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Preparation method of dialkylphosphinic acid extracting agent

A technology of dialkylphosphine and extractant, which is applied in the field of preparation of dialkylphosphinic acid extractant, can solve the problems of limited application, short reaction route, high equipment requirements, etc., and achieve cost reduction and low reaction requirements , the effect of high yield

Inactive Publication Date: 2014-11-19
TIANJIN JUDE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The same family patent CN101475588A uses a mixed initiator to obtain the target product in one step. The reaction route is short, but the reaction is carried out in a high-pressure reactor, which requires high equipment, and high-pressure reactions are inherently dangerous.
[0005] The dialkylphosphinic acid obtained from straight-chain α-olefins with more than six carbons is a white solid, which limits the application of this type of product in the field of extraction

Method used

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  • Preparation method of dialkylphosphinic acid extracting agent
  • Preparation method of dialkylphosphinic acid extracting agent
  • Preparation method of dialkylphosphinic acid extracting agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1) Synthesis of mixed olefins

[0022] Put 50g of α-octene, 800g of α-decene, and 150g of α-dodecene into a stirred 2L normal-pressure reaction flask, add 500g of 5% hydrochloric acid, then add 1g of chromocene, start stirring and heat up to At about 65°C, heat-preserve and stir for 3 hours, let stand, and separate the water layer to obtain reformed multi-branched olefins, that is, mixed olefins.

[0023] 2) Synthesis of dialkylphosphinic acid

[0024] Put 106g of sodium hypophosphite and 106g of glacial acetic acid into the normal-pressure reaction kettle brought back to the condenser in turn, start the stirring and heater, raise the temperature to 70°C, and add 300g of reformed mixed olefins after the sodium salt is completely dissolved , then add 10g of di-tert-butyl peroxide, raise the temperature to reflux (about 120°C), and keep it warm for 5 hours; add 10g of di-tert-butyl peroxide again, and keep it warm for 5 hours; repeat this 2 times, the total reaction time...

Embodiment 2

[0027] EXTRACTION AND SEPARATION EXPERIMENT OF MIXED DIALKYL PHYSININIC ACID ON NICKEL AND COBALT

[0028] The comparison of table 1 synthesis dialkyl phosphinic acid mixture and P507 nickel-cobalt separation effect

[0029]

[0030] Experimental conditions: Feed liquid—Co3.82g / L, Ni84.34g / L, pH=4.21, sulfate medium; organic phase—20% extractant + sulfonated kerosene, saponification rate 70%; grade—2 grade; Ratio O / A=1:1; mixing time—4min; temperature—12°C.

[0031] Experimental results:

[0032] The result shows that under the same extraction conditions, the dialkyl hypophosphorous acid mixture synthesized according to embodiment example 1 is compared with P507, and the extraction separation coefficient is higher by an order of magnitude. Under the same extraction conditions, the extraction performance of DDPA is better than P507.

Embodiment 3

[0034] Table 2. Test results of separation of nickel and cobalt from dialkylphosphinic acid mixtures under different Co(II) concentrations

[0035]

[0036] Test conditions: feed liquid pH=4.16, sulfate medium; organic phase—15%DDPA+sulfonated kerosene, saponification rate 70%; phase O / A=1:1; mixing time—4min; temperature—14°C.

[0037] test results:

[0038] Under the condition that the concentration of nickel ions in the stock solution is basically constant, the separation coefficient decreases with the increase of the concentration of Co(II) in the stock solution. It shows that DDPA is suitable for extracting and separating nickel and cobalt from solutions with low Co / Ni ratio, which reflects the excellent performance of the extractant.

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Abstract

The invention provides a preparation method of a dialkylphosphinic acid extracting agent. The preparation method comprises the following steps: mixing octene, decene and dodecene at a certain ratio; after catalytically reforming the mixture, catalyzing the mixture in an acidic medium by using oxide; enabling the mixture and sodium hypophosphite to be subjected to free radial substitution reaction at normal pressure to obtain a dialkylphosphinic acid mixture at high yield. The dialkylphosphinic acid mixture has extremely good extraction and separation effects for nickel and cobalt and is especially suitable for a high-nickel and low-cobalt system.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of a dialkylphosphinic acid extractant. Background technique [0002] Dialkylphosphinic acid is a kind of highly selective metal separation and extraction agent, and the representative one is di(2,4,4-trimethylpentyl)phosphinic acid (trade name Cyanex272). When it is used to separate nickel and cobalt, its separation coefficient is high, and it is the best extraction agent for nickel / cobalt separation. It is now widely used in mineral processing plants all over the world. Since dialkylphosphinic acid has different extraction activities for different metal ions at different pH values. Therefore, by adjusting the pH value of the feed liquid, it can also be applied to the selective extraction and separation of other metal ions, such as rare earth elements, transition metals such as copper, manganese, cadmium, zinc, iron, and zirconium, hafnium, uranium, thoriu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30
Inventor 多文彬
Owner TIANJIN JUDE TECH
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