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Method for synthesizing dialkyl hypophosphorous acid

A technology of dialkyl hypophosphorous acid and synthesis method, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, and organic chemistry, etc. Problems such as post-processing steps to achieve the effect of improving purity, shortening reaction time, and improving reaction rate

Active Publication Date: 2009-07-08
TSINGHUA UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

[0003] The structure of dialkylphosphinic acid contains two C-P bonds, and its formation is relatively difficult, and its synthesis often requires harsh reaction conditions and cumbersome post-processing steps, which limits the development and application of such compounds
Therefore, the method reported by Shiming Wo et al. is only applicable to the synthesis of branched dialkylphosphinic acid, and the product needs to be treated with lye, and the post-treatment process of acidification will discharge a large amount of acid-base wastewater

Method used

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  • Method for synthesizing dialkyl hypophosphorous acid
  • Method for synthesizing dialkyl hypophosphorous acid
  • Method for synthesizing dialkyl hypophosphorous acid

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Embodiment 1

[0030] Embodiment 1: the synthesis of dihexylphosphinic acid

[0031] 16.0g of NaH 2 PO 2 ·H 2 O, 16.0g of glacial acetic acid, 32.0g of 1-hexene mixed, put into a stainless steel reactor with Teflon lining, turn on the magnetic stirring, then add 0.73g of benzoyl peroxide and 1.8 g di-tert-butyl peroxide mixture, and finally add 40ml 2,2,4-trimethylpentane to the reactor, seal the reactor, start heating, and react at 120°C for 10 hours while maintaining magnetic stirring. After the reaction, cool down to room temperature naturally, open the reactor, filter the resulting mixture, remove a small amount of solids, transfer the filtrate to a separatory funnel, add 100ml of deionized water, shake, wash, discard the lower aqueous phase, and repeat this process for three times. For four times, the obtained organic phase was rotated at room temperature for one hour to collect 8.2 g of unreacted 1-hexene, and then the temperature was raised to 60°C for rotary evaporation to recover...

Embodiment 2

[0036] Embodiment 2: the synthesis of two (2,4,4-trimethylpentyl) phosphinic acid

[0037] 16.0g of NaH 2 PO 2 ·H 2 0, 16.0g glacial acetic acid, 48.6g diisobutene (containing 80% α-diisobutene and 20% β-diisobutene) mixes, packs in the stainless steel reactor with polytetrafluoroethylene liner, opens magnetic stirring, then goes to A mixture of 0.73 g of benzoyl peroxide and 1.8 g of di-tert-butyl peroxide was added to the reaction kettle, the reaction kettle was sealed, and heating was started, and the reaction was carried out at 140° C. for 15 hours while maintaining magnetic stirring. After the reaction, cool down to room temperature naturally, open the reactor, filter the resulting mixture, remove a small amount of solids, transfer the filtrate to a separatory funnel, add 100ml of deionized water, shake, wash, discard the lower aqueous phase, and repeat this process for three times. For four times, the obtained organic phase was rotated at 60°C for one hour, and 13.0 g...

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Abstract

The invention discloses a method for synthesizing a dialkyl phosphinic acid and belongs to the technical field of organic phosphorous compound preparation. The method comprises: mixing sodium hypophosphite and an alpha-alkene according to ratio and pouring the mixture in a closed reaction kettle which has a stirrer and can be heated, wherein the optimal alpha-alkene to sodium hypophosphite molar ratio is 2.2 to 2.7; mixing a low / or medium-temperature radical initiator and a high-temperature radical initiator according to a ratio of 5-0.1:1 and pouring the mixture into a reaction kettle; closing the reaction kettle and stirring the mixture for reaction for 2 to 40 hours at 40 to 200 DEG C; cooling the mixture, opening the reaction kettle, filtering the mixture and transferring a filtrate into a separating funnel and washing the filtrate; and evaporating an obtained organic phrase in a rotary mode to remove unreacted materials and solvents. A product obtained after the steps is the dialkyl phosphinic acid. The dialkyl phosphinic acid can provide a high-efficiency flotation agent or extracting agent used in the fields of ore flotation and metal iron extraction and separation. The method improves reaction rates, simplifies a post treatment process, reduces production costs and improves product purity.

Description

technical field [0001] The invention belongs to the field of preparation of organophosphorus compounds, and mainly describes a method for synthesizing dialkylphosphinic acid by using a composite free radical initiator. Background technique [0002] Dialkylphosphinic acid plays a very important role in mineral flotation, flame retardant, especially in the field of solvent extraction and separation. Since there is no ester oxygen atom in the structure of dialkylphosphinic acid, the electron-pushing effect of the alkyl group makes its pKa value larger, and it does not require higher acidity of the aqueous phase when extracting metal ions. Adjust the structure of the alkyl group to obtain the appropriate steric hindrance, so that it has high selectivity for the extraction of some specific metal ions. For example, bis(2,4,4-trimethylpentyl)phosphinic acid is a special-effect nickel and cobalt separation extractant, which requires only a small number of extraction stages to achie...

Claims

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Application Information

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IPC IPC(8): C07F9/30
Inventor 李林艳徐盛明成昌梅居中军
Owner TSINGHUA UNIV
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