CN105821224A - Method for extracting germanium in low-grade germanium concentrates through fluoride roasting process - Google Patents
Method for extracting germanium in low-grade germanium concentrates through fluoride roasting process Download PDFInfo
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- CN105821224A CN105821224A CN201610388498.2A CN201610388498A CN105821224A CN 105821224 A CN105821224 A CN 105821224A CN 201610388498 A CN201610388498 A CN 201610388498A CN 105821224 A CN105821224 A CN 105821224A
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- germanium
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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
- C22B41/00—Obtaining germanium
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
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- 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
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Abstract
The invention provides a method for extracting germanium in low-grade germanium concentrates through a fluoride roasting process, and relates to a technology for extracting germanium through chloridizing distillation by conducting fluoride roasting pretreatment on the germanium concentrates which are low in grade and difficult to treat. The method comprises the steps of fluoride roasting, hydrochloric acid distillation and germanium extracting through sodium hydroxide. The technology is simple, short in process, safe, environmentally friendly and free of corrosion to equipment, the extracting recovery rate of germanium can reach 95.6% or above, acid slag obtained in the germanium extracting process is subjected to secondary germanium extracting, the recovery rate of secondary germanium extracting reaches 91.5% or above, and the germanium grade of acid slag obtained in the secondary germanium extracting process is lowered to below 0.01%.
Description
Technical field
The present invention relates to a kind of low-grade refractory is processed germanium concentrate perfluorinated thing roasting pretreatment after carry out chlorinated distillation extract germanium method, belong to technical field of wet metallurgy.
Background technology
Germanium occupies critical role on defence and military and modern science and technology, and optical fibers germanium, infrared optics germanium, used in electronic industry germanium, pharmaceutical germanium, superconductor germanium, photoelectric source germanium etc. are all the germanium important use in every field.And germanium belongs to rare and scatter element, being distributed in the mineral such as coal, silver, stannum, zinc, copper, the extracting method of germanium is a lot, but the germanium that carries realizing high-efficient energy-saving environment friendly remains technical barrier and the study hotspot of germanium metallurgical technology field more.The brown coal germanium ore deposit of Lincang typically uses the method that chain furnace pyrogenic process extracts germanium, due to the ash in brown coal germanium ore deposit height too high, siliceous, silicon dioxide and silicates material in the germanium concentrate obtained is extracted higher through the enrichment of chain furnace pyrogenic process, leach and during distillation extraction germanium in later stage wet chlorination, germanium leaches, steam rate is difficult to breakthrough 85%, is because silicate and orthosilicic acid Si (OH) during salt adding Ore Leaching4Polymer has wrapped up part germanium and has defined SiGe coalition, and causes germanium leaching rate the highest.
For the technical barrier that the response rate in this direct salt Ore Leaching still-process is low, it is also proposed the solution of many, such as high pressure sulfuric acid leaching, aqueous slkali solvent extraction method, preparation, microwave heating method for pretreating, microwave heating alkali fusion, add Fluohydric acid. solvent extraction method etc., all there is certain effect.The know-why of the present invention has principle similarity with Fluohydric acid. solvent extraction method, but have any different, Fluohydric acid. solvent extraction method be in the solution 70-80 DEG C leach, leaching needs after completing to carry out carrying out chlorinated distillation again after the recovery of the tannin sedimentation method obtains germanium concentrate, in leaching process, Fluohydric acid. is the strongest to the corrosivity of leaching equipment and distillation equipment, the hydrogen fluoride gas produced is relatively big on operating environment impact, need to strictly protect operator.And the present invention will not produce Fluohydric acid., can directly carry out chlorinated distillation after the fired process of low-grade germanium concentrate, during distillation, fluoride will not be distilled out of, and Distallation systm and equipment will not be produced corrosion, do not produce hydrogen fluoride gas, to operator and environment non-hazardous.
Summary of the invention
The present invention is a kind of method adding fluoride roasting pretreatment germanium-containing smoke dust, carrying germanic acid slag Ti recovery, solves the germanium concentrate wet chlorination distillating method germanium response rate low, carries the germanic high second extraction germanium response rate of the acid sludge after germanium technical barrier such as low grade.
The fluorination roasting method of the present invention extracts the method for germanium in low-grade germanium concentrate, it is characterised in that the method comprises the following steps that
The first step, fluorination roasting:
Being milled to below 120 mesh by broken for fluoride, putting into after mixing with low-grade germanium concentrate heats up in Muffle furnace carries out roasting, and in 2h, Muffle furnace is warming up to 800 900 DEG C, constant temperature calcining 2-3h at such a temperature；Wherein, the weight of fluoride is the 20-30% of gross weight；
Second step, potassium cloride distillation extraction germanium:
Material roasting in above-mentioned steps is taken out and is cooled to room temperature, broken below 120 mesh that are milled to, the salt Ore Leaching 1-2h of addition 10mol/L, then distill, distillation time is 30-40min, uses the sodium hydroxide solution distillation of 10% to receive germanium；Wherein, every gram of roasting material adds hydrochloric acid 3-4mL, and 1mL water.
Described fluoride is sodium fluoride or potassium fluoride.
Described low-grade germanium concentrate is the germanic germanium concentrate at 0.5-3%.
In present invention process, relate to following chemical equation:
；
；
。
The know-why of the present invention be germanium concentrate and fluoride are mixed by a certain percentage even after carry out high-temperature roasting, the material such as silicon dioxide and silicate is made to have an effect with fluoride, the germanium by the material such as silicon dioxide and silicate parcel is made to discharge, partially fluorinated thing also can play the same role when chlorination of hydrochloric acid leaches, have an effect with silicate and silicon class polymer equally, wrapped exposed out the reacting with hydrochloric acid of germanium is made to be distilled and separate, but fluoride is because defining hexafluosilicic acid without being distilled out of, thus do not produce Fluohydric acid. and leaching equipment and distillation equipment are caused corrosivity, therefore reach to improve germanium to leach, the purpose of steam rate.
Present invention process is simple, short flow, safety and environmental protection, and germanium extraction recovery, up to more than 96.20%, puies forward the response rate that germanic acid slag uses this technique to carry out second extraction germanium and reaches more than 91.50%, and the germanium grade that secondary carries in germanic acid slag is down to less than 0.01%.
It is embodied as case
Embodiment 1:Fluorination roasting method extracts the method for germanium in low-grade germanium concentrate, it is characterised in that the method comprises the following steps that
The first step, weighs low-grade germanium concentrate 35.000g and the 15.000g sodium fluoride of germanic 2.61%, and is ground to below granularity 120 mesh, puts into Muffle kiln roasting after being sufficiently mixed uniformly, and in 2h, Muffle furnace is warmed up to 900 DEG C, constant temperature calcining 2h.Muffle furnace slightly blow-on door, is oxygen-enriched state in stove.
Second step, takes out the roasting material in the first step and is cooled to room temperature, then is crushed and be milled to below 120 mesh, accurately weigh 25.000g material in 300mL distilling flask, add 25.0mL water and the hydrochloric acid 100.0mL of 10.0mol/L, after connecting distilling apparatus, begin to warm up leaching distillation.Extraction time is 1h, has leached post-heating distillation, and has steamed germanium with the sodium hydroxide solution reception of 10.0%, and the time of chlorinated distillation is 30min, and distillation terminates rear assay and receives liquid, distills germanic amount of metal in remaining residual liquid, bottoms.The calculating employing of the germanium response rate steams amount of metal/input amount of metal and obtains, and experiment is repeated 4 times, and germanium metal recovery rate is up to more than 97.30%.
The step for that the method that blank group uses being not fill fluoride roasting, but directly weigh 25.000g germanium concentrate sample (germanic 2.61%) and add 25.0mL water and 100.0mL hydrochloric acid, just start to leach chlorinated distillation Ti recovery, experiment is repeated 4 times, and the germanium response rate obtained is difficult to breakthrough 89.70%.
Case study on implementation 2:Fluorination roasting method extracts the method for germanium in low-grade germanium concentrate, it is characterised in that the method comprises the following steps that
The first step, weigh germanic be 1.16% germanium concentrate 40.000g, and the sodium fluoride 10.000g that granularity is below 120 mesh, put into Muffle kiln roasting after being sufficiently mixed uniformly, in 2h, Muffle furnace is warmed up to 800 DEG C of constant temperature calcining 3h.Muffle fire door is slightly opened, and is oxygen-enriched state in stove.
Second step, roasting logistics in the first step is taken out and is cooled to room temperature, crushed again and be milled to below 120 mesh, accurately weigh 25.000g material in 300mL distilling flask, add 25.0mL water and the hydrochloric acid 100.0mL of 10.0mol/L, after connecting distilling apparatus, begin to warm up leaching distillation, extraction time is 1h, leach post-heating distillation, and receiving, with the sodium hydroxide solution of 10.0%, the germanium steamed, the time of chlorinated distillation is 30min, and distillation terminates rear assay and receives liquid, distills germanic amount of metal in remaining residual liquid, bottoms.The calculating employing of the germanium response rate steams amount of metal/input amount of metal and obtains, and experiment is repeated 4 times, and germanium metal recovery rate is up to more than 96.20%.
Case study on implementation 3:Fluorination roasting method extracts the method for germanium in low-grade germanium concentrate, it is characterised in that the method comprises the following steps that
The first step, by remaining for matched group in case study on implementation 1 residual acid sludge through washing post-drying, the most accurately weigh 40.000g dry acid slag (germanic 0.428%) and 10.000g sodium fluoride (below granularity 120 mesh), putting into Muffle kiln roasting after being sufficiently mixed uniformly, in 2h, Muffle furnace is warming up to 800 DEG C of constant temperature calcining 2h.
Second step, sample is taken out and is cooled to room temperature, carry out sample again crushing being milled to below 120 mesh, accurately weigh sample 25.000g material for chlorinated distillation Ti recovery, the addition of chlorinated distillation hydrochloric acid is 100.0mL, concentration is 10.0mol/L, immediately begin to add thermal distillation after adding 25.0mL water, heat and leach while distilling and using 10.0% sodium hydroxide to receive the germanium steamed, the chlorinated distillation time is 30min, and distillation terminates rear assay and receives liquid, distills germanic amount of metal in remaining residual liquid, bottoms.The calculating employing of the germanium response rate steams amount of metal/input amount of metal and obtains, and experiment is repeated 4 times, and germanium metal recovery rate is up to more than 91.50%, and remaining residue grade is down to less than 0.010%.
The step for that the method that matched group uses being not fill fluoride roasting, but directly weigh 25.000g dry acid slag specimen product (germanic 0.428%) and add 100.0mL hydrochloric acid and 25.0mL aquiform stool and start chlorinated distillation Ti recovery, experiment is repeated 4 times, and the germanium response rate obtained only has 10.30%.
Claims (3)
1. fluorination roasting method extracts the method for germanium in low-grade germanium concentrate, it is characterised in that the method comprises the following steps that
The first step, fluorination roasting:
Being milled to below 120 mesh by broken for fluoride, putting into after mixing with low-grade germanium concentrate heats up in Muffle furnace carries out roasting, and in 2h, Muffle furnace is warming up to 800-9000 DEG C, at such a temperature constant temperature calcining 2-3h；Wherein, the weight of fluoride is the 20-30% of gross weight；
Second step, potassium cloride distillation extraction germanium:
Material roasting in above-mentioned steps is taken out and is cooled to room temperature, broken below 120 mesh that are milled to, the salt Ore Leaching 1-2h of addition 10mol/L, then distill, distillation time is 30-40min, uses the sodium hydroxide solution distillation of 10% to receive germanium；Wherein, every gram of roasting material adds hydrochloric acid 3-4mL, and 1mL water.
2. fluorination roasting method as claimed in claim 1 extracts the method for germanium in low-grade germanium concentrate, it is characterised in that described fluoride be sodium fluoride or potassium fluoride.
3. fluorination roasting method as claimed in claim 1 extracts the method for germanium in low-grade germanium concentrate, it is characterised in that described low-grade germanium concentrate is the germanic germanium concentrate at 0.5-3%.
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| CN201610388498.2A CN105821224B (en) | 2016-06-06 | 2016-06-06 | It is fluorinated the method that roasting method extracts germanium in low-grade germanium concentrate |
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| CN201610388498.2A CN105821224B (en) | 2016-06-06 | 2016-06-06 | It is fluorinated the method that roasting method extracts germanium in low-grade germanium concentrate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106906364A (en) * | 2017-03-07 | 2017-06-30 | 云南临沧鑫圆锗业股份有限公司 | The process of Ti recovery from germanic fluorine containing corrosion liquid |
| CN109439897A (en) * | 2018-11-22 | 2019-03-08 | 衡阳恒荣高纯半导体材料有限公司 | Germanic organic matter produces germanium tetrachloride new process |
| CN115477501A (en) * | 2022-09-02 | 2022-12-16 | 中国矿业大学 | Resource comprehensive utilization method of germanium extraction residues |
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| CN105197938A (en) * | 2015-09-09 | 2015-12-30 | 洛阳国兴矿业科技有限公司 | Comprehensive utilization method of using acid-heating method to treat low-quality bauxite |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106906364A (en) * | 2017-03-07 | 2017-06-30 | 云南临沧鑫圆锗业股份有限公司 | The process of Ti recovery from germanic fluorine containing corrosion liquid |
| CN106906364B (en) * | 2017-03-07 | 2019-08-16 | 云南临沧鑫圆锗业股份有限公司 | The process of Ti recovery from germanic fluorine containing corrosion liquid |
| CN109439897A (en) * | 2018-11-22 | 2019-03-08 | 衡阳恒荣高纯半导体材料有限公司 | Germanic organic matter produces germanium tetrachloride new process |
| CN115477501A (en) * | 2022-09-02 | 2022-12-16 | 中国矿业大学 | Resource comprehensive utilization method of germanium extraction residues |
| CN115477501B (en) * | 2022-09-02 | 2023-02-28 | 中国矿业大学 | Resource comprehensive utilization method of germanium extraction residues |
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Inventor after: Pu Shikun Inventor after: Zhu Zhiguo Inventor after: Yang Zailei Inventor after: Xie Gao Inventor after: Wang Lifang Inventor after: Wu Wangchang Inventor after: Hu Maojiang Inventor after: Li Zhengmei Inventor after: Li Xuan Inventor before: Pu Shikun Inventor before: Zhu Zhiguo Inventor before: Yang Zailei Inventor before: Xie Gao Inventor before: Wang Lifang Inventor before: Wu Wangchang Inventor before: Hu Maojiang Inventor before: Li Zhengmei Inventor before: Li Xuan |
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Denomination of invention: Method for extracting germanium from low-grade germanium concentrate by fluorination roasting Effective date of registration: 20220113 Granted publication date: 20180615 Pledgee: Yunnan Hongta Bank Co.,Ltd. Pledgor: YUNNAN LINCANG XINYUAN GERMANIUM INDUSTRY Co.,Ltd.|YUNNAN DONGCHANG METAL PROCESSING Co.,Ltd. Registration number: Y2022530000003 |