Synthesis method of dialkyl phosphinic acid extractant

A technology of dialkyl phosphinic acid and synthesis method, applied in the field of synthesis of dialkyl phosphinic acid extractant, can solve the problems of dispersion, inability to meet the supply, scarce metal burial amount, etc., and achieve high selectivity and extraction effect Good, easy to synthesize effect

Inactive Publication Date: 2010-01-13
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In recent years, the cutting-edge technology industry has developed rapidly, and the demand for various rare metals and rare earth metals has also increas

Method used

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  • Synthesis method of dialkyl phosphinic acid extractant
  • Synthesis method of dialkyl phosphinic acid extractant
  • Synthesis method of dialkyl phosphinic acid extractant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1 Preparation of two (2,7-dimethyloctyl) phosphinic acid

[0030] Weigh 1.5g of azobisisobutyronitrile and 50g of acetic acid to prepare a solution, dissolve it and add it to the dropping device. Weigh 42.4g (0.4mol) of sodium hypophosphite monohydrate and 168g (1.2mol) of 2,7-dimethyloctene into a four-neck flask, add acetic acid as a solvent, stir until the salt dissolves, and start heating. Nitrogen is continuously fed into the reaction system, and the flow rate is controlled to prevent unreacted olefins from being taken out of the reaction phase. After the temperature rose to about 96°C, reflux began to appear in the condenser. At this temperature, evenly add the catalyst solution dropwise, control the reflux, and react for 16 hours. The reaction solution was cooled down to be processed.

Embodiment 2

[0031] Example 2 Preparation of two (2,3 dimethylheptyl) phosphinic acid

[0032] Weigh 1.5g of azobisisobutyronitrile and 50g of acetic acid to prepare a solution, dissolve it and add it to the dropping device. Weigh 42.4g (0.4mol) of sodium hypophosphite monohydrate and 151g (1.2mol) of 2,3-dimethylheptene into a four-necked flask, and add acetic acid as a solvent, stir until the salt dissolves and start heating. Nitrogen was continuously fed into the reaction system. After the temperature rose to about 94°C, reflux began to appear in the condenser. At this temperature, evenly add the catalyst solution dropwise, control the reflux, and react for 16 hours.

Embodiment 3

[0033] Example 3 Preparation of two (2-n-butylhexyl) phosphinic acid

[0034] Weigh 1.5g of azobisisobutyronitrile and 50g of acetic acid to prepare a solution, dissolve it and add it to the dropping device. Weigh 42.4g (0.4mol) of sodium hypophosphite monohydrate and 168g (1.2mol) of 2-n-butylhexene into a four-necked flask, and add acetic acid as a solvent, stir until the salt dissolves and start heating. Nitrogen was continuously fed into the reaction system. After the temperature rose to about 95°C, reflux began to appear in the condenser. At this temperature, evenly add the catalyst solution dropwise, control the reflux, and react for 16 hours.

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Abstract

The invention discloses a synthesis method of dialkyl phosphinic acid extractant, belonging to the technical field of organic extractant synthesis and the method adopts phosphine gas high pressure reaction method. The method comprises the following specific steps: step1, using decylene and phosphine to perform free radical addition reaction and obtain dialkylphosphorane; step2, oxidizing dialkylphosphorane with peroxide to oxidize the trivalent phosphorus to pentavalent phosphorus and finally obtaining dialkyl phosphinic acid. The invention has good extraction effect on metal ions such as cobalt and the like in low pH, high selectivity and simple synthesis method.

Description

technical field [0001] The invention belongs to the technical field of organic matter extraction, in particular to a synthesis method of a dialkylphosphinic acid extractant. Background technique [0002] Cu, Co, Zn, Fe and other ores in China are mostly low-grade, and the separation of these minerals is still a big problem so far. [0003] The application of alkylphosphinic acid in solvent extraction is developed with the development of cutting-edge technology industry. In recent years, the cutting-edge technology industry has developed rapidly, and the demand for various rare metals and rare earth metals has also increased sharply. However, the buried amount of these metals is scarce and scattered, and the refining technology is not yet mature, so the supply cannot be met. After the emergence of substances with special properties such as alkylphosphinic acid, and under the impetus of various other factors, the smelting industry developed and applied the method of solvent e...

Claims

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Application Information

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IPC IPC(8): C07F9/30C22B3/38
CPCY02P10/20
Inventor 成昌梅徐盛明李林艳罗军奇
Owner TSINGHUA UNIV
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