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
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[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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