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Method using catalysis transesterification to prepare n-butyl acetate cinnamate

A technology of n-butyl cinnamate and exchange reaction is applied in the field of chemical industry to achieve the effects of improving microwave absorption efficiency, simple process and good stability

Inactive Publication Date: 2015-03-11
广州善合化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no systematic research on the use of microwave control and ionic liquid catalysts in the transesterification reaction process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 1.6219g (0.01mol) methyl cinnamate and 0.2595g 1-butyl-3-methylimidazolium bisulfate into the microwave reaction tank of the WF-4000 atmospheric pressure microwave rapid reaction system (the same below), and then add 0.06 mol of n-butanol, fully mixed to obtain the reaction raw material; the reaction raw material was subjected to microwave irradiation for 30 minutes, the microwave power was set to 200W, and the microwave irradiation temperature was set to 117°C, and a light yellow product was obtained after microwave irradiation. Qualitative and quantitative analysis was carried out on the obtained product by gas-mass spectrometry, and the conversion rate of methyl cinnamate was calculated to be 31.75%.

[0033] The resulting product was assayed as follows:

[0034] 1. Determination of physical constants: The product was purified and then measured for its refractive index. The refractive index was 1.5400 (35°C), which was consistent with the measured value of the st...

Embodiment 2

[0038]Add 1.6219g (0.01mol) methyl cinnamate and 0.2595g 1-butyl-3-methylimidazolium bisulfate in microwave reaction tank, then add 0.1mol n-butanol, fully mix, obtain reaction raw material; The reaction raw materials were subjected to microwave irradiation for 30 minutes, the microwave power was set at 300 W, and the microwave irradiation temperature was set at 117° C., and a pale yellow product was obtained after microwave irradiation. Qualitative and quantitative analysis was carried out on the obtained product by gas-mass spectrometry, and the conversion rate of methyl cinnamate was calculated to be 27.55%.

[0039] The resulting product was assayed as follows:

[0040] 1. Determination of physical constants: The product was purified and measured for its refractive index. The refractive index was 1.5400 (35°C), which was consistent with the measured value of the standard product; the boiling point was 164-167°C (1333Pa), which was consistent with the literature value.

[...

Embodiment 3

[0044] Add 1.6219g (i.e. 0.01mol) methyl cinnamate and 0.1946g 1-butyl-3-methylimidazolium bisulfate into a microwave reaction tank, then add 0.08mol n-butanol, and mix well to obtain the reaction raw materials; Microwave irradiation was carried out on the reaction raw materials for 45 minutes, the microwave power was set to 300 W, and the microwave irradiation temperature was set to 80° C., and a light yellow product was obtained after microwave irradiation. Qualitative and quantitative analysis was carried out on the obtained product by gas-mass spectrometry, and the conversion rate of methyl cinnamate was calculated to be 14.11%.

[0045] The resulting product was assayed as follows:

[0046] 1. Determination of physical constants: The product was purified and measured for its refractive index. The refractive index was 1.5400 (35°C), which was consistent with the measured value of the standard product; the boiling point was 164-167°C (1333Pa), which was consistent with the ...

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Abstract

The invention belongs to the technical field of chemical industry and discloses a method using catalysis transesterification to prepare n-butyl acetate cinnamate. The method comprises evenly mixing methyl cinnamate, 1-butyl-3-methylimidazole hydrosulphate and n-butyl alcohol, using microwave with the microwave power of 100-500W to irradiate for 5-60min at the temperature of 70 DEG C to 117 DEG C, and separating to obtain the n-butyl acetate cinnamate after microwave irradiation. The conversion rate of the methyl cinnamate reaches to 36.07%. The preparation method is a novel process using microwave synergy ionic liquid catalysis transesterification to synthesize the n-butyl acetate cinnamate, has the advantages of being high in heating efficiency, short in reaction time, low in energy consumption, simple in process, easy in aftertreatment, recycling in catalysts, environmentally-friendly and the like, meets sustainable development, can save energy, is a green chemical novel method and has good industrialization prospects.

Description

technical field [0001] The invention belongs to the technical field of chemistry and chemical engineering, and relates to a method for preparing n-butyl cinnamate by catalyzing a transesterification reaction, in particular to a method for catalyzing methyl cinnamate with microwave synergistic 1-butyl-3-methylimidazolium bisulfate ionic liquid A method for preparing n-butyl cinnamate through transesterification with n-butanol. Background technique [0002] Cinnamate is an important class of synthetic fragrances, which are widely used in ingredients of food flavors and daily chemical flavors because of their special fruity or floral fragrance, and are also important raw materials for organic synthesis. N-butyl cinnamate is a balsamic ester with cocoa aroma, which is widely used in the preparation of edible and daily chemical flavors in industry. [0003] At present, the synthesis method of cinnamate is mainly the traditional strong acid catalyzed conventional heating esterifi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/618C07C67/03
CPCY02P20/584
Inventor 黎彧高虹
Owner 广州善合化工有限公司
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