claimed in claims 3-4, wherein the first stage vacuum degree is 5pa, the temperature is 600 ℃, the holding time is 75min, the second stage vacuum degree is 18pa, the temperature is 850 ℃, the second stage holding time is 1.5h, the third stage vacuum degree is 29pa, the temperature is 1250 ℃, and the holding time is 3.5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211055904.5A CN115491509A (en) | 2022-08-31 | 2022-08-31 | Vacuum purification method for multi-stage extraction of refined bismuth |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211055904.5A CN115491509A (en) | 2022-08-31 | 2022-08-31 | Vacuum purification method for multi-stage extraction of refined bismuth |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115491509A true CN115491509A (en) | 2022-12-20 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211055904.5A Pending CN115491509A (en) | 2022-08-31 | 2022-08-31 | Vacuum purification method for multi-stage extraction of refined bismuth |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115491509A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3218159A (en) * | 1961-03-13 | 1965-11-16 | Prod Semi Conducteurs Soc | Manufacture of pure bismuth |
| JPH10158754A (en) * | 1996-11-26 | 1998-06-16 | Dowa Mining Co Ltd | Production of high-purity bismuth and apparatus for production |
| CN101696469A (en) * | 2009-10-29 | 2010-04-21 | 昆明理工大学 | Method for separating multi-element alloy of lead, bismuth, gold, silver and copper |
| CN104109766A (en) * | 2014-07-31 | 2014-10-22 | 永兴鑫裕环保镍业有限公司 | Technology for separating and purifying bismuth from lead-bismuth alloy |
| CN112322904A (en) * | 2020-10-12 | 2021-02-05 | 昆明鼎邦科技股份有限公司 | Method for vacuum separation of gold, silver and copper alloy |
-
2022
- 2022-08-31 CN CN202211055904.5A patent/CN115491509A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3218159A (en) * | 1961-03-13 | 1965-11-16 | Prod Semi Conducteurs Soc | Manufacture of pure bismuth |
| JPH10158754A (en) * | 1996-11-26 | 1998-06-16 | Dowa Mining Co Ltd | Production of high-purity bismuth and apparatus for production |
| CN101696469A (en) * | 2009-10-29 | 2010-04-21 | 昆明理工大学 | Method for separating multi-element alloy of lead, bismuth, gold, silver and copper |
| CN104109766A (en) * | 2014-07-31 | 2014-10-22 | 永兴鑫裕环保镍业有限公司 | Technology for separating and purifying bismuth from lead-bismuth alloy |
| CN112322904A (en) * | 2020-10-12 | 2021-02-05 | 昆明鼎邦科技股份有限公司 | Method for vacuum separation of gold, silver and copper alloy |
Non-Patent Citations (1)
| Title |
|---|
| 陈鸿彬: "高纯试剂提纯与制备", 上海科学技术出版社, pages: 291 * |
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