Method for separating and recycling sulfur, iron and selenium from selenic acid mud

A technology for selenium acid sludge and selenium recovery, which is applied in the fields of iron, separation and recovery of sulfur and selenium, can solve the problems of low comprehensive utilization rate of elemental sulfur and complicated procedures, and achieve the effects of energy saving, simple equipment and easy operation.

Inactive Publication Date: 2010-02-17
CENT SOUTH UNIV
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AI Technical Summary

Problems solved by technology

At present, pyrometallurgy processes such as fluidized roasting are mainly used in China. Although the desulfurization rate is high, the conversion of elemental sulfur into SO 2 Secondly, selenium can be separated from other impurities by solvent extraction, vacuum distillation, ion exchange, soda ash roasting, etc., but these processes are suitable for processing materials with low selenium grades, complex procedures and comprehensive synthesis of elemental sulfur. Disadvantages such as low utilization rate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] (1) Get selenium-containing mud 100g, analyze that sulfur content is 23.80% in the slag; Selenium content is 9.10%; Iron content is 28.92%; Add kerosene control temperature and be 65 ℃, be 6: 1 at liquid-solid ratio Under the conditions, react for 0.5h; immediately filter and separate the hot kerosene rich in elemental sulfur and the desulfurization residue rich in selenium and iron; obtain 88.69g of desulfurization residue, the sulfur content in the desulfurization residue is 14.08%, the selenium content is 10.26%, The iron content is 32.61%;

[0016] (2) Add the desulfurization slag obtained above into a mixed solution containing 250 g / L sulfuric acid and 50 g / L sodium chlorate, under the condition of controlling the liquid-solid ratio to 4:1, the temperature is 80°C, react for 2 hours, filter, separate and oxidize Leaching solution and iron-containing residue; the concentration of selenium in the oxidation leaching solution reaches 29.08g / L, and the concentration of ...

Embodiment 2

[0023] (1) get selenium-containing mud 100g, analyze sulfur content in the slag and be 23.80%; Under the conditions, react for 0.5h; immediately filter and separate the hot kerosene rich in elemental sulfur and the desulfurization residue rich in selenium and iron; obtain 82.50 g of desulfurization residue, the sulfur content in the desulfurization residue is 7.64%, the selenium content is 11.03%, Iron content is 35.05%;

[0024] (2) Add the desulfurization slag obtained above into a mixed solution containing 350 g / L sulfuric acid and 150 g / L sodium chlorate, under the condition of controlling the liquid-solid ratio to 3:1, the temperature is 80°C, react for 2 hours, filter, separate and oxidize Leaching solution and iron-containing residue; the concentration of selenium in the oxidation leaching solution reaches 34.58g / L, and the concentration of iron reaches 6.83g / L;

[0025] (3)(3) The oxidation leachate obtained above is successively added sodium sulfite and 30g / L thioure...

Embodiment 3

[0029] (1) get selenium-containing mud 100g, analyze sulfur content in the slag and be 23.80%; Under the conditions, react for 0.5h; immediately filter and separate the hot kerosene rich in elemental sulfur and the desulfurization residue rich in selenium and iron; obtain 76.50 g of desulfurization residue, the selenium content in the desulfurization residue is 11.90%, and the iron content is 37.80%;

[0030] (2) Add the desulfurization slag obtained above into a mixed solution containing 300 g / L sulfuric acid and 100 g / L sodium chlorate, under the condition of controlling the liquid-solid ratio to 5:1, the temperature is 80°C, react for 2 hours, filter, separate and oxidize Leaching solution and iron-containing residue; the concentration of selenium in the oxidation leaching solution reaches 42.18g / L, and the concentration of iron reaches 9.55g / L;

[0031] (3) adding sodium sulfite and 18g / L thiourea to the oxidized leachate obtained above, and reducing to obtain selenium-pre...

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Abstract

The invention discloses a method for separating and recycling sulfur, iron and selenium from selenic acid mud, which comprises the following steps: firstly, adding elemental sulfur soaked in keroseneinto selenic acid mud, filtering and separating hot kerosine containing the elemental sulfur and desulfurization slag containing selenium and iron; separating the elemental sulfur out after cooling the hot kerosene; secondly, adding the desulfurization slag containing selenium and iron to a mixture solution of sulfuric acid and sodium chlorate, filtering and separating oxidized leaching solution and residual slag containing iron, adding sodium sulfite and thiourea into the oxidized leaching solution sequentially, and finally obtaining coarse selenium and a solution after selenium sunk throughreduction. The total recovery rate of sulfur is 97- 98%, the grade of selenium reaches 92-93%, and the total recovery rate of selenium is 94-95%. The invention has the advantages of convenient operation, simple equipment and high value in application.

Description

technical field [0001] The invention relates to a method for separating and recovering sulfur, iron and selenium from selenium-containing mud. Background technique [0002] The selenium-containing mud in the production of sulfuric acid from pyrite has a relatively high sulfur content, and appropriate methods are used to separate and recycle the sulfur from valuable metals such as selenium and iron, both in terms of resource recovery and environmental protection. are all positive. At present, pyrometallurgy processes such as fluidized roasting are mainly used in China. Although the desulfurization rate is high, the conversion of elemental sulfur into SO 2 Secondly, selenium can be separated from other impurities by solvent extraction, vacuum distillation, ion exchange, soda ash roasting, etc., but these processes are suitable for processing materials with low selenium grades, complex procedures and comprehensive synthesis of elemental sulfur. Disadvantages such as low utili...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/033C01B19/02
Inventor 张宝李倩彭春丽沈超张佳峰
Owner CENT SOUTH UNIV
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