CN112458300B - Arsenic-iron separation method of arsenic-iron-containing slag - Google Patents

Arsenic-iron separation method of arsenic-iron-containing slag Download PDF

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CN112458300B
CN112458300B CN202011380113.0A CN202011380113A CN112458300B CN 112458300 B CN112458300 B CN 112458300B CN 202011380113 A CN202011380113 A CN 202011380113A CN 112458300 B CN112458300 B CN 112458300B
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arsenic
iron
slag
filtrate
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CN112458300A (en
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易振鸿
肖超
胡石春
刘静
邓肆桌
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Guizhou Zhongwei Resources Recycling Industry Development Co ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/04Working-up slag
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C22B3/08Sulfuric acid, other sulfurated acids or salts thereof
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006Wet processes
    • C22B7/007Wet processes by acid leaching
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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Abstract

The invention provides a method for separating arsenic from iron in arsenic-containing iron slag, and relates to the field of hydrometallurgy. The arsenic-iron separation method of the arsenic-iron-containing slag comprises the following steps: mixing raw materials including arsenic-containing iron slag and sulfuric acid to obtain a first mixed solution, and performing first solid-liquid separation after a first reaction to obtain a first filtrate; mixing materials including the first filtrate and sodium sulfide to obtain a second mixed solution, and performing second solid-liquid separation after a second reaction to obtain a second filtrate and arsenous sulfide residues; and mixing materials including the second filtrate and hydrogen peroxide, adding an alkaline substance after a third reaction to obtain a third mixed solution, and performing a third solid-liquid separation after a fourth reaction to obtain a third filtrate and iron removing slag. The arsenic-iron separation method for the arsenic-iron-containing slag has the advantages of low treatment cost and good arsenic-iron separation effect, and is beneficial to environment-friendly treatment of arsenic.

Description

Arsenic-iron separation method of arsenic-iron-containing slag
Technical Field
The invention relates to the field of hydrometallurgy, in particular to a method for separating arsenic and iron from arsenic-containing iron slag.
Background
In recent years, with the development of the battery material industry, the domestic demand for nickel sulfate is increasing day by day, and the crude nickel sulfate contains impurities such as iron, copper, zinc, calcium, magnesium and the like, and purification treatment is required for preparing battery-grade nickel sulfate. The oxidation-hydrolysis precipitation method is adopted in industry to remove arsenic and iron in the crude nickel sulfate solution, and a large amount of waste residues containing ferric arsenate precipitates are generated.
Arsenic iron slag is a hazardous waste containing arsenic, which causes environmental pollution and harm to human health, and the arsenic-containing waste must be strictly treated. Therefore, the arsenic content in the iron slag is reduced, arsenic is enriched, arsenic and iron can be separated, the obtained filtrate is free of arsenic, and wastewater treatment is carried out; the amount of arsenic-containing filter residue is reduced, and the environment-friendly centralized disposal is facilitated.
In view of this, the present application is specifically proposed.
Disclosure of Invention
The invention aims to provide a method for separating arsenic and iron from arsenic-containing iron slag, which aims to solve the problems.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a method for separating arsenic and iron from arsenic-containing iron slag comprises the following steps:
mixing raw materials including arsenic-containing iron slag and sulfuric acid to obtain a first mixed solution, and performing first solid-liquid separation after a first reaction to obtain a first filtrate;
mixing materials including the first filtrate and sodium sulfide to obtain a second mixed solution, and performing second solid-liquid separation after a second reaction to obtain a second filtrate and arsenic sulfide residues;
and mixing the materials including the second filtrate and hydrogen peroxide, adding an alkaline substance after a third reaction to obtain a third mixed solution, and performing a third solid-liquid separation after a fourth reaction to obtain a third filtrate and iron-removing slag.
The reaction principle of the arsenic-iron separation method of the arsenic-iron-containing slag provided by the application comprises the following steps:
1. dissolving arsenic-containing iron slag in sulfuric acid;
2FeAsO 3 +3H 2 SO 4 ==Fe 2 (SO 4 ) 3 +2H 3 AsO 3
2. arsenous acid reacts with sodium sulfide to generate arsenic trisulfide which is insoluble in water and inorganic acid;
2H 3 AsO 3 +3Na 2 S==As 2 S 3 ↓+6NaOH
3. adding hydrogen peroxide to oxidize ferrous iron, and precipitating sodium hydroxide to remove iron;
2Fe 2+ +H 2 O 2 +2H + ==2Fe 3+ +2H 2 O
Fe 3+ +3OH - ==Fe(OH) 3 ↓。
preferably, the pH of the first mixed solution is 0.1 to 0.2.
Alternatively, the pH of the first mixed solution may be any value between 0.1, 0.15, 0.2, and 0.1-0.2.
Preferably, the temperature of the first reaction is 80-90 ℃ and the time is 0.5-1.0h.
Alternatively, the temperature of the first reaction may be any value between 80 ℃, 81 ℃, 82 ℃, 83 ℃, 84 ℃, 85 ℃, 86 ℃, 87 ℃, 88 ℃, 89 ℃, 90 ℃ and 80-90 ℃, and the time may be any value between 0.5h, 0.6h, 0.7h, 0.8h, 0.9h, 1.0h and 0.5-1.0h.
Preferably, the mass ratio of the use amount of the sulfuric acid to the arsenic-containing iron slag is (0.10-0.15): 1.
in the dissolving reaction process of the arsenic-containing iron slag (crude nickel sulfate crystal iron slag), only concentrated sulfuric acid which is 0.10-0.15 time of the weight of the arsenic-containing iron slag is needed to be added, which is beneficial to dispersing arsenic and iron in the arsenic-containing iron slag in a solution system in an ion form.
Optionally, the mass ratio of the use amount of the sulfuric acid to the arsenic-containing iron slag may be 0.1: 1. 0.11: 1. 0.12: 1. 0.13: 1. 0.14: 1. 0.15:1 and (0.10-0.15): 1, or any value between.
Preferably, the pH of the second mixed solution is 0.75 to 1.00.
In general, it is believed that arsenic can be removed by directly adding sodium sulfide to obtain arsenic sulfide precipitate, and the amount of sodium sulfide is mainly considered in terms of cost. It has been found that when arsenic and iron are present simultaneously, sodium sulfide cannot be used simply, and the interaction between arsenic and iron needs to be considered: when arsenic and iron exist simultaneously, arsenic is not easy to precipitate under the condition of low pH value; however, sodium sulfide slightly increases the pH of the system to more than 1.0, and even under strongly acidic conditions of 1.1 or 1.2 or more, iron is precipitated together with arsenic, and arsenic and iron cannot be efficiently separated. Therefore, sodium sulfide is added into the arsenic-iron-containing filtrate to adjust the pH value to 0.75-1.00, arsenic sulfide precipitate is generated through reaction, the arsenic precipitation rate reaches 97%, the iron precipitation rate is only 2%, and the arsenic sulfide precipitate stably exists in an acid solution, so that the effect of separating arsenic from iron is achieved. The technology effectively solves the problems that the slag quantity of the arsenic-containing iron slag is large, and the environmental protection treatment cost is high if the arsenic-containing iron slag is completely treated.
Alternatively, the pH of the second mixed solution may be any value between 0.75, 0.8, 0.85, 0.90, 0.95, 1.00, and 0.75-1.00.
Preferably, the time of the second reaction is 30-40min.
Alternatively, the time of the second reaction may be any value between 30min, 35min, 40min and 30-40min.
Preferably, the pH of the third mixed solution is 3.5 to 4.5;
preferably, the alkaline substance comprises sodium hydroxide.
Alternatively, the pH of the third mixed solution may be any value between 3.5, 4, 4.5, and 3.5-4.5.
Preferably, the temperature of the fourth reaction is 80-90 ℃ and the time is 0.5-1h.
Alternatively, the temperature of the fourth reaction may be any value between 80 ℃, 85 ℃, 90 ℃ and 80-90 ℃, and the time may be any value between 0.5h, 0.6h, 0.7h, 0.8h, 0.9h, 1h and 0.5-1h.
Preferably, the dosage of the hydrogen peroxide is used for oxidizing Fe in the second filtrate 2+ 2.5-3 times the theoretical amount required.
Optionally, the amount of the hydrogen peroxide is used for oxidizing Fe in the second filtrate 2+ 2.5 times, 2.6 times, 2.7 times, 2.8 times, 2.9 times, 3 times and any value between 2.5 and 3 times the theoretical amount required.
Preferably, the arsenic-containing iron slag is arsenic-containing iron slag obtained in a crude nickel refining process.
Compared with the prior art, the invention has the beneficial effects that:
according to the arsenic-iron separation method for the arsenic-iron slag, arsenic, hydrogen peroxide ferrous oxide ions and alkaline substances are removed through sulfuric acid dissolution, sodium sulfide and arsenic reaction, so that the removal rate of arsenic in the arsenic-iron slag with low iron content (the mass ratio of iron to arsenic is less than or equal to 15) reaches 97% or more, the problem that iron and arsenic are difficult to separate under the condition of low iron content is solved, and the purposes of arsenic-iron separation and arsenic centralized treatment are achieved; the method has the advantages of simple process, low material consumption and low cost, and reduces the arsenic slag treatment capacity and the treatment cost thereof.
Detailed Description
The terms as used herein:
"by 8230; \ 8230; preparation" is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of 823070, 8230composition" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of 8230' \8230"; composition "appears in a clause of the subject matter of the claims and not immediately after the subject matter, it defines only the elements described in the clause; no other elements are excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the recited range should be interpreted to include ranges of "1 to 4," "1 to 3," "1 to 2 and 4 to 5," "1 to 3 and 5," and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
In the examples, the parts and percentages are by mass unless otherwise indicated.
"part by mass" means a basic unit of measure indicating a mass ratio of a plurality of components, and 1 part may represent an arbitrary unit mass, for example, 1g or 2.689 g. If we say that the part by mass of the component A is a part by mass and the part by mass of the component B is B part by mass, the ratio of the part by mass of the component A to the part by mass of the component B is a: b. alternatively, the mass of the A component is aK and the mass of the B component is bK (K is an arbitrary number, and represents a multiple factor). It is unmistakable that, unlike the parts by mass, the sum of the parts by mass of all the components is not limited to 100 parts.
"and/or" is used to indicate that one or both of the illustrated conditions may occur, e.g., a and/or B includes (a and B) and (a or B).
Embodiments of the present invention will be described in detail below with reference to specific examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
The embodiment provides an arsenic-iron separation method of arsenic-iron-containing slag in a crude nickel refining process, which comprises the following steps:
the arsenic-containing iron slag has the following components in table 1:
TABLE 1 arsenic and iron slag composition table (unit: wt%)
Ni Fe As Moisture content Others are
0.20 3.88 0.70 46.49 48.73
Firstly, preparing a solution containing ferric sulfate and arsenate: dissolving 2kg of arsenic-containing iron slag in 240 ml of concentrated sulfuric acid, controlling the final pH to 0.1, slowly heating to 80 ℃, stirring for reacting for 1 hour, stopping the reaction, and filtering to obtain a filtrate;
step two, adding 440g of sodium sulfide into the filtrate obtained in the step one to adjust the pH value of the solution to 0.8, reacting for 30 minutes, and filtering to obtain arsenous sulfide residues and filtrate;
the composition of the arsenous sulfide slag is shown in the following table 2:
TABLE 2 ingredient table of Sulfurized arsenous slag (unit: wt%)
Ni Fe As Moisture content Others
0.091 0.46 3.71 43.26 52.48
And step three, adding hydrogen peroxide into the filtrate obtained in the step two to oxidize ferrous iron into ferric iron, adding liquid alkali to precipitate iron ions, controlling the end point pH value to be 4.5, controlling the reaction temperature to be 90 ℃, continuing to react for 0.5 hour, and filtering to obtain filtrate and iron-removing slag.
The components of the iron-removing slag are shown in the following table 3:
TABLE 3 composition of iron-removing slag (unit: wt%)
Ni Fe As Moisture content Others
0.16 4.55 0.02 47.22 48.05
Example 2
The embodiment provides an arsenic-iron separation method of arsenic-iron-containing slag in a crude nickel refining process, which comprises the following steps:
the composition of arsenic-containing iron slag was the same as in example 1.
Firstly, preparing a solution containing ferric sulfate and arsenate: dissolving 2kg of arsenic-containing iron slag in 230 ml of concentrated sulfuric acid, controlling the final pH to 0.2, slowly heating to 90 ℃, stirring for reacting for 0.5 hour, stopping the reaction, and filtering to obtain a filtrate;
step two, adding 445g of sodium sulfide into the filtrate obtained in the step one to adjust the pH value of the solution to 0.75, reacting for 32 minutes, and filtering to obtain arsenous sulfide residues and filtrate;
the composition of the arsenous sulphide slag is shown in Table 4 below:
TABLE 4 ingredients of arsenous sulfide slag Table (Unit: wt%)
Ni Fe As Moisture content Others
0.01 0.38 5.12 46.95 47.54
And step three, adding hydrogen peroxide into the filtrate obtained in the step two to oxidize ferrous iron into ferric iron, adding liquid alkali to precipitate iron ions, controlling the end point pH value to be 3.5 and the reaction temperature to be 80 ℃, continuing to react for 1.0 hour, and filtering to obtain filtrate and iron-removing slag.
The components of the iron-removing slag are shown in the following table 5:
TABLE 5 composition table of iron-removing slag (unit: wt%)
Ni Fe As Moisture content Others are
0.19 6.23 0.017 47.0 46.56
Example 3
The embodiment provides an arsenic-iron separation method of arsenic-iron-containing slag in a crude nickel refining process, which comprises the following steps:
the composition of arsenic-containing iron slag was the same as in example 1.
Firstly, preparing a solution containing ferric sulfate and arsenate: dissolving 2kg of arsenic-containing iron slag in 235 ml of concentrated sulfuric acid, controlling the final pH to 0.15, slowly heating to 85 ℃, stirring for reacting for 0.8 hour, stopping the reaction, and filtering to obtain a filtrate;
step two, adding 430g of sodium sulfide into the filtrate obtained in the step one to adjust the pH value of the solution to 0.9, reacting for 35 minutes, and filtering to obtain arsenous sulfide residues and filtrate;
the composition of the arsenous sulfide slag is shown in Table 6 below:
TABLE 6 ingredients of arsenous sulfide slag Table (Unit: wt%)
Ni Fe As Moisture content Others
0.015 0.27 5.67 45.30 48.75
And step three, adding hydrogen peroxide into the filtrate obtained in the step two to oxidize ferrous iron into ferric iron, adding liquid alkali to precipitate iron ions, controlling the end point pH value to be 4.0, controlling the reaction temperature to be 85 ℃, continuously reacting for 0.8 hour, and filtering to obtain filtrate and iron-removing slag.
The components of the iron-removing slag are shown in the following table 7:
TABLE 7 composition of iron-removing slag (unit: wt%)
Ni Fe As Moisture content Others
0.29 6.80 0.014 46.00 46.90
Example 4
The embodiment provides an arsenic-iron separation method of arsenic-iron-containing slag in a crude nickel refining process, which comprises the following steps:
the composition of the arsenic-containing iron slag was the same as in example 1.
Firstly, preparing a solution containing ferric sulfate and arsenate: dissolving 2kg of arsenic-containing iron slag in 233 ml of concentrated sulfuric acid, controlling the final pH to 0.17, slowly heating to 82 ℃, stirring for reacting for 0.6 hour, stopping the reaction, and filtering to obtain a filtrate;
step two, adding 420g of sodium sulfide into the filtrate obtained in the step one to adjust the pH value of the solution to 1.0, reacting for 40 minutes, and filtering to obtain arsenic sulfide slag and filtrate;
the composition of the arsenous sulphide slag is shown in Table 8 below:
TABLE 8 ingredients of arsenous sulfide slag Table (Unit: wt%)
Ni Fe As Moisture content Others
0.03 0.25 4.89 47.5 43.73
And step three, adding hydrogen peroxide into the filtrate obtained in the step two to oxidize ferrous iron into ferric iron, adding liquid alkali to precipitate iron ions, controlling the end point pH value to be 4.2 and the reaction temperature to be 82 ℃, continuing to react for 0.6 hour, and filtering to obtain filtrate and iron-removing slag.
The components of the iron-removing slag are shown in the following table 9:
TABLE 9 composition of iron-removing slag (unit: wt%)
Ni Fe As Moisture content Others
0.28 5.64 0.01 48.10 45.97
Comparative example 1
The embodiment provides an arsenic-iron separation method of arsenic-iron-containing slag in a crude nickel refining process, which comprises the following steps:
the composition of the arsenic-containing iron slag was the same as in example 1.
Firstly, preparing a solution containing ferric sulfate and arsenate: dissolving 2kg of arsenic-containing iron slag in 233 ml of concentrated sulfuric acid, controlling the final pH to 0.17, slowly heating to 82 ℃, stirring for reacting for 0.6 hour, stopping the reaction, and filtering to obtain a filtrate;
step two, adding 408g of sodium sulfide into the filtrate obtained in the step one to adjust the pH value of the solution to 0.7, reacting for 40 minutes, and filtering to obtain arsenous sulfide residue and filtrate;
the composition of the arsenous sulfide slag is shown in Table 10 below:
TABLE 10 ingredients of arsenic sulfide slag Table (Unit: wt%)
Ni Fe As Moisture content Others
0.03 0.87 2.54 47.0 49.56
And step three, adding hydrogen peroxide into the filtrate obtained in the step two to oxidize ferrous iron into ferric iron, adding liquid alkali to precipitate iron ions, controlling the end point pH value to be 4.2 and the reaction temperature to be 82 ℃, continuing to react for 0.6 hour, and filtering to obtain filtrate and iron-removing slag.
The components of the iron-removing slag are shown in the following table 11:
TABLE 11 composition of iron-removing slag (unit: wt%)
Ni Fe As Moisture content Others
0.28 4.72 1.25 48.5 45.25
Comparative example 2
The embodiment provides an arsenic-iron separation method of arsenic-iron-containing slag in a crude nickel refining process, which comprises the following steps:
the composition of arsenic-containing iron slag was the same as in example 1.
Firstly, preparing a solution containing ferric sulfate and arsenate: dissolving 2kg of arsenic-containing iron slag in 233 ml of concentrated sulfuric acid, controlling the final pH to 0.17, slowly heating to 82 ℃, stirring for reacting for 0.6 hour, stopping the reaction, and filtering to obtain a filtrate;
step two, adding 436g of sodium sulfide into the filtrate obtained in the step one to adjust the pH value of the solution to 1.2, reacting for 40 minutes, and filtering to obtain arsenous sulfide residues and filtrate;
the composition of the arsenous sulfide slag is shown in Table 12 below:
TABLE 12 arsenic sulfide slag composition Table (unit: wt%)
Ni Fe As Moisture content Others are
0.03 1.85 2.11 47.5 48.51
And step three, adding hydrogen peroxide into the filtrate obtained in the step two to oxidize ferrous iron into ferric iron, adding liquid alkali to precipitate iron ions, controlling the end point pH value to be 4.2, controlling the reaction temperature to be 82 ℃, continuing to react for 0.6 hour, and filtering to obtain filtrate and iron-removing slag.
The components of the iron-removing slag are shown in the following table 13:
TABLE 13 composition of iron-removing slag (unit: wt%)
Ni Fe As Moisture content Others
0.28 4.24 1.96 49.0 44.52
From the examples 1 to 4, it can be known that after arsenic-containing iron slag is dissolved by adding sulfuric acid, arsenic can be selectively precipitated by adding sodium sulfide while iron is not precipitated by controlling the temperature and acidity range of the reaction system, so that arsenic is enriched and the purpose of arsenic-iron separation is achieved; as can be seen from comparative example 1, when the pH value of the sodium sulfide adjusted in the second step is less than 0.75, the arsenic content of the generated arsenic sulfide slag is not high and iron is attached, and when the process enters the third step, the arsenic content of the generated iron slag is high; as can be seen from comparative example 2, when the pH value of the sodium sulfide in the second step is adjusted to be greater than 1.0, the arsenic content of the generated arsenic sulfide slag is not high and iron is attached, and when the process enters the third step, the arsenic content of the generated iron slag is high, so that a good iron-arsenic separation effect cannot be obtained.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Furthermore, those skilled in the art will appreciate that while some embodiments herein include some features included in other embodiments, rather than other features, combinations of features of different embodiments are meant to be within the scope of the invention and form different embodiments. For example, in the claims above, any of the claimed embodiments may be used in any combination. The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.

Claims (1)

1. A method for separating arsenic and iron from arsenic-containing iron slag, which is characterized by comprising the following steps:
mixing raw materials including arsenic-containing iron slag and sulfuric acid to obtain a first mixed solution, and carrying out first solid-liquid separation after a first reaction to obtain a first filtrate; the arsenic-containing iron slag is obtained in the crude nickel refining process, the pH value of the first mixed solution is 0.1-0.2, and the mass ratio of the use amount of the sulfuric acid to the arsenic-containing iron slag is (0.10-0.15): 1; the temperature of the first reaction is 80-90 ℃, and the time is 0.5-1.0h;
the composition of the arsenic-containing iron slag is shown in the following table (unit: wt%):
Ni Fe As moisture content Others 0.20 3.88 0.70 46.49 48.73
Mixing materials including the first filtrate and sodium sulfide to obtain a second mixed solution, and performing second solid-liquid separation after a second reaction to obtain a second filtrate and arsenous sulfide residues; the pH of the second mixed solution is 0.75-1.00; the time of the second reaction is 30-40min;
mixing materials including the second filtrate and hydrogen peroxide, adding an alkaline substance after a third reaction to obtain a third mixed solution, and performing a third solid-liquid separation after a fourth reaction to obtain a third filtrate and iron-removing residues; the pH value of the third mixed solution is 3.5-4.5, and the dosage of the hydrogen peroxide is used for oxidizing Fe in the second filtrate 2+ 2.5-3 times the theoretical amount required; the alkaline substance comprises sodium hydroxide; the temperature of the fourth reaction is 80-90 ℃ and the time is 0.5-1h.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101041498A (en) * 2007-04-29 2007-09-26 东北大学 Method for reclaiming valuable element from acidic arsenic-containing biological oxidation gold extraction waste liquor
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