Trioctylphosphine oxide compound and preparation method thereof

A technology of trioctyl phosphorus oxide and compound, applied in the field of trioctyl phosphorus oxide compound and preparation thereof, can solve the problems of unfavorable industrial application, low yield and high cost, and achieves easy control, convenient purification and enhanced safety. Effect

Active Publication Date: 2013-08-07
TIANJIN JUDE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] However, the cost of using iodine as a reactant is too high, which is extremely unfavorable for industrial applications
[0015...

Method used

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  • Trioctylphosphine oxide compound and preparation method thereof
  • Trioctylphosphine oxide compound and preparation method thereof
  • Trioctylphosphine oxide compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] The synthesis of trioctyl phosphorus oxide, taking n-octene as an example, includes the following steps:

[0051] 1) Octene addition:

[0052] Add 10g (0.114mol) of sodium hypophosphite to 50ml of acetic acid. After heating to 120°C, slowly add 30g (0.268mol) of n-octene and continue heating to 135°C for 4 hours. 31 PNMR detects the end of the reaction. After the reaction is complete, cool, add water and chloroform to separate liquids to remove acid, vacuum distillation (400Pa, 35℃) to remove organic solvents, vacuum drying (120Pa, 25℃) to obtain white solid dioctylphosphine Acid 30.8g (0.106mol). The yield was 93.2%.

[0053] 2) Trichlorosilane reduction

[0054] Put 2g (0.007mol) of dioctylphosphinic acid obtained in step 1 into a 50ml airtight reactor, add 30ml of chloroform (dehydrated) as a solvent, add 2g (0.015mol) of trichlorosilane, and react at 80°C 16 hours, 31 The end point of the reaction was detected by PNMR. After the reaction was completed, the organic solvent...

Embodiment 2

[0060] The difference from Example 2 is the process after step 2.

[0061] 1) Hydrolysis: Dissolve 2g (0.007mol) of dioctylphosphorus chloride obtained in step 2 of Example 1 in 20ml of chloroform, add distilled water to hydrolyze, 31 The end of the reaction was detected by PNMR. After the reaction was completed, lye was added for liquid separation, the water layer was removed, chloroform was distilled off under reduced pressure (400Pa, 35°C), and dried under vacuum to obtain 1.73g (0.006mol) of white solid dioctylphosphonic acid. The yield was 92.9%.

[0062] 2) Addition of octene again: Put 2g of dioctylphosphonic acid (0.007mol) into 20ml of acetic acid, heat to 120°C, slowly drop in 2.2 (0.020mol)g of octene, and continue heating to 135°C for 8 hours , 31 PNMR detects the end of the reaction. After the reaction is complete, add chloroform and distilled water to remove acetic acid, distill under reduced pressure to remove chloroform (400Pa, 35°C), vacuum dry (120Pa, 25°C) to obt...

Embodiment 3

[0064] Dissolve 2g (0.007mol) of dioctylphosphorus chloride obtained in step 2 of Example 1 in 20ml of chloroform, add 1g (0.0077mol) of n-octanol, and react at 50°C for 2 hours. 31 The end point of the reaction was detected by PNMR. After the reaction was completed, water was added and the chloroform (400Pa, 35°C) and excess n-octanol (400Pa, 65°C) were removed by distillation under reduced pressure to obtain 2.57g (0.0067 mol). Yield 95.1%

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Abstract

The invention aims to provide a trioctylphosphine oxide compound and a preparation method thereof, which is high in yield, low in cost and moderate in reaction conditions. In order to fulfill the aim of the invention, the technical scheme of the invention is that the preparation method for the trioctylphosphine oxide compound comprises the following steps of: preparing trioctylphosphine oxide from sodium hypophosphite by performing octene addition, trichlorosilane reduction, bromoalkane addition and hydrolysis in turn; or preparing the trioctylphosphine oxide from the sodium hypophosphite by performing the octene addition, the trichlorosilane reduction, the hydrolysis and the octene addition again in turn; or preparing the trioctylphosphine oxide from the sodium hypophosphite by performing the octene addition, the trichlorosilane reduction and alcoholysis in turn. According to the synthesis method provided by the invention, the selected raw materials are easy to obtain; the addition reaction is performed on the sodium hypophosphite and octene, so that the reaction conditions are moderate and are easy to control; the operation safety is enhanced; the reaction yield is high and can reach over 90 percent; the trioctylphosphine oxide is convenient to purify; and the product purity is high.

Description

Technical field [0001] The invention belongs to the field of organic chemistry, and specifically relates to a trioctyl phosphorus oxide compound and a preparation method thereof. Background technique [0002] Trioctyl phosphorus oxide compounds are usually used for the extraction of metals such as nickel, cobalt and uranium. Take uranium extraction as an example: the solution processed by the uranium metallurgical plant is a dilute solution with large volume, low uranium concentration, and high impurity content. Uranium must be separated from impurities and initially enriched. In the refining process, the processed solution is high. Concentration of uranium-containing solution, the product quality requires nuclear purity. The commonly used organic phosphine and octylamine extractants in the extraction process of uranium are tributyl phosphate (TBP), di-(2-ethylhexyl) phosphoric acid, trioctylamine, etc. [0003] In uranium hydrometallurgical plants, the extraction of sulfuric aci...

Claims

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Application Information

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IPC IPC(8): C07F9/53
Inventor 多文彬
Owner TIANJIN JUDE TECH
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