CN115216628A - Method for removing copper and arsenic from copper and arsenic-containing acidic solution - Google Patents
Method for removing copper and arsenic from copper and arsenic-containing acidic solution Download PDFInfo
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- CN115216628A CN115216628A CN202210674189.7A CN202210674189A CN115216628A CN 115216628 A CN115216628 A CN 115216628A CN 202210674189 A CN202210674189 A CN 202210674189A CN 115216628 A CN115216628 A CN 115216628A
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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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Abstract
The invention discloses a method for removing copper and arsenic from a copper-arsenic-containing acidic solution, which comprises the following steps: (1) Carrying out mixed reaction on the copper-arsenic-containing acidic solution, the copper concentrate and the reduced iron powder so as to obtain ore pulp; (2) Thickening the ore pulp so as to obtain a thickened underflow and a supernatant; (3) And (2) carrying out solid-liquid separation on the concentrated bottom flow so as to obtain a copper-arsenic-removed solution and a copper-arsenic-containing filter residue, 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 And O. Thus, cu and Cu 2 The presence of O can promote Cu 3 As is formed, the copper and arsenic in the solution can be effectively removed under the condition that the ratio of copper to arsenic is less than 3, the traditional method for oxidizing and leaching copper concentrate to supplement copper and sink 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 virulent arsenic hydride is stopped, and the downstream production is improvedAnd (5) quality of the product.
Description
Technical Field
The invention belongs to the technical field of metallurgy, and particularly relates to a method for removing copper and arsenic from a copper-arsenic-containing acidic solution.
Background
The main wet zinc smelting process of the company comprises the following steps: roasting, leaching, purifying and electrolyzing; the impurity removal 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 through reduction leaching, and according to a reaction equation of adding reduced iron powder to an acid solution containing Cu and As to remove copper and arsenic, cu (II) +2As (II) +9Fe = Fe 9 (II) +2Cu 3 As (1), directly adding reduced iron powder under the condition that the molar ratio of copper to arsenic in the reduced solution is more than 3 to ensure that the copper and the arsenic are coprecipitated into Cu 3 As, but in the case of the molar ratio of copper to arsenic being less than 3, arsenic cannot be completely removed, and the subsequent process is carried outThe effect is greater. Under the condition, the method mainly adopted at present is to supplement copper and deposit arsenic by oxidizing and leaching copper concentrate, but the method has higher oxidizing and leaching cost and larger consumption of iron powder.
Therefore, the existing method for removing copper and arsenic under the condition that the ratio of copper to arsenic is less than 3 needs to be improved.
Disclosure of Invention
The present invention is directed to solving, at least in part, one of the technical problems in the related art. Therefore, an object of the present invention 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 with a molar ratio of copper to arsenic of less than 3.
In one aspect of the invention, a method for removing copper arsenic from a copper arsenic-containing acidic solution is provided. According to an embodiment of the invention, the method comprises:
(1) Carrying out mixed reaction on the copper-arsenic-containing acidic solution, the copper concentrate and the reduced iron powder so as to obtain ore pulp;
(2) Thickening the ore pulp so as to obtain a thickened underflow and a supernatant;
(3) Carrying out solid-liquid separation on the concentrated bottom flow so as to obtain copper and arsenic removed liquid and copper and arsenic containing filter residue,
wherein, in the step (1), the molar ratio of copper to arsenic of the acid solution containing copper and arsenic 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, which is disclosed by the embodiment of the invention, the copper-arsenic-containing acidic solution with the copper-arsenic molar ratio of less than 3, and the copper-arsenic-containing acidic solution containing Cu and Cu 2 And finally, carrying out solid-liquid separation on the concentrated underflow to obtain copper-arsenic-containing liquid and copper-arsenic-containing filter residue, wherein the copper-arsenic-containing filter residue can be directly sold as a product. The application is realized by adding Cu and Cu 2 Copper concentrate of O, cu 2 O, cu can promote the formation of arsenic copper compound, remove arsenic in acid solution thoroughly, and reduce the ratio of copper to arsenic to be less than 3The arsenic in the solution is effectively removed, the traditional method for oxidizing and leaching copper concentrate to supplement copper and sink 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 virulent arsenic hydride is avoided, and the quality of downstream products is improved.
In addition, the method for removing copper and arsenic from the copper and arsenic-containing acidic solution according to the above embodiment of the invention may further have the following additional technical features:
in some embodiments of the invention, in step (1), the copper-containing arsenic 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 invention, in step (1), said copper concentrate comprises 30 to 50wt% of said Cu and 30 to 50wt% of said Cu 2 And (O). Thereby, copper and arsenic in the solution can be effectively removed when the copper-arsenic ratio is less than 3.
In some embodiments of the invention, in step (1), the Cu in the copper concentrate is in contact with the Cu 2 The ratio of the total molar amount of O to the molar amount of arsenic in the arsenic acidic solution containing copper is 1-3. Thereby, 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 invention, in step (1), the purity of metallic iron in the fine reduced iron is 95wt% or more, and the fine reduced iron having a particle size of not more than 200 meshes is not less than 80wt% of the total amount of the fine reduced iron. Thereby, copper and arsenic in the solution can be effectively removed when the copper-arsenic ratio is less than 3.
In some embodiments of the invention, the ratio of the molar amount of metallic iron to the molar amount of copper in the copper-containing arsenic acidic solution is 1 to 1.5. Thereby, 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 invention, in the step (1), the reaction temperature is 70 to 90 ℃ and the reaction time is not less than 60min. Thereby, copper and arsenic in the solution can be effectively removed when the copper-arsenic ratio is less than 3.
In some embodiments of the invention, the copper and arsenic removal liquid obtained in the step (3) is returned to the step (2) to be concentrated with the ore pulp. Therefore, the solid-liquid separation can be more thorough.
In some embodiments of the invention, the content of copper in the arsenic-containing filter residue is 30-50 wt%, and the content of arsenic is 10-30 wt%.
In some embodiments of the invention, the liquid after copper and arsenic removal contains Cu less than or equal to 0.2g/L, as less than or equal to 0.1g/L.
Additional aspects and advantages of the invention 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 invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a schematic flow diagram of a method for removing copper arsenic from an arsenic-containing acidic solution according to one embodiment of the invention;
figure 2 is a schematic flow diagram of a method for removing copper arsenic from an acidic copper arsenic-containing solution according to yet another embodiment of the invention.
Detailed Description
The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In a first aspect of the invention, a method is provided for removing copper arsenic from a copper arsenic-containing acidic solution. According to an embodiment of the invention, with reference to fig. 1, the method comprises:
s100: the copper-containing arsenic acid solution, the copper concentrate and the reduced iron powder are subjected to mixed reaction
In the step, the copper-containing arsenic acid solution with the copper-arsenic molar ratio less than 3, the copper-containing arsenic acid solution containing Cu and Cu 2 And carrying out mixed reaction on the copper concentrate of the O and the reduced iron powder to obtain ore pulp. The inventors have found that Cu and Cu 2 The presence of O can promote Cu 3 Of AsThereby effectively removing the copper and the arsenic in the solution under the condition that the copper and 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 30-50 wt% of Cu and 30-50 wt% of Cu 2 And O. The inventors have found that if Cu or Cu is present in the copper concentrate 2 Too low an amount of O will result in insufficient copper being supplied 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 the copper content of the solution. Therefore, by adopting the content of the application, the arsenic in the solution can be effectively removed 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 arsenic acidic solution containing copper is 1-3. The inventors found that if the ratio is too small, the amount of copper in the redox system is insufficient, the molar ratio to arsenic is insufficient, and arsenic precipitation is incomplete; if the ratio is too large, the cost is increased. Therefore, by adopting the ratio, the arsenic in the solution can be effectively removed 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 have found that the effect of removing copper and arsenic is not good if the purity of metallic iron in the reduced iron powder is too low or the particle size of the reduced iron powder is too large.
Further, the ratio of the molar amount of the metallic iron to the molar amount of copper in the copper-containing arsenic acid solution is 1 to 1.5. The inventors have 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 the iron powder is increased, and the production cost is increased. Therefore, the ratio of the application is favorable for Cu in the acid solution 2+ 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 effect of removing copper and arsenic is poor; if the reaction temperature is too high, the energy consumption is increased.
S200: thickening the ore pulp
In the step, the ore pulp is thickened, and the precipitate in the ore pulp is settled under the action of gravity, so that the product containing Cu is obtained 3 As, cu, and a supernatant with a lower copper-arsenic content. Specifically, the thickening process is carried out in a thickening tank. Preferably, a flocculating agent is added in the thickening process, so that the thickening effect is improved, and the thickening time is shortened. It should be noted that the specific type and amount of the flocculant can be selected by those skilled in the art according to actual needs.
S300: carrying out solid-liquid separation on the concentrated bottom flow
In the step, the concentrated bottom flow is subjected to solid-liquid separation, so that the copper and arsenic-removed liquid and the copper and arsenic-containing filter residue can be obtained. Specifically, the content of copper in the filter residue containing copper and arsenic is 30-50 wt%, and the content of arsenic is 10-30 wt%; the Cu content of the solution after copper and arsenic removal 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 those skilled in the art can select the solid-liquid separation according to actual needs, for example, the solid-liquid separation may be pressure filtration. Further, referring to fig. 2, the obtained copper and arsenic removed liquid is returned to step S200 to be concentrated with ore pulp, so that solid-liquid separation can be thorough.
The inventors have found that by adjusting the molar ratio of copper to arsenic to less than 3, a copper-containing arsenic acidic solution containing Cu and Cu 2 And finally, carrying out solid-liquid separation on the concentrated underflow to obtain copper-arsenic-containing liquid and copper-arsenic-containing filter residue, wherein the copper-arsenic-containing filter residue can be directly sold as a product. The application is realized by adding Cu and Cu 2 Copper concentrate of O, cu 2 O, cu can promote the formation of arsenic copper compound, remove arsenic in acid solution thoroughly, and make the solution have less than 3 of copper-arsenic ratioThe copper and arsenic in the copper concentrate are effectively removed, the traditional method for oxidizing and leaching copper concentrate to supplement copper and deposit 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 virulent arsenic hydride is avoided, and the quality of downstream products is improved.
The following embodiments of the present invention are described in detail, and it should be noted that the following embodiments are exemplary only, and are not to be construed as limiting the present invention. In addition, all reagents used in the following examples are commercially available or can 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: will be 100m 3 Arsenic acid solution containing copper (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 of copper concentrate (containing 41wt% Cu and 41wt% Cu 2 O) and 160kg of reduced iron powder (the purity of metallic iron is more than or equal to 95wt%, and the content of the reduced iron powder with the granularity of not more than 200 meshes is not less than 80wt% of the total content of the reduced iron powder) are mixed and reacted (the reaction temperature is 80 ℃, and the reaction time is 60 min), so that ore pulp is obtained;
and 2, step: after the reaction is finished, 0.5kg of flocculating agent is added into the ore pulp, and the ore pulp enters a thickening tank after sedimentation to obtain thickened underflow and supernatant;
and step 3: and (3) filtering the concentrated underflow by using a filter press to obtain a copper and arsenic-removed liquid (containing 0.37g/L of Cu and As0.36g/L) and a copper and arsenic-containing filter residue (containing 56.3wt% of copper and 23.5wt% of arsenic), returning the copper and arsenic-removed liquid to a concentration tank, and taking the copper and arsenic-containing filter residue as a product to be directly sold.
Example 2
Step 1: will be 100m 3 Arsenic acid solution containing copper (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 of copper concentrate (containing 41wt% Cu and 41wt% Cu 2 O) and 160kg of reduced iron powder (the purity of the metallic iron is more than or equal to 95 weight percent)The reduced iron powder with the granularity not more than 200 meshes is not less than 80 weight percent of the total amount of the reduced iron powder, and the ore pulp is obtained after the mixed reaction (the reaction temperature is 90 ℃ and the reaction time is 60 min);
step 2: after the reaction is finished, 0.5kg of flocculating agent is added into the ore pulp, and the ore pulp enters a thickening tank after sedimentation to obtain thickened underflow and supernatant;
and step 3: and (3) filtering the concentrated underflow by using a filter press to obtain a copper and arsenic-removed liquid (containing 0.12g/L of Cu and 0.13g/L of As0) and copper and arsenic-containing filter residue (containing 58.3wt% of copper and 18.5wt% of arsenic), returning the copper and arsenic-removed liquid to a concentration tank, and taking the copper and arsenic-containing filter residue as a product to be directly sold.
Comparative example 1
The difference from example 1 is that without adding copper concentrate, the post-copper and arsenic removing solution (containing Cu 0.45g/L, as 0.75.75 g/L) and the copper and arsenic containing filter residue (containing 55.6wt% of copper and 23.4wt% of arsenic) are obtained, and the post-copper and arsenic removing solution is returned to the thickening tank, and the copper and arsenic containing filter residue can be directly sold as a product.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean 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 invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer 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, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are exemplary and not to be construed as limiting the present invention, and that changes, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. A method for removing copper and arsenic from an acidic copper and arsenic containing solution, comprising:
(1) Carrying out mixed reaction on the copper-arsenic-containing acidic solution, the copper concentrate and the reduced iron powder so as to obtain ore pulp;
(2) Thickening the ore pulp to obtain a thickened underflow and a supernatant;
(3) Carrying out solid-liquid separation on the concentrated bottom flow so as to obtain copper and arsenic removed liquid and copper and arsenic containing filter residue,
wherein, in the step (1), the molar ratio of copper to arsenic of the acid solution containing copper and arsenic is less than 3, and the copper concentrate contains Cu and Cu 2 O。
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: 0.1-0.15 g/L.
3. The method of claim 1, wherein in step (1), said copper concentrate comprises 30 to 50wt% of said Cu and 30 to 50wt% of said Cu 2 O。
4. The method of claim 3, wherein in step (1), said Cu of said copper concentrate is in contact with said Cu 2 The ratio of the total molar amount of O to the molar amount of arsenic in the arsenic acidic solution containing copper is 1-3.
5. The method as set forth in claim 1 or 4, wherein in the step (1), the purity of metallic iron in the fine reduced iron is 95wt% or more, and the fine reduced iron having a particle size of not more than 200 meshes is not less than 80wt% of the total amount of the fine reduced iron.
6. The method of claim 5, wherein the ratio of the molar amount of metallic iron to the molar amount of copper in the arsenic-containing acidic solution is from 1 to 1.5.
7. The method according to claim 1, wherein in the step (1), the reaction temperature is 70 to 90 ℃ and the reaction time is not less than 60min.
8. The method according to claim 1, characterized in that the copper arsenic removal liquid obtained in the step (3) is returned to the step (2) to be concentrated with the ore pulp.
9. The method according to claim 1 or 8, wherein the copper content in the copper-arsenic containing filter residue is 30-50 wt%, and the arsenic content is 10-30 wt%.
10. The method as claimed in claim 1 or 8, wherein the Cu content of the solution after removing Cu and As is less than or equal to 0.2g/L, as and less than or equal to 0.1g/L.
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