CN113337725A - Method for enriching germanium from smelting slag - Google Patents
Method for enriching germanium from smelting slag Download PDFInfo
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- CN113337725A CN113337725A CN202110730268.0A CN202110730268A CN113337725A CN 113337725 A CN113337725 A CN 113337725A CN 202110730268 A CN202110730268 A CN 202110730268A CN 113337725 A CN113337725 A CN 113337725A
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- germanium
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- 229910052732 germanium Inorganic materials 0.000 title claims abstract description 123
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 title claims abstract description 123
- 238000003723 Smelting Methods 0.000 title claims abstract description 82
- 239000002893 slag Substances 0.000 title claims abstract description 72
- 238000000034 method Methods 0.000 title claims abstract description 26
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 10
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 claims abstract description 10
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 5
- 239000010436 fluorite Substances 0.000 claims description 5
- 229910021538 borax Inorganic materials 0.000 claims description 4
- 239000004328 sodium tetraborate Substances 0.000 claims description 4
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 4
- RHZUVFJBSILHOK-UHFFFAOYSA-N anthracen-1-ylmethanolate Chemical compound C1=CC=C2C=C3C(C[O-])=CC=CC3=CC2=C1 RHZUVFJBSILHOK-UHFFFAOYSA-N 0.000 claims description 3
- 239000003830 anthracite Substances 0.000 claims description 3
- 239000002802 bituminous coal Substances 0.000 claims description 3
- 239000006184 cosolvent Substances 0.000 claims description 2
- 239000004744 fabric Substances 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 33
- 239000000126 substance Substances 0.000 abstract description 16
- 239000000428 dust Substances 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 10
- 229910052733 gallium Inorganic materials 0.000 description 10
- 239000003245 coal Substances 0.000 description 6
- 238000000605 extraction Methods 0.000 description 6
- 238000002386 leaching Methods 0.000 description 6
- 238000000498 ball milling Methods 0.000 description 5
- 239000012141 concentrate Substances 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 description 4
- 239000002994 raw material Substances 0.000 description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-O sulfonium Chemical compound [SH3+] RWSOTUBLDIXVET-UHFFFAOYSA-O 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- KWHNXZAUGQZEDI-UHFFFAOYSA-N Cl.[Ge] Chemical compound Cl.[Ge] KWHNXZAUGQZEDI-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 235000010363 Vitex negundo Nutrition 0.000 description 1
- 244000248021 Vitex negundo Species 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000006298 dechlorination reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229940119177 germanium dioxide Drugs 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000009853 pyrometallurgy Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Images
Classifications
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- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/04—Working-up slag
-
- 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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
-
- 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
- C22B41/00—Obtaining germanium
-
- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
-
- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
- C22B7/002—Dry processes by treating with halogens, sulfur or compounds thereof; by carburising, by treating with hydrogen (hydriding)
-
- 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
Abstract
The invention discloses a method for enriching germanium from smelting slag, and belongs to the technical field of scattered metal recovery. The invention mixes the germanium-containing smelting slag, phosphogypsum, iron powder, reducing agent and fluxing agent in proportion and then grinds the mixture; and carrying out reduction matte smelting on the ground mixture to respectively obtain germanium-containing volatile substances and matte enriched substances, wherein the recovery rate of germanium in the volatile substances is more than 15 percent, the content of germanium in the volatile substances is about 0.21-0.56 percent, the recovery rate of germanium in the volatile substances is more than 80 percent, the content of germanium in the volatile substances is 0.08-0.22 percent, the content of germanium in smelting slag is less than 0.0024 percent, and the total recovery rate of germanium is more than 95.0 percent. The method has the advantages of short flow, obviously improved germanium recovery rate, mature main smelting and dust collecting equipment and potential industrialization prospect.
Description
Technical Field
The invention belongs to the technical field of scattered metal recovery, and relates to a method for enriching germanium from smelting slag.
Background
Germanium is one of strategic metals, and after most of germanium is extracted from the germanium coal mine by pyrometallurgy, a certain amount of germanium is still contained in slag, so that the recovery value is high. At present, the method for recovering the germanium-containing smelting slag comprises the following steps:
sunhoran et al disclose a method for recovering germanium from germanium extraction coal slag (patent No. 02113848.6). A method for extracting germanium again from waste germanium-extracting coal slag. The technology adopts coal slag containing 0.015-0.030% of germanium after extracting germanium as raw material, uses coke powder as reducing agent, and causes CO with volume percentage in a furnace at the furnace temperature of 1150-1250 DEG C2 10％～15％，CO 1％～4％，O22 to 5 percent of weak reducing atmosphere, and the GeO generated by reduction is oxidized into GeO2 at high temperature after being volatilized and collected in the smoke dust for recycling. The method can treat the germanium-containing coal slag with great treatment difficulty, has low treatment cost and high germanium yield, and is beneficial to changing waste into valuable and protecting the environment.
Huangping et al disclose a process for secondary recovery of germanium from germanium extraction coal slag and germanium extraction acid slag (patent number: 201310307880.2), the process of the invention includes washing deacidification and dechlorination, crushing batching, smelting, collecting germanium concentrate and germanium dioxide preparation process steps, the process of the invention enables the germanium volatility and the enrichment specific energy to be greatly improved, the recovery rate from germanium extraction waste slag to germanium concentrate can reach 73-80%, the enrichment ratio can reach 300 times of 100, the distillation recovery rate of the produced germanium concentrate germanium hydrochloric acid can reach more than 92%, the germanium content in the germanium extraction waste slag can be lower than 40g/t, and the germanium concentrate can be backfilled into a mined-out area as a filler, so as to eliminate the pollution of the germanium extraction waste slag to the environment.
The invention discloses a method for directly leaching germanium from germanium-containing slag by sulfuric acid (application publication number: 201210555576.5), which comprises the steps of taking an intermediate product of zinc hydrometallurgy as a raw material, adding water, stirring uniformly, adding a certain amount of sulfuric acid, curing, and adding water to wash the obtained filtrate, namely the experimental germanium-containing leachate. The method has the advantages of relatively mild conditions, relatively simple operation, high germanium leaching rate of over 70 percent and good practical application value.
The invention discloses a method for selectively leaching germanium and gallium from complex smelting slag or ore containing germanium and gallium (application publication No. 201310468825.1). The invention discloses a method for selectively leaching germanium and gallium from complex smelting slag or ore containing germanium and gallium under the alkaline condition of high temperature and high pressure oxygen introduction, and sequentially using calcium chloride to sink gallium and neutralizing to sink germanium after adjusting the pH value to remove impurities, so that the germanium and the gallium are selectively recovered. The invention can realize the recovery rate of germanium as high as 98 percent and the recovery rate of gallium as high as 99 percent; the effect of leaching germanium and gallium with high selectivity is achieved, and the recovery rate is high. The invention has strong raw material applicability, is not only suitable for various complex pyrometallurgical and hydrometallurgical slags containing germanium and gallium, but also suitable for ores containing germanium and gallium at high content.
In conclusion, the existing smelting slag containing germanium has low recovery rate and high cost. Based on the method, a method for enriching germanium from smelting slag is provided, and the germanium-containing smelting slag is efficiently enriched. The method is not reported in reference data.
Disclosure of Invention
The invention aims to provide a method for enriching germanium from smelting slag.
The invention provides the following technical scheme, a method for enriching germanium from smelting slag, which comprises the steps of mixing germanium-containing smelting slag, phosphogypsum, iron powder, a reducing agent and a fluxing agent in proportion and then respectively levigating; and carrying out reduction matte smelting on the ground mixture to respectively obtain germanium-containing volatile matters and matte enriched matters.
Further, in the step (1), a reducing agent is one of coke powder, anthracite and bituminous coal, a cosolvent is one of fluorite and borax, the adding amount of iron powder is 5-20% of the weight ratio of the smelting slag, the adding amount of phosphogypsum is 5-30% of the weight ratio of the smelting slag, the adding amount of the reducing agent is 5-15% of the weight ratio of the smelting slag, and the adding amount of a fluxing agent is 5-20% of the weight ratio of the smelting slag.
Further, in the step (2), the matte is reduced and smelted at the smelting temperature of 1300-1400 ℃ for 1-3 h.
The innovation points of the invention are mainly as follows:
(1) reduction matte smelting is adopted, 80% of germanium is trapped in matte, volatilization is collected by a cloth bag, and the total yield of germanium is more than 95%;
(2) because the smelting slag has high silicon content and germanium is embedded in silicate, the germanium enrichment is efficiently realized by reducing and matte smelting, and the problems of difficult filtration, large reagent consumption, high cost and the like in wet leaching are solved.
In conclusion, the recovery rate of germanium in the volatile matters containing germanium is more than 15%, the content of germanium is 0.21-0.56%, the recovery rate of germanium in the concentrate containing sulfonium is more than 80%, the content of germanium is 0.08-0.22%, the content of germanium in the smelting slag is less than 0.0024%, and the total recovery rate of germanium is more than 95.0%. The method has the advantages of short flow, obviously improved germanium recovery rate, capability of realizing high-efficiency germanium enrichment, environmental friendliness, low cost and the like, and has a potential industrial prospect due to mature main smelting and dust collecting equipment.
Drawings
FIG. 1 is a process flow diagram of the invention for germanium enrichment from smelting slag.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the following detailed description of the present invention is given with reference to specific examples:
example 1
Referring to the drawings, conditions: weighing 100kg of germanium-containing smelting slag, wherein the adding amount of iron powder is 10 wt% of the smelting slag, the adding amount of phosphogypsum is 23 wt% of the smelting slag, the adding amount of coke powder is 8 wt% of the smelting slag, and the adding amount of fluorite is 12 wt% of the smelting slag, performing ball milling and mixing, smelting and enriching germanium by using reduction matte at the smelting temperature of 1300 ℃ for 1.5h, respectively obtaining germanium-containing volatile substances and matte enriched substances, wherein the recovery rate of germanium in the former reaches 15.42% and the content of germanium is about 0.41%, the recovery rate of germanium in the latter reaches 82.01% and the content of germanium is 0.12%, the content of germanium in the smelting slag is lower than 0.0012%, and the total recovery rate of germanium reaches 96.43%.
Example 2
Referring to the drawings, conditions: weighing 250kg of germanium-containing smelting slag, wherein the adding amount of iron powder is 12% of the weight ratio of the smelting slag, the adding amount of phosphogypsum is 25% of the weight ratio of the smelting slag, the adding amount of bituminous coal is 15% of the weight ratio of the smelting slag, and the adding amount of fluorite is 12% of the weight ratio of the smelting slag, performing ball milling and mixing, smelting and enriching germanium by using reduction matte at the smelting temperature of 1400 ℃ for 2.5 hours, respectively obtaining germanium-containing volatile substances and matte enriched substances, wherein the recovery rate of germanium in the former reaches 16.25% and the content of germanium is about 0.28%, the recovery rate of germanium in the latter reaches 81.72% and the content of germanium is 0.21%, the content of germanium in the smelting slag is lower than 0.0017%, and the total recovery rate of germanium reaches 97.97%.
Example 3
Referring to the drawings, conditions: weighing 50kg of germanium-containing smelting slag, wherein the adding amount of iron powder is 15 wt% of the smelting slag, the adding amount of phosphogypsum is 22 wt% of the smelting slag, the adding amount of anthracite is 8 wt% of the smelting slag, and the adding amount of borax is 12 wt% of the smelting slag, performing ball milling and mixing, smelting and enriching germanium by using reduction sulfonium at the smelting temperature of 1320 ℃, and smelting time of 1.5h, respectively obtaining germanium-containing volatile substances and sulfonium enriched substances, wherein the recovery rate of germanium in the former reaches 15.63% and the content of germanium is about 0.52%, the recovery rate of germanium in the latter reaches 82.01% and the content of germanium is 0.14%, the content of germanium in the smelting slag is lower than 0.0012%, and the total recovery rate of germanium reaches 96.59%.
Example 4
Referring to the drawings, conditions: weighing 150kg of germanium-containing smelting slag, wherein the adding amount of iron powder is 8 wt% of the smelting slag, the adding amount of phosphogypsum is 20 wt% of the smelting slag, the adding amount of reducing agent is 9 wt% of the smelting slag, and the adding amount of fluorite is 11 wt% of the smelting slag, performing ball milling and mixing, smelting and enriching germanium by using reduction matte at the smelting temperature of 1370 ℃ for 2 hours, respectively obtaining germanium-containing volatile substances and matte enriched substances, wherein the recovery rate of germanium in the former reaches 15.32% and the content of germanium is about 0.26%, the recovery rate of germanium in the latter reaches 83.45% and the content of germanium is 0.17%, the content of germanium in the smelting slag is lower than 0.0016%, and the total recovery rate of germanium reaches 97.78%.
Example 5
Referring to the drawings, conditions: weighing 100kg of germanium-containing smelting slag, wherein the adding amount of iron powder is 6 wt% of the smelting slag, the adding amount of phosphogypsum is 24 wt% of the smelting slag, the adding amount of coke powder is 8 wt% of the smelting slag, the adding amount of borax is 11 wt% of the smelting slag, performing ball milling and mixing, smelting and enriching germanium by using reduction matte at the smelting temperature of 1350 ℃ for 2 hours, respectively obtaining germanium-containing volatile substances and matte enriched substances, wherein the recovery rate of germanium in the former reaches 15.52% and the content of germanium is about 0.31%, the recovery rate of germanium in the latter reaches 80.22% and the content of germanium is 0.19%, the content of germanium in the smelting slag is lower than 0.0015%, and the total recovery rate of germanium reaches 95.74%.
Claims (3)
1. A method for enriching germanium from smelting slag is characterized by comprising the following steps:
(1) mixing germanium-containing smelting slag, phosphogypsum, iron powder, a reducing agent and a fluxing agent in proportion and then grinding;
(2) and (3) carrying out high-temperature reduction matte smelting on the ground mixture to respectively obtain germanium-containing volatile matters and matte enriched matters, wherein the germanium-containing volatile matters are collected by a cloth bag.
2. The method of claim 1 for enriching germanium from smelting slag, characterized by: in the step (1), the reducing agent is one of coke powder, anthracite and bituminous coal, the cosolvent is one of fluorite and borax, the adding amount of iron powder is 5-20% of the weight ratio of smelting slag, the adding amount of phosphogypsum is 5-30% of the weight ratio of smelting slag, the adding amount of the reducing agent is 5-15% of the weight ratio of smelting slag, and the adding amount of the fluxing agent is 5-20% of the weight ratio of smelting slag.
3. The method of claim 1 for enriching germanium from smelting slag, characterized by: and (3) in the step (2), the matte is reduced and smelted, wherein the smelting temperature is 1300-1400 ℃, and the smelting time is 1-3 h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115181855A (en) * | 2022-07-06 | 2022-10-14 | 中国恩菲工程技术有限公司 | Method for producing alloy by enriching germanium from germanium-containing smelting slag |
| CN115505751A (en) * | 2022-10-01 | 2022-12-23 | 红河学院 | Method for enriching germanium and indium and co-producing blister copper from copper sulfide ore |
| CN115874065A (en) * | 2022-11-22 | 2023-03-31 | 云南驰宏锌锗股份有限公司 | Method for deeply purifying middle and upper clear solution by deep cone system |
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