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Method for preparing hexyl-didecyl phosphorus oxide

A technology of didecyl and phosphorus oxide, applied in the field of phosphorus chemical industry, can solve the problems of toxicity of the production method, high operation difficulty, low yield and the like, and achieve the effects of high product purity, good atom economy and simple reaction steps

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

[0025] Add 2g of didecylphosphine oxide (0.006mol), 1.26g of 1-hexene (0.015mol), 10ml of acetic acid, 0.2g of di-tert-butyl peroxide into a 25ml PTFE reactor, mix a small amount of decene, and stir to dissolve , heated up to 140°C, and reacted for 12 hours. 31 P-NMR detection reaction is complete. Add 5 wt% dilute hydrochloric acid to the reaction solution to break the emulsion and wash it, and extract it with chloroform. The organic layer is washed with water until neutral, and the chloroform and unreacted olefins are evaporated by a rotary evaporator. Recrystallization from ethanol, filtration, and vacuum drying afforded a white solid. Yield 88.6%.

Embodiment 2

[0027] Add 2g didecylphosphine oxide (0.006mol), 1.26g 1-hexene (0.015mol), 10ml acetic acid, 0.4g di-tert-butyl peroxide into a 25ml PTFE reaction kettle, mix a small amount of decene, stir to dissolve , heated up to 130°C, and reacted for 36 hours. 31 P-NMR detection reaction is complete. Add 15wt% dilute hydrochloric acid to the reaction solution to break the emulsion and wash it, and extract it with chloroform. The organic layer is washed with water until neutral, and the chloroform and unreacted olefins are evaporated by a rotary evaporator. Recrystallization from ethanol, filtration, and vacuum drying afforded a white solid. Yield 89.5%.

Embodiment 3

[0029] Add 2g of didecylphosphine oxide (0.006mol), 1.26g of 1-hexene (0.015mol), 10ml of acetic acid, 0.3g of di-tert-butyl peroxide into a 25ml PTFE reactor, mix a small amount of decene, and stir to dissolve , heated up to 135°C, and reacted for 24 hours. 31 P-NMR detection reaction is complete. Add 10wt% dilute hydrochloric acid to the reaction solution to break the emulsion and wash it, and extract it with chloroform. The organic layer is washed with water until neutral, and the chloroform and unreacted olefins are evaporated by a rotary evaporator. Recrystallization from ethanol, filtration, and vacuum drying afforded a white solid. Yield 90.0%.

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Abstract

The invention discloses a method for preparing hexyl-didecyl phosphorus oxide. The method comprises the following steps: adding didecyl phosphorus oxide, 1-hexene and di-tert-butyl peroxide in a PTFE(Polytetrafluoroethylene) reaction kettle, adding a small amount of industrial mixed decene, stirring and dissolving, rising the temperature to be 130 to 140 DEG C, reacting for 12 to 36 hours, detecting and completely reacting under <31>P-NMR (Nuclear Magnetic Resonance), adding 5 to 15 weight percent of diluted hydrochloric acid in a reaction solution for carrying out demulsifying and washing, extracting by using trichloromethane, washing an organic layer to be neutral by using water, evaporating to remove trichloromethane and unreacted olefin through a rotary evaporator, recrystalizing by using ethanol, filtering, and carrying out vacuum drying, thus obtaining white solid. The method for preparing hexyl-didecyl phosphorus 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 qualitydetection 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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