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A method for selectively removing iron from an antimony electrolyte and preparing ferrous oxalate

A ferrous oxalate and electrolyte technology, which is applied in carboxylate preparation, carboxylate preparation, chemical instruments and methods, etc., can solve the problems of large change in solution system, high acidity, and large amount of solution, and achieves no production of bismuth. The effect of secondary pollution

Inactive Publication Date: 2018-04-10
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The antimony slurry electrolyte is antimony-containing hydrochloric acid solution with high acidity (hydrochloric acid concentration 0.5-1mol / L) and low iron content (total Fe concentration 6-10g / L). The amount is large, and the acid loss is large, and the cost is high
Although the iron in the electrolyte can be removed by the above-mentioned iron removal method, it not only needs to change the electrolyte system, but also causes a large amount of loss of antimony, which makes it difficult to realize the selective separation of iron, which is not conducive to the recycling of the electrolyte and the removal of antimony. Recovery and Comprehensive Utilization of Heavy Iron Products
Although the Chinese patent CN200810241902.9 proposes a method for preparing ferrous oxalate by pickling waste liquid, this method needs to adjust the pH value of the solution system, and also needs to add iron filings to regulate the acidity of the waste liquid. The process is complicated and greatly changes the solution system. , it is difficult to meet the requirements of iron removal by antimony slurry electrolyte
However, there is no literature report on the selective iron removal method of antimony ore slurry electrolyte with the above characteristics.

Method used

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  • A method for selectively removing iron from an antimony electrolyte and preparing ferrous oxalate
  • A method for selectively removing iron from an antimony electrolyte and preparing ferrous oxalate
  • A method for selectively removing iron from an antimony electrolyte and preparing ferrous oxalate

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Effect test

Embodiment 1

[0033] Take 100mL of antimony electrolyte from an enterprise. The main components of the antimony electrolyte are: Sb 22.8, Fe13.6 in g / L, and the pH value of the electrolyte is 0.5; Sodium sulfite, the content of sodium sulfite is ≥96% by mass percentage.

[0034]Raise the temperature of the antimony electrolyte to 80°C, add oxalic acid under strong stirring conditions, the ratio of the molar amount of oxalic acid added to the total molar amount of iron and antimony ions in the electrolyte is 2:1, and the reaction time is 2h. Add sodium sulfite to the electrolyte under strong stirring, control the ratio of sodium sulfite to the total molar mass of iron and antimony ions to be 0.9:1, control the reaction temperature to 80°C, and keep the solution at 80°C to remove iron after 0.5h of reaction slag and high temperature filtrate. The high-temperature filtrate was naturally cooled to normal temperature, and filtered to obtain oxalate crystals and liquid after crystallization. Ox...

Embodiment 2

[0036] Take 100mL of antimony electrolyte from a certain enterprise. The main components of antimony electrolyte in g / L are: Sb 22.8, Fe13.6, electrolyte pH<0.5; industrial sodium oxalate, sodium oxalate content ≥ 99% by mass percentage; Industrial potassium sulfite, potassium sulfite content ≥ 98% by mass percentage.

[0037] Raise the temperature of the antimony electrolyte to 60°C, add sodium oxalate under strong stirring conditions, the ratio of the molar amount of sodium oxalate added to the total molar amount of iron and antimony ions in the electrolyte is 1.5:1, and the reaction time is 3h. Add potassium sulfite to the electrolyte under strong stirring, control the ratio of potassium sulfite to the total molar amount of iron and antimony ions to 0.6:1, control the reaction temperature to 85°C, and keep the solution at 80°C while it is hot after reacting for 0.5h Filtrate to obtain iron removal slag and high temperature filtrate. The high-temperature filtrate was natura...

Embodiment 3

[0039] Take 100mL of antimony electrolyte from an enterprise. The main components of the antimony electrolyte are: Sb 20.8, Fe20.7 in g / L. Electrolyte pH<0.5; industrial potassium oxalate, potassium oxalate content ≥99% by mass percentage; industrial sodium sulfite, sodium sulfite content ≥99.5% by mass percentage.

[0040] Raise the temperature of the antimony electrolyte to 80°C, add potassium oxalate under strong stirring conditions, the ratio of the molar amount of potassium oxalate added to the total molar amount of iron and antimony ions in the electrolyte is 2.8:1, and the reaction time is 1h. Add sodium sulfite to the electrolyte under strong stirring, control the ratio of sodium sulfite to the total molar mass of iron and antimony ions to 1:1, control the reaction temperature to 90°C, and keep the solution at 85°C for hot filtration to obtain iron removal slag after reacting for 1 hour and high temperature filtrate. The high-temperature filtrate was naturally cooled ...

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Abstract

The invention provides a selective iron removal and ferrous oxalate preparation method through an antimony electrolyte. According to the method, under the condition that the acidity is not adjusted, iron ions and antimony ions in the electrolyte are compounded through a compounding agent, then a reducing agent is added to conduct selective reduction on iron ion compounds, solid-liquid separation is conducted on the reduced electrolyte so that iron-containing compounds and the excessive compounding agent can be separated out, and finally, a precipitating agent is added to separate the compounding agent through precipitation. According to the method, the pH value does not need to be adjusted, the original electrolyte system is not damaged, and crystallization post-liquid can be directly sent back for electrolysis; the iron removal selectivity is high, the ratio of the iron removal rate to the antimony precipitation rate is larger than 80, and the purity of the ferrous oxalate in slag after purification reaches 98% or over; and the process is environment-friendly and economical, and secondary pollution is avoided.

Description

technical field [0001] The invention belongs to the technical field of non-ferrous metal smelting, and relates to a wet antimony smelting process, in particular to a method for selectively removing iron from an antimony ore slurry electrolyte and preparing high-purity ferrous oxalate. Background technique [0002] Slurry electrolysis is a process that combines ore leaching, partial leachate purification and electrolytic deposition in one device, and utilizes the anodic oxidation reaction in the electrolytic deposition process to leach valuable elements in the ore. my country's pulp electrolysis technology is at the leading level in the world. Beijing General Research Institute of Mining and Metallurgy has successfully obtained metal bismuth from bismuth concentrate by direct electrolysis through pulp electrolysis technology. Wang Chengyan and others pointed out through theoretical research that complex antimony-lead ores can also extract antimony through slurry electrolysis ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25C1/22C22B30/02C22B3/44C07C51/41C07C55/07
CPCC07C51/412C22B3/44C22B30/02C25C1/22C07C55/07Y02P10/20
Inventor 陈霖王禹昌令红斌刘伟锋张杜超杨天足
Owner CENT SOUTH UNIV
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