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Synthetic method for (2-ethylhexyl)(2,4,4'-trimehtyl amyl) phosphinic acid

A technology of trimethylpentyl and ethylhexyl, which is applied in the field of synthesis of phosphinic acid, can solve the problems of unstable source, difficult emulsification, high price, etc., and achieve simple product purification, mild reaction conditions, and simple synthesis method Effect

Inactive Publication Date: 2017-05-10
UNIV OF SCI & TECH BEIJING
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Problems solved by technology

Didecylphosphinic acid is superior to P507 and Cyanex 272 to the separation performance of nickel and cobalt, and its synthetic raw material mixed decene is a petrochemical by-product, and the price is low, but the source is unstable (Ju Zhongjun et al., the synthesis of didecylphosphinic acid and extraction performance. Chinese Journal of Nonferrous Metals. 2010,20(11):2254-2259; Li Linyan, et al., Dialkyl phosphinic acids: synthesis and applications as extraction for nickel and cobalt separation. Trans.Nonferrous Metals Soc.China.2010, 20(Suppl.1):205-210; XingPeng, et al., Cobalt separation from nickel in sulfate aqueous solution by anew extractant: didecylphosphinic acid(DDPA).Hydrometallurgy,2012,113:86-90)
Bis(2-ethylhexyl)phosphinic acid (P227) has lower acidity for heavy rare earth back extraction than P507, and its separation performance is also better than P507. Equilibrium time is long, and the raw material 2-ethyl-1-hexene of synthetic P227 is expensive, and 2-ethyl-1-hexene needs excessive in the reaction, causes cost to increase further (Du ruobing, et al., Microwave-assisted synthesis of dialkylphosphinic acids and structure-reactivity study in rare earth metal extraction.RSC Advances.2015,5:104258-104262)

Method used

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  • Synthetic method for (2-ethylhexyl)(2,4,4'-trimehtyl amyl) phosphinic acid
  • Synthetic method for (2-ethylhexyl)(2,4,4'-trimehtyl amyl) phosphinic acid

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Experimental program
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Effect test

Embodiment 1

[0023] (1) Weigh 13.2g of sodium hypophosphite, 15.0g of petroleum ether, 0.32g of di-tert-butyl peroxide, 5.8g of 2-ethyl-1-hexene, and 3ml of concentrated sulfuric acid in a 100mL polytetrafluoroethylene-lined Add magnets to the reaction kettle, seal it, place it in a small tube furnace with a magnetic stirrer, and start the stirrer to react at 135°C for 12h.

[0024] (2) Cool down to room temperature, transfer the product to a 250 mL separatory funnel, extract three times with 30 mL 4% NaOH, and combine the aqueous phases. Add 20 mL of 10% HO to the aqueous phase 2 SO 4 , then extracted 3 times with 50 mL of ether, combined the ether phases, washed 3 times with 30 mL of saturated brine, then dried with anhydrous magnesium sulfate, filtered, and removed the ether with a rotary evaporator to obtain 7.4 g of light yellow oil, with a yield of 80 %, that is, mono(2-ethylhexyl)phosphinic acid.

[0025] (3) The mono(2-ethylhexyl)phosphinic acid product obtained above and 10mL o...

Embodiment 2

[0028] (1) Weigh 26.2g of sodium hypophosphite, 30.0g of n-octane, 0.8g of di-tert-butyl peroxide, 10.0g of 2-ethyl-1-hexene, and 15.2g of glacial acetic acid in a 100mL polytetrafluoroethylene Add a magnet to the lined reaction kettle, seal it, place it in a small tube furnace with a magnetic stirrer, and start the stirrer to react at 120°C for 8 hours.

[0029] (2) Cool down to room temperature, transfer the product to a 250 mL separatory funnel, extract three times with 50 mL 6% KOH, and combine the aqueous phases. Add 50 mL of 10% HCl to the water phase, then extract 4 times with 50 mL of ether, combine the ether phases, wash with 30 mL of saturated brine for 3 times, then dry with anhydrous sodium sulfate, filter, and remove the ether with a rotary evaporator to obtain light yellow 14.1 g of oil, 89% yield, namely mono(2-ethylhexyl)phosphinic acid.

[0030](3) Mix the mono(2-ethylhexyl)phosphinic acid product obtained above with 20mL of n-octane, 15.2g of diisobutylene, ...

Embodiment 3

[0033] (1) Weigh 26.8g of sodium hypophosphite, 25.0g of cyclohexane, 0.75g of azobisisobutyronitrile, 12.2g of diisobutene, and 13.2g of glacial acetic acid in a reaction kettle with a 100mL polytetrafluoroethylene liner, and add Magnet, sealed, placed in a small tube furnace with a magnetic stirrer under it, and reacted at 80°C for 16h with the stirrer turned on.

[0034] (2) Cool down to room temperature, transfer the product to a 250 mL separatory funnel, extract three times with 50 mL 6% KOH, and combine the aqueous phases. Add 50 mL of 10% HCl to the water phase, then extract with 50 mL of petroleum ether for 3 times, combine the petroleum ether phases, wash with 30 mL of saturated brine for 3 times, then dry with anhydrous sodium sulfate, filter, and remove the ether with a rotary evaporator to obtain 13.0 g of light yellow oily substance, yield 67%.

[0035] (3) Mix the monoalkylphosphinic acid product obtained above with 15mL cyclohexane, 24.2g 2-ethyl-1-hexene, 4.2g...

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Abstract

The invention provides a synthetic method for (2-ethylhexyl)(2,4,4'-trimehtyl amyl) phosphinic acid, and belongs to the technical field of wet metallurgy. The method comprises the following steps of performing a free radical addition reaction on 2-ehtyl-1-hexene and sodium hypophosphite or hypophosphorous acid, synthesizing a mono(2-ethylhexyl) phosphinic acid intermediate, then reacting with diisobutylene, and generating (2-ethylhexyl)(2,4,4'-trimethyl amyl) phosphinic acid; or firstly performing the free radical addition reaction on diisobutylene and sodium hypophosphite or hypophosphorous acid, synthesizing a mono(2,4,4'-trimethyl amyl) phosphinic acid intermediate, then reacting with 2-ehtyl-1-hexene, and generating a target compound. The reverse extraction acidity of the extraction agent phosphinic acid in the invention for heavy rare earth ions is lower than P507, the saturated extraction capacity is higher than that of Cyanex 272, the extraction balance time is shorter than P227, the synthetic method is mild in reaction condition, easy to implement, few in side reactions and simple in production purification, and the compound is suitable for large-scale production.

Description

technical field [0001] The invention relates to the technical field of hydrometallurgy, in particular to a method for synthesizing (2-ethylhexyl)(2,4,4'-trimethylpentyl)phosphinic acid. Background technique [0002] 2-Ethylhexyl phosphate-2-ethylhexyl ester (P507) and dialkylphosphinic acid represented by bis(2,4,4'-trimethylpentyl)phosphinic acid (Cyanex 272) are It is an effective extractant for extracting and separating rare earth and nickel and cobalt. P507 can efficiently separate light and medium rare earths, but it has high acidity, poor selectivity and slow extraction rate for heavy rare earths. The acidity of Cyanex 272 for heavy rare earth stripping is much lower than that of P507, and the separation performance of heavy rare earth and nickel-cobalt is better than that of P507, but its saturation load is low and it is easy to emulsify. Didecylphosphinic acid is superior to P507 and Cyanex 272 to the separation performance of nickel and cobalt, and its synthetic r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30C22B3/38
CPCC07F9/30C22B3/3842Y02P10/20
Inventor 王俊莲
Owner UNIV OF SCI & TECH BEIJING
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