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Method for preparing didecyl phosphine oxide

A technology of didecylphosphine chloride and phosphine oxide, which is applied in the field of phosphorus chemical industry, can solve the problems of production method toxicity, high operation difficulty, and low yield, and achieve high product purity, good atom economy, and simple reaction steps Effect

Inactive Publication Date: 2018-10-02
四川中环检测有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] Trioctylphosphine oxide is widely used in the extraction of uranium in industry, usually with different proportions of D 2 EHPA combined, the extraction efficiency is very high, but the trialkylphosphorus oxide that has been industrialized is only trioctylphosphorus oxide. Therefore, the research and development of other industrialized production routes of trialkylphosphorus oxide is very important for finding new high-efficiency extractants. of great significance
However, as we all know, the Grignard reaction has many disadvantages: the operation is difficult, the conditions for preparing the Grignard reagent are very strict, the Grignard reagent is extremely sensitive to water and oxygen, and the yield is generally very low
[0013] Neutral phosphorus-type extractants are widely used in the extraction process of uranium. They generally have high selectivity to uranium and certain chemical radiation stability. However, only tri-n-octyl phosphorus oxide has been industrially produced in the market , and the production method or toxicity is relatively large, or the yield is low, still need to be improved, and need to develop the production method of more kinds of trialkylphosphine oxide

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add didecylphosphorus chloride to distilled water at room temperature, stir and hydrolyze for 10 minutes, adjust to pH > 13 with 5wt% NaOH solution, extract with chloroform, take the organic layer, wash with distilled water until neutral, and evaporate the organic layer with a rotary evaporator. layer solvent, dissolved in acetic acid, filtered, and the filter residue was discarded, adding chloroform and distilled water to extract the filtrate, collecting the organic layer, washing with distilled water until neutral, and drying in vacuo to obtain a white solid with a yield of 98%.

Embodiment 2

[0024] Add didecylphosphorus chloride to distilled water at room temperature, stir and hydrolyze for 30 minutes, adjust to pH > 13 with 15wt% NaOH solution, extract with chloroform, take the organic layer, wash with distilled water until neutral, and evaporate the organic layer by rotary evaporator. layer solvent, dissolved in acetic acid, filtered, and the filter residue was discarded, adding chloroform and distilled water to extract the filtrate, collecting the organic layer, washing with distilled water until neutral, and drying in vacuo to obtain a white solid with a yield of 99%.

Embodiment 3

[0026] Add didecylphosphorus chloride to distilled water at room temperature, stir and hydrolyze for 20 minutes, adjust to pH > 13 with 10wt% NaOH solution, extract with chloroform, take the organic layer, wash with distilled water until neutral, and evaporate the organic layer by rotary evaporator. layer solvent, dissolved in acetic acid, filtered, and the filter residue was discarded, added chloroform and distilled water to extract the filtrate, collected the organic layer, washed with distilled water until neutral, and dried in vacuo to obtain a white solid with a yield of 100%.

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Abstract

The invention discloses a method for preparing didecyl phosphine oxide. The method comprises the following steps: adding distilled water in didecyl phosphine oxide under room temperature, stirring andhydrolyzing for 10 to 30 minutes, regulating PH (Potential of Hydrogen) to be greater than 13 by using 5 to 15 weight percent of NaOH solution, extracting by using trichloromethane, taking an organiclayer, washing to be neutral by using the distilled water, evaporating to remove a solvent in the organic layer through a rotary evaporator, dissolving by using acetic acid, filtering, and discardingfilter residue; adding trichloromethane and the distilled water for extracting filtrate, collecting the organic layer, washing to be neutral by using the distilled water, and carrying out vacuum drying, thus obtaining white solid. The method for preparing didecyl phosphine oxide, disclosed by the invention, is simple in steps, is green and environmentally friendly and is good in atom economy, a product is high in purity, separation is easy, and an industrial prospect is obtained; the product is applied to industries of water quality detection and sewage treatment.

Description

technical field [0001] The invention belongs to the technical field of phosphorus chemical industry, and in particular relates to a method for preparing trialkyl phosphorus oxides. Background technique [0002] Extraction refers to the partial or complete entry of a compound into one solvent because of differences in solubility (partition coefficient) in two solvents that have little or no solubility in each other. With enough extractions, the compound goes completely into one of the solvents. [0003] There are many kinds of extractants, generally including inorganic and organic extractants. Most of the extractants used in industrial production are organic extractants, which have good solubility in organic solvents. The purpose of making it soluble in organic solvents is to increase its solubility with the metal to be extracted, enhance its extraction performance, and at the same time reduce its volatility, viscosity, and water solubility. Organic extractants are widely ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/53
CPCC07F9/5304
Inventor 闵成勇何明联刘良彬蒲冬勤谢林
Owner 四川中环检测有限公司
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