Method for preparing trioctylphosphine oxide by hydrolysis addition

Abstract

The invention discloses a method for preparing trioctylphosphine oxide by hydrolysis addition. The method comprises the following steps: adding dioctylphosphine oxide, 1-octene, an acetic acid solventand di-tert-butyl peroxide into a polytetrafluoro reactor, adding a small amount of industrial mixed decene, and performing stirring for dissolving; raising the temperature to 130-140 DEG C, performing reaction for 12-36 hours, and enabling the 31P-NMR detection reaction to be completed; adding 5-15wt% of dilute hydrochloric acid into the reaction liquid to perform demulsification washing, and performing extraction with trichloromethane; washing an organic layer to be neutral with water; removing trichloromethane and unreacted olefin by evaporation with a rotary evaporator; performing recrystallization with ethanol; and performing filtration and vacuum drying to obtain a white solid. The preparation method disclosed by the invention has the advantages that the reaction steps are simple and environmentally friendly, the atom economy is good, and the product is high in purity and easy to separate and has industrialized prospects. The obtained product is applied to water quality detection and sewage treatment industries.

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 ...

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