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A kind of phenoxycarboxylic acid rare earth solution aluminum removal extractant

A technology of phenoxycarboxylic acid and rare earth solution, which is applied in the field of phenoxycarboxylic acid extractant and rare earth solution high-efficiency aluminum removal extractant. problem, to achieve the effect of stable extraction performance, less loss of extractant, and strong hydrophobicity

Active Publication Date: 2021-12-21
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the raw material of chlorinated naphthenic acid is still a mixture of naphthenic acids, the problem of complex components has not changed fundamentally, the water solubility of some components and the active reactivity of some chemical bonds have not changed, and the long-term operation of the aluminum removal process of this system does not Stablize
[0005] Patent CN1710119A discloses a long-chain fatty acid as an extractant, alcohols or N235 or petroleum sulfoxide as a cosolvent, and kerosene as a diluent to form a long-chain fatty acid-cosolvent-kerosene extraction organic phase aluminum removal system. Long-chain fatty acids belong to C18 unsaturated fatty acids, and there are two typical disadvantages. One is that long-chain fatty acids are very easy to form esters and water-insoluble precipitates with metal ions, which is difficult to use stably in industry; the other is that long-chain fatty acids themselves have monotonous or polyunsaturated bonds. These unsaturated bonds are easy to oxidize and break in complex environments such as metal ions, acids, and alkalis. The extraction agent is extremely unstable, and it is difficult to achieve the goal of aluminum removal in a long-term and stable manner.

Method used

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  • A kind of phenoxycarboxylic acid rare earth solution aluminum removal extractant
  • A kind of phenoxycarboxylic acid rare earth solution aluminum removal extractant
  • A kind of phenoxycarboxylic acid rare earth solution aluminum removal extractant

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Second-octyl o-phenoxyacetic acid has a phenoxycarboxylic acid structure and a pKa value of 5.35. It is easily soluble in conventional organic solvents but hardly soluble in water. It can be used as an extractant for aluminum removal in rare earth solutions. Take 2.8761g of sec-octyl-o-phenoxyacetic acid (purity 92%, 0.01mol) into a 100mL volumetric flask, add sec-octyl alcohol and kerosene at a volume ratio of 1:3 to make a 0.1mol / L Aluminum extractant, add 50mL of 0.1mol / L NaOH solution, fully mix and saponify for 20min (saponification rate 50%). After standing to remove the water phase, take the saponification extractant 4mL and 2mL of AlCl 3 (0.01mol / L) and GdCl 3 (0.01mol / L) mixed solution (pH=3.5) was mixed at room temperature for 20min, left to stand for phase separation, and the aqueous phase analysis of the raffinate in the lower layer showed that the extraction rate of aluminum was 30.28%, the distribution ratio was 0.4344, and the extraction rate of gadolini...

Embodiment 2

[0028] Sec-nonyl-p-phenoxypropionic acid has a phenoxycarboxylic acid structure and a pKa value of 5.23. It is easily soluble in conventional organic solvents but hardly soluble in water. It can be used as an extractant for aluminum removal in rare earth solutions. Take 3.1784g of sec-nonyl-p-phenoxy propionic acid (purity 92%, 0.01mol) into a 50mL volumetric flask, add isooctyl alcohol and toluene with a volume ratio of 2:10 to form a 0.2mol / L aluminum removal extraction agent, add 0.1mol / L NaOH solution 50mL, fully mix and saponify for 20min (saponification rate 50%). After standing to remove the water phase, take the saponification extractant 4mL and 4mL of AlCl 3 (0.01mol / L) and EuCl 3 (0.01mol / L) mixed solution (pH=3.5) was mixed at room temperature for 20min, left to stand for phase separation, and the aqueous phase of the raffinate in the lower layer was taken for analysis. The extraction rate of aluminum was 32.41%, the distribution ratio was 0.4795, and the extractio...

Embodiment 3

[0031]S-octyl-p-phenoxyacetic acid has a phenoxycarboxylic acid structure and a pKa value of 5.19. It is easily soluble in conventional organic solvents but hardly soluble in water. It can be used as an extractant for aluminum removal in rare earth solutions. Take 2.8735g of sec-octyl-p-phenoxyacetic acid (purity 92%, 0.01mol) to a 25mL volumetric flask, add TBP and n-heptane with a volume ratio of 3:10 to form a 0.4mol / L aluminum removal extractant , add 50mL of 0.1mol / L NaOH solution, fully mix and saponify for 20min (saponification rate 50%). After standing to remove the water phase, take the saponification extractant 4mL and 8mL of AlCl 3 (0.01mol / L) and GdCl 3 (0.01mol / L) mixed solution (pH=3.5) was mixed at room temperature for 20min, left to stand for phase separation, and the aqueous phase analysis of the raffinate in the lower layer showed that the extraction rate of aluminum was 35.32%, the distribution ratio was 0.5461, and the extraction rate of gadolinium was 0.5...

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Abstract

The present invention relates to a kind of phenoxycarboxylic acid extraction agent for efficient aluminum removal in rare earth solution, which has a typical structure of benzene ring and carboxylic acid group, wherein a carbon atom on the benzene ring is connected with carboxylic acid oxygen functional group (‑O‑(CH 2 ) n ‑COOH), the other five carbon atoms are connected to R1, R2, R3, R4 and R5 functional groups respectively, and the effective component is a single compound. Phenoxycarboxylic acid, cosolvent, and diluent are used to form a phenoxycarboxylic acid-cosolvent-diluent to extract the aluminum removal system of the organic phase, which has the characteristics of preferentially extracting aluminum ions, and can achieve efficient removal of impurity aluminum ions in rare earth solutions. The extraction agent has the characteristics of single active ingredient, small pKa value, stable extraction performance, etc., and is suitable for use as an efficient aluminum removal extraction agent for rare earth solutions.

Description

【Technical field】 [0001] The invention relates to a rare earth solution high-efficiency aluminum removal extractant, in particular to a phenoxycarboxylic acid extractant with a low pKa value, belonging to the field of rare earth extraction and separation. 【Background technique】 [0002] Rare earth and aluminum elements are often associated together, such as the southern ionic rare earth ore contains a large amount of Al(H 2 O) 3+ 6 and Al(OH) n (3-n)+ The form of aluminum adsorbed on the ore, northern bastnaesite also contains a large amount of aluminum, which is similar to rare earth metals in nature, and is often leached together with rare earth metals, making the impurity aluminum content in the rare earth solution 0.1-10g / L; Another example is that NdFeB waste often contains aluminum impurities brought in during the material manufacturing process. In the solution after hydrochloric acid leaching, the aluminum content is 0.5-5g / L; another example is rare earth mines a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B3/32C22B59/00
CPCC22B59/00Y02P10/20
Inventor 张香平李福建闫俊俊董海峰白璐张锁江
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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