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Method for preparing benzaldehyde by taking hydroxypropyl-beta-cyclodextrin as accelerating agent

A technology of cyclodextrin and hydroxypropyl, which is applied in the field of benzaldehyde production, can solve problems such as limited application, limited solubility, and unsatisfactory yield of benzaldehyde, so as to improve solubility, increase reaction rate, and avoid product polymerization and disproportionation Effect

Active Publication Date: 2010-02-17
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the limited solubility of β-cyclodextrin in water (1.85g / 100mL, 25°C), its application is greatly limited, and the yield of benzaldehyde is not ideal

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 25mL 2% NaOH aqueous solution (mass percentage) and 1mmol 2-hydroxypropyl-β-cyclodextrin mixture (substitution degree 3.9) into a 100mL flask respectively, and stir at 0°C until hydroxypropyl-β-cyclodextrin Dissolve, then add 1mmol cinnamaldehyde, react for 7h and extract with 50mL ethyl acetate, the obtained ethyl acetate phase is concentrated under reduced pressure to remove ethyl acetate to obtain benzaldehyde with a yield of 23%.

Embodiment 2

[0024] Add 25mL 2% NaOH aqueous solution (mass percentage) and 1mmol 2-hydroxypropyl-β-cyclodextrin (substitution degree 3.9) to a 100mL three-necked flask respectively, and stir at 50°C until 2-hydroxypropyl-β-cyclodextrin Dextrin was dissolved, then 1 mmol cinnamaldehyde was added, and after reacting for 5 h, it was extracted with 50 mL ethyl acetate, and the obtained ethyl acetate phase was concentrated under reduced pressure to remove ethyl acetate to obtain benzaldehyde with a yield of 70%.

Embodiment 3

[0026] Add 25mL 2% NaOH aqueous solution (mass percentage) and 1mmol 2-hydroxypropyl-β-cyclodextrin (substitution degree 3.9) to a 100mL three-necked flask respectively, and stir at 100°C until 2-hydroxypropyl-β-cyclodextrin Dextrin was dissolved, then 1 mmol cinnamaldehyde was added, and after reacting for 1 h, it was extracted with 50 mL butyl acetate, and the obtained butyl acetate phase was concentrated under reduced pressure to remove butyl acetate to obtain benzaldehyde with a yield of 35%.

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Abstract

The invention discloses a method for preparing benzaldehyde by taking hydroxypropyl-beta-cyclodextrin as an accelerating agent. The method comprises the following steps: taking cinnamon oil or cinnamaldehyde as raw material, hydroxypropyl-beta-cyclodextrin as an accelerating agent and alkaline water which formed by one or more mixtures of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, ethanolamine, diethanol amine, triethanolamine and triethylamine and is used as a solvent react; after reaction, carrying out extraction concentration by using ester solvent, methanol, acetone or acetonitrile as an organic solvent to obtain the benzaldehyde. The method has the advantages of simple process, low energy consumption, low / no pollution, environmental protection, highbenzaldehyde yield and natural degree, and the like.

Description

technical field [0001] The invention relates to a production technology of benzaldehyde. Background technique [0002] Benzaldehyde is the second most used spice in the world. It has been widely used in food, health care products, cosmetics and other industries. It is also an important pharmaceutical intermediate. The natural benzaldehyde used in the food industry in the world has reached 3000 tons every year, and its annual demand is still increasing. The traditional production method of natural benzaldehyde is to use the bitter almonds containing amygdalin as raw material, through enzymatic hydrolysis, alkali washing and other processes; Removal of benzaldehyde is a qualified product, resulting in complicated production process and high cost of benzaldehyde. [0003] Another source of synthesizing natural benzaldehyde is cinnamon oil. my country has rich cinnamon oil resources. The use of cinnamon oil or its rich cinnamaldehyde to produce natural benzaldehyde has attract...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/54C07C45/67B01J31/06
Inventor 纪红兵陈鸿雁周贤太
Owner SUN YAT SEN UNIV
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