CN113292051A - Separation and recovery method of arsenic selenide - Google Patents
Separation and recovery method of arsenic selenide Download PDFInfo
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- CN113292051A CN113292051A CN202110524824.9A CN202110524824A CN113292051A CN 113292051 A CN113292051 A CN 113292051A CN 202110524824 A CN202110524824 A CN 202110524824A CN 113292051 A CN113292051 A CN 113292051A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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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
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/045—Leaching using electrochemical 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/12—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions
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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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/04—Obtaining arsenic
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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
- C22B7/00—Working 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
- C22B7/006—Wet processes
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention provides a method for separating and recovering arsenic selenide, and relates to the technical field of resource recovery. The method for separating and recovering the arsenic selenide provided by the invention comprises the following steps: (1) mixing arsenic selenide powder with water, and adding an alkaline compound into a mixing system; (2) adding oxidant into the mixed system until the potential value of the mixed system is-500-300 mv, stirring and filtering to obtain crude selenium and leachate; (3) adding a precipitator into the leaching solution, stirring and filtering to obtain an arsenic-containing compound and an arsenic-precipitating filtrate. Controlling the potential in the oxidation leaching process under the alkaline condition and controlling the oxidation process to recover the selenium in the arsenic selenide defective product in a simple substance form; arsenic is finally recovered in the form of calcium arsenate, and the calcium arsenate can be further used for producing other arsenic-containing products, so that selenium and arsenic are effectively separated and recovered, the selenium and arsenic separation effect is good, and the recovery rate is high; and the recovery process has the advantages of simple equipment, short flow, low cost, safety and environmental friendliness, and is suitable for industrial application.
Description
Technical Field
The invention relates to the technical field of resource recovery, in particular to a method for separating and recovering arsenic selenide.
Background
Arsenic selenide is a black crystal or dark brown solid, of the formula As2Se3Molecular weight of 386.72, specific gravity of 4.75, low toxicity, and important application in infrared optics field. Arsenic selenide is generally obtained by mixing and melting the elements arsenic and selenium according to a proportion, and a certain amount of defective products are generated in the processing process. Selenium is a rare metal and is a raw material for producing selenium compounds, and the selenium compounds are widely used as glass decolorants, colorants, feed additives and the like; in addition, selenium also has important application in the fields of electronics, solar energy and the like, and has high application value. Arsenic and its compounds are not only raw materials for alloy smelting, agricultural chemicals and medicines, pigments and other industries, but also toxic substances, and when not properly utilized, have great harm to the environment and human body. Therefore, the separation and recovery of selenium and arsenic are of great significance for comprehensive utilization of resources, reduction of production cost and prevention and treatment of environmental pollution.
No arsenic selenide recovery method exists at present, and Chinese patent CN108033431A discloses a method for separating and recovering selenium from a chalcogenide glass waste material, wherein strong alkali is adopted for leaching, and leaching solution is mixed with sulfuric acid and an oxidant for precipitating selenium, so that selenium is separated from germanium and arsenic. Needs strong alkali for leaching, needs sulfuric acid in the selenium precipitation step, and has the problems of long flow, large consumption of auxiliary materials, high operation cost and the like.
Disclosure of Invention
The invention mainly aims to provide a method for separating and recovering arsenic selenide, and aims to solve the problems that the current method for recovering selenium and arsenic compounds needs to be leached by strong base, strong acid needs to be added in the selenium precipitation step, and therefore the method has long flow, large auxiliary material consumption, high operation cost and the like.
In order to realize the purpose, the invention provides a method for separating and recovering arsenic selenide, which comprises the following steps:
(1) mixing arsenic selenide powder with water, adding an alkaline compound into a mixed system until the pH value of the mixed system is 11-13, and then heating the mixed system to 60-75 ℃;
(2) adding oxidant into the mixed system until the potential value of the mixed system is-500-300 mv, stirring and filtering to obtain crude selenium and leachate;
(3) adding a precipitator into the leaching solution, stirring and filtering to obtain an arsenic-containing compound and an arsenic-precipitating filtrate.
According to the technical scheme, arsenic selenide powder is used as a recovery raw material, selenium in the arsenic selenide is-2-valent, arsenic is + 3-valent, a proper amount of oxidant is added under an alkaline condition to control the potential to be proper, the selenium is firstly oxidized to be 0-valent, and the arsenic is leached into a solution in a form of + 3-valent or + 5-valent, so that the effective separation of the selenium and the arsenic is realized; then adding a precipitator to the leachate to precipitate arsenic in the form of calcium arsenite or calcium arsenate. Taking the case that the oxidant is hydrogen peroxide and the precipitator is calcium hydroxide, the reaction formula involved in the recovery process is as follows:
As2Se3+6OH-+3H2O2＝3Se↓+2AsO3 3-+6H2O
As2Se3+6OH-+5H2O2＝3Se↓+2AsO4 3-+8H2O
2Na3AsO3+3Ca(OH)2＝Ca3(AsO3)2↓+6NaOH
2Na3AsO4+3Ca(OH)2＝Ca3(AsO4)2↓+6NaOH
according to the technical scheme, by controlling the pH value of the mixed system to be 11-13, strong alkali leaching and consumption of a large amount of auxiliary materials such as acid and alkali are avoided in a weak alkaline system, and meanwhile, harmful gases such as hydrogen selenide and the like can be avoided under the traditional acidic condition by adopting alkaline condition treatment.
As a preferred embodiment of the method for separating and recovering arsenic selenide according to the present invention, the alkaline compound in the step (1) includes at least one of sodium hydroxide, potassium hydroxide, and sodium carbonate.
The inventor finds that the separation effect of selenium and arsenic can be optimized by mixing one or more of sodium hydroxide, potassium hydroxide and sodium carbonate as alkaline compounds with arsenic selenide through a large amount of experimental researches, so that the recovery rates of two metal elements are improved.
As a preferred embodiment of the method for separating and recovering arsenic selenide, in the step (1), the arsenic selenide powder and water are mixed according to the following ratio: and mixing water in a mass ratio of 1: 6-8.
The inventor finds that, after a great deal of experimental research, the arsenic selenide powder: under the solid-liquid ratio of 1: 6-8, the materials can be fully stirred and mixed, and the volume of a mixing system is not too high and waste is avoided while arsenic is fully dissolved.
As a preferred embodiment of the method for separating and recovering arsenic selenide, in the step (1), the arsenic selenide powder comprises the following components in percentage by mass: 61-62% of selenium and 38-39% of arsenic; the particle size of the arsenic selenide powder is 20-50 meshes.
In the technical scheme of the invention, the arsenic selenide used as the recovery raw material comprises the following elements: 61-62% of selenium and 38-39% of arsenic. Through a large number of experimental researches, the inventor discovers that the arsenic selenide is pulverized into powder with the particle size of 20-50 meshes, and the powder can show a better dissolution rate in a subsequent reaction after being mixed with water, so that the leaching efficiency is improved.
As a preferred embodiment of the method for separating and recovering arsenic selenide, in the step (2), the oxidant includes at least one of hydrogen peroxide, potassium permanganate and sodium hypochlorite.
In the technical scheme of the invention, the oxidant can play an oxidizing role under an alkaline condition.
As a preferable embodiment of the method for separating and recovering arsenic selenide, the stirring time in the step (2) is 0.5-1 h, and the stirring time in the step (3) is 0.5-1 h.
In the preferred embodiment of the method for separating and recovering arsenic selenide, in the step (2), the pH value of the mixing system is maintained between 11 and 13, and the temperature of the mixing system is maintained between 60 and 75 ℃.
The weak base condition is favorable for arsenic dissolution, selenium dissolution and auxiliary material saving; the appropriate temperature can provide the reaction power.
As a preferred embodiment of the method for separating and recovering arsenic selenide according to the present invention, in the step (3), the precipitant is any one of calcium hydroxide, calcium oxide, and calcium chloride.
The calcium hydroxide, calcium oxide and calcium chloride have certain solubility, can provide calcium ions and promote arsenic precipitation.
As a preferable embodiment of the method for separating and recovering arsenic selenide, the mass ratio of Ca ions in the precipitator to As ions in the leaching solution is 0.8-0.9: 1.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the technical scheme, the potential in the oxidation leaching process is controlled under the alkaline condition, the oxidation process is controlled, and the selenium in the arsenic selenide defective product is recovered in a simple substance form; arsenic is finally recovered in the form of calcium arsenate, and the calcium arsenate can be further used for producing other arsenic-containing products, so that selenium and arsenic are effectively separated and recovered, the selenium and arsenic separation effect is good, and the recovery rate is high;
(2) the recovery method has the advantages of simple equipment, short flow, low cost, safety and environmental friendliness, and is suitable for industrial application.
Drawings
Fig. 1 is a simplified process flow diagram of the separation and recovery process of arsenic selenide.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the following specific examples.
Example 1
The separation and recovery method of the embodiment comprises the following steps:
(1) crushing and ball-milling inferior arsenic selenide containing 61.3 percent of selenium and 38.7 percent of arsenic by adopting crushing and ball-milling equipment, sieving the inferior arsenic selenide by a 30-mesh sieve to obtain arsenic selenide powder, adding 800mL of water into a reactor, adding 100g of the arsenic selenide powder at the stirring speed of 300r/min, continuously adding sodium hydroxide to adjust the pH value of a mixing system to 11, and heating the mixing system to 60 ℃;
(2) slowly adding hydrogen peroxide into the mixed system obtained in the step (1), stopping adding when the potential value of the mixed system is-500 mv, stirring for 0.5h, controlling the pH value of the mixed system to be 11-13 and the temperature to be 60-75 ℃, and then performing suction filtration to separate first-stage filter residue and leachate, wherein the first-stage filter residue is dried to obtain crude selenium;
(3) adding 56g of calcium hydroxide into the leachate obtained in the step (2), stirring for 0.5h, and filtering to separate second-stage filter residue and arsenic-precipitating filtrate, wherein the second-stage filter residue is dried to obtain the arsenic-containing compound.
The product obtained in each step of this example is shown in table 1 below.
TABLE 1 product condition table obtained in each step of example 1
The calculation method of the selenium recovery rate in the step (2) comprises the following steps: (the mass of the crude selenium is multiplied by the mass fraction of the selenium in the crude selenium)/the mass of the selenium in the raw materials;
the calculation method of the arsenic recovery rate in the step (3) comprises the following steps: (mass of arsenic-containing compound x mass fraction of arsenic in mass of arsenic-containing compound)/mass of arsenic in the raw material;
the calculated recovery rate of selenium in example 1 was 99.3% and the recovery rate of arsenic was 98.1%.
Example 2
The separation and recovery method of the embodiment comprises the following steps:
(1) crushing and ball-milling inferior arsenic selenide containing 61.3 percent of selenium and 38.7 percent of arsenic by adopting crushing and ball-milling equipment, sieving the inferior arsenic selenide by a 30-mesh sieve to obtain arsenic selenide powder, adding 700mL of water into a reactor, adding 100g of the arsenic selenide powder at the stirring speed of 400r/min, continuously adding sodium hydroxide to adjust the pH value of a mixing system to 12, and heating the mixing system to 60 ℃;
(2) slowly adding potassium permanganate into the mixed system obtained in the step (1), stopping adding when the potential value of the mixed system is-400 mv, stirring for 1h, controlling the pH value of the mixed system to be 11-13 and the temperature to be 60-75 ℃, and then performing suction filtration to separate first-stage filter residue and leachate, wherein the first-stage filter residue is dried to obtain crude selenium;
(3) adding 43g of calcium oxide into the leachate obtained in the step (2), stirring for 1h, and filtering to separate second-stage filter residue and arsenic-precipitating filtrate, wherein the second-stage filter residue is dried to obtain the arsenic-containing compound.
The product obtained in each step of this example is shown in table 2 below.
TABLE 2 product condition table obtained in each step of example 2
The method for calculating the recovery rates of selenium and arsenic in this example is the same as that in example 1.
The calculated recovery rate of selenium in example 2 was 98.8% and the recovery rate of arsenic was 98.2%.
Example 3
The separation and recovery method of the embodiment comprises the following steps:
(1) crushing and ball-milling inferior arsenic selenide containing 61.3 percent of selenium and 38.7 percent of arsenic by adopting crushing and ball-milling equipment, sieving the inferior arsenic selenide by a 30-mesh sieve to obtain arsenic selenide powder, adding 600mL of water into a reactor, adding 100g of the arsenic selenide powder at the stirring speed of 500r/min, continuously adding sodium hydroxide to adjust the pH value of a mixed system to 13, and heating the mixed system to 60 ℃;
(2) slowly adding sodium hypochlorite into the mixed system obtained in the step (1), stopping adding when the potential value of the mixed system is-300 mv, stirring for 1h, controlling the pH value of the mixed system to be 11-13 and the temperature to be 60-75 ℃, and performing suction filtration to separate first-stage filter residue and leachate, wherein the first-stage filter residue is dried to obtain crude selenium;
(3) and (3) adding 63g of calcium hydroxide into the leachate obtained in the step (2), stirring for 1h, and filtering and separating second-stage filter residue and arsenic-deposited filtrate, wherein the second-stage filter residue is dried to obtain the arsenic-containing compound.
The product obtained in each step of this example is shown in Table 3 below.
TABLE 3 product condition table obtained in each step of example 3
The method for calculating the recovery rates of selenium and arsenic in this example is the same as that in example 1.
The calculated recovery rate of selenium in example 3 was 98.4% and the recovery rate of arsenic was 98.3%.
Comparative example 1
The separation and recovery method of the comparative example comprises the following steps:
(1) crushing and ball-milling inferior arsenic selenide containing 61.3 percent of selenium and 38.7 percent of arsenic by adopting crushing and ball-milling equipment, sieving the inferior arsenic selenide by a 30-mesh sieve to obtain arsenic selenide powder, adding 800mL of water into a reactor, adding 100g of the arsenic selenide powder at the stirring speed of 300r/min, continuously adding sodium hydroxide to adjust the pH value of a mixing system to 11, and heating the mixing system to 60 ℃;
(2) and (2) slowly adding hydrogen peroxide into the mixed system obtained in the step (1), stopping adding when the potential value of the mixed system is-550 mv, stirring for 0.5h, controlling the pH value of the mixed system to be 11-13 and the temperature to be 60-75 ℃, and performing suction filtration to separate first-stage filter residue and leachate, wherein the first-stage filter residue is dried to obtain crude selenium.
The product obtained in each step of this comparative example is shown in Table 4 below.
TABLE 4 product condition obtained in each step of comparative example 1
The method for calculating the recovery rates of selenium and arsenic in the comparative example is the same as that of example 1.
The calculated result shows that the recovery rate of selenium in the comparative example 1 is 82.1%, the recovery rate of selenium is low, more selenium in the leaching solution cannot be precipitated, and part of arsenic in the leaching residue is not leached, so that the effect is not ideal.
Comparative example 2
The separation and recovery method of the comparative example comprises the following steps:
(1) crushing and ball-milling inferior arsenic selenide containing 61.3 percent of selenium and 38.7 percent of arsenic by adopting crushing and ball-milling equipment, sieving the inferior arsenic selenide by a 30-mesh sieve to obtain arsenic selenide powder, adding 700mL of water into a reactor, adding 100g of the arsenic selenide powder at the stirring speed of 400r/min, continuously adding sodium hydroxide to adjust the pH value of a mixing system to 12, and heating the mixing system to 60 ℃;
(2) slowly adding potassium permanganate into the mixed system obtained in the step (1), stopping adding when the potential value of the mixed system is-250 mv, stirring for 1h, controlling the pH value of the mixed system to be 11-13 and the temperature to be 60-75 ℃, and then performing suction filtration to separate first-stage filter residue and leachate, wherein the first-stage filter residue is dried to obtain crude selenium.
The product obtained in each step of this comparative example is shown in table 5 below.
TABLE 5 product condition obtained in each step of comparative example 2
The method for calculating the recovery rates of selenium and arsenic in the comparative example is the same as that of example 1.
The calculated recovery rate of the selenium in the comparative example 2 is 82.2%, the recovery rate of the selenium is low, more selenium in the leaching solution cannot be precipitated, and the effect is not ideal.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (9)
1. A method for separating and recovering arsenic selenide is characterized by comprising the following steps:
(1) mixing arsenic selenide powder with water, adding an alkaline compound into a mixed system until the pH value of the mixed system is 11-13, and then heating the mixed system to 60-75 ℃;
(2) adding oxidant into the mixed system until the potential value of the mixed system is-500-300 mv, stirring and filtering to obtain crude selenium and leachate;
(3) adding a precipitator into the leaching solution, stirring and filtering to obtain an arsenic-containing compound and an arsenic-precipitating filtrate.
2. The separation and recovery method according to claim 1, wherein the basic compound in the step (1) includes at least one of sodium hydroxide, potassium hydroxide, and sodium carbonate.
3. The separation and recovery method according to claim 1, wherein the arsenic selenide powder and the water in the step (1) are mixed in a ratio of the arsenic selenide powder: and mixing water in a mass ratio of 1: 6-8.
4. The separation and recovery method according to claim 1, wherein the arsenic selenide powder in the step (1) comprises the following components in percentage by mass: 61-62% of selenium and 38-39% of arsenic; the particle size of the arsenic selenide powder is 20-50 meshes.
5. The separation and recovery method according to claim 1, wherein the oxidant in step (2) comprises at least one of hydrogen peroxide, potassium permanganate and sodium hypochlorite.
6. The separation and recovery method according to claim 1, wherein the stirring time in the step (2) is 0.5 to 1 hour, and the stirring time in the step (3) is 0.5 to 1 hour.
7. The separation and recovery method according to claim 1, wherein the pH value of the mixed system in the step (2) is maintained between 11 and 13, and the temperature of the mixed system is maintained between 60 and 75 ℃.
8. The separation and recovery method according to claim 1, wherein the precipitant in the step (3) is any one of calcium hydroxide, calcium oxide and calcium chloride.
9. The separation and recovery method according to claim 8, wherein the mass ratio of Ca ions in the precipitant to As ions in the leachate is 0.8 to 0.9: 1.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101928838A (en) * | 2010-09-08 | 2010-12-29 | 中南大学 | Method for removing and recovering arsenic from lead anode slime |
| CN104911358A (en) * | 2015-06-10 | 2015-09-16 | 中南大学 | Method for separating arsenic and selenium from copper anode slime alkaline leach liquor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101928838A (en) * | 2010-09-08 | 2010-12-29 | 中南大学 | Method for removing and recovering arsenic from lead anode slime |
| CN104911358A (en) * | 2015-06-10 | 2015-09-16 | 中南大学 | Method for separating arsenic and selenium from copper anode slime alkaline leach liquor |
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