Extraction method of lithium in spodumene, adsorption material for extraction of lithium and preparation method thereof

A technology of adsorption materials and extraction methods, applied in chemical instruments and methods, other chemical processes, lithium carbonate;/acid carbonate, etc., can solve the problems of large acid-base consumption and poor extraction effect, and achieve Long service life, good extraction effect, and the effect of reducing production costs

Active Publication Date: 2020-01-31
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] One of the objectives of the present invention is to overcome the disadvantages of relatively poor extraction effect and large acid-base consumption when extracting lithium from spodumene by using the existing sulfuric acid process, and to provide a lithium extraction method in spodumene The adsorption material for extraction and the preparation method thereof, the adsorption material of the present invention has a strong selective adsorption capacity for lithium, can be effectively used for the extraction of lithium in the sulfuric acid spodumene, the extraction efficiency is high and the impurity removal treatment is effectively reduced acid-base consumption

Method used

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  • Extraction method of lithium in spodumene, adsorption material for extraction of lithium and preparation method thereof
  • Extraction method of lithium in spodumene, adsorption material for extraction of lithium and preparation method thereof
  • Extraction method of lithium in spodumene, adsorption material for extraction of lithium and preparation method thereof

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preparation example Construction

[0042] The preparation method of adsorption material of the present invention specifically comprises the following steps:

[0043] (1) React 1,3-dibromopropane, catechol and NaOH at a molar ratio of 1:(2-3):(2-3), preferably a molar ratio of 1:2:2. Specifically, first add 1,3-dibromopropane and catechol into the reaction flask, stir and heat up to 120-140°C, add NaOH aqueous solution within 1-2h and stir for 5-10h; Pour the liquid into 5N NaOH aqueous solution, add an appropriate amount of CH 2 Cl 2 , filter to remove solid impurities, adjust the filtrate to be neutral with HCl solution, and then use CH 2 Cl 2 Extraction, anhydrous Na 2 SO 4 Dry, remove the solvent with a rotary evaporator, and pass through the column with silica gel powder to obtain product A, and the structural formula of product A is as follows:

[0044]

[0045] (2) React the product A, LiOH and epichlorohydrin at a molar ratio of 1:(2-3):(1-2), preferably a molar ratio of 1:2:1. Specifically, un...

Embodiment 1

[0062] The preparation process of the adsorbent material of the present embodiment is as follows:

[0063] (1) React 1,3-dibromopropane, catechol and NaOH at a molar ratio of 1:2:2. Specifically, first add 1,3-dibromopropane and catechol into the reaction flask, stir and heat up to 120°C, add NaOH aqueous solution within 1h and stir for 5h; then pour the reaction mixture into 5N NaOH In the aqueous solution, add an appropriate amount of CH 2 Cl 2 , filter to remove solid impurities, adjust the filtrate to be neutral with HCl solution, and then use CH 2 Cl 2 Extraction, anhydrous Na 2 SO 4 Dry, remove the solvent with a rotary evaporator, and pass through a column with silica gel powder to obtain product A.

[0064] (2) The product A, LiOH and epichlorohydrin were reacted in a molar ratio of 1:2:1. Specifically, under the protection of nitrogen, the product A, LiOH, H 2 Add O into the reaction flask, heat up to 90°C and stir until completely dissolved; cool down to 40°C...

Embodiment 2

[0074] The preparation process of the adsorbent material of the present embodiment is as follows:

[0075] (1) 1,3-dibromopropane, catechol and NaOH were reacted at a molar ratio of 1:2.5:2.5. Specifically, first add 1,3-dibromopropane and catechol into the reaction flask, stir and heat up to 125°C, add NaOH aqueous solution within 1.5h and stir for 6h; then pour the reaction mixture into 5N NaOH aqueous solution, adding an appropriate amount of CH 2 Cl 2 , filter to remove solid impurities, adjust the filtrate to be neutral with HCl, then use CH 2 Cl 2 Extraction, anhydrous Na 2 SO 4 Dry, remove the solvent with a rotary evaporator, and pass through a column with silica gel powder to obtain product A.

[0076] (2) The product A, LiOH and epichlorohydrin were reacted in a molar ratio of 1:2.5:1.5. Specifically, under the protection of nitrogen, the product A, LiOH, H 2 Add O into the reaction flask, heat up to 92°C and stir until completely dissolved; drop the temperat...

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Abstract

The invention discloses an extraction method of lithium in spodumene, and an adsorption material for extraction of lithium and a preparation method thereof, belonging to the technical field of lithiumresource extraction. The adsorption material disclosed by the invention is a 4-aminodibenzo-14-crown-4 crown ether derivative loaded on the surface of SiO2. According to the method for extracting lithium from spodumene in the invention, a sulfuric acid method is adopted for extraction; spodumene is subjected to roasting transformation-sulfated roasting-leaching to obtain a lithium sulfate solution; then the adsorption material is adopted for adsorption treatment of the obtained lithium sulfate solution; finally, the adsorption material is washed and desorbed, a pure sodium carbonate solutionis added, heating is performed for lithium precipitation, and washing and drying are carried out to obtain a lithium carbonate product. The adsorption material disclosed by the invention has strong capacity in selective adsorption of lithium, can be effectively used for extracting lithium from spodumene via the sulfuric acid method, is high in extraction efficiency, realizes a high enrichment effect on lithium ions, and overcomes the defects of an existing sulfuric acid method extraction process.

Description

technical field [0001] The invention belongs to the technical field of lithium resource extraction, and more specifically relates to a lithium extraction method in spodumene, an adsorption material for extraction and a preparation method thereof. Background technique [0002] Lithium is the lightest metal in nature. It is chemically active and can form compounds with various elements. It is widely used in lithium batteries, nuclear power generation, aerospace, lubricant materials, heat-resistant glass and other fields. In recent years, lithium has shown great application prospects in the field of new energy due to its superior performance of high energy density and high electrochemical potential (3.045V). Especially with the successful application of lithium-ion batteries in electric vehicles and hybrid vehicles, the demand for lithium in the world is increasing rapidly, so the full development and utilization of lithium resources is imminent. [0003] Lithium ore resources...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/08B01J20/22B01J20/30
CPCC01D15/08B01J20/22
Inventor 赵卓徐亮张福元童碧海田勇攀姚永林程衔锟熊延杭
Owner ANHUI UNIVERSITY OF TECHNOLOGY
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