Method for separating antimony and iron by extraction-water decomposition in a mixed solution of antimony and iron

A mixed solution and extraction technology, which is applied in the field of non-ferrous metallurgy, can solve the problems of poor separation of antimony and iron, poor selectivity of P204, poor extraction selectivity, etc., achieve complete separation of antimony and iron, reduce reagents The effect of short consumption and process flow

Active Publication Date: 2019-12-31
杨婷
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Problems solved by technology

Patent CN107557579A discloses a method for extracting and separating antimony-iron in an acidic complex antimony-containing solution, which is still a traditional extraction process in essence, and the extraction selectivity is not good under multivalent conditions
In the process of research on the separation process of antimony and iron, Zhang Yinsheng, Wang Chengyan, etc. proposed to use P204 as the extraction agent to extract iron from antimony and iron solution in the paper "P204 Extraction and Separation of Antimony and Iron" published in Nonferrous Metals (Smelting Part). , leaving antimony in the original solution, due to the complex valence state in the solution and the poor selectivity of P204, the extraction rate of iron is only 30% to 50%, while the extraction rate of antimony is as high as about 20%, so the separation of antimony and iron is not complete
[0005] Other replacement methods and evaporation methods have not solved the separation problem of antimony and iron in the mixed high acid solution of antimony and iron

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  • Method for separating antimony and iron by extraction-water decomposition in a mixed solution of antimony and iron
  • Method for separating antimony and iron by extraction-water decomposition in a mixed solution of antimony and iron
  • Method for separating antimony and iron by extraction-water decomposition in a mixed solution of antimony and iron

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Embodiment 1

[0042] This example provides a method for separating antimony and iron by extraction-water decomposition in the mixed solution of antimony and iron.

[0043] The composition (g / L) of the antimony-iron mixed solution as the test raw material is: Sb T 35.2, Sb 5+ 1.29 Fe T 21.4 Fe 3+ 2.08. The acidity is 1.3g / L; the iron powder used for valence adjustment is reduced iron powder with a purity of Fe>98%.

[0044] Specific steps are as follows:

[0045] S1. Valence state adjustment: Weigh 500 mL of the antimony-iron mixed solution of the above ingredients, add 1.2 g of reduced iron powder (1.5 times the theoretical amount), and react at 50 ° C for 2 h; separate the supernatant and analyze the Sb in the solution 5+ and Fe 3+ The concentrations are 0.07g / L and 0.14g / L respectively, and the calculated reduction rates of antimony and iron are 94.57% and 93.27% respectively;

[0046] S2. Extraction: Take all the adjustment solution obtained in step S1, add 200mL of organic phase...

Embodiment 2

[0049] This example provides a method for separating antimony and iron by extraction-water decomposition in the mixed solution of antimony and iron.

[0050] The antimony-iron mixed solution and reduced iron powder as test raw materials are the same as in Example 1.

[0051] Specific steps are as follows:

[0052] S1. Valence state adjustment: Weigh 500mL of antimony-iron solution of the above components, add 0.96g of reduced iron powder (1.2 times the theoretical amount), and react at 70°C for 2h; separate the supernatant and analyze the Sb in the solution 5+ and Fe 3+ The concentrations are 0.09g / L and 0.10g / L respectively, and the calculated reduction rates of antimony and iron are 99.74% and 99.53% respectively;

[0053] S2. Extraction: Take all the adjustment solution obtained in step S1, add 180mL organic phase extractant, and its composition is: N235 concentration is 35.0%, TBP concentration is 17.0%, and sec-octanol concentration is 4.0%. Three countercurrent extrac...

Embodiment 3

[0056] This example provides a method for separating antimony and iron by extraction-water decomposition in the mixed solution of antimony and iron.

[0057] The iron antimony solution and reduced iron powder as test raw materials are the same as in Example 1.

[0058] Specific steps are as follows:

[0059] S1. Valence state adjustment: Weigh 1000mL of the antimony-iron solution of the above components, add 1.76g of reduced iron powder (1.1 times the theoretical amount), and react at 70°C for 1h; separate the supernatant and analyze the Sb in the solution 5+ and Fe 3+ The concentrations are 0.11g / L and 0.14g / L respectively, and the calculated reduction rates of antimony and iron are 91.47% and 93.27% respectively;

[0060] S2. Extraction: Take all the adjusted solution obtained in step S1, and add 500 mL of organic phase extractant, which is composed of: N235 concentration of 25.0%, TBP concentration of 15.0%, and sec-octanol concentration of 6.0%. Carry out four counter-c...

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Abstract

The invention discloses a method for extracting-water-splitting and separating antimony and iron in an antimony-iron mixed solution, belonging to the field of non-ferrous metal metallurgy. The method firstly uses iron powder to reduce high-valent antimony iron ions in an antimony-iron mixed solution to a low-valent iron Divalent iron ion and trivalent antimony ion are filtered and separated to obtain low-valent antimony iron solution, and then use quaternary ammonium salt extractant to extract and separate antimony from it, to obtain antimony-rich organic phase and ferrous raffinate, the latter can be directly opened; The antimony-rich organic phase does not carry out back extraction, but is directly water-decomposed to generate antimony oxychloride, and at the same time, the quaternary ammonium salt extractant is regenerated. The method realizes the separation problem of antimony and iron through valence adjustment and extraction process, and the separation of antimony and iron is complete; and the innovative water splitting step is used to directly complete the dissociation of antimony, which cancels the traditional stripping process and obtains antimony products in one step. and regeneration extraction agent, simplifying the process, reducing the consumption of reagents, and solving the problem of separation and separate utilization of antimony iron solution in the antimony hydrometallurgy process.

Description

technical field [0001] The invention belongs to the field of nonferrous metal metallurgy, and more specifically relates to a method for separating antimony and iron by extraction-water decomposition in a mixed solution of antimony and iron. Background technique [0002] Antimony is widely used in the fields of metallurgy, materials, chemicals, and building materials. my country is the world's largest antimony resource country, accounting for more than 80% of global reserves. The smelting of antimony is mainly based on sulfide ore, mainly including pyrotechnics and wet processes. The pyrotechnic process mainly adopts blast furnace volatilization roasting (smelting)-reduction smelting process, and there is a low concentration of SO 2 With the disadvantages of flue gas pollution, high energy consumption and large amount of smoke and dust, with the increasing environmental protection requirements, this process has not adapted to the development requirements. [0003] Since the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B3/44C22B3/28C22B30/02
CPCC22B3/44C22B30/02C22B3/288Y02P10/20
Inventor 叶龙刚欧阳臻胡宇杰胡洵璞陈艺锋夏志美肖利
Owner 杨婷
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