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Method for preparing arsenic trioxide by utilizing arsenic sulfide residues

A technology of arsenic trioxide and arsenic sulfide, which is applied in arsenic oxide/arsenic hydroxide/oxyacid arsenic, chemical instruments and methods, arsenic compounds, etc. The problems of high consumption and price, to achieve the effect of saving equipment investment and production costs, efficient extraction and recycling, and broad prospects for industrial application

Inactive Publication Date: 2019-07-19
CENT SOUTH UNIV +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, there are two main methods for preparing arsenic trioxide from arsenic sulfide slag: (1) fire treatment such as redox roasting to recover arsenic in the form of arsenic trioxide, which has the advantages of mature technology and short process, but there is environmental pollution Serious, high investment costs and other shortcomings have been basically eliminated; 2) wet treatment, wet treatment in the prior art mainly includes copper sulfate replacement method, oxygen pressure leaching method, alkali leaching method and high iron sulfate method, etc., but these There are still many shortcomings in the method, such as the consumption of copper powder in the copper sulfate replacement method is large, the copper recovery is difficult, and the cost is high
[0005] The arsenic sulfide slag is leached by oxygen pressure leaching, and then passed through a reducing agent such as SO 2 Preparation of arsenic trioxide by reduction, but the oxidation efficiency is low, and the high-salt process requires high equipment, and new impurities need to be introduced, which will affect the quality of arsenic trioxide, and further purification is required
Alkaline leaching method is incomplete and the consumption and price of sodium hydroxide are high. The process of ferric sulfate method is complicated and costly. The iron in the prepared arsenic trioxide is easy to exceed the standard, which makes the purity and whiteness difficult to meet the requirements.
[0006] The Chinese invention patent application with the application number 201710203220.8 discloses a process for extracting arsenic from arsenic sulfide waste residue by an all-wet method. Specifically, oxygen is used to perform high-pressure leaching of arsenic filter cake, and then the arsenic filter cake is used to reduce the oxygen pressure leaching solution to prepare arsenic trioxide. However, there are also high oxygen pressure leaching temperatures, low leaching efficiency, and the need to use high-pressure equipment, which requires high equipment investment.

Method used

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  • Method for preparing arsenic trioxide by utilizing arsenic sulfide residues
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Embodiment 1

[0037] Embodiments of the present invention provide a method for preparing arsenic trioxide from arsenic sulfide slag, such as figure 1 As shown, it specifically includes the following steps:

[0038] (1) Fully mix the arsenic sulfide slag with a content of 40% and water, and the water consumption is calculated as 200ml / 100g (arsenic sulfide slag), and slowly add hydrogen peroxide (mass fraction is 30%) in a water bath at 60°C with stirring. , for oxidation, the oxidation time is 60min, 30% hydrogen peroxide is calculated as 300g / 100g arsenic sulfide slag, after the oxidation reaction is completed, the solution is filtered and the filtrate is collected, the arsenic content of the obtained filter residue is 98%. Pentavalent arsenic accounts for 92% of the total arsenic in the filtrate;

[0039](2) adding an equivalent mass ratio of 40% arsenic sulfide slag to the filtrate obtained in step (1), mixing fully, that is, the content of arsenic sulfide added in step (2) is equal to ...

Embodiment 2

[0042] The embodiment of the present invention provides a method for preparing arsenic trioxide by using arsenic sulfide slag, which specifically includes the following steps:

[0043] (1) Mix arsenic sulfide residue with 50% arsenic sulfide slag and water fully, the water consumption is calculated as 300ml / 100g arsenic sulfide slag, slowly add 30% hydrogen peroxide in a water bath at 80°C under agitation, and oxidize, and the oxidation time For 15 minutes, 30% hydrogen peroxide is calculated as 400g / 100g of arsenic sulfide slag. After the oxidation reaction is completed, the solution is filtered and the filtrate is collected. The arsenic content of the obtained filter residue is 98%. 95% of total arsenic;

[0044] (2) to step (1) gained filtrate, add the content of equivalent mass proportion to be 50% arsenic sulfide slag and mix fully, and water bath pan reduces reaction at 72 ℃, and the molar concentration of arsenic sulfide in the control reaction system is 0.3028mol / L, ...

Embodiment 3

[0047] The embodiment of the present invention provides a method for preparing arsenic trioxide by using arsenic sulfide slag, which specifically includes the following steps:

[0048] (1) Mix arsenic sulfide residue with 60% arsenic sulfide slag and water fully, the water consumption is calculated as 400ml / 100g arsenic sulfide slag, slowly add 30% hydrogen peroxide in a water bath at 70°C under agitation, and oxidize, and the oxidation time For 45 minutes, 30% hydrogen peroxide is calculated as 500g / 100g of arsenic sulfide slag. After the oxidation reaction is completed, the solution is filtered and the filtrate is collected. The arsenic content of the obtained filter residue is 98%. The pentavalent arsenic in the obtained filtrate accounts for 99% of total arsenic;

[0049] (2) Add the arsenic sulfide slag with the content of 60% to the filtrate obtained in step (1) and mix fully, and a reduction reaction occurs in a water bath at 90° C., and the reduction reaction time is 4...

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Abstract

The invention discloses a method for preparing arsenic trioxide by utilizing arsenic sulfide residues. The method comprises the following steps: oxidizing arsenic sulfide residues with hydrogen peroxide under atmospheric conditions, filtering and collecting the filtrate; oxidizing the arsenic sulfide residues with the filtrate, and filtering and collecting the filtrate; evaporating and concentrating, cooling and crystallizing, thereby obtaining the arsenic trioxide. According to the method disclosed by the invention, the arsenic sulfide residues are oxidized with the hydrogen peroxide, the operation is rapid and efficient, the arsenic sulfide residues are oxidized with the product, heat produced by the oxidization process of the hydrogen peroxide is favorable for latter reactions, any newimpurity is not introduced in the whole process, and the purity of the obtained arsenic trioxide is higher than 99%. The filtrate containing pentavalent arsenic doped with specific residual hydrogen peroxide is oxidized again, and the reaction temperature and the concentration of arsenic sulfide in the reaction system are controlled, so that the oxidizing reaction efficiency can be effectively improved, and the recycling rate of the arsenic sulfide can be effectively improved by controlling the content of SO4<2-> in the recycled arsenic sulfide residues; secondary pollution in the process is avoided, high-pressure equipment is not needed, the cost is reduced, the conditions are simple and mild, and the application prospects are excellent.

Description

technical field [0001] The invention belongs to the technical field of resource waste recycling, and relates to the recycling technology of arsenic sulfide slag, in particular to a method for preparing arsenic trioxide by using arsenic sulfide slag. Background technique [0002] Non-ferrous metal smelting ores are mainly sulfide ores. During pyro-smelting (including drying, sintering, roasting, smelting, blowing, fuming, volatilization, casting, etc.), a large amount of flue gas containing sulfur dioxide will be produced. The smelting flue gas is mainly It is used to prepare sulfuric acid; at the same time, smoke is also carried in the flue gas. In order to ensure the quality of sulfuric acid, impurities such as smoke and dust must be removed from the flue gas. Flue gas is usually treated by a combination of dry and wet methods. Wet dust collection makes the dust and water fully contact, and impurities such as arsenic dust, sulfur trioxide, fluorine, and chlorine in the flue...

Claims

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Application Information

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IPC IPC(8): C01G28/00
CPCC01G28/005C01P2006/80
Inventor 王庆伟曲胜利潘青林柴立元高伟荣李青竹岑家山蒋国民董准勤郑九林
Owner CENT SOUTH UNIV
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