Method for preparing anisaldehyde

An anisaldehyde and ozonation technology, applied in the direction of ozonolysis preparation, organic chemistry, etc., to achieve the effects of facilitating industrial production, solving equipment corrosion, and long half-life

Inactive Publication Date: 2010-08-04
GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Due to the limitation of resources, foreign studies on ozonation mainly focus on chain unsat

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Mix anethole, acetone and water with a mass ratio of 20:20:1 to obtain reaction raw materials; 3 h -1 The flow rate of every kilogram of reaction raw materials is fed into ozone and oxygen mixed gas to carry out ozonation reaction; after the ozonation reaction is completed, continue to pass oxygen gas for 15 minutes to drive out excess ozone to obtain an ozonated reaction liquid; in the ozone and oxygen mixed gas, ozone The mass percentage content is 5%;

[0027] The height-to-diameter ratio of the bubbling reaction tower (made of glass) is 10:1, and a condensation jacket is added outside the bubbling reaction tower, and the condensation area is 0.32m 2 For each kilogram of reaction raw material, a gas distributor is installed at the bottom of the bubbling reaction tower, the aperture of the gas distributor is 50 μm, and the bubbling area of ​​the gas distributor is 0.008m 2 For every kilogram of reaction raw material, a low-temperature reflux condensing device is...

Embodiment 2

[0030] (1) Mix anethole, acetone and water with a mass ratio of 20:88:12 to obtain the reaction materials; 3 h -1 The flow rate of every kilogram of reaction raw materials is fed into ozone and oxygen mixed gas, and the ozonation reaction is carried out for 1.0h; After the ozonation reaction is completed, continue to pass oxygen for 15min to drive out excess ozone to obtain an ozonated reaction liquid; the ozone and oxygen mixed gas The mass percent composition of ozone in the medium is 5%;

[0031] The height-to-diameter ratio of the bubbling reaction tower is 20:1, and a condensation jacket is added outside the bubbling reaction tower, and the condensation area is 0.50m 2 / kg reaction raw materials, the bottom of the bubbling reaction tower is equipped with a gas distributor, the aperture of the gas distributor is 5μm, and the bubbling area of ​​the gas distributor is 0.01m 2 / kg of reaction raw materials, the top of the bubbling reaction tower is equipped with a low-tempe...

Embodiment 3

[0034] (1) Mix anethole, methyl ethyl ketone and water with a mass ratio of 20:51:9 to obtain the reaction raw materials; add the reaction raw materials into the bubbling reaction tower, control the reaction temperature at 25°C, and use 0.24m 3 h -1 The flow rate of every kilogram of reaction raw materials is passed into ozone and oxygen mixed gas, and carries out ozonation reaction 1.2h; After ozonation reaction finishes, continue to pass oxygen 25min to drive out excess ozone, obtain ozonated reaction liquid; Described ozone and oxygen mixed gas The mass percent composition of ozone in the medium is 2%;

[0035] The height-to-diameter ratio of the bubbling reaction tower is 20:1, and a condensation jacket is added outside the bubbling reaction tower, and the condensation area is 0.50m 2 / kg reaction raw materials, the bottom of the bubbling reaction tower is equipped with a gas distributor, the aperture of the gas distributor is 5μm, and the bubbling area of ​​the gas distr...

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PUM

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Abstract

The invention discloses a method for preparing anisaldehyde. The method comprises the following steps: (1) mixing anethole, organic solvents and water to obtain reaction materials; adding the reaction materials into a bubble reaction tower and introducing mixed gas of ozone and oxygen to carry out ozonization reaction; continuing introducing oxygen to expel redundant ozone after the ozonization reaction is over to obtain ozonization reaction liquid; and (2) heating anhydrous sodium sulfite solution to 60-80 DEG C and dropwise adding the ozonization reaction liquid to carry out reduction reaction; continuing reacting for 30-60min after dropwise adding the ozonization reaction liquid, cooling and standing the reactant and dividing the liquid to obtain the coarse anisaldehyde; and removing the organic solvents by distillation to obtain the anisaldehyde product. The method avoids a little side reaction in the process of ozonization, lowers the equipment and production cost, solves the keyproblems confronted by industrialized production, such as equipment corrosion due to presence of acetic acid, heavy environmental pollution and the like, and opens up a way for large-scale industrialized production.

Description

technical field [0001] The invention belongs to the field of perfume preparation, in particular to a method for preparing anisaldehyde by ozonation reaction of anethole using an organic solvent and water as a composite solvent. Background technique [0002] Anisaldehyde (anisaldehyde, anisic aldehyde, p-methoxybenzaldehyde) is also known as Oshirahama, and its chemical name is p-methoxybenzaldehyde. The pure product is a colorless or light yellow liquid with a strong hawthorn flower aroma, long-lasting aroma and strong antioxidant properties. Density is 1.123g / ml (20°C), melting point is 2.5°C, boiling point is 249.5°C, 144~200°C (28kPa), 134~135°C (1.6kPa), 83°C (0.267kPa), relative density is 1.1191(15 / 4 °C), the refractive index is 1.5720 (20 °C), and the flash point is 117.8 °C. Slightly soluble in water, easily soluble in ethanol and ether. Molecular formula is C 8 h 8 o 2 , the molecular weight is 136.15. [0003] Because anisaldehyde has a long-lasting hawthorn...

Claims

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Application Information

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IPC IPC(8): C07C47/575C07C45/40
Inventor 哈成勇于静沈敏敏甘露邓莲丽
Owner GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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