Method for preparing dioctyl phosphine oxide

A technology of dioctylphosphine oxide and dioctylphosphine chloride, 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 reaction Effects in simple steps

Inactive Publication Date: 2018-06-29
四川中环检测有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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

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Effect test

Embodiment 1

[0022] Dioctylphosphorus chloride was added to distilled water at room temperature, stirred and hydrolyzed for 10 minutes, adjusted to pH > 13 with 5wt% NaOH solution, extracted with chloroform, the organic layer was taken, washed with distilled water until neutral, and evaporated to remove the organic layer by 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] Dioctylphosphorus chloride was added to distilled water at room temperature, stirred and hydrolyzed for 30 minutes, adjusted to pH > 13 with 15wt% NaOH solution, extracted with chloroform, and the organic layer was taken, washed with distilled water until neutral, and evaporated by a rotary evaporator to remove the organic layer. 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 98.5%.

Embodiment 3

[0026] Dioctylphosphorus chloride was added to distilled water at room temperature, stirred and hydrolyzed for 20 minutes, adjusted to pH > 13 with 10wt% NaOH solution, extracted with chloroform, and the organic layer was taken, washed with distilled water until neutral, and evaporated by a rotary evaporator to remove the organic layer. 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%.

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Abstract

The invention discloses a method for preparing dioctyl phosphine oxide. The method comprises the following steps: adding dioctyl phosphorus chloride into distilled water at room temperature, stirringand hydrolyzing for 10 to 30 minutes; adjusting with 5 to 15 weight percent of NaOH solution until a pH value is greater than 13; extracting with trichloromethane, taking an organic layer, and washingto neutral with the distilled water; evaporating by using a rotary evaporator to remove an organic layer solvent; dissolving with acetic acid, filtering and discarding filter residues; adding the trichloromethane and the distilled water; extracting filtrate and collecting an organic layer; and washing with the distilled water to neutral, and carrying out vacuum drying to obtain white solid. The preparation method disclosed by the invention has the advantages of simple reaction steps, greenness, environmental protection, high atom economy, high purity of a product, easiness in separation and industrial prospect. The product disclosed by the invention is applied to water quality detection and sewage treatment industry.

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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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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