Solid acid catalysts with dual-center ionic liquid structures and preparation method and application thereof

A technology of solid acid catalyst and ionic liquid, which is applied in the direction of physical/chemical process catalyst, organic compound/hydride/coordination complex catalyst, carboxylate preparation, etc., which can solve the limitation of industrial application of ionic liquid and poor stability , synthesis difficulties and other problems, to achieve the effect of low cost, simple synthesis method and high synthesis purity

Inactive Publication Date: 2015-11-11
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these ionic liquids have low melting point, high viscosity, low acidity, poor stability, and difficult synthesis, which

Method used

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  • Solid acid catalysts with dual-center ionic liquid structures and preparation method and application thereof
  • Solid acid catalysts with dual-center ionic liquid structures and preparation method and application thereof
  • Solid acid catalysts with dual-center ionic liquid structures and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1: pyrazine bishydrogensulfate

[0017] Add 40.05g of pyrazine to a 250mL three-neck round bottom flask, and accurately weigh 98.08g of concentrated sulfuric acid to prepare a 50% dilute sulfuric acid aqueous solution by mass. Add it into a three-necked round-bottomed flask containing pyrazine, raise the temperature to 100°C and continue the reaction for 16 hours after the completion of the dropwise addition, and remove the water by rotary evaporation after the reaction. weight to give a tan solid. The product yield is 98%. Its chemical structural formula is:

[0018]

[0019] Characterization results: elemental analysis theoretical value C: 17.39%, H: 2.90%, N: 10.14%, measured value C: 17.42%, H: 2.98%, N: 10.10%. H NMR 1 HNMR (D 2 0, 300 MHz), δ = 8.646 (s, 4H, CH). Its melting point was measured by DSC scanning: 108.2°C.

Embodiment 2

[0020] Example 2: 2,2'-bipyridyl bishydrogensulfate

[0021] Add 39.05g of 2,2'-bipyridine to a 250mL three-neck round-bottom flask, and accurately weigh 49.04g of concentrated sulfuric acid to prepare a 50% dilute sulfuric acid aqueous solution by weight. Dilute sulfuric acid was slowly added dropwise into a three-necked round-bottomed flask containing 2,2'-bipyridine. After the dropwise addition, the temperature was raised to 100°C and the reaction continued for 8 hours. After the reaction was completed, the water was removed by rotary evaporation. The obtained sample was extracted three times with benzene and ether. And vacuum-dried at 80°C to constant weight to obtain a pink solid. The product yield is 99%. Its chemical structural formula is:

[0022]

[0023] Characterization results: elemental analysis theoretical values ​​C: 34.09%, H: 3.41%, N: 7.95%, measured values ​​C: 34.05%, H: 3.40%, N: 7.98%. H NMR 1 HNMR (D 2 0, 300 MHz), δ=7.515 (t, 2H, CH), 7.970 (t, ...

Embodiment 3

[0024] Embodiment 3: 1,10-phenanthroline dihydrogensulfate

[0025] Add 49.55g of 1,10-phenanthroline to a 250mL three-necked round-bottom flask, and accurately weigh 49.04g of concentrated sulfuric acid to prepare a 50% dilute sulfuric acid aqueous solution at room temperature. Slowly add dilute sulfuric acid into a three-necked round-bottomed flask containing 1,10-phenanthroline. After the addition, the temperature is raised to 100°C and the reaction is continued for 10 hours. After the reaction, the water is removed by rotary evaporation, and the obtained sample is repeatedly extracted with benzene and ether. three times, and dried under vacuum at 80 °C to constant weight to obtain a gray solid. The product yield is 99%. Its chemical structural formula is:

[0026]

[0027] Characterization results: elemental analysis theoretical values ​​C: 38.30%, H: 3.19%, N: 7.45%, measured values ​​C: 38.00%, H: 3.41%, N: 7.33%. H NMR 1 HNMR (D 2 0, 300 MHz), δ=7.407 (s, 2H, CH...

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Abstract

The invention discloses solid acid catalysts with dual-center ionic liquid structures. The cations of the solid acid catalysts with the dual-center ionic liquid structures are dications with symmetrical structures and containing nitrogen heterocyclic compounds, and the anions thereof are inorganic or organic strong acid anions. The solid acid catalysts with the dual-center ionic liquid structures, provided by the invention, have relatively high acidity, are good in stability, and can meet requirements for synthesis of most organic acid esters. The preparation process of the solid acid catalysts with the dual-center ionic liquid structures is simple, the product yield and purity are high, no byproduct is produced, and the synthesis cost is low; the solid acid catalysts with the dual-center ionic liquid structures are quite suitable for industrial production. The invention further discloses the preparation method of the solid acid catalysts with the dual-center ionic liquid structures.

Description

technical field [0001] The invention relates to a solid acid catalyst with a dual-center ionic liquid structure and a preparation method thereof. Background technique [0002] Ionic liquids refer to organic molten salts composed entirely of anions and cations at room temperature and nearby temperatures. As a hotspot of green and sustainable chemistry research, ionic liquids are widely used in organic reactions, liquid phase separation, gas Absorption, electrochemistry and other fields have great application potential. Since Wilkes reported the first tetrafluoroborate imidazole ionic liquid stable to both water and air in 1992, ionic liquids have been developed rapidly. Early ionic liquids can be roughly divided into four categories: pyridinium salts, imidazolium salts, quaternary ammonium salts, and quaternary phosphorus salts. Subsequently, ions with pyrazoles, piperazines, pyrroles, morpholines, thiazoles, azolines, guanidines, imidazoles, benzotriazines, sulfoniums, et...

Claims

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Application Information

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IPC IPC(8): B01J31/02C07C69/24C07C67/08C07C69/40C07C69/14C07C69/18C07C69/145
Inventor 吴有庭陈永乐胡兴邦
Owner NANJING UNIV
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