CN115215303A - Method for extracting tellurium dioxide from tellurium copper slag - Google Patents
Method for extracting tellurium dioxide from tellurium copper slag Download PDFInfo
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- C01B19/00—Selenium; Tellurium; Compounds thereof
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Abstract
The invention discloses a method for extracting tellurium dioxide from tellurium copper slag, which relates to the technical field of copper smelting and solves the technical problem of low tellurium recovery rate of the existing purification method, and the method comprises the steps of sequentially carrying out acid leaching, oxidation and filtration on wet tellurium copper slag to obtain acid leaching oxidation filter washing slag and acid leaching oxidation filter washing liquid, then carrying out alkali leaching and filtration on the acid leaching oxidation filter washing slag to obtain alkali leaching filter washing slag and alkali leaching washing liquid, and then carrying out wet purification and drying on the alkali leaching filter washing liquid to obtain tellurium dioxide solid; the method effectively improves the recovery rate of tellurium.
Description
Technical Field
The invention relates to the technical field of copper smelting, in particular to the technical field of a method for extracting tellurium dioxide from tellurium copper slag.
Background
The tellurium copper slag is a Cu2Te displacer recovered when copper anode slime is treated by a Kaldor furnace, and particularly, the process of extracting selenium and tellurium by adopting an oxygen pressure leaching method enables the tellurium to be nearly 100% leached and transferred into a solution, then reduction treatment is carried out through sulfur dioxide, and the Cu2Te displacer is obtained by adopting copper scrap for displacement in an environment of normal pressure and 80 ℃.
The tellurium copper slag has a low content of tellurium element, which is only about 20%, and in order to purify the tellurium element, the following method is generally adopted: the tellurium copper slag is sulfated and roasted, then alkaline leached to separate tellurium, and finally purified to recover metal tellurium.
The purification method has the defect of low tellurium recovery rate.
Disclosure of Invention
The invention aims to: in order to solve the technical problems, the invention provides a method for extracting tellurium dioxide from tellurium copper slag.
The invention specifically adopts the following technical scheme for realizing the purpose:
the method comprises the steps of sequentially carrying out acid leaching, oxidation and filtration on wet tellurium copper slag to obtain acid leaching oxidation filter washing slag and acid leaching oxidation filter washing liquid, then carrying out alkaline leaching and filtration on the acid leaching oxidation filter washing slag to obtain alkaline leaching washing slag and alkaline leaching washing liquid, and then carrying out wet purification and drying on the alkaline leaching washing liquid to obtain a tellurium dioxide solid.
Further, before acid leaching and oxidizing the wet tellurium-copper slag, preparing wet tellurium-copper slag ore pulp and a composite oxidant solution.
Further, the concrete steps of preparing the wet tellurium copper slag ore pulp are as follows:
adding Xg wet tellurium-copper slag into a container, then adding Yml water, and stirring to obtain wet tellurium-copper slag ore pulp, wherein the drying amount of the wet tellurium-copper slag is 64%, and X: y =0.625;
the specific steps for preparing the composite oxidant solution are as follows:
adding Ag water into a container, sequentially adding a Bg oxidant and Cg salt, and dissolving the oxidant and the salt to obtain a composite oxidant solution, wherein A: b: c: x =50:11:5:100.
further, the specific steps of acid leaching the wet tellurium copper slag slurry are as follows:
adding the wet tellurium copper slag ore pulp into a container, and sequentially adding Dml industrial sulfuric acid and Eg copper sulfate pentahydrate under the condition of stirring the wet tellurium copper slag ore pulp to obtain acid leaching ore pulp, wherein C: d: e =25:40:32.
further, the specific steps of oxidizing the acid leaching ore pulp are as follows:
heating the acid leaching ore pulp, heating to 90 ℃, continuously introducing air into the acid leaching ore pulp, stirring, dripping the composite oxidant solution into the acid leaching ore pulp for less than 2 hours, and continuously reacting for 1-1.5 hours after dripping to obtain an acid leaching oxidation solution.
Further, the specific steps of filtering the acid leaching oxidation solution are as follows:
(1) Filtering while the solution is hot to obtain acid leaching oxidation filter residue and acid leaching oxidation filtrate;
(2) Washing the acid leaching oxidation filter residue for 3 times by using Fml hot water of 80-85 ℃, combining the washed hot water and the acid leaching oxidation filter liquor to obtain an acid leaching oxidation filter washing liquor, wherein the washed acid leaching oxidation filter residue is acid leaching oxidation filter washing residue, and E: f = 2.
Further, the specific steps of carrying out alkaline leaching on the acid leaching oxidation filter washing slag comprise:
adding acid leaching oxidation filter washing slag and Gml water into a container, stirring, adding Hg sodium hydroxide solid and Jg industrial sodium sulfide in portions, adding to 60-80 ℃, and stirring for reacting for 1H to obtain an alkaline leaching solution, wherein F: G: H: J = 600750.
Further, the specific steps of filtering the alkaline leaching solution are as follows:
(1) Filtering while hot to obtain alkaline leaching filter residue and alkaline leaching filtrate;
(2) And washing the alkaline leaching filter residue for 3 times by adopting hot water of Fml80-85 ℃, combining the washed hot water and the alkaline leaching filtrate to obtain alkaline leaching washing liquor, wherein the washed alkaline leaching filter residue is alkaline leaching washing residue.
Further, the specific steps of wet purification and drying of the alkaline leaching washing solution are as follows:
(1) Preparing a dilute sulfuric acid solution: adding 1 part of 98% reagent-grade sulfuric acid into 3 parts of water to obtain a dilute sulfuric acid solution for later use;
(2) Adding an alkali leaching lotion into a container, sequentially adding Kg of EDTA solution, mg anhydrous calcium chloride powder and Mg sodium sulfide powder under the condition of normal-temperature stirring, continuously stirring for reacting for 2 hours, and standing for 24 hours, wherein H: k: m = 150;
(3) Filtering the solution after the reaction to obtain filtrate;
(4) Adding the filtrate into a container, heating to 60 deg.C, adding dilute sulfuric acid solution under stirring, and stopping when the pH value of the solution is 3.0-5.0;
(5) Vacuum filtering while the solution is hot to obtain precipitate and waste water;
(6) Washing the precipitate with Kml of 80-85 deg.C hot water for 3 times;
(7) And drying the washed precipitate to obtain a tellurium dioxide solid.
A method for extracting tellurium dioxide from tellurium copper slag comprises the following steps:
(1) Preparing wet tellurium copper slag ore pulp: adding 500g of wet tellurium-copper slag into a container, adding 800ml of water, and stirring to obtain wet tellurium-copper slag slurry, wherein the drying amount of the wet tellurium-copper slag is 64%;
(2) Preparing a composite oxidant solution:
firstly, adding 250g of water into a container, then sequentially adding 55g of oxidant and 25g of salt, and dissolving the oxidant and the salt to obtain a composite oxidant solution;
(3) Acid leaching the wet tellurium copper slag slurry:
adding wet tellurium copper slag ore pulp into the container, and sequentially adding 40ml of industrial sulfuric acid and 32g of copper sulfate pentahydrate under the condition of stirring the wet tellurium copper slag ore pulp to obtain acid leaching ore pulp;
(4) Oxidizing acid leaching ore pulp:
heating the acid leaching ore pulp, heating to 90 ℃, continuously introducing air into the acid leaching ore pulp, stirring, dripping the composite oxidant solution into the acid leaching ore pulp for less than 2 hours, and continuously reacting for 1-1.5 hours after dripping to obtain an acid leaching oxidation solution;
(5) Filtering the acid leaching oxidation solution:
filtering while hot to obtain acid leaching oxidation filter residue and acid leaching oxidation filtrate;
washing the acid leaching oxidation filter residue for 3 times by using 1200ml of hot water with the temperature of 80-85 ℃, combining the washed hot water with the acid leaching oxidation filtrate to obtain an acid leaching oxidation filter washing liquid, wherein the washed acid leaching oxidation filter residue is acid leaching oxidation filter washing residue;
(6) Carrying out alkaline leaching on acid leaching oxidation filter washing residues:
adding acid leaching oxidation filter washing slag and 1500ml of water into a container, stirring, adding 150g of sodium hydroxide solid and 58g of industrial sodium sulfide in batches, heating to 60-80 ℃, and stirring for reacting for 1h to obtain an alkaline leaching solution;
(7) Filtering the alkaline leaching solution:
filtering while hot to obtain alkaline leaching filter residue and alkaline leaching filtrate;
washing the alkaline leaching residue with 1200ml of hot water at 80-85 deg.C for 3 times, mixing the washed hot water with the alkaline leaching filtrate to obtain alkaline leaching washing liquid, and collecting the washed alkaline leaching residue as alkaline leaching washing residue.
(8) Wet purification and drying of the alkaline leaching washing solution:
preparing a dilute sulfuric acid solution: adding 1 part of 98% reagent-grade sulfuric acid into 3 parts of water to obtain a dilute sulfuric acid solution for later use;
adding an alkali leaching lotion into a container, sequentially adding 0.1g of EDTA solution, 5g of anhydrous calcium chloride powder and 5g of sodium sulfide powder under the condition of stirring at normal temperature, continuously stirring for reacting for 2 hours, and standing for 24 hours;
filtering the solution after reaction to obtain filtrate and filter residue;
adding the filtrate into a container, heating to 60 deg.C, adding dilute sulfuric acid solution under stirring, and stopping when the pH value of the solution is 3.0-5.0;
vacuum filtering while the solution is hot to obtain precipitate and waste water;
washing the precipitate with 2000ml of 80-85 deg.C hot water for 3 times;
and drying the washed precipitate to obtain tellurium dioxide solid.
The invention has the following beneficial effects:
(1) Oxidizing the acid leached tellurium-copper slag by using a proper amount of oxidant, on one hand, removing copper in the tellurium-copper slag, on the other hand, generating tellurite acid or tellurite which is easily dissolved in alkali liquor, and avoiding excessive oxidation of the tellurium-copper slag to form Na2Te04 compound and Cu3Te06 compound which are difficultly dissolved in the alkali liquor
(2) Converting silver in the tellurium copper slag into silver chloride precipitate by adopting industrial salt, so that the tellurium can be conveniently and smoothly leached out;
(3) Tellurium in acid leaching oxidation filter washing slag exists mainly in forms of TeO2, cuTeO3 and the like, silver exists in forms of AgCl, ag2O and the like, selenium Se, seO2, seO3, cuSeO3 and the like, and two elements of sulfur and selenium are close to tellurium in chemical property, but tellurium is more alkaline, tellurium dioxide is easily dissolved in a strong alkaline solution to generate tellurite (such as Na2TeO3 and the like), and an alkaline leaching method can selectively dissolve out substances soluble in the alkaline solution, so that tellurium is dissolved in the alkaline solution and most metals are retained in the alkaline leaching filter washing slag;
(4) The invention adds proper amount of sodium sulfide and calcium chloride into the alkaline leaching washing solution, namely sodium tellurite solution, can remove impurities insoluble in alkali liquor and impurities such as Cu, pb, si, etc., purifies the sodium tellurite solution after impurity removal, neutralizes the sodium tellurite solution with dilute sulfuric acid until the pH value is 3-5, and the precipitate is washed and dried to obtain the refined tellurium dioxide product.
Detailed Description
The embodiment provides a method for extracting tellurium dioxide from tellurium copper slag, which comprises the following steps:
(1) Preparing wet tellurium copper slag ore pulp: adding 500g of wet tellurium-copper slag into a container, adding 800ml of water, and stirring to obtain wet tellurium-copper slag slurry, wherein the drying amount of the wet tellurium-copper slag is 64%, and the solid content of the tellurium-copper slag is 320g;
(2) Preparing a composite oxidant solution:
firstly, adding 250g of water into a container, then sequentially adding 55g of oxidant and 25g of salt, and dissolving the oxidant and the salt to obtain a composite oxidant solution, wherein specifically, the oxidant is industrial sodium hydroxide and meets GB/T209-2018;
(3) Acid leaching the wet tellurium copper slag slurry:
adding wet tellurium copper slag ore pulp into the container, and sequentially adding 40ml of 93% industrial sulfuric acid and 32g of blue vitriol under the condition of stirring the wet tellurium copper slag ore pulp to obtain acid leaching ore pulp;
(4) Oxidizing acid leaching ore pulp:
heating the acid leaching pulp, heating to 90 ℃, continuously introducing air into the acid leaching pulp, stirring, dripping a composite oxidant solution into the acid leaching pulp for 1.5 hours, and continuously reacting for 1.5 hours after dripping to obtain an acid leaching oxidation solution;
(5) Filtering the acid leaching oxidation solution:
filtering while hot to obtain acid leaching oxidation filter residue and acid leaching oxidation filtrate;
washing the acid leaching oxidation filter residue for 3 times by using 1200ml of hot water with the temperature of 85 ℃, combining the washed hot water with the acid leaching oxidation filter residue to obtain an acid leaching oxidation filter washing liquid, wherein the washed acid leaching oxidation filter residue is acid leaching oxidation filter washing residue, the moisture content is 466.46g, and the dry basis content is about 65.8%;
(6) Carrying out alkaline leaching on acid leaching oxidation filter washing residues:
adding acid leaching oxidation filter washing residues and 1500ml of water into a container, stirring, adding 150g of sodium hydroxide solid and 58g of industrial sodium sulfide in batches, adding the sodium hydroxide solid and the industrial sodium sulfide in 5 batches sequentially, namely adding 30g of sodium hydroxide solid and 11.6g of industrial sodium sulfide into each batch, heating to 70 ℃, and stirring for reacting for 1 hour to obtain an alkaline leaching solution;
(7) Filtering the alkaline leaching solution:
filtering while hot to obtain alkaline leaching filter residue and alkaline leaching filtrate;
and washing the alkaline leaching filter residue for 3 times by using 1200ml of hot water with the temperature of 85 ℃, combining the washed hot water with the alkaline leaching filtrate to obtain alkaline leaching washing liquor, wherein the washed alkaline leaching filter residue is alkaline leaching washing residue.
(8) Wet purification and drying are carried out on the alkaline leaching and filtering washing liquid:
preparing a dilute sulfuric acid solution: adding 1 part of 98% reagent-grade sulfuric acid into 3 parts of water to obtain a dilute sulfuric acid solution for later use;
adding an alkali lixiviation washing solution into a container, sequentially adding 0.1g of EDTA solution, 5g of anhydrous calcium chloride powder and 5g of sodium sulfide powder under the condition of stirring at normal temperature, continuously stirring for reacting for 2 hours, and standing for 24 hours;
filtering the solution after reaction to obtain filtrate and filter residue;
adding the filtrate into a container, heating to 60 deg.C, adding dilute sulfuric acid solution under stirring, and stopping when the pH value of the solution is 3.5;
vacuum filtering while the solution is hot to obtain precipitate and waste water;
washing the precipitate with 2000ml of hot water at 85 ℃ for 3 times;
and drying the washed precipitate to obtain tellurium dioxide solid.
Specifically, the container in the embodiment is a 3000ml beaker, the sodium sulfide content of industrial sodium sulfide is not less than 60%, the industrial salt meets GB/T5462-2015, and the sodium hydroxide solid adopts industrial sodium hydroxide and meets GB/T209-2018.
See tables 1-4 for specific experimental results.
Table 1: acid leaching oxidation experiment result and balance table
The tellurium-copper slag in table 1 is the weight of solid, the acid leaching oxidation filter washing slag is the dry basis content, as can be seen from table 1, 67.42% of copper in the tellurium-copper slag is converted into copper sulfate after acid leaching oxidation and enters the acid leaching oxidation filter washing liquid, and the acid leaching oxidation filter washing liquid has less impurity content of tellurium, silver, selenium and the like, and can be used for preparing crude copper sulfate and also can be returned to a copper electrolysis (electrodeposition) workshop to be used as a raw material for extracting electrolytic copper. The recovery rates of tellurium, silver and selenium in the acid leaching oxidation filter residue are respectively 99.07%, 99.98% and 97.94%, tellurium, silver and selenium are mainly enriched in the acid leaching oxidation filter residue, the enrichment degree is high, and good conditions are created for the next alkaline leaching.
Table 2: alkaline leaching experiment result and balance table
In table 2, the alkaline leaching, filtering and washing slag is the dried weight, and is silver-selenium slag enriched with silver and selenium, as can be seen from table 2, when the acid leaching, oxidizing, filtering and washing slag is subjected to alkaline leaching, 92.49% of tellurium can be converted into sodium tellurite to be leached into an alkaline solution, but the solution contains a small amount of impurity components such as copper, selenium, lead and silicon which are easily dissolved in the alkaline solution, and the impurity components need to be further removed and purified to be used for electrodeposition of tellurium; the alkaline leaching residue is enriched with 100% of silver and 94.21% of selenium, wherein the contents of copper, tellurium, silver and selenium respectively reach 12.11%, 2.68%, 56.75% and 12.87%, and the alkaline leaching residue can be returned to a KALDO (Kaldo) furnace smelting system or subjected to secondary acid leaching oxidation to respectively recover copper, tellurium, silver and selenium.
Table 3: wet purification experimental result and balance table
Table 4: tellurium dioxide solid all-element analysis result table
In table 3, the filtered residue can be returned to the high pressure leaching process of the KALDO furnace for secondary recovery of copper and tellurium, and the tellurium dioxide solid is the weight after drying, as can be seen from tables 3 and 4, after the alkaline leaching washing liquid is subjected to wet purification, the filtered residue is mainly enriched with elements such as copper, tellurium, lead and sulfur, wherein the copper content is 7.03% and the tellurium content is 9.31%, the filtered residue can be returned to the high pressure leaching process of the KALDO furnace for secondary recovery of copper and tellurium, the wet purification can remove metal impurities such as copper and lead in the alkaline leaching washing liquid, the removal rate is more than 96.9%, selenium element forms SeO2 when being neutralized in dilute sulfuric acid, the precipitate is completely enriched in the precipitate, after the alkaline leaching washing liquid is subjected to wet purification and drying, the grade of the precipitated tellurium dioxide solid is 87.62%, the tellurium recovery rate is 95.83%, and the recovery rate is high.
Claims (9)
1. The method is characterized in that acid leaching, oxidation and filtration are sequentially carried out on wet tellurium copper slag to obtain acid leaching oxidation filter washing slag and acid leaching oxidation filter washing liquid, then alkali leaching and filtration are carried out on the acid leaching oxidation filter washing slag to obtain alkali leaching washing liquid, and then wet purification and drying are carried out on the alkali leaching filter washing liquid to obtain tellurium dioxide solid.
2. The method for extracting tellurium dioxide from tellurium copper slag according to claim 1, wherein before acid leaching and oxidizing the wet tellurium copper slag, ore pulp of the wet tellurium copper slag and a composite oxidant solution are prepared.
3. The method for extracting tellurium dioxide from tellurium copper slag according to claim 2, wherein the concrete steps of preparing the ore pulp of the wet tellurium copper slag are as follows:
adding Xg wet tellurium copper slag into a container, adding Yml water, and stirring to obtain wet tellurium copper slag ore pulp, wherein the drying amount of the wet tellurium copper slag is 64%, and X: y =0.625;
the specific steps for preparing the composite oxidant solution are as follows:
adding Ag water into a container, sequentially adding a Bg oxidant and Cg salt, and dissolving the oxidant and the salt to obtain a composite oxidant solution, wherein A: b: c: x =50:11:5:100.
4. the method for extracting tellurium dioxide from tellurium copper slag according to claim 3, wherein the specific steps of acid leaching of the wet tellurium copper slag slurry are as follows:
adding wet tellurium copper slag ore pulp into the container, and sequentially adding Dml industrial sulfuric acid and Eg blue vitriol under the condition of stirring the wet tellurium copper slag ore pulp to obtain acid leaching ore pulp, wherein C: d: e =25:40:32.
5. the method for extracting tellurium dioxide from tellurium copper slag according to claim 4, wherein the specific steps of oxidizing the acid leaching pulp are as follows:
heating the acid leaching pulp, raising the temperature to 90 ℃, continuously introducing air into the acid leaching pulp, stirring, dripping the composite oxidant solution into the acid leaching pulp for less than 2 hours, and continuously reacting for 1-1.5 hours after dripping to obtain an acid leaching oxidation solution.
6. The method for extracting tellurium dioxide from tellurium copper slag according to claim 5, wherein the specific steps of filtering the acid leaching oxidation solution are as follows:
(1) Filtering while the solution is hot to obtain acid leaching oxidation filter residue and acid leaching oxidation filtrate;
(2) Washing the acid leaching oxidation filter residue for 3 times by using Fml hot water of 80-85 ℃, combining the washed hot water and the acid leaching oxidation filter liquor to obtain an acid leaching oxidation filter washing liquor, wherein the washed acid leaching oxidation filter residue is acid leaching oxidation filter washing residue, and E: f = 2.
7. The method for extracting tellurium dioxide from tellurium copper slag according to claim 6, wherein the specific steps of carrying out alkaline leaching on the acid leaching oxidation filter washing slag are as follows:
adding acid leaching oxidation filter washing slag and Gml water into a container, stirring, adding Hg sodium hydroxide solid and Jg industrial sodium sulfide in portions, heating to 60-80 ℃, and stirring for reacting for 1H to obtain an alkaline leaching solution, wherein F: G: H: J =600 750.
8. The method for extracting tellurium dioxide from tellurium copper slag according to claim 7, wherein the specific steps of filtering the alkaline leaching solution are as follows:
(1) Filtering while hot to obtain alkaline leaching filter residue and alkaline leaching filtrate;
(2) And washing the alkaline leaching filter residue for 3 times by adopting hot water of Fml80-85 ℃, combining the washed hot water with the alkaline leaching filtrate to obtain alkaline leaching washing liquor, wherein the washed alkaline leaching filter residue is alkaline leaching washing residue.
9. The method for extracting tellurium dioxide from tellurium copper slag according to claim 8, wherein the specific steps of performing wet purification and drying on the alkaline leaching washing solution are as follows:
(1) Preparing a dilute sulfuric acid solution: adding 1 part of 98% reagent-grade sulfuric acid into 3 parts of water to obtain a dilute sulfuric acid solution for later use;
(2) Adding an alkali lixiviation washing solution into a container, sequentially adding Kg of EDTA solution, mg anhydrous calcium chloride powder and Mg sodium sulfide powder under the condition of stirring at normal temperature, continuously stirring for reacting for 2 hours, and standing for 24 hours, wherein H: k: m = 150;
(3) Filtering the solution after the reaction to obtain filtrate and filter residue;
(4) Adding the filtrate into a container, heating to 60 deg.C, adding dilute sulfuric acid solution under stirring, and stopping when the pH value of the solution is 3.0-5.0;
(5) Vacuum filtering while the solution is hot to obtain precipitate and waste water;
(6) Washing the precipitate with Kml of 80-85 deg.C hot water for 3 times;
(7) And drying the washed precipitate to obtain a tellurium dioxide solid.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002105554A (en) * | 2000-09-28 | 2002-04-10 | Furukawa Co Ltd | Method for recovering tellurium |
| CN104928483A (en) * | 2015-05-15 | 2015-09-23 | 西北矿冶研究院 | Method for comprehensively recovering silver, selenium, tellurium and copper from copper telluride residues |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002105554A (en) * | 2000-09-28 | 2002-04-10 | Furukawa Co Ltd | Method for recovering tellurium |
| CN104928483A (en) * | 2015-05-15 | 2015-09-23 | 西北矿冶研究院 | Method for comprehensively recovering silver, selenium, tellurium and copper from copper telluride residues |
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