Novel industrialized synthesis technique for preparing cinnamic acid from cinnamic aldehyde by catalytic oxidation

A technology of catalytic oxidation and cinnamaldehyde, which is applied in the preparation of organic compounds, carboxylate preparation, physical/chemical process catalysts, etc., can solve the problems of inability to realize the industrial production of cinnamic acid, silver catalyst poisoning, and easy mass adsorption, etc., to achieve Achieve industrialized mass production, short reaction time, and reduce production costs

Inactive Publication Date: 2012-12-19
湖北远成赛创科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is prone to catalyst falling off, and the loss of silver is relatively large. The catalyst needs to be filtered and recovered, and the process is relatively cumbersome.
Moreover, since the carrier carbon in the Ag / C catalyst is a non-polar adsorbent, it is easy to adsorb a large amount of cinnamaldehyde, causing silver to be completely wrapped by cinnamaldehyde and causing catalyst poisoning.
Therefore, in process control, the rate of addition of cinnamaldehyde must be below 2ml / min, which makes this method impossible to realize the industrialized production of cinnamic acid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (A) Add sodium hydroxide, purified water, and catalyst into the reaction kettle and stir to mix. The mass ratio of sodium hydroxide, purified water, and catalyst is 8:180:2.2. After feeding pure oxygen for 5 minutes, add dropwise Cinnamaldehyde, the dropping speed of cinnamaldehyde is controlled at 30mL / min, the dropping time is 80min, and the oxygen flow is continued to stir for 30min during the dropping process, the stirring speed is 200r / min, and the oxygen flow rate is 5m 3 / h, the temperature is 40°C, the pressure in the reaction kettle is 3.5atm, after the reaction is completed, let it stand for 25min to make the catalyst settle, and realize the separation of the sodium cinnamate solution and the catalyst generated by the reaction in the reaction kettle;

[0021] The catalyst is nano-silver particles, and its preparation steps are: first mix and dissolve silver nitrate and pure water according to the mass ratio = 17:36, then add sodium hydroxide solution to adjust ...

Embodiment 2

[0024] (A) Add sodium hydroxide, purified water, and catalyst into the reactor and stir to mix. The mass ratio of sodium hydroxide, purified water, and catalyst is 40:180:1.1. After feeding pure oxygen for 10 minutes, add dropwise Cinnamaldehyde, the dropping speed of cinnamaldehyde is controlled at 40mL / min, the dropping time is 60min, and the oxygen flow is continued to stir for 40min during the dropping process, the stirring speed is 500r / min, and the oxygen flow rate is 10m 3 / h, the temperature is 50°C, the pressure in the reaction kettle is 3.0atm, after the reaction is completed, let it stand for 40min to make the catalyst settle, and realize the separation of the sodium cinnamate solution and the catalyst generated by the reaction in the reaction kettle;

[0025] The catalyst is nano-silver particles, and its preparation steps are: first mix and dissolve silver nitrate and pure water according to the mass ratio = 17:40, then add sodium hydroxide solution to adjust the p...

Embodiment 3

[0028] (A) Add sodium hydroxide, purified water, and catalyst into the reaction kettle and stir and mix. The mass ratio of sodium hydroxide, purified water, and catalyst is 25:180:1.5. After feeding pure oxygen for 8 minutes, add dropwise Cinnamaldehyde, the dropping speed of cinnamaldehyde is controlled at 60mL / min, the dropping time is 40min, and the oxygen flow is continued to stir for 60min during the dropping process, the stirring speed is 800r / min, and the oxygen flow rate is 15m 3 / h, the temperature is 60°C, the pressure in the reaction kettle is 4.0atm, after the reaction is completed, let it stand for 30min to make the catalyst settle, and realize the separation of the sodium cinnamate solution and the catalyst generated by the reaction in the reaction kettle;

[0029] The catalyst is nano-silver particles, and the preparation steps are as follows: first mix and dissolve silver nitrate and pure water at a mass ratio of 17:40, then add sodium hydroxide solution to adju...

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Abstract

The invention belongs to the technical field of intermediate synthesis in fine chemical engineering, and particularly relates to a novel industrialized synthesis technique for preparing cinnamic acid from cinnamic aldehyde by catalytic oxidation. The technique comprises the following steps: (A) adding sodium hydroxide, pure water and catalyst mixed solution in a mass ratio of (8-40):180:(1.1-2.2) into a reaction kettle, stirring, introducing pure oxygen, dropwisely adding cinnamic aldehyde into the mixed solution at proper rate to generate sodium cinnamate, and standing for 10-40 minutes to deposit the catalyst; and (B) leading out the sodium cinnamate solution obtained in the step (A), carrying out acid precipitation at 70-80 DEG C, keeping the reaction for 15-40 minutes, and naturally cooling to room temperature, thereby obtaining the cinnamic acid. The catalyst is nano silver particles. By adopting the supporter-free nano silver particles as the catalyst for the first time, the invention solves the problems of catalyst poisoning, high shedding tendency, high loss and the like, simplifies the production technique, greatly lowers the production cost, has the advantage of high yield, and implements industrialized mass production.

Description

technical field [0001] The invention belongs to the technical field of synthesis of fine chemical intermediates, and specifically refers to a new industrial synthesis process for preparing cinnamic acid by catalytic oxidation of cinnamaldehyde. Background technique [0002] Cinnamic acid is a very important chemical raw material, which is widely used in the fields of medicine, spices, food additives, plastics and photosensitive materials, and is in short supply in China. At present, the synthesis methods of cinnamic acid include Perkin method, styrene-carbon tetrachloride method, 1,3,3,3-tetrachlorophenylpropane hydrolysis method and cinnamaldehyde catalytic oxidation method. [0003] The Perkin method is the preparation of cinnamic acid from benzaldehyde and acetic anhydride under the catalysis of anhydrous sodium (potassium) acetate. Due to the many side reactions, low yield and serious pollution of this process, this method has been eliminated. [0004] The styrene-carb...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C57/44C07C51/235B01J23/50
Inventor 叶思叶传发朱如慧
Owner 湖北远成赛创科技有限公司
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