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Application and method of a kind of immobilized ionic liquid in catalytic synthesis of n-butyl carboxylate

An ionic liquid, a technology for synthesizing carboxylic acid, applied in chemical instruments and methods, preparation of carboxylic acid esters, preparation of organic compounds, etc. simple effect

Active Publication Date: 2022-02-11
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, most ionic liquids have high selectivity for catalyzed esterification reactions, and there is no clear guideline for how to choose ionic liquids for specific esterification reactions.

Method used

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  • Application and method of a kind of immobilized ionic liquid in catalytic synthesis of n-butyl carboxylate
  • Application and method of a kind of immobilized ionic liquid in catalytic synthesis of n-butyl carboxylate
  • Application and method of a kind of immobilized ionic liquid in catalytic synthesis of n-butyl carboxylate

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Experimental program
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Effect test

Embodiment 1～12

[0019]

[0020] The concrete experimental process of embodiment 1-12 is:

[0021] Respectively weigh carboxylic acid, n-butanol, immobilized ionic liquid and water-carrying agent cyclohexane into a three-necked flask equipped with a reflux condenser, a water separator, and a magnetic stirrer, and heat to reflux for reaction. After the reaction, Cyclohexane was removed by rotary evaporation, the remaining reactants were removed by washing with saturated sodium chloride solution and saturated sodium carbonate solution, and the product n-butyl formate was obtained after drying over anhydrous magnesium sulfate, and the immobilized ionic liquid could be reused after recovery and drying.

Embodiment 13

[0023] The immobilized 1-methyl-3-ethylimidazolium bisulfate ionic liquid that embodiment 1 reclaims, the immobilized 1-methyl-3-butylimidazolium bisulfate ionic liquid that embodiment 5 reclaims and implement The immobilized 1-methyl-3-octylimidazolium bisulfate ionic liquid recovered in Example 9 was washed and dried at 80°C for recycling. In other experimental conditions, it was the same as in Example 1, Example 5 and Example 9. Under the same premise, the effect of catalytic esterification reaction is shown in Table 1.

[0024] Table 1 Experiments on the cyclic use of immobilized ionic liquids

[0025]

[0026] It can be seen from the results in Table 1 that the selected immobilized ionic liquid in the present invention can be used more than 5 times without regeneration in catalyzing the esterification reaction.

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Abstract

The invention relates to the technical field of organic synthesis, and specifically discloses the application and method of a solid-supported ionic liquid in catalytically synthesizing n-butyl carboxylate. The carrier in the solid-supported ionic liquid is silica gel, and the ionic liquid is wherein base, butyl or octyl, the carboxylic acid used for the n-butyl carboxylic acid is a C1-C4 carboxylic acid, and its synthesis method is to add the immobilized ionic liquid, water-carrying agent, carboxylic acid and n-butanol In the reactor, reflux for 0.5 to 6 hours. The selected immobilized ionic liquid in the present invention is cheap, simple to prepare, and environmentally friendly, and has high selectivity to the esterification reaction of C1-C4 carboxylic acid and n-butanol, and the amount of ionic liquid is small, and the catalytic efficient.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to the application and method of a solid-supported ionic liquid in catalytically synthesizing n-butyl carboxylate. Background technique [0002] Esterification is one of the important reactions in organic synthesis, and it is widely used in chemical products such as spices, plasticizers, and solvents. With the development of the economy, higher requirements are put forward for the industrial production of ester products. In the traditional esterification reaction using concentrated sulfuric acid as a strong acid catalyst, there are problems such as strong corrosion, difficult disposal of waste liquid, and many side reactions. Afterwards, various heteropolyacids studied as catalysts have problems such as low catalytic efficiency, easy volatilization, and difficulty in recycling. However, traditional solid-supported acid catalysts also have problems such as low selectivity...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C69/003
Inventor 刘冉张珂刘晨张娟赵地顺
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY