Extractant, preparation method and application thereof

An extraction agent and reaction technology, applied in the field of extraction agent and its preparation, can solve the problems of difficult operation and low extraction efficiency, and achieve the effects of no secondary pollution, easy solid-liquid separation, and large processing capacity

Active Publication Date: 2020-04-17
XIAMEN INST OF RARE EARTH MATERIALS
View PDF3 Cites 13 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide an extractant and its preparation method and application to solve the

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Extractant, preparation method and application thereof
  • Extractant, preparation method and application thereof
  • Extractant, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0051] A kind of preparation method of above-mentioned extractant, comprises the steps:

[0052] (1) phenolic compound reacts with alkali, obtains corresponding phenate compound;

[0053] (2) the phenoxide compound and the halogenated carboxylic acid derivative or the halogenated carboxylic acid salt react in a solvent to obtain an intermediate;

[0054] (3) The intermediate is acidified to obtain the extractant.

[0055] Further, in the step (1), the reaction temperature is 40-60°C.

[0056] Further, in the step (2), the pH of the reaction is 10-12, and the reaction temperature is 60-110° C. During the step (2), solid sodium hydroxide is used to control the pH value of the reaction process to be alkaline, but it cannot exceed 10.

[0057] A method for enriching rare earth elements from low-concentration rare earth ore leachate, comprising the following steps:

[0058] (1) using alkaline compound to saponify the above-mentioned extractant to obtain saponified extractant; ...

Embodiment 1

[0073] Example 1 Synthesis of 2-(4-butoxyphenoxy)acetic acid (BPAA)

[0074] Weigh 0.05mol of 4-n-butoxyphenol and dissolve it in 100mL of ethanol and water, the mass ratio of ethanol to water is 1:1. Add 0.05 mol of solid sodium hydroxide, slowly heat to 50°C and stir for 30 minutes. Weigh 0.08 mol of sodium chloroacetate and dissolve it in ethanol, add 0.2 g of KI, slowly add to the three-neck flask, then continue to slowly heat to 110°C, condense and reflux for 5 hours. During the control reaction, the pH value was about 10. Use a rotary evaporator to remove ethanol, use 3mol / L hydrochloric acid to acidify, control the pH value to about 2-3, produce a brown solid, filter, and use deionized water to wash to neutral, and then recrystallize with toluene several times BPAA with a yield of 86% and a purity of 98% was obtained.

[0075] NMR spectrum such as figure 1

[0076] BPAA: 1 H NMR (500MHz, DMSO-d6) δ12.95(s,1H),6.84(s,4H),4.59(s,2H),3.89(t,J=6.5Hz,2H),1.69-1.62(m, ...

Embodiment 2

[0077] Example 2 Synthesis of 4-(4-butoxyphenoxy)butanoic acid (BPBA)

[0078] Weigh 0.05mol of 4-n-butoxyphenol into a three-necked flask, add 100mL of ethanol, add 0.5g of KI, weigh 0.05mol of solid sodium hydroxide, add it and slowly heat and stir, control the temperature at 40°C, and react 1 Cool down to room temperature after 1 hour, add 4-bromobutyrate methyl ester dissolved in ethanol (40mL) slowly in five times, and slowly heat to 60°C when adding 4-bromobutyrate methyl ester for the first time, and the temperature rise should not be too fast . When methyl 4-bromobutyrate is added completely, continue to heat up to 110°C, during which time solid sodium hydroxide is used to control the pH value of the reaction process to 12, react for 12 hours, then add 50mL of deionized water for ester hydrolysis reaction, continue After 3 hours of reaction, it was cooled to room temperature. Use a rotary evaporator to remove ethanol, use 3mol / L hydrochloric acid to acidify to produc...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
Solubilityaaaaaaaaaa
Login to view more

Abstract

The invention relates to the field of separation and enrichment of metals, in particular to an extractant, a preparation method and application thereof. The preparation method comprises the followingsteps that a phenol compound reacts with a halogenated carboxylic acid derivative or halogenated carboxylate in a solvent, then acidifying is carried out, and the phenoxy carboxylic acid extractant issynthesized. The prepared extractant can be used for enriching rare earth in rare earth mineral leachate after being saponified by an alkaline compound; compared with the existing extractant, the extractant has the advantages of being higher in precipitation capacity, high in precipitation efficiency and large in precipitation particles, facilitating the separation of a rare earth extraction complex and a water phase and improving the production efficiency; and moreover, the extractant can further be used for selectively recovering/separating valuable metals from different industries.

Description

technical field [0001] The invention relates to the field of separation and enrichment of metals, in particular to an extractant and its preparation method and application. Background technique [0002] In order to effectively recover and enrich low-concentration REEs, some classical methods, such as solvent extraction and chemical precipitation, are widely used to extract REEs from the leachate and wastewater of ion-adsorbed REE ores. The solvent extraction method has the advantages of continuous operation, high efficiency, low cost, and easy large-scale production, and can achieve the purpose of separating and enriching rare earths from most impurities. Recently, researchers developed a non-saponifiable centrifugal extraction process using 2-ethylhexyl phosphate mono-2-ethylhexyl (P507) and di-(2-ethylhexyl) phosphate (P204) from low concentrations of Ion adsorption rare earth ore leach solution enriches rare earth elements. This process can respectively obtain heavy rar...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C22B3/32C22B59/00C22B15/00C22B23/00C22B60/02
CPCC22B15/0086C22B23/00C22B59/00C22B60/0291C22B3/326Y02P10/20
Inventor 孙晓琦倪帅男陈倩文高云郭向广
Owner XIAMEN INST OF RARE EARTH MATERIALS
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap