Industrial preparation method of high-yield cinnamaldehyde

A cinnamaldehyde, high-yield technology, applied in the field of cinnamaldehyde preparation, can solve problems such as poor economic benefits, insufficient yield, equipment corrosion, etc., achieve the effects of reducing thermal damage, improving product yield and purity, and avoiding pollution

Inactive Publication Date: 2012-10-10
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

Because benzaldehyde is insoluble in water, this method belongs to two-phase reaction, and the yield is too low, the yield is less than 60%, and the economic benefit is poor
The process of synthesizing cinnamaldehyde by this method is simple, and the environmental pollution is relatively small, but the yield is too low, less than 50%, and under the condition of high temperature and high pressure, the organic chemical reaction in near-critical water will seriously corrode the equipment. At the same time, this method is adopted overinvestment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] First configure the aqueous solution: take 2.25kg of PEG-400 and add it to 1 ton of deionized water, stir evenly, and set aside.

[0030] A. Before feeding, nitrogen purging is used to remove the oxygen in the reaction vessel, and then 50kg of strong basic anion exchange resin and the prepared aqueous solution of PEG-400 are added through the feeding kettle. The strong basic anion exchange resin used is Nanjing D201 macroporous strongly basic styrene-based anion exchange resin produced by the resin factory, then add 450kg of benzaldehyde and stir for half an hour;

[0031] B. Control the temperature at 15-20°C, add dropwise 450kg of 30% mass percent acetaldehyde aqueous solution while stirring, and add dropwise for 1 hour. After the dropwise addition, control the temperature at 25°C, and react for 3.5 hours;

[0032] C. After the reaction is completed, the reaction liquid is washed with water, and then multi-stage static stratification is carried out: put the material i...

Embodiment 2

[0035] First prepare the aqueous solution: take 2 kg of PEG-400 and add it to 1 ton of deionized water, stir evenly, and set aside.

[0036] A. Before feeding, nitrogen purging is used to remove the oxygen in the reaction vessel, and then 50kg of strong basic anion exchange resin and the prepared PEG-400 aqueous solution are added through the feeding kettle. The strong basic anion exchange resin used is Rohm &Hass Co. (Rohm and Haas company) produces Amberjet 4400 OH, then add benzaldehyde 400kg, stir for half an hour;

[0037] B. Control the temperature at 15-20°C, add dropwise 400kg of acetaldehyde aqueous solution with a mass percentage of 40% while stirring, and add the time for 1.5 hours. After the dropwise addition, control the temperature at 28°C and react for 4 hours;

[0038] C. After the reaction is completed, the reaction liquid is washed with water, and then multi-stage static stratification is carried out: put the material into the static equipment and let it stan...

Embodiment 3

[0041] First configure the aqueous solution: take 2.3kg of PEG-400 and add it to 1 ton of deionized water, stir evenly, and set aside.

[0042] A. Before feeding, use nitrogen purge to remove the oxygen in the reaction vessel, and then add 50kg of strong basic anion exchange resin and the configured PEG-400 aqueous solution through the feeding kettle. The strong basic anion exchange resin used is Mitsubishi Diaion PA produced by Chemical Industries Co.Ltd. (Mitsubishi Chemical Corporation), then add 460kg of benzaldehyde and stir for half an hour;

[0043] B. Control the temperature at 15-20°C, add 250kg of acetaldehyde aqueous solution with a mass percentage of 50% dropwise while stirring, and add dropwise for 2 hours. After the dropwise addition, control the temperature at 30°C and react for 5 hours.

[0044] C. After the reaction is completed, the reaction liquid is washed with water, and then multi-stage static stratification is carried out: put the material into the stati...

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PUM

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Abstract

The invention provides an industrial preparation method of high-yield cinnamaldehyde. The method includes the following steps of: A, adding a solid catalyst and a water solution of polyethylene glycol 400 to a reaction vessel, then adding benzaldehyde; B, adding dropwisely 30 % to 50% by mass of an acetaldehyde water solution slowly with stirring, after the dropwisely adding, controlling the temperature from 25 DEG C to 30 DEG C for a reaction for 3 to 5 hours; C, performing washing after the completion of the reaction, and allowing the mixture to stand for delamination; and D, performing distillation after separating out an oil layer to obtain the cinnamaldehyde. The method in the invention is advantaged in operational simplicity, easiness in obtaining raw materials and in preparation of the catalyst, simple recovery, environmental friendliness, continuous operation, fast forward reaction speed compared with common processes, low probability of a side reaction, reduced unit energy consumption of a product as well as stable quality, high yield, and high purity of the produced cinnamaldehyde.

Description

technical field [0001] The invention relates to a preparation method of cinnamaldehyde, in particular to an industrial preparation method of high-yield cinnamaldehyde. Background technique [0002] Cinnamaldehyde, also known as phenylacrolein, is an oily substance with strong cinnamon aroma and pungent taste. It is a commonly used spice with functions of sterilization, insurance, deodorization and good fragrance retention. Therefore, cinnamaldehyde is widely used as a flavor enhancer for beverages and foods and as a spice for cosmetics, and it is also an important organic synthesis intermediate. Studies in recent years have proved that cinnamaldehyde also has the function of inhibiting the carcinogen Aspergillus flavus, which has attracted more attention. [0003] At present, cinnamaldehyde has the following several industrial preparation methods: [0004] 1. Under alkaline conditions, benzaldehyde and acetaldehyde undergo a condensation reaction, and the mixture is distil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/232C07C45/74
CPCY02P20/584
Inventor 叶思朱如慧杨洁韩洪杰徐海林
Owner 湖北远成赛创科技有限公司
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