Method for preparing dioctyl phosphorus chloride

Abstract

The invention discloses a method for preparing dioctyl phosphorus chloride. The method comprises the following steps: adding dioctyl phosphinic acid and trichlorosilane in a PTFE (Polytetrafluoroethylene) reaction kettle, wherein trichlorosilane is excessive; adding an organic solvent, stirring and dissolving, rising the temperature to be 60 to 100 DEG C, reacting for 6 to 24 hours, detecting andcompletely reacting under <31>P-NMR (Nuclear Magnetic Resonance), and evaporating to remove the organic solvent and residual trichlorosilane by a rotary evaporator, thus obtaining light green liquid-dioctyl phosphorus chloride. The method for preparing the dioctyl phosphorus chloride, 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 preparation method of a trialkyl phosphorus oxide intermediate, dialkyl phosphorus chloride. 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 ...

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