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Purifying method of pulp electrolyte containing antimony concentrates

A technology of electrolyte and pulp, applied in the field of purification of pulp electrolyte, can solve the problems of slow stripping speed, increased treatment, insufficient phase separation time, etc., to reduce emulsification and aging, prolong the service period, and realize the effect of recycling.

Active Publication Date: 2018-04-17
ZHUZHOU SMELTER GRP
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

When treating complex antimony-gold concentrates with slurry electrolysis process, antimony is selectively leached in the anode area, and metal antimony is deposited and precipitated in the cathode, reaching a balance. However, about 4% of the iron in the raw material is leached into the solution, and the iron continues to accumulate, thus affecting The entire electrolysis process is carried out normally; at the same time, the organic flotation agent added in the early flotation process of the complex antimony-gold concentrate and the oil unloaded during the operation of various equipment reduce the current efficiency of antimony electrolysis and increase the unit power consumption. Therefore, it is necessary to purify, remove iron and reduce oil in the slurry electrolyte, so as to maintain the concentration of iron ions in a reasonable area
[0003] Chen Yongqiang, Liu Yong, Wang Chengyan, etc. mentioned in the "continuous expansion test of electrolysis of high arsenic antimony gold concentrate pulp electrolysis" published in the twelfth issue of nonferrous metals (smelting part) in 2015, and mentioned extraction and removal of iron, and hydrochloric acid back extraction was used in the process; Zhang Yinsheng, Wang Chengyan, Jiang Peihai, etc. published in the second issue of Nonferrous Metals (Smelting Part) in 2003 "P204 Extraction and Separation of Iron Antimony Process Research" mentioned extraction and removal of iron, washing of loaded organic phase, hydrochloric acid back extraction and back extraction The N235 iron extraction process of iron in the liquid is composed of processes such as iron extraction. The deficiencies in these two studies are: ① The iron ion in the anolyte of the slurry electrolysis in the production site exists in the form of Fe 2+ , while Fe 3+ The content is less than 1g / L, P204 mainly extracts Fe 3+ , Fe 2+ The amount of extraction is less; ② due to Fe 3+ The stripping speed in hydrochloric acid is slow, and the organic phase after stripping also contains a certain amount of Fe 3+ , so that the extraction capacity of the organic phase decreases, and it is easy to cause the emulsification of the organic phase; ③The phase separation time in the extraction and washing process is not enough, resulting in incomplete phase separation between the organic phase and the water phase, so that antimony is entrained in the organic phase, resulting in the recovery of antimony ④ N235 is used to extract iron again in the stripping liquid, which leads to high production cost and is difficult to apply in industrial production
[0004] Zhang Yonglu, Wang Chengyan, Yin Fei, etc. published in the fourth issue of Nonferrous Metals (Smelting Part) in 2016, "Research on the Separation of Antimony and Iron in Pulp Electrolytic Solution" mentioned that iron filings were used to replace antimony to achieve the separation of antimony and iron. In this study There are deficiencies: 1. sponge antimony is easy to oxidize, causing the recovery rate of antimony to decline; 2. iron is difficult to control in the production site, and the iron content in sponge antimony is high, and antimony is difficult to handle; 3. after the replacement, the liquid is ferrous chloride solution, which contains a lot of lead, Heavy metal ions such as copper and arsenic are added to the treatment of heavy metal ions such as lead, copper and arsenic when used in the wastewater treatment of mineral processing plants
[0005] The method currently adopted by Xinlong Mining Co., Ltd. to remove iron from the slurry electrolyte is to add ammonium bicarbonate to the slurry electrolyte, so that antimony and iron can be precipitated together. There are shortcomings: ① Antimony slag is difficult to recycle, stockpiling, antimony recovery ②When ammonium bicarbonate is used for precipitation, a large amount of ammonia gas is released, which affects the environment, and the production cost is high; Electrolytic efficiency and blocked pipelines affect production and high production costs

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  • Purifying method of pulp electrolyte containing antimony concentrates

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Embodiment 1

[0028] The ore slurry electrolyte composition of the antimony concentrate that the present invention adopts is following mass concentration (unit g / L): Fe 2+ 26.01, Fe 3+ 0.68, Sn 0.035, SiO 2 0.18, As 0.048, Sb 32.27, H + 28.53. Follow these steps:

[0029] Step A: Under the condition of oxidation temperature of 40°C and stirring time of 300 minutes, oxidant air is blown in, and activated carbon is added to absorb for 5 minutes at the end of the reaction, and Fe in the oxidation solution 3+ , Fe 2+ , Sb mass concentrations were 8g / L, 18.37g / L and 32.08g / L.

[0030] Step B: The extraction is a two-stage extraction. The organic phase of the extraction is a mixed organic phase composed of P204 with a volume fraction of 25%, 200# kerosene with a volume fraction of 74%, and TBP with a volume fraction of 1%. The volume ratio of the organic phase to the aqueous phase is 1 : 2, extraction time is 15 minutes, temperature is 15 ℃, clarification time 10 minutes; Gained raffina...

Embodiment 2

[0037] The ore slurry electrolyte composition of the antimony concentrate that the present invention adopts is following mass concentration (unit g / L): Fe 2+ 26.01, Fe 3+ 0.68, Sn 0.035, SiO 2 0.18, As 0.048, Sb 32.27, H + 28.53. Follow these steps:

[0038] Step A: Under the conditions of oxidation temperature 75°C and stirring time of 60 minutes, oxidant oxygen is blown in, and at the end of the reaction, activated carbon is added for adsorption for 10 minutes, and Fe in the oxidation solution 3+ , Fe 2+ , Sb mass concentrations were 13g / L, 14.08g / L and 32.31g / L.

[0039] Step B: the extraction is a two-stage extraction, and the extracted organic phase is a mixed organic phase composed of P204 with a volume fraction of 35%, sulfonated common kerosene with a volume fraction of 64% and TBP with a volume fraction of 1%, and the volume of the organic phase and the aqueous phase is The ratio is 1:4, the extraction time is 5 minutes, the temperature is 40°C, and the clar...

Embodiment 3

[0046] The ore slurry electrolyte composition of the antimony concentrate that the present invention adopts is following mass concentration (unit g / L): Fe 2+ 26.01, Fe 3+ 0.68, Sn 0.035, SiO 2 0.18, As 0.048, Sb 32.27, H + 28.53. Follow these steps:

[0047] Step A: Under the condition of oxidation temperature of 60°C and stirring time of 150 minutes, oxidant air is blown in, and activated carbon is added to absorb for 5 minutes at the end of the reaction, and Fe in the oxidation solution 3+ , Fe 2+ , Sb mass concentrations were 10g / L, 16.76g / L and 32.36g / L.

[0048] Step B: The extraction is a 3-stage extraction, and the extracted organic phase is a mixed organic phase composed of P204 with a volume fraction of 30%, 200# kerosene with a volume fraction of 68%, and TBP with a volume fraction of 2%, and the volume ratio of the organic phase to the aqueous phase is 1 : 3, the extraction time is 10 minutes, the temperature is 25 ℃, and the clarification time is 20 minut...

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Abstract

The invention discloses a purifying method of pulp electrolyte containing antimony concentrates. The purifying method comprises the following steps: (A) oxidation: part of divalent iron ions are oxidized as trivalent iron ions; (B) extraction: oxide liquid and an organic phase are mixed in a mixing tank for extraction; (C) washing: less antimony in the organic phase is transferred into washing liquid; (D) blank: a washing organic phase flows to clarifying tank component phases on a blank stage by the mixing tank; (E) reverse extraction: such substances as iron, copper and silicon dioxide in the organic phase are transferred into sodium carbonate solution to generate precipitations; and (F) regeneration: the reversely extracted organic phase is mixed with a prepared regeneration agent in the mixing tank for regeneration. The purifying method solves the problem the entrainment problem of antimony in the organic phase, and realizes recycling of the organic phase.

Description

technical field [0001] The invention relates to a method for separating valuable metal antimony from impurity iron ions and harmful organic substances in an antimony electrolyte, in particular to a method for purifying an antimony-containing concentrate slurry electrolyte. Background technique [0002] The modern metallurgical production methods of metal antimony are mainly divided into two categories: fire method and wet method. At present, antimony by fire method is the main method. Antimony smelting by fire method is mainly volatile roasting-reduction smelting method, that is, antimony trioxide is produced first, and then crude antimony is produced by reduction smelting; antimony smelting by wet method mainly includes two methods: alkaline leaching and acid leaching. The process of antimony smelting by pyrometallurgy has the problems of long process, many returning materials, difficult separation of antimony and lead, and accumulation of polysulfides in alkaline wet antim...

Claims

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Application Information

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IPC IPC(8): C25B1/00C22B3/44C22B3/38C22B30/02
CPCC22B3/44C22B30/02C25B1/00C22B3/3846Y02P10/20Y02P20/584
Inventor 廖贻鹏林文军张磊唐亦秋杨益
Owner ZHUZHOU SMELTER GRP
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