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Synthesis method of natural anisaldehyde

A technology of natural anethole and synthesis method, which is applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve the problems of high investment cost, limited promotion, etc., and achieves reduction of solid waste, cost reduction, less corrosive effect

Active Publication Date: 2020-03-17
ANHUI SHENGNUOBEI CHEM TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method has good selectivity, few by-products, high anisaldehyde yield, good quality, and easy control of reaction conditions, but the investment cost is relatively large, which limits the promotion of the method

Method used

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  • Synthesis method of natural anisaldehyde
  • Synthesis method of natural anisaldehyde
  • Synthesis method of natural anisaldehyde

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preparation example Construction

[0022] According to the present invention object is to provide a kind of synthetic method of anisaldehyde, this method comprises the following steps:

[0023] Step 1. Add natural anethole, catalyst and solvent into the reaction vessel, mix and heat up.

[0024] In step 1, the anethole and the solvent are firstly added into the reaction vessel, stirred and mixed evenly, and then the catalyst is added, and evenly dispersed in the reaction solution under the stirring condition.

[0025] In a preferred mode of the present invention, the reaction vessel is connected to a reflux device for cooling and refluxing the volatilized solvent during the heating reaction.

[0026] The purity of the natural anethole should not be lower than 90%. If the content of the raw material anethole is too low, impurities will be introduced from the source, which will make it more difficult to store the product anisaldehyde, so that the purity of the product cannot meet the requirements for use.

[002...

Embodiment Embodiment 1

[0061] Put 148g of natural anethole (the purity of anethole is 90%) into the reaction vessel, then add 200g of methanol and mix well, then add 1.5g of cobalt acetate, 0.5g of copper acetate and 2.0g of disodium hydrogen phosphate The mixture was stirred and dispersed, and the reaction system was heated to 50°C. Then, after the oxygen was treated by the micro-nano bubble generator, it was passed into the flask by the gas distributor to carry out the oxidation reaction. The oxygen flow rate was controlled at 200mL / min, and the reflux reaction was started. . Until the mass fraction of anethole is less than 1%, the heating is stopped, and the reaction is terminated, and the reaction time is 6 hours. The conversion rate of anethole was sampled and tested to be 99%, and the selectivity of anisaldehyde was 90.8%.

[0062] Cobalt acetate, copper acetate and disodium hydrogen phosphate are washed out with water, and the recovered catalyst is applied to the next batch of reactions. Th...

Embodiment 2

[0067] Carry out experiment by embodiment 1, difference is only: catalyst is 1.5g cobalt acetate, 0.5g copper acetate and 2.0g dipotassium hydrogen phosphate. The reaction time was 6 hours, and the product was distilled under reduced pressure to obtain 118.2 g (purity: 95.3%). The conversion rate and selectivity of anisehole were 99.5% and 92.4%, respectively, and the yield of anisaldehyde was 92%.

[0068] Qualitative and quantitative analysis was performed on the components of the distillate after solvent separation by chromatography-mass spectrometry.

[0069] The test results are shown in the table below:

[0070] Product composition and content in the embodiment 2 of table 2

[0071]

[0072] As can be seen from the experimental results in Example 1 and Example 2, when disodium hydrogen phosphate and dipotassium hydrogen phosphate were co-catalysts, the conversion rate and selectivity of the reaction system did not change much, indicating that the main role played in...

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Abstract

The invention provides a synthesis method of natural anisaldehyde. In the method, natural anethole is adopted as a raw material, oxygen or air is adopted as an oxidant, and the anisaldehyde is prepared under the action of a catalyst. The product obtained by this method has a pure aroma and excellent quality, which are obviously better than these of anisaldehyde obtained by pure chemical synthesismethods. The catalyst and solvent used in the method can be recycled and reused, thus reducing the cost and reducing generation of three wastes. The clean oxygen or air is adopted as the oxidant, thesource is wide, the reaction condition is mild, and corrosion is low, thus facilitating industrial production of the anisaldehyde.

Description

technical field [0001] The invention belongs to the technical field of spices and fine chemicals, and in particular relates to a method for synthesizing anisaldehyde. Background technique [0002] Anisaldehyde was first produced by Cahours in the 18th century when anise oil was treated with dilute nitric acid, and gradually attracted people's attention due to its unique aroma. There are many ways to synthesize anisaldehyde. It can be obtained by organic synthesis of many petrochemical raw materials, and it can also be obtained by oxidation of natural product star anise essential oil-anethole, and anisaldehyde obtained by oxidation of anethole has the best aroma. [0003] With the increasing shortage of petrochemical raw material resources and rising prices, and our country is rich in natural anethole, the production of anisaldehyde by oxidation of natural anethole can make good use of natural resources, which has gradually attracted people's attention. People use manganese ...

Claims

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Application Information

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IPC IPC(8): C07C45/36C07C47/575
CPCC07C45/36C07C47/575Y02P20/584
Inventor 陈和平保志学
Owner ANHUI SHENGNUOBEI CHEM TECH
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