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Method for extracting battery-grade lithium carbonate from magnesium sulfate subtype salt lake brine

A magnesium sulfate subtype and salt lake brine technology, applied in the direction of lithium carbonate;/acid carbonate, etc., can solve the problems of inability to produce battery-grade lithium carbonate products, imperfect process combination, and large loss of lithium ions. To achieve the effect of controllable product quality, low production cost and saving investment

Pending Publication Date: 2019-04-12
青海中信国安锂业发展有限公司
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  • Abstract
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  • Claims
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Problems solved by technology

Chinese patent CN104961143A, Chinese patent CN100408705C and Chinese patent CN103074502A announced the method of using nanofiltration membrane separation process for salt lake brine to extract lithium, which has been applied on an industrial scale in Qinghai Salt Lake in my country, but there are several aspects in the current nanofiltration membrane process for lithium extraction The problems need to be improved: First, the existing nanofiltration membrane separation method cannot produce battery-grade lithium carbonate products due to the imperfect process combination, and the market application is limited
Second, the nanofiltration membranes are all low-pressure membranes, and the maximum operating pressure they can withstand should not be higher than 4.0MPa, resulting in a dilution factor of brine as high as 14 to 20 times and a particularly high water consumption.
The third is that the current nanofiltration process has high requirements on raw materials, and the lithium ion mass concentration in the old brine must not be lower than 4.0g. L-1, leading to a large loss of lithium ions in the enrichment process of potassium extraction old brine

Method used

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  • Method for extracting battery-grade lithium carbonate from magnesium sulfate subtype salt lake brine
  • Method for extracting battery-grade lithium carbonate from magnesium sulfate subtype salt lake brine
  • Method for extracting battery-grade lithium carbonate from magnesium sulfate subtype salt lake brine

Examples

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Effect test

Embodiment 1

[0053] The raw material is taken from the old brine after potassium extraction from the Dachaidan Salt Lake in Qaidam Basin, Qinghai. It has the chemical composition shown in Table 1. From the composition analysis, the water chemical type of the brine system belongs to the magnesium sulfate subtype.

[0054] Table 1 Chemical composition of the brine from the Dachaidan Salt Lake in Qinghai Qaidam Basin

[0055]

[0056] ⑴ Extract 1.00m 3 Table 1 Extract potassium and old brine, add fly ash at 1% of the weight of the old brine, turn on the stirring, 10 minutes later, use the slurry pump to drive into the plate and frame filter press to filter, and obtain the filter residue 40Kg, and the refined filtrate is 0.96 m. 3 , Control filtrate NTU <20, SDI <200.

[0057] ⑵Dilute with production water once to refine the old brine 10 times to 9.6m 3 , Use a centrifugal pump to filter into the ultrafiltration device, close the concentrated water valve, and control the filtrate NTU 3 , Put into PP s...

Embodiment 2

[0064] The raw materials are taken from the old brine after potassium extraction from the Jinel Salt Lake in Dongtai, Qaidam Basin, Qinghai. It has the chemical composition shown in Table 2. From the composition analysis, the water chemical type of the brine system belongs to the magnesium sulfate subtype. This example and the examples 1 Compared with the method provided, the selected raw materials and operating conditions are different, and the adaptability of the method under different raw materials and operating conditions is mainly investigated.

[0065] Table 2 Chemical composition of the brine from the Jinel Salt Lake in Dongtai, Qaidam Basin, Qinghai Province

[0066]

[0067] ⑴ Extract 1.00m 3 Table 2 Extract potassium and old brine, add fly ash at 1% of the weight of the old brine, turn on the stirring, 10 minutes later, use the slurry pump to drive into the plate and frame filter press to filter, obtain the filter residue 38Kg, the first refined filtrate 0.98 m 3 , Control...

Embodiment 3

[0075] The raw material is taken from the old brine after potassium extraction from the Xitaijinel Salt Lake in the Qaidam Basin, Qinghai Province, and has the chemical composition shown in Table 3. From the composition analysis, the water chemical type of the brine system belongs to the magnesium sulfate subtype. This example and the examples 2 Compared with the method provided, the selected raw materials and operating conditions are different, and the adaptability of the method under different raw materials and operating conditions is mainly investigated.

[0076] Table 3 The chemical composition of the brine from the Jinel Salt Lake in Xitai, Qaidam Basin, Qinghai Province

[0077]

[0078] ⑴ Extract 1.00m 3 Table 3 Extract potassium and old brine, add fly ash according to 1% of the weight ratio of the old brine, start stirring, 10 minutes later, use a slurry pump to drive into the plate and frame filter press to filter, obtain the filter residue 44Kg, the refined filtrate is 0.9...

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Abstract

The invention relates to a method for extracting battery-grade lithium carbonate from magnesium sulfate subtype salt lake brine. The method includes the following steps that (1) fly ash is added intopotassium extraction old brine, and filtration is carried out to obtain primarily refined old brine; (2) the primarily refined old brine is diluted and then pumped into an ultrafiltration device to obtain secondarily refined old brine; (3) the secondarily refined old brine is pumped into a three-stage high-pressure nanofiltration membrane device, and pressure is applied to obtain lithium-rich liquor and concentrated liquor; (4) the lithium-rich liquor is subjected to RO membrane+MVR forced evaporation two-stage concentration to obtain a high-lithium solution and purified water respectively; (5) the high-lithium solution is injected into a boron resin exchange column to obtain a boron-removed high-lithium solution; (6) the boron-removed high-lithium solution to subjected to pH value regulation and then filtered to obtain a refined high-lithium solution; (7) a sodium carbonate solution is added into the refined high-lithium solution for a reaction, and filtration is carried out to obtaincrude lithium carbonate and precipitate lithium mother liquor respectively; (8) the crude lithium carbonate precipitate is subjected to washing, filtration, drying and smashing to obtain a battery-grade lithium carbonate product. The method is simple in process, low in water consumption, low in investment and excellent in product quality.

Description

Technical field [0001] The invention relates to the field of inorganic salt chemical industry, in particular to a method for extracting battery grade lithium carbonate from magnesium sulfate subtype salt lake brine. Background technique [0002] Lithium is silver-white, soft, and the lightest metal in the periodic table. It has the highest electrochemical potential, excellent ductility and catalytic properties. Its special properties make lithium and its compounds useful in the national economy, military industry, and aerospace. The department is widely used. In recent years, with the launch of new electric vehicle products from major international manufacturers such as Tesla Moto, GM, TOYOTA, and BMW, lithium as a strategic resource has increasingly shown a huge market application prospect. [0003] Lithium has no elemental form in nature, but mainly exists in granite pegmatite deposits (spodumene, lepidolite, lapholite, etc.), brine and seawater in compound form. According to p...

Claims

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Application Information

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IPC IPC(8): C01D15/08
CPCC01D15/08C01P2006/80
Inventor 李陇岗秦佳政余明祥苏建军权彩兄
Owner 青海中信国安锂业发展有限公司
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