Preparation method of dialkyl phosphinic acid

A technology of dihydrocarbyl phosphinic acid and halogenated hydrocarbons, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problem of many reaction steps, small steric hindrance and complex process and other problems, to achieve the effects of reducing production costs, mild reaction conditions, and low energy consumption

Inactive Publication Date: 2014-08-27
TSINGHUA UNIV
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Problems solved by technology

In this method, there is no P=O bond in the phosphorus trichloride molecule, and the steric hindrance is small. When it reacts with the Grignard reagent, the three Cl atoms in the phosphorus trichloride may all be replaced to generate trihydrocarbyl phosphine. Therefore, the yield of dihydrocarbylphosphinic acid is lower
In addition, there are many reaction steps and the reaction cycle is long
[0004] It can be seen that the yield of dihydrocarbylphosphinic acid in large-scale production is not high at present, and the process is relatively complicated and the cost is high, so the in-depth research and application of this type of compound are seriously affected

Method used

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  • Preparation method of dialkyl phosphinic acid
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  • Preparation method of dialkyl phosphinic acid

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preparation example Construction

[0017] Please also refer to figure 2 as well as image 3 , the preparation method of the dihydrocarbyl phosphinic acid provided by the present invention, the preparation method comprises the following steps:

[0018] Step 1, metal magnesium, halogenated hydrocarbon and solvent are mixed and reacted to obtain a Grignard reagent.

[0019] The Grignard reagent refers to the reaction of organic halogen compounds (halogenated hydrocarbons, active halogenated aromatic hydrocarbons) and metal magnesium in a solvent to form an organic magnesium reagent. The process is specifically:

[0020] Put a certain amount of metal magnesium bars into a three-necked flask with stirring, reflux and drying devices, then add a small amount of solvent, just to immerse the metal magnesium bars, and then add a small amount of mixture of halogenated hydrocarbons and solvents to initiate the reaction, heat Until the system obviously reacts, continue to add the above mixed solution dropwise after a fe...

Embodiment 1

[0037] Put 2.16g metal magnesium strips (0.09mol) into a three-necked flask equipped with a stirring, reflux, drying device and a constant pressure dropping funnel, and add 5mL of ether to immerse the magnesium strips. Mix 11.6g of brominated isooctane (0.06mol) with 30mL of diethyl ether and place in a constant pressure dropping funnel. First add about 1 / 10 volume of the above mixed solution into the flask, and heat until the system obviously reacts. After 10 minutes, under the state of maintaining reflux, continue to slowly add the rest of the above mixed solution dropwise. After the dropwise addition, maintain reflux and react for about 2 hours. After the reaction, the system was cooled to room temperature. 3.67g POCl 3 (0.024mol) mixed with 10ml of diethyl ether, placed in a constant pressure dropping funnel and slowly added dropwise to the above reaction system, and continued to stir for about 1 hour after the dropwise addition was completed. Then add 60 mL of H with a...

Embodiment 2

[0040] Put 2.16g metal magnesium bars (0.09mol) into a three-neck flask equipped with stirring, reflux, drying device and constant pressure dropping funnel, add 5mL tetrahydrofuran to immerse the magnesium bars. Mix 7.4g of bromohexane (0.045mol) with 60mL of tetrahydrofuran and place in a constant pressure dropping funnel. First add about 1 / 10 volume of the above mixed solution into the flask, and heat until the system obviously reacts. After 10 minutes, under the condition of maintaining reflux, continue to slowly add the rest of the above mixed solution dropwise. After the dropwise addition, maintain reflux and react for about 4 hours. After the reaction, the system was cooled to room temperature. 2.28g POCl 3 (0.015mol) mixed with 20mL tetrahydrofuran, placed in a constant pressure dropping funnel and slowly added dropwise to the above reaction system, and continued to stir for about 1 hour after the dropwise addition was completed. Then add 50 mL of H with a molar conc...

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Abstract

The invention relates to a preparation method of dialkyl phosphinic acid. The preparation method comprises the following steps: mixing magnesium metal, halohydrocarbon and a first solvent and carrying out a reaction to obtain a Grignard reagent; adding phosphorus oxychloride into the Grignard reagent and carrying out a reaction to obtain a dialkyl phosphoryl chloride coarse product; and adding an organic acid to hydrolyze dialkyl phosphoryl chloride in the dialkyl phosphoryl chloride coarse product to dialkyl phosphinic acid.

Description

technical field [0001] The invention relates to a method for preparing an organophosphorus compound, in particular to a method for preparing a dihydrocarbyl phosphinic acid. Background technique [0002] As a neutral phosphorus extractant, dihydrocarbyl phosphinic acid has been widely studied and applied in the extraction and separation of organic matter, post-treatment of high-level waste liquid, and extraction and separation of non-ferrous and rare earth metals. [0003] At present, the synthesis routes of dihydrocarbyl phosphinic acid mainly include Grignard reagent-phosphite method, free radical addition method, and Grignard reagent-phosphorus trichloride method. Grignard reagent-phosphite method for the synthesis of dihydrocarbyl phosphinic acid first reacts phosphorus trichloride with ethanol to generate diethyl phosphite, then reacts with Grignard reagent to generate dihydrocarbyl phosphine oxide, and finally oxidizes to dihydrocarbyl phosphonic acid . In this metho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30
Inventor 李林艳徐盛明黄华林王学军刘欣
Owner TSINGHUA UNIV
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