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A kind of immobilized ionic liquid and preparation method thereof

A technology of ionic liquid and cation, which is applied in the field of immobilized ionic liquid and its preparation, can solve the problems of low impurity removal efficiency and low recovery rate of rare earth ions, and achieve the goals of protecting the environment, superior impurity removal performance, and overcoming secondary pollution Effect

Active Publication Date: 2020-02-18
INST OF APPLIED CHEM JIANGXI ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, the immobilized ionic liquids in the prior art have low removal efficiency for iron and aluminum non-rare earth impurity ions, and pretreatment for removal of impurities is required, resulting in low recovery rate of rare earth ions

Method used

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  • A kind of immobilized ionic liquid and preparation method thereof
  • A kind of immobilized ionic liquid and preparation method thereof
  • A kind of immobilized ionic liquid and preparation method thereof

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preparation example Construction

[0027] The above-mentioned immobilized ionic liquid preparation method comprises the following steps:

[0028] (1) prepare dialkyl diglycol amic acid;

[0029] Dissolve dialkylamine and diglycolic anhydride in a low-polarity organic solvent, stir and react at room temperature for 48 hours, wash the resulting solution with dilute hydrochloric acid solution to remove residual diisooctylamine, and rotary evaporate to remove ethyl acetate and a small amount of water to obtain dialkyl diglycol amic acid. Low polar organic solvents include ethyl acetate, tetrahydrofuran, toluene, hexane or kerosene; ethyl acetate is preferred. To ensure complete reaction of diglycolic anhydride, the present invention sets the molar ratio of dialkylamine to diglycolic anhydride to be 1.0-1.5:1.

[0030] Dialkylamines are preferred: diisooctylamine, di-n-octylamine, di-n-hexylamine or di-n-decylamine.

[0031] The dialkyl diglycol amic acid prepared by selecting the above raw materials is: dioctyl ...

Embodiment 1

[0040] (1) Diisooctylamine and diglycolic anhydride with a molar ratio of 1.1:1 were dissolved in ethyl acetate, stirred and reacted at room temperature for 48 hours, and the resulting solution was washed with dilute hydrochloric acid solution to remove residual diisooctylamine, Ethyl acetate and a small amount of water were removed by rotary evaporation to obtain di(2-ethylhexyl) diglycol amic acid;

[0041] (2) Put chlorine-type strong basic polystyrene resin in a chromatographic column, and use 2wt% sodium hydroxide solution to flow through the resin layer to carry out anion exchange. After the alkali washing is completed, rinse with deionized water until the pH value is neutral to obtain a strongly basic polystyrene resin in the form of hydroxide.

[0042](3) Swell 20.0g of hydroxide-type strongly basic polystyrene resin in N,N-dimethylformamide for 1h to make a suspension, and then 29.1g of bis(2-ethylhexyl) diglycolamide Dissolve the acid in N,N-dimethylformamide, add i...

Embodiment 2

[0045] (1) Dissolve di-n-octylamine and diglycolic anhydride with a molar ratio of 1.3:1 in ethyl acetate, stir and react at room temperature for 48 hours, and use dilute hydrochloric acid solution to wash the resulting solution to remove residual di-n-octylamine, Ethyl acetate and a small amount of water are removed by rotary evaporation to obtain dioctyl diglycol amic acid;

[0046] (2) Put chlorine-type strong basic polystyrene resin in a chromatographic column, and use 2wt% sodium hydroxide solution to flow through the resin layer to carry out anion exchange. After the alkali washing is completed, rinse with deionized water until the pH value is neutral to obtain a strongly basic polystyrene resin in the form of hydroxide.

[0047] (3) Swell 15.0g of hydroxide-type strongly basic polystyrene resin in N,N-dimethylformamide for 1h to make a suspension, then dissolve 19.3g of dioctyl diglycol amic acid in N, Add N-dimethylformamide to the suspension of the above-mentioned hy...

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Abstract

The present invention provides an immobilized ionic liquid and a preparation method thereof, wherein the cation of the immobilized ionic liquid is a trialkylbenzyl ammonium cation shown in formula (I), and the anion of the immobilized ionic liquid is Deprotonated dialkyl diglycol amic acid shown in formula (II): in formula (I), R 1 and R 2 is methyl, R 3 Be methyl or hydroxyethyl; In formula (II), R 4 and R 5 Each is independently an alkyl group and at least one is an alkyl group having at least 6 carbon atoms. The immobilized ionic liquid and the preparation method thereof provided by the invention can preferentially extract rare earth ions, have high impurity removal efficiency for iron and aluminum impurity ions, thereby have a high recovery rate for low-concentration rare earths, and improve the utilization rate of rare earth resources.

Description

technical field [0001] The invention relates to the field of separation materials, in particular to an immobilized ionic liquid and a preparation method thereof. Background technique [0002] With the development and popularization of in-situ leaching technology for ion-type rare earth ores, rich ores are preferentially mined and utilized, resulting in a gradual decline in the grade of rare earths in ion-type rare earth ores, resulting in low rare earth leaching rates and low concentrations of rare earths in leachate. It is still difficult to effectively enrich and recover these low-concentration rare earth resources. At present, when solvent extraction is used to recover rare earths from low-concentration rare earth solutions, due to the low concentration of rare earths in the leach solution, the extraction ratio is large, the phase interface is unclear and the entrainment is serious, causing secondary pollution and other problems. In recent years, in order to overcome the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F8/30C08F8/12C08F112/14C22B59/00C22B3/32
CPCC08F8/30C22B59/00C22B3/284C08F8/12C08F112/14Y02P10/20
Inventor 崔红敏冯雪娇石劲松晏南富翁雅青邓朝阳
Owner INST OF APPLIED CHEM JIANGXI ACAD OF SCI