CN111575488A - Method for separating, enriching and extracting arsenic, tungsten and germanium-containing waste in sections - Google Patents
Method for separating, enriching and extracting arsenic, tungsten and germanium-containing waste in sections Download PDFInfo
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- CN111575488A CN111575488A CN202010478574.5A CN202010478574A CN111575488A CN 111575488 A CN111575488 A CN 111575488A CN 202010478574 A CN202010478574 A CN 202010478574A CN 111575488 A CN111575488 A CN 111575488A
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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
- C22B7/001—Dry 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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/14—Agglomerating; Briquetting; Binding; Granulating
- C22B1/24—Binding; Briquetting ; Granulating
- C22B1/2406—Binding; Briquetting ; Granulating pelletizing
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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
- C22B1/14—Agglomerating; Briquetting; Binding; Granulating
- C22B1/24—Binding; Briquetting ; Granulating
- C22B1/248—Binding; Briquetting ; Granulating of metal scrap or alloys
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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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/04—Obtaining arsenic
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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
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/36—Obtaining tungsten
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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
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/34—Electrolytic production, recovery or refining of metals by electrolysis of melts of metals not provided for in groups C25C3/02 - C25C3/32
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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
Abstract
The invention discloses a method for separating, enriching and extracting arsenic, tungsten and germanium wastes by stages, which relates to the field of industrial waste treatment and recycling and is exclusive. Grinding and mixing wastes containing arsenic, tungsten and germanium and any combination of ferrous phosphide, phosphorus oxide, ferrous sulfide, sulfur, activated carbon powder and coke powder according to a certain proportion to ensure that the materials are fully contacted to obtain a mixed material, and adding water into the mixed material for granulation to obtain mixed pellets; and then placing the mixed pellets in a vacuum smelting furnace, and carrying out separation treatment according to the conditions of multi-stage temperature rise, temperature reduction and vacuum degree. The method realizes the step-by-step separation and recovery of the waste containing arsenic, tungsten and germanium, and the final residue is not a dangerous waste, can be recycled, has the characteristics of high efficiency, environmental protection and high recycling degree, and is suitable for large-scale industrial application.
Description
Technical Field
The invention relates to the field of industrial waste treatment and recycling, in particular to a sectional separation, enrichment and extraction method for waste containing arsenic, tungsten and germanium.
Background
Germanium, a rare earth metal, has been widely used in semiconductor, electronic and optical devices. Germanium is also a strategic reserve metal in many countries. According to the distribution of germanium application fields, the global germanium usage is mainly in optical fibers, infrared devices and chemical catalysts, accounting for 30%, 22% and 34%, respectively. However, as the amount of germanium used increases, the germanium resource is scarce on a global scale. The global germanium reserves are 8600 tons only, and the gold reserves are 1/10. It is because of this contradiction that the market price of germanium is increasing, with a price of $ 2000/kg 5/month in 2015.
Germanium metal does not have a separate mineral reserve in nature, but is associated with some minerals, such as sphalerite and the like. Germanium-containing waste (such as germanium-containing smoke) is generally only filled in landfills as coal burnout residue, and some germanium-containing smoke contains germanium, which if not utilized, can cause resource waste and environmental pollution. The germanium-containing smoke dust generated after burning coal is usually treated by landfill, and the germanium-containing smoke dust generally contains rich germanium resources. In addition, the wastes are often associated with metal tungsten oxides and the like, and the resource value is higher.
From an environmental point of view, the germanium-containing waste is only treated in landfills and can only enter hazardous waste landfills. Not only is land resource consumed, but also landfill cost is increased. In view of resources, the lignite soot with such a high germanium content is not reused, which results in a great waste of resources. If the waste water can be reasonably recycled, the economic benefit is considerable. China is the second largest germanium resource country in the world, has proved that the germanium mining area is 35, has the reserve of about 3500 metal tons in China and the reserve of about 9600 metal tons in China among the reserves of 8600 metal tons of germanium which have been proved in the world, and has obvious advantages in the world. At present, China has become a major world China for producing and consuming germanium, so that the recovery of germanium resources in germanium-containing smoke dust can not only generate economic value, but also relieve the inevitable requirement of continuously increasing the consumption of germanium in China and the contradiction between the relative shortage of germanium resources.
The waste residue after germanium extraction in the waste is generally treated as toxic arsenic-containing waste residue. At present, the curing and stabilizing treatment technology is generally adopted for treating toxic arsenic-containing waste residues at home and abroad, wherein the cement curing technology is widely applied due to the low price and easy obtaining of curing materials, low treatment cost and good effect, and a plurality of scholars study the mechanism and effect of cement curing arsenic-containing waste residues from different angles. However, after long-term use of the arsenic-containing cured cement, the arsenic is gradually released when the cured cement is exposed to environmental media such as water and soil, so that the concentration of arsenic in the environmental media is increased, and the arsenic-containing cured cement has potential environmental risks. The research reports on arsenic removal from fly ash are few, and researches on elution of arsenic from fly ash by using a nitric acid and sulfuric acid pickling method are available, but the removal rate of arsenic is not high and is only about 60%, and wet-process arsenic removal also has the problems of waste acid and wastewater pollution and the like.
Therefore, those skilled in the art have made efforts to develop a method that can extract arsenic, tungsten, germanium in stages.
Disclosure of Invention
In view of the above defects in the prior art, the technical problem to be solved by the invention is that the invention overcomes the problems of complex process, low recovery rate and large output of waste acid and wastewater in the traditional wet method precious metal recovery process. In order to achieve the aim, the invention provides a sectional separation, enrichment and extraction method of waste containing arsenic, tungsten and germanium, which is characterized by comprising the following steps of: step 1, grinding and mixing waste containing arsenic, tungsten and germanium and any combination of ferrous phosphide, phosphorus oxide, ferrous sulfide, sulfur, activated carbon powder and coke powder according to a certain proportion to ensure that the materials are fully contacted to obtain a mixed material, and adding water into the mixed material for granulation to obtain a mixed pellet; and 2, placing the mixed pellets in a vacuum smelting furnace, and performing separation treatment according to the conditions of multi-stage temperature rise, temperature reduction and vacuum degree.
Further, the waste containing arsenic, tungsten and germanium in the step 1 is one of lignite smoke dust, fly ash and tailings.
Further, the proportioning in step 1 is that the contents of the ferrous phosphide, the phosphorus oxide, the ferrous sulfide, the sulfur, the activated carbon powder and the coke powder relative to the arsenic, the tungsten and the germanium waste are respectively 0-20 wt.%, 0-15 wt.%, 0-20 wt.%, 0-25 wt.%, 0-40 wt.% and 0-40 wt.%.
Further, the step 2 further comprises the following steps: step 2.1, raising the temperature in the furnace to 200-2-104Pa, raising the temperature in the furnace to 350-500 ℃, maintaining for 3-5h, volatilizing and separating out oxides, sulfides and phosphides of arsenic, and obtaining residue rich in germanium and tungsten; 2.2, increasing the temperature in the furnace to 800-; and 2.3, adding the residual residues into a smelting furnace, adding any combination of sodium chlorate, calcium chloride, calcium carbonate, magnesium chloride, sodium fluoride, calcium fluoride and potassium tungstate, and performing high-temperature electrochemical fusion deposition to obtain tungsten.
Further, the maintaining time of the step 2.1 is 2-3 h.
Further, the maintaining time of the step 2.2 is 1-5 h.
Further, in step 2.2, the vacuum state is 0.01-100 Pa.
Further, step 2.3 the sodium chlorate, calcium chloride, calcium carbonate, magnesium chloride, sodium fluoride, calcium fluoride, potassium tungstate are added in an amount of 0-40 wt.%, 0-20 wt.%, 0-30 wt.%, 0-5 wt.% of the arsenic, tungsten, germanium waste, respectively.
Further, the high temperature in step 2.3 is 400-900 ℃.
Further, the electrochemical fused deposition potential of the step 2.3 is-1V-1.5V.
The invention has the following technical effects:
1) the waste containing arsenic, tungsten and germanium is separated and recycled step by step, and the final residue is not a dangerous waste and can be recycled, so that the method has the characteristics of high efficiency, environmental protection and high recycling degree, and is suitable for large-scale industrial application;
2) the recovery rate and the enrichment rate of rare metals are high. The recovery rate of the rare metals exceeds 98%, and the enrichment rate exceeds 20-40 times that of the rare metals recovered by the traditional wet method;
3) the treatment process is clean and does not discharge any toxic and harmful substances to the environment. The final residue is not hazardous waste and can enter a general industrial waste landfill;
4) the whole process is applied to enrichment and separation of rare metals, and the process flow is simple and easy to operate and realize.
The conception, the specific structure and the technical effects of the present invention will be further described with reference to the accompanying drawings to fully understand the objects, the features and the effects of the present invention.
Drawings
FIG. 1 is a process flow diagram of a preferred embodiment of the present invention.
Detailed Description
The technical contents of the preferred embodiments of the present invention will be more clearly and easily understood by referring to the drawings attached to the specification. The present invention may be embodied in many different forms of embodiments and the scope of the invention is not limited to the embodiments set forth herein.
Example 1
As shown in fig. 1, 50g of waste (brown coal dust, fly ash, tailings, etc.) powder containing arsenic, tungsten and germanium is first added with 10 wt.% of ferrous phosphide, 15 wt.% of phosphorus oxide, 20 wt.% of ferrous sulfide, 15 wt.% of sulfur, 40 wt.% of activated carbon powder and 10 wt.% of coke powder based on the mass of the waste powder, and then ground and mixed, so that the materials are fully contacted, and a mixed material is obtained. And adding water into the mixed material for granulation to obtain mixed pellets. And (3) placing the mixed powder in a vacuum smelting furnace, and carrying out separation treatment under the conditions of multi-stage temperature rise, temperature reduction and vacuum degree. And (3) raising the temperature in the furnace to 350 ℃ under normal pressure, maintaining for 3 hours, vacuumizing the vacuum furnace after the mixed materials are fully reacted, maintaining the pressure in the furnace at 1000Pa, raising the temperature in the furnace to 450 ℃, and volatilizing and separating arsenic oxide, sulfide, phosphide and the like to obtain the residue rich in germanium and tungsten. Raising the temperature in the furnace to 950 ℃, performing secondary volatilization on the germanium and tungsten-rich residues enriched in the vacuum smelting furnace, reducing the pressure in the vacuum furnace to 1Pa in a vacuum state, maintaining for 4 hours, and volatilizing and separating germanium metal, germanium oxide and phosphide to obtain residual residues. And (4) dissolving the volatile germanium and the oxide thereof by using acid, and hydrolyzing to obtain pure germanium. And (3) dissolving the residual residue by hydrochloric acid, and adding 20 wt.% of sodium chlorate, 10 wt.% of calcium chloride, 20 wt.% of calcium carbonate, 15 wt.% of sodium fluoride, 10 wt.% of calcium fluoride and 5 wt.% of potassium tungstate according to the mass of tungsten in the residue to perform high-temperature melting-electrochemical fractional deposition on tungsten, wherein the melting temperature is controlled at 750 ℃, and the deposition potential is 1.5V, so as to obtain a tungsten product.
Example 2
Firstly, 1kg of waste (lignite smoke dust, fly ash, tailings and the like) powder containing arsenic, tungsten and germanium is ground and mixed by adding 10 wt.% of ferrous phosphide, 20 wt.% of phosphorus oxide, 10 wt.% of ferrous sulfide, 15 wt.% of sulfur, 20 wt.% of activated carbon powder and 20 wt.% of coke powder based on the mass of the waste powder, so that the materials are fully contacted to obtain a mixed material. And adding water into the mixed material for granulation to obtain mixed pellets. And (3) placing the mixed powder in a vacuum smelting furnace, and carrying out separation treatment under the conditions of multi-stage temperature rise, temperature reduction and vacuum degree. And (3) raising the temperature in the furnace to 300 ℃ under normal pressure, maintaining for 4 hours, vacuumizing the vacuum furnace after the mixed materials are fully reacted, maintaining the pressure in the furnace at 10000Pa, raising the temperature in the furnace to 450 ℃, and volatilizing and separating arsenic oxide, sulfide and phosphide to obtain the residue rich in germanium and tungsten. Raising the temperature in the furnace to 950 ℃, performing secondary volatilization on the germanium and tungsten-rich residues enriched in the vacuum smelting furnace, reducing the pressure in the vacuum furnace to 100Pa in a vacuum state, maintaining for 4 hours, and volatilizing and separating germanium metal, germanium oxide and phosphide to obtain residual residues. And (4) dissolving the volatile germanium and the oxide thereof by using acid, and hydrolyzing to obtain pure germanium. And (3) dissolving the residual residues by hydrochloric acid, adding 20 wt% of sodium chlorate, 20 wt% of calcium chloride, 10 wt% of sodium fluoride, 10 wt% of calcium fluoride and 5 wt% of potassium tungstate according to the mass of tungsten in the residues, and performing high-temperature melting-electrochemical fractional deposition to obtain tungsten under the conditions that the melting temperature is controlled at 850 ℃ and the deposition potential is 1.3V, thereby obtaining a tungsten product.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (10)
1. A sectional separation, enrichment and extraction method of waste containing arsenic, tungsten and germanium is characterized by comprising the following steps:
step 1, grinding and mixing waste containing arsenic, tungsten and germanium and any combination of ferrous phosphide, phosphorus oxide, ferrous sulfide, sulfur, activated carbon powder and coke powder according to a certain proportion to ensure that the materials are fully contacted to obtain a mixed material, and adding water into the mixed material for granulation to obtain a mixed pellet;
and 2, placing the mixed pellets in a vacuum smelting furnace, and performing separation treatment according to the conditions of multi-stage temperature rise, temperature reduction and vacuum degree.
2. The method for fractional separation, enrichment and extraction of arsenic, tungsten and germanium containing waste as claimed in claim 1, characterized in that the arsenic, tungsten and germanium containing waste of step 1 is one of lignite soot, fly ash and tailings.
3. The method for fractional separation, enrichment and extraction of arsenic, tungsten and germanium containing waste as claimed in claim 1, wherein the proportioning in step 1 is that the content of the ferrous phosphide, the phosphorus oxide, the ferrous sulfide, the sulfur, the activated carbon powder and the coke powder is 0-20 wt.%, 0-15 wt.%, 0-20 wt.%, 0-25 wt.%, 0-40 wt.% and 0-40 wt.%, respectively, relative to the arsenic, tungsten and germanium containing waste.
4. The method for the fractional separation, enrichment and extraction of arsenic, tungsten and germanium containing waste as claimed in claim 1, characterized in that said step 2 further comprises the following steps:
step 2.1, raising the temperature in the furnace to 200-2-104Pa, raising the temperature in the furnace to 350-500 ℃, maintaining for 3-5h, volatilizing and separating out oxides, sulfides and phosphides of arsenic, and obtaining residue rich in germanium and tungsten;
2.2, increasing the temperature in the furnace to 800-;
and 2.3, adding the residual residues into a smelting furnace, adding any combination of sodium chlorate, calcium chloride, calcium carbonate, magnesium chloride, sodium fluoride, calcium fluoride and potassium tungstate, and performing high-temperature electrochemical fusion deposition to obtain tungsten.
5. The method for fractional separation, enrichment and extraction of arsenic, tungsten, germanium containing waste according to claim 4, characterised in that step 2.1 is maintained for a period of time comprised between 2 and 3 hours.
6. The method for fractional separation, enrichment and extraction of arsenic, tungsten, germanium containing waste according to claim 4, characterised in that step 2.2 is maintained for a period of 1-5 hours.
7. The method for fractional separation, enrichment and extraction of arsenic, tungsten, germanium containing waste according to claim 4, characterised in that step 2.2 the vacuum state is 0.01-100 Pa.
8. The process for fractional separation, enrichment and extraction of arsenic, tungsten and germanium containing waste as claimed in claim 4, characterized in that step 2.3 the sodium chlorate, calcium chloride, calcium carbonate, magnesium chloride, sodium fluoride, calcium fluoride, potassium tungstate are added in amounts of 0-40 wt.%, 0-20 wt.%, 0-30 wt.%, 0-5 wt.% of the arsenic, tungsten, germanium waste, respectively.
9. The method as claimed in claim 4, wherein the step 2.3 comprises a step of high temperature of 400-900 ℃.
10. The method for fractional separation, enrichment and extraction of arsenic, tungsten and germanium containing waste as claimed in claim 4, characterized in that step 2.3 the electrochemical fused deposition potential is between-1V and 1.5V.
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Cited By (2)
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| 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 |
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Application publication date: 20200825 |