Extracting agent for rare earth extraction separation, preparing method thereof and extraction separation method using same

An extraction agent and extraction technology, applied in the direction of improving process efficiency, etc., can solve problems such as insufficient separation coefficient, decline in extraction capacity, and increase in economic cost, and achieve the effect of good extraction phenomenon, maintenance of separation coefficient, and low cost

Active Publication Date: 2018-08-28
XIAMEN INST OF RARE EARTH MATERIALS
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  • Application Information

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Problems solved by technology

Although this extraction method can produce high-purity and high-yield yttrium oxide, there are many shortcomings in the extraction process of naphthenic acid, mainly because it is a by-product of the petroleum industry, its composition is complex, and it is easy to slowly undergo esterification with mixed alcohols. As a result, the extraction capacity is significantly reduced, and it needs to be replaced every few years, which not only wastes resources, but also may pollute the environment and greatly increase economic costs.
Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, designed and synthesized a carboxylic acid type extractant code-named CA12 (Ye Weizhen, Xu Qingren, Qian Yunfang, "Extractant for Separation of Rare Earth Metals" 93112500.6, 1994-03-30); invented by China Patent CN 99118261.8 discloses a process for separating yttrium oxide based on CA12, practice shows that the separation coefficient of CA12 to heavy rare earths (such as Er, Tm, Yb, Lu) and Y is not high enough

Method used

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  • Extracting agent for rare earth extraction separation, preparing method thereof and extraction separation method using same
  • Extracting agent for rare earth extraction separation, preparing method thereof and extraction separation method using same
  • Extracting agent for rare earth extraction separation, preparing method thereof and extraction separation method using same

Examples

Experimental program
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Effect test

Embodiment 1

[0079] 1) Synthetic extractant ortho-sec-octylphenoxy substituted n-propionic acid

[0080] Get 2.17 kilograms of 3-chloro-n-propionic acid, add 5 liters of water, slowly add 1.4 kilograms of potassium carbonate, adjust the pH value to 9, and obtain 3-chloro-n-propionic acid sodium solution; Under stirring conditions, add 4.13 kg of ortho-sec-octylphenol, and slowly add 0.46 kg of sodium metal. After the reaction is complete, heat up to 90 degrees Celsius and keep warm for half an hour to obtain a solution of ortho-sec-octylphenol sodium. Turn on stirring and heating, raise the temperature to 110 degrees Celsius, slowly add the 3-chloro-n-propionate sodium solution into the ortho-second-octylsodium phenolate solution, cool to room temperature after reacting for 1 hour, add 6 moles per liter of hydrochloric acid 5 1 liter for acidification, after washing 4 times, rotary evaporation to remove solvent, 160 degrees centigrade vacuum distillation, to obtain ortho-secondary octylphe...

Embodiment 2

[0096] 1) Synthetic extractant p-n-nonylphenoxy substituted isopropionic acid

[0097]Take 2.17 kg of 2-chloropropionic acid, add 5 liters of water, slowly add 1.4 kg of potassium carbonate, adjust the pH value to 9, and obtain a 2-chloropropionic acid sodium solution; Next, add 4.47 kg of p-n-nonylphenol, slowly add 2 kg of sodium hydroxide and raise the temperature to 90 degrees Celsius, react for half an hour, heat up to 110 degrees Celsius, slowly add 2-chloropropionate sodium solution to the p-normal In sodium nonylphenolate solution, react for 1 hour and then cool to room temperature, add 5 liters of hydrochloric acid with 6 moles per liter for acidification, wash 4 times with water, remove solvent by rotary evaporation, and distill under reduced pressure at 170 degrees Celsius to obtain para-n-nonyl The phenoxy substituted isopropionic acid product has a yield of 96.3%. After acid-base titration and NMR characterization, the purity of p-n-nonylphenoxy substituted isopro...

Embodiment 3

[0106] 1) Synthetic extractant p-n-nonylphenoxy substituted isopropionic acid

[0107] With embodiment 2.

[0108] 2) Prepare the organic phase: take 460 ml of p-n-nonylphenoxy substituted isopropionic acid obtained in step 1), mix it with 100 ml of tributyl phosphate and 260# solvent kerosene to obtain the organic phase, and extract The agent concentration is 0.80 mol / liter, and the volume ratio of tributyl phosphate is 10%. Add 88 milliliters of concentrated ammonia water to make the degree of saponification of the extractant in the organic phase reach 80%.

[0109] 3) Preparation of yttrium-containing rare earth feed liquid

[0110] With embodiment 2.

[0111] 4) Extraction and separation: such as figure 1 As shown, the whole extraction process was carried out in a mixed-settler tank, including 20 stages of extraction (n=60), 15 stages of washing (m=30) and 6 stages of back extraction (k=6). The mass flow ratio of the organic phase, the rare earth material liquid conta...

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Abstract

The invention discloses an extracting agent for rare earth extraction separation, a preparing method thereof and an extraction separation method using the extracting agent. The extraction separation method comprises the following steps of (1), mixing one or a plurality of diluents in an extracting agent which is represented by a formula (I) and/or a formula (II), and obtaining an organic phase; (2), mixing the organic phase obtained in the step (1) with yttrium-containing rare earth material solution, performing selective extraction for keeping the yttrium in a water phase and making poor-yttrium rare earth enter an organic phase, namely realizing extraction of rare earth yttrium. The extracting agent and the extraction separation method are advantageous in that 1, high selectivity of theextracting agent in rare earth extraction separation is realized, not only is a separation coefficient between light rare earth and yttrium kept, but also a separation range between heavy rare earth and the yttrium is improved; 2, the organic phase of the process can be cycled by more than one year without remarkable concentration reduction; 3, high extraction phenomenon and no emulsification arerealized; and 4, simple synthesis and low cost of the extracting agent are realized.

Description

technical field [0001] The invention belongs to the technical field of rare earth extraction and separation, and relates to an extraction agent for rare earth extraction and separation, a preparation method thereof and an extraction and separation method using the extraction agent, in particular to an extraction agent for extraction and separation of yttrium-containing rare earths, a preparation method thereof and An extraction and separation method for extracting yttrium-containing rare earths by using the extractant. Background technique [0002] As a type of heavy rare earth, yttrium is widely used in rare earth aluminum alloys, functional ceramics, lasers, phosphors and other fields. In the existing technology, the separation of yttrium mainly adopts the extraction and separation method based on naphthenic acid (code name NA). Using naphthenic acid-mixed alcohol-kerosene as the organic phase, high-purity yttrium oxide is prepared from a rare earth mixture with a yttrium...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B59/00C22B3/32
CPCC22B59/00C22B3/32Y02P10/20
Inventor 孙晓琦王艳良董亚敏
Owner XIAMEN INST OF RARE EARTH MATERIALS
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