Method for recovering alkali, selenium and arsenic in arsenic-alkali residue from antimony smelting

A technology of arsenic-alkali slag and arsenic-alkali slag, which is applied in the field of antimony smelting arsenic-alkali slag disposal, selenium and arsenic, and recovery of alkali from arsenic-alkali slag, which can solve the problem of unrealized component recovery, unstable product components, and affecting glass quality and other issues, to achieve good economic and environmental benefits, high utilization, and reduce production costs

Active Publication Date: 2019-08-20
CENT SOUTH UNIV
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

For example, the sodium arsenate compound salt method is to recover the antimony in the arsenic-alkali slag by water leaching, concentrate and evaporate the leachate to dryness, and dry the physical water to obtain the sodium arsenate compound salt. This compound salt is still a hazardous solid waste, although it can be used as glass Clarifying agent, but the product components are unstable, which is easy to affect the quality of the glass. Now the environmental protection requirements are stricter, and its use is strictly restricted. At the same time, the sodium arsenate compound salt contains valuable components that can be recycled, and relevant recovery of components
CN 200410013369.2 discloses a method for separating and recovering sodium arsenate and alkali by fractional crystallization. The method uses the difference in solubility between sodium arsenate and sodium carbonate at high temperature to realize the separation and recovery of arsenic and alkali. The one-step crystallization product is mainly sodium arsenate At the same time, it also contains a small amount of alkali, and the second-step crystallization product is crude alkali, which is returned to the antimony smelting crude antimony refining dearsenic process, but the crude alkali contains 2.29% arsenic, which will cause a vicious circle of arsenic in the smelting system
CN200410023055.0 discloses a pollution-free arsenic-alkali slag treatment technology, which utilizes CO 2 Dealkalization, the carbonate after washing is returned to antimony smelting, and the aqueous solution system is circulated, but the arsenic content in the carbonate is high, and the arsenic content is still about 1% after washing. In addition, hydrogen sulfide will be produced during the dearsenization of sodium sulfide. The environment is relatively poor, and the sodium sulfate in the dearsenic solution is subsequently treated with barium hydroxide, and the treatment cost is relatively high

Method used

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  • Method for recovering alkali, selenium and arsenic in arsenic-alkali residue from antimony smelting
  • Method for recovering alkali, selenium and arsenic in arsenic-alkali residue from antimony smelting

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The method is used to treat the secondary arsenic-alkali slag of an antimony smelter in Hunan, and the moisture content of the arsenic-alkali slag is 31.2%. Break the arsenic-alkali slag to less than 5mm, then take 1.2kg of arsenic-alkali slag and leaching with water for 1 hour under the conditions of liquid-solid ratio 3mL / g, stirring speed 100r / min and leaching temperature 95°C, filter and wash to obtain antimony slag and arsenic-alkali solution. The alkali leaching rate of arsenic-alkali slag leaching and washing process is 100%, and the leaching rates of As, Sb and Se are 98.4%, 1.8% and 97.9%, respectively. Table 1 shows the content of relevant components in arsenic-alkali slag and antimony slag (dry basis), and Table 2 shows the content of relevant components in arsenic-alkali solution.

[0036] Table 1 Arsenic-alkali slag and antimony slag related component content (%)

[0037]

[0038] Related component content (g / L) in table 2 arsenic alkali solution

[0...

Embodiment 2

[0050] The experimental conditions of the arsenic-alkali slag used in this example, the leaching and washing of the arsenic-alkali slag, and the twice recovery of alkali by carbon dioxide are the same as those in Example 1. Adjust the pH of the secondary crystallization mother liquor to 2.9 with sulfuric acid, heat to 100° C. and keep the temperature for 20 minutes, and filter while it is hot to obtain black selenium and deselenized liquid. The direct yield of selenium is 81.3%, and the content of relevant components in black selenium is shown in Table 4. Show. CO produced during pH adjustment by sulfuric acid 2 Return to the alkali recovery process for recycling.

[0051] The solution after deselenization was fed with SO at 25°C and a stirring speed of 200r / min. 2 Reduce As(V) to As(III), then concentrate the reduced solution by 3.8 times, then cool and crystallize at 25°C, and filter to obtain crude arsenic trioxide and arsenic-removed solution. The direct yield of arsenic...

Embodiment 3

[0055] The method is used to treat the secondary arsenic-alkali slag of an antimony smelter in Hunan, and the moisture content of the arsenic-alkali slag is 29.1%. Crush the arsenic-alkali slag to less than 5mm, then take 1.2kg of arsenic-alkali slag and leaching with water for 1 hour under the conditions of liquid-solid ratio 3.5mL / g, stirring speed 100r / min and leaching temperature 105°C, filter and wash to obtain antimony slag and arsenic-alkali solution. The alkali leaching rate of arsenic-alkali slag leaching and washing process is 100%, and the leaching rates of As, Sb and Se are 99.4%, 2.1% and 98.9%, respectively. Table 5 shows the content of relevant components in arsenic-alkali slag and antimony slag (dry basis), and Table 6 shows the content of relevant components in arsenic-alkali solution.

[0056] Table 5 Arsenic-alkali slag and antimony slag related component content (%)

[0057]

[0058] Related component content (g / L) in table 6 arsenic-alkali mixed solut...

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Abstract

The invention discloses a method for recovering alkali, selenium and arsenic in arsenic-alkali residue from antimony smelting, comprising the following steps: (1) immersing arsenic-alkali residue in water, filtering and washing to obtain antimony slag and an arsenic-alkali solution; (2) concentrating the arsenic-alkali solution until concentration of arsenic is 12-17 g / L, introducing CO2 to obtainsodium hydrogen carbonate and primary crystallization mother liquor, concentrating the primary crystallization mother liquor until concentration of arsenic is 48-60 g / L, and introducing CO2 to obtainsodium hydrogen carbonate and secondary crystallization mother liquor; (3) using acid to regulate pH of the secondary crystallization mother liquor to 1-4, heating and reacting to obtain black selenium and a selenium-removed solution; and (4) carrying out SO2 reduction on the selenium-removed solution, conducting evaporation and concentration, cooling for crystallization and filtering to obtain arsenic trioxide and an arsenic-removed solution. By the above method, efficient recovery of alkali, selenium and arsenic in arsenic-alkali residue is realized, and effective enrichment of antimony isalso realized, oxidation for deep antimony removal is not required, arsenic-alkali separation is thorough, no sodium arsenate composite salt is generated, and acid consumption and use amount of a reducing agent are low. In addition, the process is concise, and the method has good economic and environmental benefits.

Description

technical field [0001] The invention relates to a method for disposing of arsenic-alkali slag from antimony smelting, in particular to a method for recovering alkali, selenium and arsenic from the arsenic-alkali slag, and belongs to the technical field of comprehensive recycling of metallurgical solid waste. Background technique [0002] my country's antimony resource reserves and output both rank first in the world, mainly concentrated in the Lengshuijiang tin mine area of ​​Hunan Province. The antimony ore reserves in this area account for more than 60% of the world's total reserves, and the output of antimony products accounts for 80% of the world's total output. At present, 95% of my country's antimony smelting production adopts pyrometallurgical smelting process. In the crude antimony refining process, soda ash is usually added to remove arsenic to obtain refined antimony, and at the same time, solid waste residue containing arsenic will be produced, that is, arsenic-alk...

Claims

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Application Information

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IPC IPC(8): C01D7/12C01B19/02C01G28/00C22B7/00C22B30/04
CPCC01B19/02C01D7/12C01G28/005C01P2006/80C22B7/006C22B30/04Y02P10/20
Inventor 郑雅杰龙华
Owner CENT SOUTH UNIV
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