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Organic heteropoly hybrid catalyst for esterification reaction and preparation method thereof

A technology for esterification reaction and heteropoly acid, which is applied in the preparation of organic compounds, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc., to achieve convenient recovery, simple synthesis process and high yield Effect

Inactive Publication Date: 2012-10-03
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, organic heteropolyacid salt catalysts with BrΦnsted acidity are still very rare, and the recovery and reuse performance of such catalysts need to be further improved

Method used

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  • Organic heteropoly hybrid catalyst for esterification reaction and preparation method thereof
  • Organic heteropoly hybrid catalyst for esterification reaction and preparation method thereof
  • Organic heteropoly hybrid catalyst for esterification reaction and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 60mL of distilled water, 0.58g of polyvinylpyrrolidone and 5.0g of 12-phosphotungstic acid into a 100mL round bottom flask, and stir at 50°C for 12h. The solvent was removed by rotary evaporation, washed repeatedly with ethanol, and dried at 100° C. for 12 hours to obtain 5.3 g of polyvinylpyrrolidone-phosphotungstic acid hybrid catalyst (PVP-PW). IR (KBr, v / cm -1 )( figure 1 ) characterization results are: 1643, 1296, 1080, 983, 889, 804cm -1 .

[0019] In a 50mL three-necked flask equipped with a magnetic stirrer, a spherical condenser and a water separator, add 0.2g catalyst PVP-PW, 30mmol acetic acid and 36mmol n-butanol, heat the oil bath to 110°C, and react for 1.5h. The results of the catalytic reactions are shown in Table 1.

Embodiment 2

[0021] Add 60mL of distilled water, 0.52g of methylpyrrolidone and 5.0g of 12-phosphotungstic acid into a 100mL round bottom flask, and stir at 50°C for 12h. The solvent was removed by rotary evaporation, washed repeatedly with ethanol, and dried at 100°C for 12 hours to obtain 5.2 g of methylpyrrolidone-phosphotungstic acid hybrid catalyst ([NMP] 3 PW).

[0022] The resulting catalyst [NMP] 3 PW is used for the esterification reaction of acetic acid and n-butanol, carried out according to the method described in Example 1, and the results of the catalytic reaction are shown in Table 1.

Embodiment 3

[0024] Add 60mL of distilled water, 0.59g of caprolactam and 5.0g of 12-phosphotungstic acid into a 100mL round bottom flask, and stir at 50°C for 12h. The solvent was removed by rotary evaporation, washed repeatedly with ethanol, and dried at 100°C for 12 hours to obtain 5.2 g of caprolactam-phosphotungstic acid hybrid catalyst ([CLA] 3 PW).

[0025] The resulting catalyst [CLA] 3 PW is used for the esterification reaction of acetic acid and n-butanol, carried out according to the method described in Example 1, and the results of the catalytic reaction are shown in Table 1.

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PUM

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Abstract

The invention discloses an organic heteropoly hybrid catalyst for an esterification reaction. The organic components comprise polyvinyl pyrrolidone, methyl-pyrrolidone and caprolactam. The heteropoly acid is 12-phosphotungstic acid, 12-phosphomolybdic acid and 12-silicotungstic acid. The preparation method comprises the step that the organic components and the heteropoly acids are subjected to protonation to obtain the organic heteropoly hybrid catalyst. The invention has the advantages that the preparation process of the catalyst is simple and practicable; and the obtained catalyst is suitable for the esterification reaction of many kinds of carboxylic acids and alcohol, and has the characteristics of high catalytic activity and selectivity, convenient recycling, and stable reutilization performance, thereby being an environment-friendly novel solid acid catalyst.

Description

technical field [0001] The invention relates to the preparation and application of a solid acid catalyst, in particular to a preparation method of an organic heteropolyacid hybrid catalyst and its application in the esterification reaction of carboxylic acid and alcohol. Background technique [0002] Carboxylate is an important class of fine chemicals widely used in fragrances, cosmetics, surfactants, medical drugs, etc. The traditional esterification reaction mainly uses H 2 SO 4 , HF, H 3 PO 4 Such as inorganic liquid acid as a catalyst, not only the separation and reuse of the catalyst are difficult, but also there are problems such as equipment corrosion and environmental pollution. Therefore, solid acid catalysts that can be easily recovered and reused have received extensive attention. [0003] Heteropolyacids are a class of strong inorganic solid acids with redox properties, and are widely used as catalysts for many acid-catalyzed and oxidation reactions. Howeve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/18B01J31/16C07C67/08C07C69/14C07C69/704C07C69/24C07C69/78C07C69/40
Inventor 冷炎张书源蒋平平
Owner JIANGNAN UNIV
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