CN112662898A - Method for efficiently extracting germanium from zinc-germanium leaching solution - Google Patents
Method for efficiently extracting germanium from zinc-germanium leaching solution Download PDFInfo
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- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 229910052732 germanium Inorganic materials 0.000 title claims abstract description 79
- MRZMQYCKIIJOSW-UHFFFAOYSA-N germanium zinc Chemical compound [Zn].[Ge] MRZMQYCKIIJOSW-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000002386 leaching Methods 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 27
- 229920001864 tannin Polymers 0.000 claims abstract description 76
- 235000018553 tannin Nutrition 0.000 claims abstract description 76
- 239000001648 tannin Substances 0.000 claims abstract description 76
- 239000007788 liquid Substances 0.000 claims abstract description 21
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000001263 FEMA 3042 Substances 0.000 claims abstract description 17
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims abstract description 17
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims abstract description 17
- 229940033123 tannic acid Drugs 0.000 claims abstract description 17
- 235000015523 tannic acid Nutrition 0.000 claims abstract description 17
- 229920002258 tannic acid Polymers 0.000 claims abstract description 17
- 238000001556 precipitation Methods 0.000 claims abstract description 15
- 239000012629 purifying agent Substances 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 6
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 claims description 10
- 239000002893 slag Substances 0.000 claims description 8
- 235000011437 Amygdalus communis Nutrition 0.000 claims description 5
- 241000218652 Larix Species 0.000 claims description 5
- 235000005590 Larix decidua Nutrition 0.000 claims description 5
- 241000220304 Prunus dulcis Species 0.000 claims description 5
- 235000020224 almond Nutrition 0.000 claims description 5
- 210000000051 wattle Anatomy 0.000 claims description 5
- 239000011347 resin Substances 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 4
- 239000012535 impurity Substances 0.000 abstract description 10
- 150000002500 ions Chemical class 0.000 abstract description 8
- 238000000605 extraction Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 239000000706 filtrate Substances 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract description 2
- 238000009854 hydrometallurgy Methods 0.000 abstract description 2
- 238000009856 non-ferrous metallurgy Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 20
- 239000011701 zinc Substances 0.000 description 12
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 6
- 229910052785 arsenic Inorganic materials 0.000 description 6
- 238000009616 inductively coupled plasma Methods 0.000 description 6
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- 229910052725 zinc Inorganic materials 0.000 description 5
- 230000008021 deposition Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000000349 field-emission scanning electron micrograph Methods 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000011549 displacement method Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- -1 solar cell Substances 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 229920002253 Tannate Polymers 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- JQJCSZOEVBFDKO-UHFFFAOYSA-N lead zinc Chemical compound [Zn].[Pb] JQJCSZOEVBFDKO-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000004065 semiconductor Substances 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
- 239000011787 zinc oxide Substances 0.000 description 1
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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 relates to a method for efficiently extracting germanium from zinc-germanium leaching solution, belonging to the technical field of hydrometallurgy in nonferrous metallurgy. Adding a purifying agent into a zinc-germanium leaching solution, reacting for 10-20 min under the condition of stirring to obtain a solution system A, and carrying out solid-liquid separation to obtain a solution B; adding tannin extract into the solution B, reacting for 1-10 min under the stirring condition, slowly adding tannic acid, reacting for 10-20 min to obtain a system C, performing solid-liquid separation to obtain germanium precipitation liquid and tannin germanium residues, and washing the tannin germanium residues to obtain tannin germanium. According to the invention, a purifying agent is added to react with impurity ions to generate insoluble substances, filtrate with high germanium content and low impurity element content is obtained by filtering, germanium is sequentially precipitated after tannin extract and tannic acid are added, the germanium precipitation rate reaches 98.9%, the germanium content in the tannin germanium reaches 5%, the purity of the tannin germanium is improved, the tannin extract is lower in price, the production cost is reduced, and the existing germanium precipitation process can be obviously optimized. The method has the characteristics of low labor intensity, high germanium extraction rate and low production cost.
Description
Technical Field
The invention relates to a method for efficiently extracting germanium from zinc-germanium leaching solution, belonging to the technical field of hydrometallurgy in nonferrous metallurgy.
Background
Germanium (Ge) belongs to rare dispersion metal, is extremely dispersed in the crust, is mainly associated with bauxite, lead-zinc ore and coal mine, is the most important semiconductor material except silicon, is widely used in the fields of optical fiber, solar cell, medicine, catalyst and the like, is also an indispensable important metal in the fields of national defense aviation, space development and the like, and is an important strategic reserve resource in China. At present, representative enterprises in China mainly extract germanium from leachate obtained by acid leaching of zinc smelting byproducts, and the main methods comprise a zinc powder displacement method, an extraction method and a tannin precipitation method, wherein the zinc powder displacement and extraction method have the defects of environmental pollution, high price of an extracting agent, incapability of recycling and the like, so the tannin precipitation method is widely applied at present. However, tannic acid reacts with other impurity ions such as iron and arsenic, so that the consumption of tannic acid is increased, the grade of germanium concentrate is influenced, and the cost of tannic acid is high (5.5 ten thousand per ton), so that the optimization of the germanium precipitation process is more important.
Disclosure of Invention
The invention provides a method for efficiently extracting germanium from zinc-germanium leachate aiming at the problems of more impurity metals, high tannin dosage and the like in the prior art.
A method for efficiently extracting germanium from zinc-germanium leaching solution comprises the following specific steps:
(1) adding a purifying agent into the zinc-germanium leaching solution, reacting for 10-20 min under the condition of stirring to obtain a solution system A, and carrying out solid-liquid separation to obtain a solution B;
(2) adding tannin extract into the solution B obtained in the step (1), reacting for 1-10 min under the stirring condition, slowly adding tannic acid, reacting for 10-20 min to obtain a system C, performing solid-liquid separation to obtain germanium precipitation liquid and tannin germanium slag, and washing the tannin germanium slag to obtain tannin germanium;
the purifying agent in the step (1) is catechol, biochar or D001 resin, and the adding amount of the purifying agent is 5-10 g/L;
the tannin extract in the step (2) is wattle bark, almond bark or larch tannin extract, and the addition amount of the tannin extract is 5-15 times of the mass of germanium in the zinc-germanium leaching solution in the step (1);
preferably, the tannin mass content in the tannin extract is 90-95%;
and (2) adding the tannin in an amount which is 10-20 times of the mass of the germanium in the zinc-germanium leaching solution in the step (1).
Furthermore, the zinc-germanium leachate is leachate after acid leaching of zinc oxide smoke dust containing germanium, and the main component elements comprise Zn, Ge, Fe, Mg and As, wherein Zn is 100-200 g/L, Ge is 50-100 Mg/L, Fe is 5-10 g/L, Mg is 60-100 g/L, and As is 0.5-1 g/L.
The invention has the beneficial effects that:
according to the method, the purifying agent can react with impurity ions such as iron and arsenic to form insoluble substances, and the filtrate obtained by filtering is low in impurity ion content and high in germanium content, so that the complexing of the impurity ions and tannin can be reduced, the using amount of tannic acid is reduced, and the purity of tannin and germanium can be improved; the tannin extract and the tannic acid of different types are added in the process of tannin germanium precipitation, and the cost of the tannin extract is lower than that of the tannic acid, and the tannin extract and the tannic acid are added discontinuously, so that the tannin and the germanium are fully complexed, and the germanium precipitation rate is improved.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is an FE-SEM image (3000 times) of germanium tannin of example 3;
FIG. 3 is an FE-SEM image (10000 times) of germanium tannate of example 3;
FIG. 4 is a distribution diagram of the particle size of germanium tannin of example 3.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
Example 1: a method for efficiently extracting germanium from zinc-germanium leachate (see figure 1) comprises the following steps:
(1) adding a purifying agent (catechol) into the zinc-germanium leaching solution, reacting for 10min under stirring to precipitate impurity ions such as arsenic, iron and the like with the catechol to obtain a solution system A, and carrying out solid-liquid separation to obtain a solution B; wherein the zinc content in the zinc-germanium leaching solution is 100g/L, the Ge content is 50Mg/L, the Fe content is 5g/L, the Mg content is 60g/L, the As content is 0.5g/L, and the addition amount of a purifying agent (catechol) is 5 g/L; the pH value of the solution system A is 1; the Zn content in the solution B is 98.9g/L, the Ge content is 49.5Mg/L, the Fe content is 2.1g/L, the Mg content is 59.3g/L, the As content is 0.2g/L, and the pH value of the solution system B is 1;
(2) adding tannin extract (wattle bark tannin extract) into the solution B in the step (1), reacting for 1min under stirring, slowly adding tannic acid at a constant speed within 30s, reacting for 10min to obtain a system C, performing solid-liquid separation to obtain germanium precipitation liquid and tannin germanium residue, and washing the tannin germanium residue to obtain tannin germanium; wherein the tannin content in the tannin extract (wattle bark tannin extract) is 90 percent, the addition amount of the tannin extract (wattle bark tannin extract) is 5 times of the mass of germanium in the zinc-germanium leaching solution in the step (1), and the addition amount of tannic acid is 10 times of the mass of germanium in the zinc-germanium leaching solution in the step (1);
the liquid after germanium deposition is detected by adopting an ICP (inductively coupled plasma generator) to obtain:
Ge 3.5mg/L；Zn 97.7g/L；Fe 1.23g/L；Mg 55.4g/L；As 0.05g/L；
in the embodiment, the germanium precipitation rate is 83.5%, and the germanium content in the tannin germanium reaches 3.5%.
Example 2: a method for efficiently extracting germanium from zinc-germanium leachate (see figure 1) comprises the following steps:
(1) adding a purifying agent (biochar) into the zinc-germanium leaching solution, reacting for 15min under stirring to enable impurity ions such as arsenic and iron to be adsorbed and precipitated with the biochar to obtain a solution system A, and carrying out solid-liquid separation to obtain a solution B; wherein the zinc content in the zinc-germanium leaching solution is 150g/L, the Ge content is 75Mg/L, the Fe content is 7.5g/L, the Mg content is 80g/L, the As content is 0.75g/L, and the addition amount of a purifying agent (biochar) is 7.5 g/L; the pH value of the solution system A is 1.5; the Zn content in the solution B is 149.2g/L, the Ge content is 74.5Mg/L, the Fe content is 3.8g/L, the Mg content is 79.3g/L, and the As content is 0.28 g/L; the pH value of the solution system B is 1.5;
(2) adding tannin extract (almond skin tannin extract) into the solution B in the step (1), reacting for 5min under stirring, slowly adding tannic acid at a constant speed within 45s, reacting for 15min to obtain a system C, performing solid-liquid separation to obtain germanium precipitation liquid and tannin germanium slag, and washing the tannin germanium slag to obtain tannin germanium; wherein the tannin content in the tannin extract (almond skin tannin extract) is 92.5 percent, the addition amount of the tannin extract (almond skin tannin extract) is 10 times of the mass of germanium in the zinc-germanium leaching solution in the step (1), and the addition amount of tannic acid is 15 times of the mass of germanium in the zinc-germanium leaching solution in the step (1);
the liquid after germanium deposition is detected by adopting an ICP (inductively coupled plasma generator) to obtain:
Ge 1.84mg/L；Zn 138.30g/L；Fe 1.31g/L；Mg 69.7g/L；As 0.1g/L；
in the embodiment, the germanium precipitation rate is 93.4%, and the germanium content in the tannin germanium reaches 4.25%.
Example 3: a method for efficiently extracting germanium from zinc-germanium leachate (see figure 1) comprises the following steps:
(1) adding a purifying agent (D001 resin) into the zinc-germanium leaching solution, reacting for 20min under stirring to allow impurity ions such as arsenic and iron to be adsorbed and precipitated with charcoal to obtain a solution system A, and performing solid-liquid separation to obtain a solution B; wherein the zinc content in the zinc-germanium leaching solution is 200g/L, the Ge content is 100Mg/L, the Fe content is 10g/L, the Mg content is 100g/L, the As content is 1g/L, and the addition amount of a purifying agent (D001 resin) is 10.0 g/L; the pH value of the solution system A is 3.0; the Zn content in the solution B is 199.3g/L, the Ge content is 99.5Mg/L, the Fe content is 3.2g/L, the Mg content is 99.6g/L, and the As content is 0.23 g/L; the pH value of the solution system A is 3.0;
(2) adding tannin extract (larch tannin extract) into the solution B in the step (1), reacting for 10min under the stirring condition, slowly adding tannic acid at a constant speed within 60s, reacting for 15min to obtain a system C, performing solid-liquid separation to obtain germanium-precipitated liquid and tannin germanium slag, and washing the tannin germanium slag to obtain tannin germanium; wherein the tannin content in the tannin extract (larch tannin extract) is 95%, the addition amount of the tannin extract (larch tannin extract) is 15 times of the mass of germanium in the zinc-germanium leaching solution in the step (1), and the addition amount of tannic acid is 20 times of the mass of germanium in the zinc-germanium leaching solution in the step (1);
the liquid after germanium deposition is detected by adopting an ICP (inductively coupled plasma generator) to obtain:
Ge 0.7mg/L；Zn 186.4g/L；Fe 2.46g/L；；Mg 88.4g/L；As 0.12g/L；
in the embodiment, the germanium precipitation rate is 98.9%, and the germanium content in the tannin germanium reaches 5%;
the FE-SEM image and the particle size distribution diagram of the tannin germanium in the embodiment are shown in FIGS. 2-4, and it can be seen from FIGS. 2-4 that:
the tannin germanium is irregular block-shaped substance formed by agglomeration of three-dimensional spheres, and the particle diameter of the tannin germanium is about 39.481 μm.
Claims (5)
1. A method for efficiently extracting germanium from a zinc-germanium leaching solution is characterized by comprising the following specific steps:
(1) adding a purifying agent into the zinc-germanium leaching solution, reacting for 10-20 min under the condition of stirring to obtain a solution system A, and carrying out solid-liquid separation to obtain a solution B;
(2) adding tannin extract into the solution B in the step (1), reacting for 1-10 min under the stirring condition, slowly adding tannic acid, reacting for 10-20 min to obtain a system C, performing solid-liquid separation to obtain germanium precipitation liquid and tannin germanium slag, and washing the tannin germanium slag to obtain tannin germanium.
2. The method for efficiently extracting germanium from a zinc-germanium leachate according to claim 1, wherein the method comprises the following steps: the purifying agent in the step (1) is catechol, biochar or D001 resin, and the adding amount of the purifying agent is 5-10 g/L.
3. The method for efficiently extracting germanium from a zinc-germanium leachate according to claim 1, wherein the method comprises the following steps: the tannin extract in the step (2) is wattle bark, almond bark or larch tannin extract, and the addition amount of the tannin extract is 5-15 times of the mass of germanium in the zinc-germanium leaching solution in the step (1).
4. The method for efficiently extracting germanium from a zinc-germanium leachate according to claim 3, wherein the method comprises the following steps: the tannin mass content in the tannin extract is 90-95%.
5. The method for efficiently extracting germanium from a zinc-germanium leachate according to claim 1, wherein the method comprises the following steps: and (2) adding tannin in an amount which is 10-20 times of the mass of germanium in the zinc-germanium leaching solution in the step (1).
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Cited By (4)
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| CN113355535A (en) * | 2021-06-03 | 2021-09-07 | 昆明理工大学 | Method and device for purifying tannin germanium slag by combining ultrasonic wave with air floatation method |
| CN114672673A (en) * | 2022-03-09 | 2022-06-28 | 昆明理工大学 | Method for circularly precipitating germanium by using tannic acid |
| CN115109929A (en) * | 2022-01-21 | 2022-09-27 | 昆明理工大学 | Method for directly preparing coarse germanium dioxide from tannin germanium slag |
| CN115537584A (en) * | 2022-11-29 | 2022-12-30 | 昆明理工大学 | Method for strengthening tannin germanium precipitation through ultrasonic and tannic acid modification |
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