Functionalized polyacid ionic liquid catalyst and preparation method as well as method for catalytically synthesizing isobornyl acetate by using functionalized polyacid ionic liquid catalyst

A technology of isobornyl acetate and ionic liquid, which is applied in the direction of physical/chemical process catalyst, organic compound/hydride/coordination complex catalyst, carboxylate preparation, etc., and can solve the problem of low yield of isobornyl acetate , low esterification reaction rate, poor thermal stability and other problems, to achieve the effect of simple synthesis method, good stability and mild reaction conditions

Active Publication Date: 2018-04-13
HENAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, the acidic cation exchange resin catalyst shows good catalytic activity and is a commercial solid acid catalyst with excellent performance, but it also has some defects, such as poor thermal stability, easy poisoning and deactivation, and mass transfer problems
[0003] In summary, there are still some difficulties and challenges in how to efficiently and selectively convert camphene and acetic acid into isobornyl acetate, such as low esterification reaction rate and low yield of isobornyl acetate.

Method used

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  • Functionalized polyacid ionic liquid catalyst and preparation method as well as method for catalytically synthesizing isobornyl acetate by using functionalized polyacid ionic liquid catalyst
  • Functionalized polyacid ionic liquid catalyst and preparation method as well as method for catalytically synthesizing isobornyl acetate by using functionalized polyacid ionic liquid catalyst

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Embodiment 1

[0031] A kind of preparation method of functionalized multi-acid ionic liquid catalyst, described method comprises the following steps:

[0032] (1) Take a certain amount of pentamethyldiethylenetriamine (0.2mol) and 1,4-butyl sultone (0.4mol) in a round bottom flask, slowly heat up to 60°C under stirring, and react quickly to obtain white solid. The obtained solid was washed three times with ethyl acetate and filtered, then vacuum-dried at 80° C. for 12 h, and the obtained white solid was an ylide.

[0033] (2) Take a certain amount of ylide (0.1 mol) and place it in a round bottom flask, and place it in a water bath at 80°C. Take 0.1mol of phosphotungstic acid (H 3 PW 12 o 40 ) was dissolved in distilled water and added dropwise to a round bottom flask, stirred and refluxed for 18h. After the reaction, the water was distilled off under reduced pressure to obtain a light yellow solid, which was washed three times with ether and toluene in sequence, and dried in vacuum at...

Embodiment 2

[0038] A method for synthesizing isobornyl acetate by functionalization multi-acid ionic liquid catalysis, comprises the following steps: in reactor, add acetic acid 18.02g (0.3mol) successively, camphene 13.62g (0.1mol) and embodiment [Bis-Bs-PMDETA](1 / 2Zn)HSiW prepared in 1 12 o 40 Catalyst 1.84g (accounting for 7wt% of raw material total mass), stirring and heating up to reaction temperature 60 ℃, constant temperature reaction 3h, the transformation rate of camphene is 92%, the selectivity of isobornyl acetate is 96%, and isoformyl acetate The yield of brain ester was 88%.

Embodiment 3

[0040] A method for synthesizing isobornyl acetate by functionalization multi-acid ionic liquid catalysis, comprises the following steps: in reactor, add acetic acid 6.01g (0.1mol) successively, camphene 27.25g (0.2mol) and embodiment [Bis-Bs-PMDETA](1 / 2Cu)PMo prepared in 1 12 o 40 Catalyst 0.98g (accounting for 5wt% of raw material gross mass), stirring and heating up to reaction temperature 100 ℃, constant temperature reaction 1h, the conversion rate of camphene is 44%, the selectivity of isobornyl acetate is 89%, and isoformyl acetate The yield of brain ester was 39%.

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Abstract

The invention discloses a functionalized polyacid ionic liquid catalyst and a preparation method as well as a method for catalytically synthesizing isobornyl acetate by using the functionalized polyacid ionic liquid catalyst. The method for catalytically synthesizing the isobornyl acetate comprises the following steps: taking camphene and acetic acid as raw materials, taking functionalized polyacid ionic liquid as a catalyst and carrying out esterification reaction to obtain the isobornyl acetate. According to the functionalized polyacid ionic liquid catalyst disclosed by the invention, the conversion rate of the camphene is as high as 92 percent, the selectivity of the isobornyl acetate is as high as 96 percent and the yield of the isobornyl acetate reaches 88 percent. The method disclosed by the invention has the advantages of high activity of the catalyst, good activity, mild reaction conditions, high yield of a product, easy separation of the catalyst and a product and the like.

Description

technical field [0001] The invention relates to a functionalized multi-acid ionic liquid catalyst, a preparation method and a method for using it to catalyze the synthesis of isobornyl acetate, and relates to the field of functionalized multi-acid ionic liquids, the field of catalyst synthesis and the catalysis of isobornyl acetate synthetic field. Background technique [0002] Isobornyl acetate is a colorless crystalline powder with the smell of rosin and camphor. It is an important chemical intermediate and is mainly used in the fields of synthesizing camphor, flavors and fragrances. Concentrated sulfuric acid is mainly used as a catalyst in the traditional production of isobornyl acetate in industry, but it is gradually eliminated due to problems such as environmental pollution, corrosion of equipment, and many side reactions. Many environmentally friendly acid catalysts have replaced concentrated sulfuric acid in the esterification process of isobornyl acetate synthesis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02C07C69/14C07C67/04
CPCB01J31/0279B01J2231/321C07C67/04C07C69/14Y02P20/584
Inventor 刘勇翟翠萍王建红刘威华乔聪震牛景杨
Owner HENAN UNIVERSITY
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