Alpha-hydroxy-2-ethylhexyl phosphinic acid extracting agent as well as preparation method and application thereof

A technology of base phosphinic acid and extractant, which is applied in the field of α-hydroxy-2-ethylhexylphosphinic acid extractant and its preparation, can solve the problems of easy occurrence of side reactions, high toxicity and the like, and achieves easy industrial popularization and application , good selectivity, the effect of improving extraction capacity

Active Publication Date: 2022-04-15
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reactive reagents of phosphorus sources such as phosphorus oxychloride, phosphorus pentachloride, and phosphorus pentoxide have strong activity, but there are also problems such as high toxicity and easy occurrence of side reactions.

Method used

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  • Alpha-hydroxy-2-ethylhexyl phosphinic acid extracting agent as well as preparation method and application thereof
  • Alpha-hydroxy-2-ethylhexyl phosphinic acid extracting agent as well as preparation method and application thereof
  • Alpha-hydroxy-2-ethylhexyl phosphinic acid extracting agent as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Preparation of α-Hydroxy-2-Ethylhexylphosphinic Acid

[0037] 1) Take 47.4mL (288mmol) of 2-ethylhexylaldehyde, 47.0mL (432mmol) of 50% hypophosphorous acid, 6mL of concentrated hydrochloric acid, and 70mL of 1,4-dioxane in a reaction flask, add a magnet, heat, and condense Reflux and react at 80°C for 5h;

[0038] 2) The reacted mixture was lowered to room temperature, washed several times with 10% aqueous sodium hydroxide solution until the pH of the aqueous phase was >10, and the aqueous phase was combined and retained. The aqueous phase was acidified to pH31 The results of P NMR spectrum analysis are as follows: figure 1 as shown, 13 The results of C NMR spectrum analysis are as follows: figure 2 Shown, the infrared spectrum analysis result of α-hydroxyl-2-ethylhexylphosphinic acid is as follows image 3 As shown, the mass spectrometric analysis results of α-hydroxy-2-ethylhexylphosphinic acid are as follows Figure 4 As shown, the analysis results confirmed t...

Embodiment 2

[0040] Preparation of α-Hydroxy-2-Ethylhexylphosphinic Acid

[0041] 1) Take 47.4mL (288mmol) of 2-ethylhexylaldehyde, 47.0mL (432mmol) of 50% hypophosphorous acid, 5mL of concentrated sulfuric acid, and 70mL of tetrahydrofuran in a reaction flask, add a magnet, heat, condense and reflux, and react at 90°C 5h;

[0042] 2) The reacted mixture was lowered to room temperature, washed several times with 10% aqueous sodium hydroxide solution until the pH of the aqueous phase was >10, and the aqueous phase was combined and retained. The aqueous phase was acidified to pH<3 with 10% sulfuric acid, extracted three times with 30 mL of ethyl acetate, and the organic phase was combined and retained. Finally, the organic phase was washed three times with saturated brine, dried over anhydrous sodium sulfate, filtered, and distilled under reduced pressure at 55° C. to obtain a light yellow transparent oily liquid with a yield of 81.44%.

Embodiment 3

[0044] Extraction Performance of α-Hydroxy-2-Ethylhexylphosphinic Acid for Manganese and Magnesium

[0045] Mn in manganese magnesium solution 2+ The concentration is 5.5g / L, Mg 2+ The concentration is 2.4g / L, and the extractants are α-hydroxy-2-ethylhexylphosphinic acid, α-hydroxyoctylphosphinic acid, P204, α-hydroxy-2-ethylhexylphosphinic acid, P204 The diluent is kerosene, and the diluent of α-hydroxyoctylphosphinic acid is acetone. The extractant and the diluent are mixed to form an organic phase, the concentration of the extractant is 20%, and the organic phase is saponified by 30% aqueous sodium hydroxide solution, and the saponification rate is 30%; the organic phase and the manganese-magnesium solution are mixed, O / A=1:2, the extraction time is 10min, and the standing time is 30min; after the primary extraction, the extraction rates of manganese and magnesium in the manganese-magnesium mixed solution by the three extraction systems are shown in Table 1. As can be s...

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Abstract

The invention provides an alpha-hydroxy-2-ethylhexyl phosphinic acid extraction agent and a preparation method and application thereof.The preparation method comprises the step that 2-ethylhexyl aldehyde and hypophosphorous acid are subjected to an addition reaction under the condition of an acid catalyst to generate the alpha-hydroxy-2-ethylhexyl phosphinic acid extraction agent which can be applied to recovery of multiple metal ions, and the extraction agent is environmentally friendly and environmentally friendly. For example, manganese, magnesium, rare earth metals and the like in the manganese-magnesium solution are recovered; extracting and separating manganese and magnesium in the manganese-magnesium solution to obtain a raffinate which is a magnesium-rich low-manganese solution, adding carbonate to form a magnesium-containing precipitate, and washing and calcining to obtain a magnesium oxide product; the preparation method of the extraction agent is simple, the extraction efficiency of metal ions is high, the extraction agent is particularly used for recycling manganese and magnesium in a manganese-magnesium solution, the separation efficiency and the product quality can be improved, and resource utilization of manganese and magnesium is achieved.

Description

technical field [0001] The invention relates to the field of hydrometallurgy, in particular to α-hydroxy-2-ethylhexylphosphinic acid extractant and its preparation method and application. Background technique [0002] Solvent extraction is a separation technique developed rapidly in the 20th century. It is an effective method for separating, enriching, and extracting useful substances in a solution. This separation technology has simple equipment, short production cycle, and is convenient for continuous operation. It can cooperate with other purification steps such as crystallization and distillation, and it is easy to realize automatic control. It is applicable to various scales and occupies an irreplaceable position in environmental protection and industrial development. [0003] Extractant is the core and key of extraction technology. Organophosphorus compounds have good extraction properties for metal ions and have been widely used in the field of hydrometallurgy. At p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/38C22B7/00C22B26/22C22B47/00C22B59/00
CPCC22B26/22C22B47/00C22B59/00C22B7/006Y02P10/20
Inventor 王帅郭永娜钟宏杨佳
Owner CENT SOUTH UNIV
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