CN115216628B - Method for removing copper and arsenic from copper-arsenic-containing acidic solution - Google Patents
Method for removing copper and arsenic from copper-arsenic-containing acidic solution Download PDFInfo
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- CN115216628B CN115216628B CN202210674189.7A CN202210674189A CN115216628B CN 115216628 B CN115216628 B CN 115216628B CN 202210674189 A CN202210674189 A CN 202210674189A CN 115216628 B CN115216628 B CN 115216628B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical 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
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
- C22B19/26—Refining solutions containing zinc values, e.g. obtained by leaching zinc ores
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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
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Abstract
The application discloses a method for removing copper and arsenic from copper-arsenic-containing acid solution, which comprises the following steps: (1) Mixing and reacting the copper-arsenic-containing acid solution, copper concentrate and reduced iron powder to obtain ore pulp; (2) Concentrating the pulp to obtain a concentrated underflow and a supernatant; (3) Subjecting the dense underflow to solid-liquid separation to obtain a copper and arsenic removed liquor and a copper and arsenic containing filter residue, wherein in step (1), the copper and arsenic containing acidic solution has a copper and arsenic molar ratio of less than 3, and the copper concentrate comprises Cu and Cu 2 O. Thereby, cu and Cu 2 The presence of O can promote Cu 3 As is formed, so that copper and arsenic in the solution can be effectively removed under the condition that the copper-arsenic ratio is less than 3, the traditional method for oxidizing and leaching copper concentrate to supplement copper and precipitate arsenic is avoided, the oxidizing and leaching cost is reduced, the consumption of iron powder is reduced, the production cost is saved, good conditions can be created for downstream processes, the generation of highly toxic arsine is stopped, and the quality of downstream products is improved.
Description
Technical Field
The application belongs to the technical field of metallurgy, and particularly relates to a method for removing copper and arsenic from copper-arsenic-containing acidic solution.
Background
The main process of zinc hydrometallurgy of the company comprises the following steps: roasting, leaching, purifying and electrolyzing; the impurity removing process comprises the following steps: low-acid leaching-reduction leaching-copper removal-neutralization-iron removal, wherein valuable metals and impurities in the calcine enter a wet system in the leaching process, arsenic in the calcine enters a reduction leaching solution after reduction leaching, and according to a reaction equation 6Cu (II) +2As (II) +9Fe=9Fe (II) +2Cu by adding reduced iron powder into an acidic solution containing Cu and As to remove copper and arsenic 3 As (1), under the condition that the molar ratio of copper to arsenic in the reduced liquid is more than 3, the copper and arsenic can be coprecipitated into Cu by directly adding reduced iron powder 3 As, however, under the condition that the molar ratio of copper to arsenic is less than 3, arsenic cannot be thoroughly removed, and the influence on the subsequent process is large. Under the condition, the method mainly adopted at present is copper concentrate oxidation leaching to supplement copper and precipitate arsenic, but the method has higher oxidation leaching cost and higher iron powder consumption.
Therefore, the existing method for removing copper and arsenic under the condition that the copper-arsenic ratio is less than 3 needs to be improved.
Disclosure of Invention
The present application aims to solve at least one of the technical problems in the related art to some extent. Therefore, an object of the present application is to provide a method for removing copper and arsenic from an acidic solution containing copper and arsenic, by which copper and arsenic in the solution can be effectively removed at a molar ratio of copper and arsenic of less than 3.
In one aspect of the application, a method for removing copper and arsenic from an acidic copper-and arsenic-containing solution is provided. According to an embodiment of the application, the method comprises:
(1) Mixing and reacting the copper-arsenic-containing acid solution, copper concentrate and reduced iron powder to obtain ore pulp;
(2) Concentrating the pulp to obtain a concentrated underflow and a supernatant;
(3) Carrying out solid-liquid separation on the dense underflow so as to obtain copper and arsenic removed liquid and copper and arsenic contained filter residues,
wherein in the step (1), the copper-arsenic molar ratio of the copper-arsenic-containing acidic solution is less than 3, and the copper concentrate contains Cu and Cu 2 O。
According to the method for removing copper and arsenic from the copper-arsenic-containing acidic solution, the copper-arsenic-containing acidic solution with the copper and arsenic molar ratio less than 3 comprises Cu and Cu 2 Mixing the copper concentrate of O with reduced iron powder, concentrating ore pulp obtained by the reaction to obtain a concentrated bottom flow and a supernatant, and finally carrying out solid-liquid separation on the concentrated bottom flow to obtain a copper-arsenic-removed liquid and copper-arsenic-containing filter residues, wherein the copper-arsenic-containing filter residues can be directly sold as products. The application is realized by adding Cu and Cu 2 Copper concentrate of O, cu 2 The O, cu can promote the formation of arsenic-copper compounds, and thoroughly remove arsenic in an acidic solution, so that the arsenic in the solution can be effectively removed under the condition that the copper-arsenic ratio is less than 3, the traditional method for oxidizing and leaching copper concentrate to supplement copper and precipitate arsenic is avoided, the oxidizing and leaching cost is reduced, the consumption of iron powder is reduced, the production cost is saved, good conditions can be created for downstream procedures, the generation of highly toxic arsine is avoided, and the quality of downstream products is improved.
In addition, the method for removing copper and arsenic from copper-arsenic-containing acidic solution according to the above embodiment of the present application may have the following additional technical features:
in some embodiments of the application, in step (1), the copper-arsenic-containing acidic solution comprises Cu: 1.0-2.0 g/L, as: 0.5-1.5 g/L, H 2 SO 4 ：28～32g/L、Fe 2+ : 35-45 g/L and In: 0.1-0.15 g/L.
In some embodiments of the application, in step (1), the copper concentrate comprises 30 to 50wt% of the Cu and 30 to 50wt% of the Cu 2 O. Thus, copper and arsenic in the solution can be effectively removed when the copper-arsenic ratio is less than 3.
In some embodiments of the application, in step (1), the Cu and the Cu in the copper concentrate 2 The ratio of the total molar amount of O to the molar amount of arsenic in the copper-arsenic-containing acidic solution is 1 to 3. Thus, copper and arsenic in the solution can be effectively removed when the copper-arsenic ratio is less than 3.
In some embodiments of the present application, in the step (1), the reduced iron powder has a metallic iron purity of 95wt% or more and a particle size of not more than 200 mesh of not less than 80wt% of the total amount of the reduced iron powder. Thus, copper and arsenic in the solution can be effectively removed when the copper-arsenic ratio is less than 3.
In some embodiments of the application, the ratio of the molar amount of metallic iron to the molar amount of copper in the copper-arsenic-containing acidic solution is 1 to 1.5. Thus, copper and arsenic in the solution can be effectively removed when the copper-arsenic ratio is less than 3.
In some embodiments of the application, in step (1), the reaction temperature is 70-90 ℃ and the reaction time is not less than 60min. Thus, copper and arsenic in the solution can be effectively removed when the copper-arsenic ratio is less than 3.
In some embodiments of the present application, the copper and arsenic removed solution obtained in step (3) is returned to step (2) to be thickened with the pulp. Thus, the solid-liquid separation can be more thorough.
In some embodiments of the present application, the copper content of the copper-bearing arsenic-bearing filter residue is 30-50 wt% and the arsenic content is 10-30 wt%.
In some embodiments of the application, the copper and arsenic removal liquid contains Cu which is less than or equal to 0.2g/L, as which is less than or equal to 0.1g/L.
Additional aspects and advantages of the application will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the application.
Drawings
The foregoing and/or additional aspects and advantages of the application will become apparent and may be better understood from the following description of embodiments taken in conjunction with the accompanying drawings in which:
FIG. 1 is a schematic flow diagram of a method for removing copper and arsenic from an acidic copper-arsenic-containing solution according to one embodiment of the application;
fig. 2 is a schematic flow diagram of a method for removing copper and arsenic from an acidic copper-arsenic-containing solution according to yet another embodiment of the application.
Detailed Description
The embodiments described below by referring to the drawings are illustrative and intended to explain the present application and should not be construed as limiting the application.
In a first aspect of the application, the application provides a method for removing copper and arsenic from an acidic copper-and arsenic-containing solution. Referring to fig. 1, according to an embodiment of the present application, the method includes:
s100: mixing copper-arsenic-containing acid solution, copper concentrate and reduced iron powder for reaction
In this step, the copper-arsenic acid solution containing Cu and Cu is prepared by mixing copper-arsenic acid solution with a copper-arsenic molar ratio of less than 3 2 And (3) carrying out a mixing reaction on the copper concentrate of O and reduced iron powder to obtain ore pulp. The inventors found that Cu and Cu 2 The presence of O can promote Cu 3 As is formed, so that copper and arsenic in the solution can be effectively removed under the condition that the copper-arsenic ratio is less than 3. Specifically, the copper-arsenic-containing acidic solution is from a wet system in a zinc hydrometallurgy process, and comprises the following components: cu: 1.0-2.0 g/L, as: 0.5-1.5 g/L, H 2 SO 4 ：28～32g/L、Fe 2+ : 35-45 g/L and In: 0.1-0.15 g/L.
Further, the copper concentrate contains 30 to 50 weight percent of Cu and 30 to 50 weight percent of Cu 2 O. The inventors found that if Cu or Cu in copper concentrate 2 Too low an amount of O can result in insufficient copper being fed to completely precipitate the arsenic; if Cu or Cu in copper concentrate 2 The content of O is too high, and the dosage of iron powder needs to be increased to reduce copper content of the solution. Therefore, the content of the application is beneficial to effectively removing arsenic in the solution under the condition that the copper-arsenic ratio is less than 3, and the cost is controlled.
Further, cu and Cu in the copper concentrate 2 The ratio of the total molar amount of O to the molar amount of arsenic in the copper-arsenic-containing acidic solution is 1 to 3. The inventors found that if the ratio is too small, the amount of copper in the redox system is insufficient, the molar ratio of copper to arsenic is insufficient, and arsenic precipitation is incomplete; and if the ratio is too large, the cost is increased. Therefore, the ratio of the application is beneficial to effectively removing arsenic in the solution under the condition that the copper-arsenic ratio is less than 3, and the cost is controlled.
Further, the purity of the metallic iron in the reduced iron powder is more than or equal to 95wt%, and the reduced iron powder with the granularity not more than 200 meshes is not less than 80wt% of the total amount of the reduced iron powder. The inventors found that if the purity of the metallic iron in the reduced iron powder is too low or the particle size of the reduced iron powder is too large, the copper and arsenic removal effect is poor.
Further, the ratio of the molar amount of the metallic iron to the molar amount of copper in the copper-arsenic-containing acidic solution is 1 to 1.5. The inventors found that if the ratio is too small, cu in the acidic solution 2+ Incomplete precipitation; if the ratio is too large, the consumption of iron powder is increased, and the production cost is increased. Thus, the ratio of the application is favorable for Cu in the acid solution 2+ And (5) fully precipitating and controlling the cost.
Further, the reaction temperature is 70-90 ℃ and the reaction time is not less than 60min. The inventor finds that if the reaction temperature is too low or the reaction time is too short, the copper and arsenic removal effect is poor; if the reaction temperature is too high, the energy consumption increases.
S200: concentrating the ore pulp
In the step, the ore pulp is thickened, and the sediment in the ore pulp is settled by utilizing the gravity action, thus obtaining the Cu-containing material 3 As、A dense underflow of Cu and a supernatant liquid with lower content of copper and arsenic. Specifically, the above-described thickening process is performed in a thickening tank. Preferably, the flocculant is added during the thickening process, thereby improving the thickening effect and shortening the thickening time. It should be noted that the specific type and addition amount of the flocculant may be selected by those skilled in the art according to actual needs.
S300: solid-liquid separation is carried out on the dense underflow
In the step, the dense underflow is subjected to solid-liquid separation, so that copper and arsenic removed liquid and copper and arsenic contained filter residues can be obtained. Specifically, the content of copper in the copper-bearing arsenic filter residue is 30-50wt% and the content of arsenic is 10-30wt%; the Cu content of the copper-arsenic removing liquid is less than or equal to 0.2g/L, as and less than or equal to 0.1g/L. The specific mode of the solid-liquid separation is not particularly limited, and may be selected according to actual needs by those skilled in the art, and may be, for example, press filtration. Further, referring to fig. 2, the obtained copper and arsenic removed solution is returned to step S200 to be concentrated with the pulp, so that the solid-liquid separation can be more thorough.
The inventors found that by bringing a copper-arsenic-containing acidic solution having a copper-arsenic molar ratio of less than 3, a copper-arsenic-containing acidic solution containing Cu and Cu 2 Mixing the copper concentrate of O with reduced iron powder, concentrating ore pulp obtained by the reaction to obtain a concentrated bottom flow and a supernatant, and finally carrying out solid-liquid separation on the concentrated bottom flow to obtain a copper-arsenic-removed liquid and copper-arsenic-containing filter residues, wherein the copper-arsenic-containing filter residues can be directly sold as products. The application is realized by adding Cu and Cu 2 Copper concentrate of O, cu 2 The O, cu can promote the formation of arsenic-copper compounds and thoroughly remove arsenic in an acidic solution, so that copper and arsenic in the solution can be effectively removed under the condition that the copper-arsenic ratio is less than 3, the traditional method for copper supplementing and arsenic precipitating by oxidizing and leaching copper concentrate is avoided, the oxidizing and leaching cost is reduced, the consumption of iron powder is reduced, the production cost is saved, good conditions can be created for downstream procedures, the generation of highly toxic arsine is avoided, and the quality of downstream products is improved.
The following detailed description of embodiments of the application is provided for the purpose of illustration only and is not to be construed as limiting the application. In addition, all reagents employed in the examples below are commercially available or may be synthesized according to methods herein or known, and are readily available to those skilled in the art for reaction conditions not listed, if not explicitly stated.
Example 1
Step 1: 100m of 3 Copper-arsenic-containing acidic solution (Cu: 1.23g/L, as:1.27g/L, H) 2 SO 4 ：30g/L、Fe 2+ :42g/L and In:0.12 g/L), 300kg copper concentrate (containing 41wt% Cu and 41wt% Cu 2 O) and 160kg of reduced iron powder (the purity of the metal iron is more than or equal to 95wt percent, the granularity of the reduced iron powder is not more than 200 meshes and is not less than 80wt percent of the total amount of the reduced iron powder) are mixed for reaction (the reaction temperature is 80 ℃ and the reaction time is 60 min) to obtain ore pulp;
step 2: adding 0.5kg of flocculant into ore pulp after the reaction is finished, and settling the mixture and then entering a thickening tank to obtain thickened underflow and supernatant;
step 3: filtering the dense underflow by using a filter press to obtain copper and arsenic removed liquid (containing 0.37g/L of Cu and 0.36g/L of As) and copper and arsenic-containing filter residues (the copper content is 56.3wt percent and the arsenic content is 23.5wt percent), and returning the copper and arsenic removed liquid to the dense pond, wherein the copper and arsenic-containing filter residues can be directly sold as products.
Example 2
Step 1: 100m of 3 Copper-arsenic-containing acidic solution (Cu: 1.23g/L, as:1.27g/L, H) 2 SO 4 ：30g/L、Fe 2+ :42g/L and In:0.12 g/L), 400kg copper concentrate (containing 41wt% Cu and 41wt% Cu 2 O) and 160kg of reduced iron powder (the purity of the metal iron is more than or equal to 95wt percent, the granularity of the reduced iron powder is not more than 200 meshes and is not less than 80wt percent of the total amount of the reduced iron powder) are mixed for reaction (the reaction temperature is 90 ℃ and the reaction time is 60 min) to obtain ore pulp;
step 2: adding 0.5kg of flocculant into ore pulp after the reaction is finished, and settling the mixture and then entering a thickening tank to obtain thickened underflow and supernatant;
step 3: filtering the dense underflow by using a filter press to obtain copper and arsenic removed liquid (containing Cu 0.12g/L and As0.13 g/L) and copper and arsenic containing filter residues (the copper content is 58.3wt percent and the arsenic content is 18.5wt percent), and returning the copper and arsenic removed liquid to the dense pond, wherein the copper and arsenic containing filter residues can be directly sold as products.
Comparative example 1
The difference from example 1 is that copper concentrate is not added, a copper-arsenic-removed liquor (containing Cu 0.45g/L, as 0.75.75 g/L) and copper-arsenic-containing filter residues (the copper content is 55.6wt% and the arsenic content is 23.4 wt%) are obtained, and the copper-arsenic-removed liquor is returned to a thickening tank, and the copper-arsenic-containing filter residues can be directly sold as products.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present application. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
While embodiments of the present application have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the application, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the application.
Claims (8)
1. A method for removing copper and arsenic from an acidic copper and arsenic-containing solution comprising:
(1) Mixing and reacting the copper-arsenic-containing acid solution, copper concentrate and reduced iron powder to obtain ore pulp;
(2) Concentrating the pulp to obtain a concentrated underflow and a supernatant;
(3) Carrying out solid-liquid separation on the dense underflow so as to obtain copper and arsenic removed liquid and copper and arsenic contained filter residues,
wherein in the step (1), the copper-arsenic molar ratio of the copper-arsenic-containing acidic solution is less than 3, and the copper concentrate contains Cu and Cu 2 O，
In the step (1), the copper concentrate contains 30-50wt% of Cu and 30-50wt% of Cu 2 O；
In step (1), the Cu and the Cu in the copper concentrate 2 The ratio of the total molar amount of O to the molar amount of arsenic in the copper-arsenic-containing acidic solution is 1-3.
2. The method of claim 1, wherein in step (1), the copper-arsenic-containing acidic solution comprises: cu: 1.0-2.0 g/L, as: 0.5-1.5 g/L, H 2 SO 4 ：28~32g/L、Fe 2+ : 35-45 g/L and In:0.1 to 0.15g/L.
3. The method according to claim 1, wherein in the step (1), the purity of metallic iron in the reduced iron powder is not less than 95% by weight, and the reduced iron powder having a particle size of not more than 200 mesh is not less than 80% by weight of the total amount of the reduced iron powder.
4. A method according to claim 3, wherein the ratio of the molar amount of metallic iron to the molar amount of copper in the copper-arsenic-containing acidic solution is 1 to 1.5.
5. The method according to claim 1, wherein in the step (1), the reaction temperature is 70-90 ℃ and the reaction time is not less than 60min.
6. The method according to claim 1, wherein the copper and arsenic removal liquid obtained in the step (3) is returned to the step (2) to be thickened with the ore pulp.
7. The method according to claim 1 or 6, wherein the copper content of the copper-arsenic-containing filter residue is 30-50wt% and the arsenic content is 10-30wt%.
8. The method according to claim 1 or 6, wherein the copper and arsenic removing liquid contains Cu less than or equal to 0.2g/L, as less than or equal to 0.1g/L.
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