Polymeric solid acid catalyst for esterification reaction and preparation method thereof

A technology of solid acid catalyst and esterification reaction, applied in the direction of preparation of organic compounds, organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, etc., can solve pollution, equipment corrosion environment, catalyst separation and Difficulty in reuse and other problems, to achieve the effect of simple filtration recovery, high catalytic activity, and simple reuse

Inactive Publication Date: 2015-04-22
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most of the esters produced in industry are based on H 2 SO 4 , HF or H 3 PO 4 Such as inorganic liquid acid as a catalyst, but this method has great disadvantages: not only the separation and reuse of the catalyst is very difficult, but also brings serious equipment corrosion and environmental pollution problems
[0004] In order to solve the problems referred to above, the present invention adopts free radical polymerization to make the polymeric solid acid catalyst containing polysilsesquioxane (POSS) to synthesize carboxylate, and this method has not yet been reported

Method used

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  • Polymeric solid acid catalyst for esterification reaction and preparation method thereof
  • Polymeric solid acid catalyst for esterification reaction and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0015] Preparation of octavinyl POSS: In a round bottom flask, add 20mL vinyltriethoxysilane and 100mL ethanol, stir and mix evenly, slowly add 8mL of 37% hydrochloric acid and 6mL deionized water dropwise, at 25°C After stirring for 24 h, the white solid was filtered out, washed three times with ethanol, and then recrystallized with a mixed solution of tetrahydrofuran and methanol (1:3 by volume), and the obtained crystal was vacuum-dried at 80° C. for 10 h to obtain octavinyl POSS.

[0016] Polymerized solid acid catalyst POSS-SO 3 Preparation of H: The octavinyl POSS and sodium p-styrenesulfonate obtained above are added to a mixed solvent of tetrahydrofuran and deionized water (volume ratio is 10:1) according to a molar ratio of 1:8, and a certain amount of The initiator azobisisobutyronitrile AIBN (1% of the total mass of octavinyl POSS and sodium p-styrene sulfonate), then stirred at 25°C for 4h, filtered or centrifuged to separate the solid product, and washed three tim...

Embodiment 2

[0018] In a 100mL round bottom flask, add acetic acid and n-butanol (molar ratio is 1: 1.2), then add the solid acid catalyst POSS-SO with a mass of 2% of the total mass of the reactant 3 H, at a reaction temperature of 120°C, reflux to separate water, and stirred for 2 hours. According to chromatographic analysis, the conversion rate of acetic acid was 99%, and the selectivity of butyl acetate was 100%.

Embodiment 3

[0020] In a 100mL round bottom flask, add acetic acid and benzyl alcohol (molar ratio is 1: 1.2), then add the solid acid catalyst POSS-SO 3 H, at a reaction temperature of 150°C, reflux to separate water, and stirred for 6 hours. According to chromatographic analysis, the conversion rate of acetic acid was 92%, and the selectivity of benzyl acetate was 100%.

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Abstract

The invention discloses a polymeric solid acid catalyst for esterification reaction and a preparation method thereof. The preparation method comprises the following steps: copolymerizing octavinyl polysilsesquioxane and sodium p-styrenesulfonate under the initiation of azobisisobutyronitrile, and carrying out ion exchange on the obtained polymer to obtain the polymeric solid acid catalyst. The preparation method of the polymeric solid acid catalyst is simple and is easy to operate, and the prepared polymeric solid acid catalyst is used for esterification reaction, has high catalytic activity and selectivity, can be easily filtered and recovered and can be used repeatedly for 6 times with the catalytic activity being not reduced significantly.

Description

technical field [0001] The invention relates to a preparation method of a novel solid acid for esterification reaction, which uses free radical polymerization to prepare POSS-SO 3 The invention discloses an H polymerization type solid acid catalyst, which belongs to the technical field of fine organic chemical industry. Background technique [0002] Carboxylate esters are an important class of fine chemicals, widely used in the fields of fragrances, cosmetics, surfactants and medicines. At present, the industrial production of various esters is mostly based on H 2 SO 4 , HF or H 3 PO 4 Such as inorganic liquid acid as catalyst, but this method has great disadvantages: not only the separation and reuse of the catalyst is very difficult, but also brings serious equipment corrosion and environmental pollution problems. Therefore, searching for new esterification catalysts that can replace liquid acids has become a hot spot in current research and development. [0003] Sol...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): B01J31/10C07C67/08C07C69/14C07C69/157C07C69/704C07C69/58C07C69/18
Inventor冷炎赵计伟蒋平平
OwnerJIANGNAN UNIV