CN108048672B - Extraction furnace and extraction method for extracting germanium in low-grade germanium concentrate by thermal reduction and volatilization - Google Patents
Extraction furnace and extraction method for extracting germanium in low-grade germanium concentrate by thermal reduction and volatilization Download PDFInfo
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- CN108048672B CN108048672B CN201810115436.3A CN201810115436A CN108048672B CN 108048672 B CN108048672 B CN 108048672B CN 201810115436 A CN201810115436 A CN 201810115436A CN 108048672 B CN108048672 B CN 108048672B
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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
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/06—Dry methods smelting of sulfides or formation of mattes by carbides or the like
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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
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/16—Dry methods smelting of sulfides or formation of mattes with volatilisation or condensation of the metal being produced
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Abstract
An extraction furnace and an extraction method for extracting germanium in low-grade germanium concentrate by thermal reduction volatilization, in particular to an extraction furnace and an extraction method for extracting germanium in low-grade germanium concentrate by adopting a high-temperature thermal reduction volatilization method. The extraction furnace comprises a volatilizing furnace, a cooler and a dust collector which are sequentially connected, wherein the volatilizing furnace comprises a shell, a furnace body, a partition plate, a guide rail, heat insulation cotton and heating resistance wires, the shell is sleeved outside the furnace body, the heat insulation cotton is filled in a gap between the shell and the furnace body, and the heating resistance wires are arranged on the outer wall of the furnace body; the two partition boards are vertically fixed on the top inner wall of the furnace body, divide the interior of the furnace body into three parts, and respectively comprise a preheating area, a high-temperature constant-temperature area and a cooling area from front to back; the guide rail is arranged in the middle of the furnace body at a lower position. According to the invention, the three-section germanium extraction furnace is adopted, the germanium extraction flow is optimized, the heat loss is reduced, the enrichment multiple of germanium ore smelting and the grade of germanium concentrate are improved, the grade of the obtained germanium concentrate is high and can reach more than 20%, and the subsequent process is facilitated.
Description
Technical Field
The invention relates to germanium recovery and extraction equipment, in particular to an extraction furnace and an extraction method for extracting germanium in low-grade germanium concentrate by adopting a high-temperature thermal reduction volatilization method.
Background
In recent years, along with continuous exploitation of germanium ore resources, high-quality germanium ores are reduced, the content of germanium is continuously reduced, and the grade of germanium concentrate obtained by traditional pyrometallurgical equipment, technology and technology is reduced, and is generally in the range of 0.5% -2%. The current treatment process for germanium ore at home and abroad mainly comprises the following steps: ion exchange method, liquid membrane extraction method, classical chlorination method, zinc powder displacement method, tannin precipitation method, etc. The method for extracting germanium from coal is classified into fire smelting method, water smelting method and extraction method. The hydrometallurgy method is to directly extract germanium from coal, has simple process, but high consumption of hydrochloric acid and high industrialization cost; extraction is limited by few efficient extractants, which are expensive, and is mainly Lix63, kelexl100, TOA, ywl, etc. Some foreign enterprises mainly adopt medium-temperature or high-temperature carbonization coal to extract germanium in lignite, so that germanium compounds are volatilized and enriched in tar, and then germanium is extracted by a wet method; the research of Beijing mining and metallurgy institute develops a process for extracting and recovering germanium by using the HGS98 germanium extractant; zinc powder replacement method is adopted in plant smelting plants to comprehensively recover germanium; the Hoboken company of belgium has studied the process of reducing volatilisation germanium extraction in a shaft furnace. However, in the above process method and research, the grade of the commonly obtained germanium concentrate is low, the enrichment multiple of the germanium concentrate is not high, the recovery rate of the germanium extraction by chlorination in the back-end process is low, the production cost is high, and the three wastes are generated: the problem of high harmless treatment pressure of residual acid, residues and waste gas.
The U.S. patent office discloses a process for direct carbonization of coal at temperatures above 800 ℃ to volatilize and enrich germanium compounds in tar, followed by extraction of germanium from the coal by solvent extraction and co-precipitation. In addition, the patent application of Tokyo corporation in Japan also adopts a carbonization method to extract germanium, and the technology mainly relates to electrostatic separation of ligneous parts of lignite, carbonization and germanium enrichment and the like.
Disclosure of Invention
The invention aims to solve the problems existing in the existing germanium ore treatment, and provides an extraction furnace and an extraction method for extracting germanium in low-grade germanium concentrate by adopting a high-temperature thermal reduction volatilization method.
The invention relates to an extraction furnace for extracting germanium in low-grade germanium concentrate by thermal reduction volatilization, which is characterized by comprising a volatilization furnace, a cooler and a dust collector which are sequentially connected, wherein the volatilization furnace comprises a shell, a furnace body, a partition plate, a guide rail, heat insulation cotton and heating resistance wires, the shell is sleeved outside the furnace body, the heat insulation cotton is filled in a gap between the shell and the furnace body, and the heating resistance wires are arranged on the outer wall of the furnace body; the two partition boards are vertically fixed on the top inner wall of the furnace body, divide the interior of the furnace body into three parts, and respectively comprise a preheating area, a high-temperature constant-temperature area and a cooling area from front to back; the guide rail is arranged in the middle of the furnace body at a lower position, the height of the guide rail is lower than the lowest point of the partition plate, a tray filled with low-grade lignite germanium concentrate is placed on the guide rail, and the tray slides on the guide rail.
The cooler is also provided with a volatile gas collecting pipe, the cooler is connected with the furnace body through the volatile gas collecting pipe, and an air inlet of the volatile gas collecting pipe is fixed at the top of the furnace body in the high-temperature constant-temperature area.
The lower part of the furnace body is also provided with an air inlet through which inert gas is filled into the furnace body.
The extraction method for extracting germanium in low-grade germanium concentrate by thermal reduction and volatilization is characterized by comprising the following steps of:
1) Argon is filled into the furnace body through the air inlet hole and continuously introduced for 30 minutes, and the air flow is 240-300m 3 And/h, filling argon into the furnace body completely;
2) Uniformly mixing low-grade lignite germanium concentrate and potassium borohydride, spreading the mixture into a material tray, placing the material tray on a guide rail, and feeding the material tray into a furnace body from an inlet of the furnace body;
3) Pushing the material tray into a preheating zone through a guide rail for preheating, wherein the temperature of the preheating zone is 300-500 ℃, and the preheating time is 1 hour;
4) The preheated material tray enters a high-temperature constant-temperature region again through a guide rail, and is subjected to high Wen Zhe reduction volatilization at 1100-1150 ℃ for 2 hours;
5) The volatilized germanium-containing smoke dust enters a cooler through a volatilized gas collecting pipe to be cooled;
6) Cooling the germanium-containing smoke dust to 200 ℃, then entering a dust collector, and filtering, collecting dust and enriching through a cloth bag to obtain high-grade germanium concentrate with the germanium content of more than 20%;
7) And 4) feeding the material tray after the germanium is volatilized at the high temperature in the step 4) into a cooling area through a track for cooling.
In the step 2), 7.5-10 parts by mass of potassium borohydride is added to every 100 parts by mass of low-grade germanium concentrate.
The performance of the invention is measured: determining germanium content by potassium iodate titration method, firstly adopting H 3 PO 4 + KMnO 4 Decomposing smoke germanium concentrate; adding hydrochloric acid for distillation, wherein the initial acidity is strictly controlled at 6mol/L; when the germanium content in the germanium concentrate is measured, 100mL of 6mol/L hydrochloric acid solution is used for receiving the distilled liquid, and sodium hypophosphite can be used for reduction measurement after 2/3 of distilled liquid is distilled out.
Compared with the prior art, the invention has the beneficial effects that:
(1) The novel designed three-section germanium extracting furnace is adopted, the germanium extracting flow is optimized through the three-section structural design, the heat in the furnace is utilized to the maximum extent, the heat loss is reduced, and the energy saving, emission reduction and high-efficiency recycling of germanium extracting are realized;
(2) The reduction volatilizing germanium extraction process of the argon, potassium borohydride and three-section germanium extraction furnace improves the enrichment factor of germanium ore smelting and the grade of germanium concentrate, solves the problems that the recovery rate of germanium extraction by chlorination in the subsequent process is reduced, the production cost is greatly increased, and the generated three wastes: the problem of high pressure of innocent treatment of residual acid, residues and waste gas;
(3) The introduction of the inert gas argon is used as the carrier gas of volatile components, so that the problems that germanium smoke dust is easy to adhere to the pipe wall and block in the cooling pipeline in the traditional dust collection system are effectively solved, and meanwhile, the inert gas atmosphere is formed to isolateAir, prevents the generated CeO from being oxidized into CeO 2 ；
(4) The introduction of the reducing agent potassium borohydride solves the defect that the C in the lignite is used as the reducing agent in the germanium ore lignite, so that germanium cannot be reduced to the maximum extent to be volatilized into CeO;
(5) The obtained germanium concentrate has high grade which can reach more than 20 percent, and is favorable for the process of extracting germanium by the rear end further wet method.
Drawings
FIG. 1 is a schematic view of the structure of the extraction furnace of the present invention.
FIG. 2 is a schematic diagram of a cross-sectional structure of an extraction furnace according to the present invention.
FIG. 3 is a schematic diagram of the end face structure of the extraction furnace according to the present invention.
FIG. 4 is a schematic process diagram of the extraction method of the present invention.
The device comprises a cooler 1, a dust collector 2, a shell 3, a furnace body 4, a partition board 5, a guide rail 6, heat insulation cotton 7, a heating resistance wire 8, a preheating zone 9, a high-temperature constant-temperature zone 10, a cooling zone 11, a volatile gas collecting pipe 12 and an air inlet hole 13.
Detailed Description
Example 1: the utility model provides an extraction furnace of germanium in low-grade germanium concentrate is volatilized in thermal reduction, includes volatilize stove, cooler 1 and dust collector 2 that connect in proper order, volatilize the stove including shell 3, furnace body 4, baffle 5, guide rail 6, thermal-insulated cotton 7 and heating resistance wire 8, shell 3 suit is outside furnace body 4, thermal-insulated cotton 7 fills in the clearance between shell 3 and the furnace body 4, heating resistance wire 8 sets up on furnace body 4 outer wall; the two partition boards 5 are vertically fixed on the top inner wall of the furnace body 4, divide the interior of the furnace body 4 into three parts, and respectively comprise a preheating area 9, a high-temperature constant-temperature area 10 and a cooling area 11 from front to back; the guide rail 6 is arranged in the middle of the furnace body 4 and is lower than the lowest point of the partition plate 5, a tray filled with low-grade lignite germanium concentrate is placed on the guide rail 6, and the tray slides on the guide rail 6. The cooler 1 is also provided with a volatile gas collecting pipe 12, the cooler 1 is connected with the furnace body 4 through the volatile gas collecting pipe 12, and an air inlet of the volatile gas collecting pipe 12 is fixed at the top of the furnace body 4 in the high-temperature constant-temperature region 10. The lower part of the furnace body 4 is also provided with an air inlet hole 13, and inert gas is filled into the furnace body 4 through the air inlet hole 13.
The extraction method for extracting germanium in low-grade germanium concentrate by thermal reduction and volatilization comprises the following steps:
1) Argon is filled into the furnace body 4 through the air inlet hole 13 and continuously introduced for 30 minutes, and the air flow is 240-300m 3 And/h, filling argon into the furnace body 4;
2) Uniformly mixing low-grade lignite germanium concentrate and potassium borohydride, spreading the mixture into a material tray, adding 7.5-10 parts by mass of potassium borohydride into every 100 parts by mass of low-grade germanium concentrate, placing the material tray on a guide rail 6, and feeding the material tray into a hearth from an inlet of a furnace body 4 through a push rod;
3) Pushing the material tray into a preheating zone 9 for preheating, wherein the temperature in the preheating zone 9 is 300-500 ℃, and the preheating time is 1 hour;
4) Pushing the preheated material tray into a high-temperature constant-temperature region 10 through a guide rail 6, and carrying out high-temperature reduction and volatilization of germanium at 1100-1150 ℃ for 2 hours;
5) The reduced and volatilized germanium-containing smoke dust enters the cooler 1 through the volatilized gas collecting pipe 12 for cooling;
6) After the germanium-containing smoke dust is cooled to 200 ℃, the smoke dust enters a bag dust collector 2, dust collection and enrichment are carried out, and high-grade germanium concentrate with the germanium content of more than 20% is obtained;
7) The material tray after the high-temperature volatilization in the step 4) enters a cooling zone 11 through a track to be cooled and then is discharged.
After the potassium borohydride reducing agent is added, the germanium volatilization rate is obviously improved, when the added mass ratio is 8.5%, the germanium volatilization rate reaches the end, the adding amount is continuously increased, and the volatilization rate is hardly continuously increased, so that the optimal adding mass ratio is 8.5%, and experimental data are shown in the following table:
。
some common industrial reducing agents, such as coke, iron powder and the like, have far less reducing effect than potassium borohydride KBH 4 The product potassium borate can also be used as disinfectantIndustrial application, good economic benefit and safety and environmental protection. Experimental data are as follows:
。
argon belongs to single-molecule gas, is relatively more stable and is rarely reacted with metals, and nitrogen is called inert gas only because the bond energy of a nitrogen-nitrogen triple bond is particularly large and is not easy to break for reaction, and the argon and some metals can react slowly; so that argon has more application area and better protection effect than nitrogen. Meanwhile, the relative atomic mass of argon is much larger than that of nitrogen molecules, so that air can be better discharged. The contrast effect of argon and air is as follows:
。
Claims (2)
1. the extraction method is characterized in that the extraction method is based on an extraction furnace, the extraction furnace comprises a volatilization furnace, a cooler (1) and a dust collector (2) which are sequentially connected, the volatilization furnace comprises a shell (3), a furnace body (4), a baffle plate (5), a guide rail (6), heat insulation cotton (7) and heating resistance wires (8), the shell (3) is sleeved outside the furnace body (4), the heat insulation cotton (7) is filled in a gap between the shell (3) and the furnace body (4), and the heating resistance wires (8) are arranged on the outer wall of the furnace body (4); the two partition boards (5) are vertically fixed on the top inner wall of the furnace body (4), divide the interior of the furnace body (4) into three parts, and are respectively a preheating area (9), a high-temperature constant-temperature area (10) and a cooling area (11) from front to back; the guide rail (6) is arranged in the middle of the furnace body (4) and is lower than the lowest point of the partition plate (5), a tray filled with low-grade lignite germanium concentrate is placed on the guide rail (6), and the tray slides on the guide rail (6); the cooler (1) is also provided with a volatile gas collecting pipe (12), the cooler (1) is connected with the furnace body (4) through the volatile gas collecting pipe (12), and an air inlet of the volatile gas collecting pipe (12) is fixed at the top of the furnace body (4) of the high-temperature constant-temperature region (10); the lower part of the furnace body (4) is also provided with an air inlet hole (13), and inert gas is filled into the furnace body (4) through the air inlet hole (13);
the extraction method of the extraction furnace comprises the following steps:
1) Argon is filled into the furnace body (4) through the air inlet hole (13) and continuously introduced for 30 minutes, and the air flow is 240-300m 3 And/h, filling argon into the furnace body (4);
2) Uniformly mixing low-grade lignite germanium concentrate and potassium borohydride, spreading the mixture into a material tray, adding potassium borohydride into every 100 parts by mass of low-grade germanium concentrate, placing the material tray on a guide rail (6), and feeding the material tray into a hearth from an inlet of a furnace body (4) through a push rod;
3) Pushing the material tray into a preheating zone (9) for preheating, wherein the temperature in the preheating zone (9) is 300-500 ℃, and the preheating time is 1 hour;
4) Pushing the preheated material tray into a high-temperature constant-temperature area (10) through a guide rail (6), and carrying out high-temperature reduction and volatilization of germanium at 1100-1150 ℃ for 2 hours;
5) The reduced and volatilized germanium-containing smoke dust enters a cooler (1) through a volatilized gas collecting pipe (12) for cooling;
6) After the germanium-containing smoke dust is cooled to 200 ℃, the smoke dust enters a dust collector (2), dust collection and enrichment are carried out, and high-grade germanium concentrate with the germanium content of more than 20% is obtained;
7) The material tray after the high-temperature volatilization in the step 4) enters a cooling area (11) through a track to be cooled and then is discharged.
2. The method for extracting germanium from low-grade germanium concentrate by thermal reduction and volatilization according to claim 1, wherein in the step 2), 7.5 to 10 parts by mass of potassium borohydride is added per 100 parts by mass of low-grade germanium concentrate.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57205321A (en) * | 1981-06-06 | 1982-12-16 | Nippon Telegr & Teleph Corp <Ntt> | Separating and recovering method for germanium from glass composition containing germanium |
| CN101680054A (en) * | 2007-05-24 | 2010-03-24 | 保尔伍斯股份有限公司 | Method for the valorisation of zinc- and sulphate-rich residue |
| CN102031397A (en) * | 2010-10-25 | 2011-04-27 | 云南天浩稀贵金属股份有限公司 | Method for reducing high-purity germanium dioxide into germanium ingots continuously |
| CN104805316A (en) * | 2015-05-07 | 2015-07-29 | 云南临沧鑫圆锗业股份有限公司 | Method for extracting germanium by thermally reducing and volatilizing germanium ores |
| CN205821424U (en) * | 2016-07-25 | 2016-12-21 | 云南临沧鑫圆锗业股份有限公司 | Dry distilling germanic brown coal volatilizing and enriching extracts germanium device |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10156003B2 (en) * | 2015-05-07 | 2018-12-18 | Yunnan Lincang Xinyuan Germanium Industry Co.,Ltd. | Method of extracting germanium from germanium deposit using thermal reduction process |
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- 2018-02-06 CN CN201810115436.3A patent/CN108048672B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57205321A (en) * | 1981-06-06 | 1982-12-16 | Nippon Telegr & Teleph Corp <Ntt> | Separating and recovering method for germanium from glass composition containing germanium |
| CN101680054A (en) * | 2007-05-24 | 2010-03-24 | 保尔伍斯股份有限公司 | Method for the valorisation of zinc- and sulphate-rich residue |
| CN102031397A (en) * | 2010-10-25 | 2011-04-27 | 云南天浩稀贵金属股份有限公司 | Method for reducing high-purity germanium dioxide into germanium ingots continuously |
| CN104805316A (en) * | 2015-05-07 | 2015-07-29 | 云南临沧鑫圆锗业股份有限公司 | Method for extracting germanium by thermally reducing and volatilizing germanium ores |
| CN205821424U (en) * | 2016-07-25 | 2016-12-21 | 云南临沧鑫圆锗业股份有限公司 | Dry distilling germanic brown coal volatilizing and enriching extracts germanium device |
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