System method for extracting lithium-containing brine from lepidolite and manufacturing lithium salt

A lepidolite and brine technology, applied in lithium carbonate;/acid carbonate, silicate, lithium halide, etc., can solve the problems of long leaching time, poor selectivity, and product quality decline, etc. Achieve the effect of improving the comprehensive added value, the overall process is simple, and the product quality is stable

Active Publication Date: 2020-05-12
CHANGSHA YUANPENG CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantages of the sulfuric acid method are: ① a large amount of sulfuric acid is required during leaching, and a large amount of aluminum elements are leached, resulting in a large amount of neutralization slag, a large amount of solid waste and difficult to handle; ② long leaching time, more than 8 hours, energy consumption High, low production efficiency; ③ During leaching, hydrofluoric acid volatilizes, which is extremely corrosive to equipment and unfriendly to the environment; ④ High impurities, product quality is average, especially residual potassium, rubidium and cesium in brine, which will be quantified brought into the product, resulting in a decline in product quality
This process needs to add a large amount of sodium sulfate, and the selectivity is not good; a single sodium sulfate has a low melting point, and it is easy to form a low-eutectic molten mass with mica, resulting in wall agglomeration during roasting, which increases the difficulty of subsequent processing and is not conducive to industrial production. ; more suitable for high-grade lepidolite, with limited scope of application; there is no good comprehensive utilization method for lithium extraction tailings slag and fluorine; this technology does not provide an effective technical route for subsequent treatment of high-sodium lithium-containing brine
[0010] The advantage of the sulfate method is that the roasting conversion rate in the early stage is high, and the disadvantage is that a large amount of sodium sulfate, potassium sulfate and lithium sulfate are easily generated in the solution to form Li (2-X-Y) Na X K Y SO 4 Type double salt, resulting in lower yield and efficiency in the later stage; the price of potassium sulfate is more than 6 times higher than that of sodium sulfate, so in the design, it should be as possible to adopt the technical route with wide application range, good reaction selectivity and lower cost

Method used

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  • System method for extracting lithium-containing brine from lepidolite and manufacturing lithium salt
  • System method for extracting lithium-containing brine from lepidolite and manufacturing lithium salt
  • System method for extracting lithium-containing brine from lepidolite and manufacturing lithium salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] (1) Take 300g of lepidolite with a lithium oxide content of 2.8%, add 90g of sodium sulfate and 60g of calcium sulfate, finely grind and mix evenly to obtain a mixture;

[0075] (2) Roast the mixture at 1050°C for 10 minutes to obtain the roasted material;

[0076] (3) After cooling, add 600mL of water, stir for 30min, and filter to obtain filtrate and filter residue;

[0077] Table 1 Lepidolite data, %

[0078]

[0079] Table 2 filtrate data, g / L

[0080]

[0081] Table 3 Residue data, %

[0082]

[0083] (4) The obtained filtrate is lithium-containing brine, and the obtained filter residue is lithium extraction tailings.

Embodiment 2

[0085] (1) Take 300g of lepidolite with a lithium oxide content of 3.5%, add 60g of sodium sulfate, 60g of calcium sulfate, and 30g of concentrated sulfuric acid (98%), and mix evenly to obtain a mixture;

[0086] (2) Roast at 850°C for 30 minutes, absorb tail gas with a mixed solution of calcium carbonate and calcium hydroxide, and obtain roasted material and tail gas absorption slag;

[0087] (3) Add 600mL of water to the baking material, stir for 30min, and separate the solid and liquid to obtain the filtrate and filter residue;

[0088] (4) Solid-liquid separation of acid-absorbing tail gas slag;

[0089] Table 4 Lepidolite data, %

[0090]

[0091] Table 5 filtrate data, g / L

[0092]

[0093] Table 6 Residue data, %

[0094]

[0095] Table 7 Absorption acid tail gas slag data (approximate value), %

[0096]

[0097] (5) The obtained filtrate is lithium-containing brine, the obtained filter residue is lithium extraction tailings, and the obtained acid gas s...

Embodiment 3

[0099] (1) Take 10000g of lepidolite with a lithium oxide content of 3.9%, add 1500g of sodium sulfate and 1500g of calcium sulfate, finely grind and mix evenly, add 4000g of concentrated sulfuric acid (98%), and roast at 750°C for 300min to obtain a roasted material; The mixed solution of calcium carbonate and calcium hydroxide absorbs tail gas to obtain roasted material and tail gas slag;

[0100] (2) Add 20,000mL of water to the roasting material, stir for 30 minutes, and separate the solid and liquid to obtain the filtrate and filter residue;

[0101] (3) Solid-liquid separation of acid-absorbing tail gas slag;

[0102] Table 8 Lepidolite data, %

[0103]

[0104] Table 9 filtrate data, g / L

[0105]

[0106] Table 10 Residue data, %

[0107]

[0108] Table 11 Absorption acid tail gas slag data (approximate value), %

[0109]

[0110] (4) The obtained filtrate is the lithium-containing brine, the obtained filter residue is the lithium extraction tailings res...

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Abstract

The invention discloses a system method for extracting lithium-containing brine from lepidolite and manufacturing lithium salt. The system method comprises the following steps: material mixing, roasting, brine preparation, lithium salt preparation and comprehensive utilization of tailing slag. According to the invention, sulfuric acid double salt and sulfuric acid (selected) are used as auxiliarymaterials to be mixed with the lepidolite for reaction; the system method is applicable to extraction of lithium in high-content and low-content lepidolite; good selectivity is achieved during extraction; the extraction rate of lithium is 95.5%-97.5%; and the extraction rates of K, Rb and Cs are smaller than 30%; the obtained brine is neutral and can be used for directly preparing lithium hydroxide monohydrate, lithium chloride or lithium carbonate, and the total yield of lithium is more than 92%; the process is high in flexibility, can produce single-variety lithium salt, and can jointly produce two or more varieties of lithium salt; and fluorine in the lepidolite can be separated and recovered, so the additional value is increased, and the lithium extraction tailing slag can be comprehensively utilized. The system method provided by the invention has the following advantages: the whole process is short in flow, low in cost and friendly to the environment; and the system method has good economic benefits and social benefits and good industrial application values.

Description

technical field [0001] The invention relates to a systematic method for extracting lithium-containing brine from lepidolite and producing lithium salt, which is suitable for extracting lithium-containing brine from lepidolite and producing lithium salt (lithium hydroxide monohydrate, lithium chloride, lithium carbonate), It belongs to the technical field of rare metal extraction. Background technique [0002] Lithium salts currently produced on a large scale include lithium carbonate, lithium hydroxide monohydrate, lithium chloride, lithium fluoride, lithium sulfide, lithium dihydrogen phosphate, and lithium hexafluorophosphate. Among them, the production scale of lithium carbonate, lithium hydroxide monohydrate and lithium chloride ranks the top three, and the three can be transformed into each other, and they are also the basic materials for the preparation of other lithium salts. [0003] Lithium carbonate is widely used in glass, ceramics, lubricants, medicine and other...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/04C01D15/08C01D15/02C01F11/22C01B33/26
CPCC01D15/02C01D15/04C01D15/08C01F11/22C01B33/26
Inventor 姚丽吕运征吕运凤
Owner CHANGSHA YUANPENG CHEM TECH
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