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Sulfonic- functionalized caprolactam acidic ion liquid and preparation method thereof

An acidic ionic liquid, caprolactam technology, applied in organic chemistry and other directions, can solve problems such as preparations that have not been reported, and achieve the effects of easy availability of raw materials, strong adjustability, and easy promotion and use

Active Publication Date: 2011-07-13
溧阳常大技术转移中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no report on the preparation of sulfonic acid functionalized caprolactam Brφnsted acidic ionic liquid

Method used

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  • Sulfonic- functionalized caprolactam acidic ion liquid and preparation method thereof
  • Sulfonic- functionalized caprolactam acidic ion liquid and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Preparation of ionic liquid IL1: 50mmol (5.7g) of caprolactam and 10mL of water were fully dissolved, placed at room temperature or in an ice-water bath, then 55mmol (7.6g) of 1,4-butane sultone was added, and the reaction temperature was 25? C, reacted for 24h, then added 50mmol (4.9g) of sulfuric acid and 10mL of acetonitrile, refluxed for 6h, evaporated the obtained liquid to remove the solvent, washed with toluene to remove non-ionic residues, and dried in vacuum at 70°C to obtain colorless 17.2 g of transparent viscous liquid is IL1, and the yield is 95%. Its structural characterization data and physical parameters are shown in Table 1.

Embodiment 2

[0025] Preparation of ionic liquid IL2: the same method as in Example 1, replacing sulfuric acid with p-toluenesulfonic acid, the yield was 97%. Its structural characterization data and physical parameters are shown in Table 1.

Embodiment 3

[0027] Preparation of ionic liquid IL3: same as in Example 1, replacing sulfuric acid with formic acid, the yield was 85%. Its structural characterization data and physical parameters are shown in Table 1.

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Abstract

The invention relates to a chemical product and a preparation technology thereof, in particular to sulfonic-functionalized caprolactam acidic ion liquid and a preparation method thereof. The ion liquid has the following structural general formula shown in the specification, wherein B<-> is selected from the following anions: hydrogen sulfate radicals, p-toluene sulfate radicals, formate radicals, phosphate radicals, and acetate radicals. The preparation method comprises the steps of: firstly, mixing a caprolactam water solution with the concentration of 5-10mol / L with 1,4-butane sultone in the molar ratio of 1:1.1 for reaction for 6-24 h at the temperature of 25-80 DEG C; and then, reacting a reaction product with conjugate acid of the paired anion B<-> in the molar ratio of 1:1 for 4-6h. The preparation method provided by the invention has the advantages that the raw materials are cheap and are easy to obtain and the synthesis steps are simple and convenient and are easy to popularize and apply; the varieties of anions can be adjusted as required so as to satisfy requirements on different acidities so that stronger adjustability is achieved; and the synthesized ion liquid is more degradable than ion liquid of imidazole and pyridine, and is more environmental-friendly and recyclable.

Description

technical field [0001] The invention relates to a chemical product and its preparation technology, in particular to a sulfonic acid functionalized caprolactam Brφnsted (Bronsted acid) acidic ionic liquid and a preparation method thereof. Background technique [0002] Room temperature ionic liquids have been successfully used in organic synthesis due to their unique physical and chemical properties, such as non-volatile, non-flammable, relatively wide liquid temperature range, adjustable solubility, recyclable use and excellent electrochemical properties. , electrochemistry and materials science and many other fields. Various properties of ionic liquids at room temperature depend on the structures of anions and cations. In principle, room temperature ionic liquids can be designed according to requirements, and many room temperature ionic liquids can be obtained by changing the types of cations and anions, so there are various types of room temperature ionic liquids. [0003...

Claims

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Application Information

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IPC IPC(8): C07D223/08
Inventor 陈群吕琳何明阳尹芳华
Owner 溧阳常大技术转移中心有限公司
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