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Preparation method for high-purity ionic liquid

An ionic liquid and high-purity technology, applied in the field of high-purity ionic liquid preparation, can solve the problems of lack of method specificity, high product impurity content and high synthesis cost, and achieve the effects of simple process, good product quality and low cost.

Inactive Publication Date: 2012-06-27
NANJING UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The purpose of the present invention is to overcome the defects of high product impurity content, high synthesis cost and lack of commonality in the existing ionic liquid synthesis method, to provide a simple process, good product quality, low cost, and the The method of unifying ionic liquids under a common technology has good industrialization prospects

Method used

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  • Preparation method for high-purity ionic liquid
  • Preparation method for high-purity ionic liquid
  • Preparation method for high-purity ionic liquid

Examples

Experimental program
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Effect test

Embodiment 1

[0041] The preparation of embodiment 1,1-methyl-3-butylimidazole acetic acid ionic liquid

[0042] Step 1, metathesis reaction synthesis 1-methyl-3-butyl imidazole base

[0043] Dissolve 214.2g of 1-methyl-3-butylimidazolium chloride (0.9mol) in 300g of absolute ethanol, place in a 1L reactor, dissolve 50.4g of potassium hydroxide (0.9mol) in 250g of anhydrous Slowly add ethanol to the reactor, and react at room temperature for 12 hours under full stirring, and filter to remove potassium chloride precipitate after the reaction, to obtain a 1-methyl-3-butylimidazole alkali solution with a mass content of about 28% , The yield (based on 1-methyl-3-butylimidazole base) is about 95%.

[0044] Step 2, ion exchange to remove chloride ions

[0045] Pack 201×7 strong base anion exchange resin (chlorine type) in a glass column with a size of Φ16×500mm, and the filling height is 450mm. First wash the resin with 100mL deionized water, then rinse with 100mL 4% NaOH, then rinse with 150...

Embodiment 2～3

[0055] Change step 1 potassium hydroxide consumption, other conditions are identical with embodiment 1, and the results are shown in Table 1

Embodiment 4～5

[0057] Change the concentration of hydroxide in step 2, other conditions are identical with embodiment 1, the results are shown in Table 1

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Abstract

A preparation method for a high-purity ionic liquid is disclosed, which orderly comprises five steps of metathetical reaction, ion exchange for removing halide ions, ion exchange for removing potassium ions, acid-alkali neutralization and solvent recovery. The method specifically comprises the following steps of: performing stirring reaction on the haloid of a target cation and potassium hydroxide for 2-24 hours in ethanol, and filtering to remove potassium halide, so as to obtain an alkaline liquid containing the target cation; adding water to dilute, and removing the residual halide ions and potassium ions through an anion exchange unit and a cation exchange unit orderly; and performing neutralization reaction for 2-6 hours with the conjugate acid of a target anion to obtain ionic liquid solution, filtering to remove solid insoluble substances, evaporating to recover a solvent, and drying to obtain the high-purity ionic liquid. Showed in the figure, the method disclosed by the invention is simple in technical process, good in the quality of product, low in cost, capable of unifying a plurality of ionic liquids in common technology, and with great industrialization prospect.

Description

technical field [0001] The invention relates to a preparation method of a high-purity ionic liquid that can be scaled up industrially. technical background [0002] Ionic liquids are salts composed of organic cations and inorganic or organic anions that are liquid at or near room temperature. Since it is completely composed of ions, ionic liquids have many advantages that conventional solvents do not have, such as low melting point, non-volatile, good thermal stability, strong solubility, and adjustable properties. Therefore, ionic liquids can be used as green solvents in industrial production, and their properties can also be adjusted by designing and changing their structures to achieve specific application purposes such as catalysis, separation, and material preparation. [0003] At present, non-chloroaluminate ionic liquids are mainly synthesized by a two-step method. The first step is the alkylation reaction of tertiary amines and halogenated hydrocarbons, and the sec...

Claims

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Application Information

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IPC IPC(8): C07D233/58C07C211/63C07C209/68C07F9/54C07D213/20
Inventor 吴有庭蔡大牛黄宽胡兴邦张志炳
Owner NANJING UNIV
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