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Method for recovering lithium from lithium-containing wastewater

A technology for recovering lithium and waste water, applied in the field of lithium recovery, can solve problems such as high investment cost, equipment corrosion, difficult stripping, etc., and achieve the effect of short process flow, low equipment investment and good selectivity

Active Publication Date: 2020-11-17
HUNAN BRUNP RECYCLING TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, the extraction systems that have undergone industrial experiments in China or have been applied to industrial production include amide extractants (N503, N523), neutral phosphine extractants TBP, ketone The extractant DIBK, the extraction system needs to add ferric chloride as a co-extractant, and the extraction with ferric chloride as a co-extractant needs to be carried out under acidic conditions to ensure that FeCl4 -Generate and prevent Fe3+ hydrolysis; and the back extraction of Li+ requires a strong acid solution above 6mol / L, which leads to serious corrosion of equipment, and FeCl 3Emulsification occurs during use; it is difficult to extract iron after it is combined with organic matter. On the one hand, it will increase the density and viscosity of the organic matter, making it difficult to separate phases (centrifugal extractors are generally used for lithium extraction from salt lakes, and the investment cost is high. ), on the other hand will reduce the organic loading

Method used

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  • Method for recovering lithium from lithium-containing wastewater

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Experimental program
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Effect test

Embodiment 1

[0032] A method for reclaiming lithium from lithium-containing wastewater, comprising the steps of:

[0033] (1) Adopt sulfuric acid to adjust the pH of lithium-containing waste water to be 2.0, detect wherein Li + =3.7g / L, Na + =21g / L;

[0034] (2) 40% C272 (bis(2,4,4-trimethylpentyl) phosphonic acid), 20% TBP (tributyl phosphate) and 40% sulfonated kerosene are formulated into an organic phase by mass percentage, Take 100mL of the organic phase and saponify it with 5mol / L sodium hydroxide according to 1.4 times the lithium concentration in the lithium-containing wastewater. After saponification, no phase separation is required. Place 100mL of the organic phase after saponification and 100mL of the lithium-containing wastewater into a separatory funnel. Vibrate at a rotation speed of 240 rpm, extract at a temperature of 40° C. for 4 minutes, and stand still to separate phases to obtain an organic phase containing lithium ions and a raffinate.

[0035] The detection results...

Embodiment 2

[0037] A method for reclaiming lithium from lithium-containing wastewater, comprising the steps of:

[0038] (1) Adopt sulfuric acid to adjust the pH of lithium-containing waste water to be 4.0, detect wherein Li + =3.7g / L, Na + =21g / L;

[0039] (2) 40% C272 (bis(2,4,4-trimethylpentyl) phosphonic acid), 20% TBP (tributyl phosphate) and 40% sulfonated kerosene are formulated into an organic phase by mass percentage, Take 100mL of the organic phase and saponify it with 5mol / L sodium hydroxide according to 1.4 times the lithium concentration in the lithium-containing wastewater. After saponification, no phase separation is required. Take 100mL of the saponified organic phase and 100mL of the lithium-containing wastewater and place them in a separatory funnel. Shake at a rotation speed of 240 rpm, extract at a temperature of 40° C. for 4 minutes, and stand still to separate phases to obtain an organic phase containing lithium ions and a raffinate.

[0040] The detection results...

Embodiment 3

[0042] A method for reclaiming lithium from lithium-containing wastewater, comprising the steps of:

[0043] (1) Sulfuric acid is used to adjust the pH of lithium-containing wastewater to 6.0, and Li + =3.7g / L, Na + =21g / L;

[0044] (2) 40% C272 (two (2,4,4-trimethylpentyl) phosphonic acid), 20% TBP (tributyl phosphate) and 40% sulfonated kerosene by volume percentage are made into an organic phase, Take 100mL of the organic phase and saponify it with 5mol / L sodium hydroxide according to 1.4 times the lithium concentration in the lithium-containing wastewater. Shake at 240rpm, extract at 40°C for 4min, and stand still to separate the phases to obtain an organic phase containing lithium ions and a raffinate.

[0045] The detection results of lithium content in the raffinate are shown in Table 1, and the extraction rate of lithium is 58.6%.

[0046] Table 1 Extraction of lithium-containing wastewater by C272 and TBP combined extractant at different pH

[0047] Wast...

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Abstract

The invention belongs to the field of hydrometallurgy, and discloses a method for recovering lithium from lithium-containing wastewater. The method comprises the following steps of (1) regulating thepH value of the lithium-containing wastewater to be acidic or neutral; and (2) preparing an organic phase, performing saponifying, adding the lithium-containing wastewater for extraction, and separating out a water phase to obtain a loaded organic phase containing lithium ions. A solution for adjusting the pH value of the lithium-containing wastewater is sulfuric acid; and the organic phase comprises the following components including an extraction agent, a synergist and a diluent. According to a combined extraction agent system, ferric trichloride does not need to be added to serve as a co-extraction agent, and the emulsification phenomenon caused by Fe<3+> hydrolysis is avoided; and the combined extraction agent system is good in lithium-sodium selectivity and high in loading capacity, Li in the wastewater can be reduced from 3.7 g / L to 0.126 g / L through four-stage counter-current extraction, and the extraction rate can reach 96.6%.

Description

technical field [0001] The invention relates to the field of hydrometallurgy, in particular to a method for recovering lithium from lithium-containing wastewater. Background technique [0002] Lithium is an important rare element, known as "energy metal" and "important element that drives the world forward". Lithium metal and its compounds have been widely used in the fields of electronics, metallurgy, chemical industry, medicine, nuclear energy, aerospace and energy. Lithium resources exist in the form of solid ore and salt lake brine. Due to the abundant lithium resources in salt lakes and low production costs, the current lithium extraction field that is relatively mature in research and large-scale production is the extraction of lithium in salt lakes. [0003] Scientific researchers have done a lot of research work on the extraction of lithium, and developed a variety of technologies, including precipitation calcination, membrane separation technology, adsorption techn...

Claims

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Application Information

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IPC IPC(8): C22B26/12C22B7/00C22B3/38
CPCC22B26/12C22B7/006C22B3/408Y02P10/20C02F1/26C02F2101/10C02F1/66B01D11/0492C22B3/38
Inventor 张荣荣李生康刘黄华刘勇奇巩勤学李长东
Owner HUNAN BRUNP RECYCLING TECH
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