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Preparation method and application of a kind of dialkylphosphinic acid compound or its salt

A technology of alkylphosphinic acid and compound, which is applied in the field of preparation of dialkylphosphinic acid compounds or their salts, and can solve problems such as harsh reaction conditions, many side reactions, and long reaction time

Active Publication Date: 2017-04-12
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to overcome the defects of low conversion rate, long reaction time, many side reactions and harsh reaction conditions in the existing preparation method of dialkylphosphinic acid compounds or their salts, and provide Preparation method and application of a kind of dialkylphosphinic acid compound or its salt

Method used

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  • Preparation method and application of a kind of dialkylphosphinic acid compound or its salt
  • Preparation method and application of a kind of dialkylphosphinic acid compound or its salt
  • Preparation method and application of a kind of dialkylphosphinic acid compound or its salt

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Experimental program
Comparison scheme
Effect test

Embodiment 1 2

[0099] The synthesis of embodiment 1 two (n-octyl) phosphinic acid:

[0100]

[0101] Sodium hypophosphite monohydrate 10.6g (0.1mol), glacial acetic acid 15mL (0.26mol), N,N-dimethylformamide (DMF) 80mL, 1-octene 22.4g (0.2mol), azobisiso 3.3g (0.02mol) of butyronitrile was reacted at 130°C for 1h. After adding 3.3 g (0.02 mol) of the initiator azobisisobutyronitrile, the reaction was continued at 130° C. for 1 h. After the reaction, cool down, wash the reaction liquid twice with water, wash once with saturated saline, add 8% (wt) NaOH solution to wash, add 20% (wt) sulfuric acid solution to acidify, extract twice with ether, combine the organic phases, and wash with water After washing, it was dried over anhydrous sodium sulfate, filtered with suction, and the solvent was removed under reduced pressure to obtain 23.4 g of the product with a yield of 80.7%.

[0102] 31 P NMR: Di(n-octyl)phosphinic acid: δ: 59.7ppm, 98.3% (purity, by peak value)

[0103] Neutralization ...

Embodiment 2

[0104] The synthesis of embodiment 2 two (2,4,4-trimethylpentyl) phosphinic acid

[0105]

[0106] Sodium hypophosphite monohydrate 10.6g (0.1mol), glacial acetic acid 10mL (0.175mol), 2,4,4-trimethyl-1-pentene 30g (0.27mol), benzoyl peroxide 4.8g (0.02 mol), DMF80mL were added to the microwave synthesis reactor in sequence, heated to 135°C under microwave conditions, and reacted for 2h. After adding 4.8 g (0.02 mol) of initiator benzoyl peroxide, the reaction was continued at 135°C for 2 h, and the above process was repeated 3 times (0.1 mol of initiator was added during the entire reaction process). After the reaction, cool down, wash the reaction solution twice with water, once with saturated saline, add 8% (wt) NaOH solution for washing, add 20% (wt) hydrochloric acid solution to acidify, extract twice with ether, combine the organic phases, and wash with water After washing, it was dried over anhydrous sodium sulfate, filtered with suction, and the solvent was removed...

Embodiment 3

[0109] The synthesis of two (3,3-dimethylbutyl) phosphinic acid of embodiment 3

[0110]

[0111] Sodium hypophosphite monohydrate 10.6g (0.1mol), glacial acetic acid 5mL (0.089mol), ethylene glycol monomethyl ether 75mL, 3,3-dimethyl-1-butene 16.8g (0.2mol), peroxidized 4 mL (0.021 mol) of tert-butyl benzoate was sequentially added to a microwave synthesis reactor, and heated to 90°C for 1 h under microwave conditions. After adding 4 mL of initiator tert-butyl peroxybenzoate, the reaction was continued at 90° C. for 1 h. Wash twice with water, once with saturated saline, add 8% (wt) NaOH solution to wash, add 20% (wt) sulfuric acid solution to acidify, extract twice with ether, combine organic phases, wash with water, and dry over anhydrous sodium sulfate. Suction filtration and desolventization under reduced pressure gave 17.5 g of the product with a yield of 74.8%.

[0112] 31 P NMR: bis(3,3-dimethylbutyl) phosphinic acid: δ: 61.7ppm, 95.6% (purity, by peak value)

...

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Abstract

The invention discloses a preparation method and an application of dialkyl phosphinate compounds and salts thereof. The method for preparing a compound shown as a formula I comprises the following steps: carrying out a free radical addition reaction shown as the following formula between a compound shown as a formula A1 and a compound shown as a formula B in an inert solvent under closed and / or microwave conditions in the presence of acids and initiators. The invention also discloses the compound shown as the formula I as well as an application thereof in separation of a metal-containing mixture. The invention further discloses an extraction agent composition and an extraction method. The preparation method is high in conversion rate, the reaction time is shortened to be 2-10 hours, the side reactions and byproducts are reduced, and the product purity is high.

Description

technical field [0001] The invention relates to a preparation method and application of a dialkylphosphinic acid compound or a salt thereof. Background technique [0002] The separation and purification of rare earth is currently the most widely used solvent extraction, and the most widely used rare earth extractant is the extractant P507 (the main component is 2-B 2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester), the extractant has excellent extraction performance and good separation coefficient, and can effectively separate rare earth elements. However, there are also shortcomings such as high acidity in stripping and serious pollution of three wastes, and the separation factor in the extraction of heavy rare earths needs to be further improved. [0003] In the second half of the 20th century, the American Cytec Corporation (CYTEC) produced Cyanex272 as a nickel-cobalt separation extractant, which has been widely used and has a good separation factor for the separati...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/30C22B3/38
CPCY02P10/20
Inventor 肖吉昌杜若冰王振兴张燕辉张婷
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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