Method for catalytically synthesizing ethyl cinnamate by using microporous molecular sieve

A technology of microporous molecular sieve and ethyl cinnamate, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid esters, etc., can solve the problems of non-renewable catalytic activity, expensive production cost of catalysts, difficult application, etc., to achieve Target product selectivity solution, target product selectivity is high, and the effect of reducing production cost

Pending Publication Date: 2021-09-17
LIAONING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

SO 4 2- /TiO 2 Solid superacid is an acid whose acid strength is stronger than 100% sulfuric acid, but it has the advantages of non-corrosive equipment, high reactivity, good selectivity, easy separation, etc., but the acid has small specific surface area, irregular pore structure and catalytic activity. Defects such as almost no regeneration make it difficult for the catalyst to be applied in industrial

Method used

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  • Method for catalytically synthesizing ethyl cinnamate by using microporous molecular sieve
  • Method for catalytically synthesizing ethyl cinnamate by using microporous molecular sieve
  • Method for catalytically synthesizing ethyl cinnamate by using microporous molecular sieve

Examples

Experimental program
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Example Embodiment

[0015] Example 1:

[0016] A. all add 1.0 g cinnamic acid and 10.0 g ethanol in three lining polytetrafluoroethylene reactors, obtain cinnamic acid ethanol solution;

[0017] b. Add 0.5 g H-ZSM-5 molecular sieve, 0.5 g H-Y molecular sieve and 0.5 g H-β molecular sieve to the ethanol solution of cinnamic acid, respectively, at 150 ℃, 160 ℃, 170 ℃, 180 ℃, 190 ℃ Reaction 8h under the reaction temperature;

[0018] c. The reaction product obtained in step b is subjected to on-line analysis by a chromatograph after vacuum distillation, and is determined to be ethyl cinnamate, and the conversion rate and selectivity of ethyl cinnamate are shown in Table 1.

[0019] Table 1

[0020]

[0021] Note *: (result after chromatographic normalization calculation); **: (result after chromatographic normalization calculation)

Example Embodiment

[0022] Example 2:

[0023] A. all add 1.0 g cinnamic acid and 10.0 g ethanol in three lining polytetrafluoroethylene reactors, obtain cinnamic acid ethanol solution;

[0024] b. Add 0.5 g of cinnamic acid ethanol solution and name it β-5% P 2 o 5 , β-10% P 2 o 5 or β-10 % SO 3 The modified microporous molecular sieve was reacted at 180 ℃ for 8 h;

[0025] The β-5 % P 2 o 5 , β-10% P 2 o 5 The preparation method is: impregnating strip-shaped H-β molecular sieves in NH 4 h 2 PO 4 solution for 12 h, the solid was dried at 100 °C, and then calcined at 550 °C for 4 h in an air atmosphere to obtain β-5 % P 2 o 5 , β-10% P 2 o 5 , the NH 4 h 2 PO 4 2H 2 The concentration of O is represented by P 2 o 5 The mass ratio to strip β-type molecular sieve is 5.0%, 10.0% shall prevail;

[0026] β-10% SO 3 The preparation method is: impregnating strip-shaped H-β molecular sieves in (NH 4 ) 2 SO 4 solution for 12 h, the solid was dried at 100 °C, and then calcined at 5...

Example Embodiment

[0031] Example 3:

[0032] A. all add 1.0 g cinnamic acid and 10.0 g ethanol in six lining polytetrafluoroethylene reactors, obtain cinnamic acid ethanol solution;

[0033] b. Add 0.025 g, 0.065 g, 0.125 g, 0.250 g, 0.750 g and 1.000 g of H-β molecular sieve to the ethanol solution of cinnamic acid, and react at a temperature of 180 °C for 8 h;

[0034] c. The reaction product obtained in step b is subjected to on-line analysis by a chromatograph after vacuum distillation, and is determined to be ethyl cinnamate, and the conversion rate and selectivity of ethyl cinnamate are shown in Table 3.

[0035] table 3

[0036]

[0037] Note *: (result after chromatographic normalization calculation); **: (result after chromatographic normalization calculation)

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Abstract

The invention discloses a method for catalytically synthesizing ethyl cinnamate by using a microporous molecular sieve. The method comprises the following steps: dissolving cinnamic acid in ethanol to obtain a cinnamic acid ethanol solution, wherein the mass ratio of cinnamic acid to ethanol being 1: (1.5-50); adding a catalyst into the cinnamic acid ethanol solution, and carrying out a reaction for 2-72 h at a temperature of 150-300 DEG C, wherein the catalyst is a microporous hydrogen type molecular sieve or a modified microporous molecular sieve, and the mass ratio of the catalyst to cinnamic acid is (0.025-1.5): 1; and carrying out reduced pressure distillation on the reaction product obtained in the step b to obtain ethyl cinnamate. The method has the advantages of high target product selectivity, high activity of the microporous hydrogen molecular sieve or modified microporous molecular sieve, reusability and activity regeneration, effective reduction of the preparation cost of ethyl cinnamate, and suitableness for industrial production.

Description

technical field [0001] The invention relates to a method for preparing ethyl cinnamate, in particular to a method for catalytically synthesizing ethyl cinnamate by using microporous molecular sieves. Background technique [0002] Ethyl cinnamate is also known as β-phenyl acrylate ethyl, 3-phenylpropionate ethyl, the molecular formula is PhCH=CHCOOEt, exists in natural plants such as the volatile oil of Eleuthero jujube, and has fruit (sweet orange and grape, etc.) aroma It is mainly used in cigarette flavoring agent and preparation of essence, etc. [0003] In the past, ethyl cinnamate was synthesized industrially by Claisen condensation of ethyl acetate and benzaldehyde under the action of sodium metal or by esterification of cinnamic acid and ethanol under the catalysis of sulfuric acid. question. The former is dangerous to operate due to the instability of metallic sodium; the latter is highly corrosive due to the strong corrosiveness of concentrated sulfuric acid, whic...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/618
CPCC07C67/08C07C69/618
Inventor 陈立东赵柳宋胜杰李昊楠毕明莉王思越郭颖
Owner LIAONING NORMAL UNIVERSITY
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