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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AI-Extracted Technical Summary

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

Result shows, use microporous hydrogen type molecular sieve or its modification microporous molecular sieve as catalyzer, catalyzed cinnamic acid and ethanol esterification reaction synthetic high value-added ethyl cinnamate at lower...

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.

Application Domain

Organic compound preparationCarboxylic acid esters preparation

Technology Topic

ChemistryEthyl ester +8

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Examples

Experimental program(4)
Effect test(1)

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 550 °C for 4 h in an air atmosphere to obtain β-10 % SO 3 , the (NH 4 ) 2 SO 4 Concentration is obtained by roasting at 550 ℃ for 4 h 3 The mass ratio to the bar-shaped β-type molecular sieve is 10.0%;

[0027] c. The reaction product obtained in step b is subjected to on-line analysis through 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 2.

[0028] Table 2

[0029]

[0030] Note *: (result after chromatographic normalization calculation); **: (result after chromatographic normalization calculation)

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)

PUM

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