A kind of recyclable waste acid recovery extraction agent and preparation method thereof
An extraction agent and extraction technology, which are applied in the preparation of amino-substituted functional groups, separation methods, solvent extraction, etc., can solve the problems of acetic acid that cannot be reused, and achieve the effects of low loss rate, little environmental pollution, and no waste residue.
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Embodiment 1
[0024] Synthesis of N,N-Di-n-octyl-N-(1-phenylethyl)amine
[0025] In a 100mL round bottom flask, under nitrogen protection, dissolve 1.74g of sodium iodide and 19mL of n-octane bromide in 30mL of methanol, then add 14g of potassium carbonate and 6.5mL of α-methylbenzylamine, and heat to reflux until TLC monitors the reaction After completion, evaporate the solvent, filter, wash the filter cake with ethyl acetate, wash the filtrate twice with 30 mL of saturated brine, and dry the organic phase with anhydrous magnesium sulfate. It was filtered, concentrated, and separated by column chromatography (petroleum ether / ethyl acetate=40:1) to obtain 10.5 g of a colorless liquid with a yield of 60.7%.
[0026] Colorless liquid; 1H NMR (300MHz, CDCl3) δ (ppm): 0.89 (t, J = 6.6Hz, 6H), 1.24-1.43 (m, 28H), 2.33-2.44 (m, 4H), 3.83 (q, J =6.9Hz,1H),7.18-7.37(m,5H)
[0027] Using this compound as an extractant, the sulfuric acid extraction rate is 85.4%, and the stripping efficiency reache...
Embodiment 2
[0029] Synthesis of N,N-Di-n-octyl-N-(1-phenylethyl)amine
[0030] In a 100mL round bottom flask, under nitrogen protection, 1.80g of potassium iodide and 19mL of bromo-octane were dissolved in 40mL of tetrahydrofuran, then 18g of sodium carbonate and 10mL of α-methylbenzylamine were added, heated to reflux until the reaction was monitored by TLC, evaporated Remove the solvent, filter, wash the filter cake with ethyl acetate, wash the filtrate twice with 30 mL of saturated brine, and dry the organic phase with anhydrous magnesium sulfate. It was filtered, concentrated, and separated by column chromatography (petroleum ether / ethyl acetate=40:1) to obtain 12.5 g of a colorless liquid with a yield of 65.8%.
Embodiment 3
[0032] Synthesis of N,N-Di-n-octyl-N-benzylamine
[0033] In a 100mL round bottom flask, under nitrogen protection, 1.74g of sodium iodide and 19mL of n-octane bromide were dissolved in 30mL of ethanol, then 14g of potassium carbonate and 7.5g of benzylamine were added, heated to reflux until the completion of the reaction monitored by TLC, evaporated solvent, filtered, and the filter cake was washed with ethyl acetate, the filtrate was washed twice with 30 mL of saturated brine, and the organic phase was dried over anhydrous magnesium sulfate. It was filtered, concentrated, and separated by column chromatography (petroleum ether / ethyl acetate=40:1) to obtain 13.5 g of a colorless liquid with a yield of 74.1%.
[0034] Colorless liquid; 1H NMR (300MHz, CDCl3) δ (ppm): 0.88 (t, J = 6.6Hz, 6H), 1.24-1.43 (m, 28H), 2.32-2.45 (m, 4H), 3.93 (S, 2H ),7.18-7.37(m,5H).
[0035] Using this compound as an extractant, the sulfuric acid extraction rate is 90.2%, and the stripping effici...
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