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.

Active Publication Date: 2018-12-07
成都奥斯汀生物医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This patent only extracts acetic acid from the reaction system, and also needs to add alkali to regenerate the extractant, and the extracted acetic acid cannot be reused through simple treatment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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PUM

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Abstract

The invention provides a recyclable waste acid recycling extraction agent and a preparation method thereof. The extraction agent is tertiary amine with the molecular formula R1R2NR3, wherein R1 and R2 in the formula are C8-C10 straight-chain alkanes, and R3 in the formula is alpha-ethylbenzene or methylbenzene. The preparation method of the extraction agent comprises the steps that alkyl halide, alpha-methylbenzylamine or benzylamine, a catalyst and alkali are added into a solvent, after heating reflux is conducted, the solvent is removed through evaporation, water is added, extraction is conducted with ethyl acetate, and after an organic phase is dried, concentration is conducted to obtain the product. The extraction agent is low in loss rate along with an aqueous solution, little in pollution to the environment and capable of achieving acid recycling and reducing acid emission and environmental pollution.

Description

technical field [0001] The invention belongs to the technical field of waste acid recovery, and in particular relates to a recyclable waste acid recovery extraction agent and a preparation method thereof. Background technique [0002] Sulfuric acid is widely used in the fields of medicine, organic synthesis, especially metallurgy, and the resulting waste acid reaches more than 20 million tons per year, which poses a great threat to the environment. The treatment of traditional waste acid not only consumes a large amount of alkali, but also increases equipment investment and complicates the process. Some acid leaching solutions cannot be neutralized with alkali, otherwise it will lead to complete failure of the process. It can be seen that the treatment of waste acid has become the key to the sustainable development of related industries in our country. [0003] At present, the methods for treating waste acid in my country mainly include: acid-base waste acid neutralization...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/08C07C211/27B01D11/04
CPCB01D11/0492C07C209/08C07C211/27
Inventor 骆文凯支永刚
Owner 成都奥斯汀生物医药科技有限公司
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