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Method for converting safrole into iso-safrole

A technology of isosafrole and safrole, which is applied in the field of natural flavor and fragrance processing, can solve the problems of resource waste, air organic matter pollution, etc., and achieve the effects of reducing oxidation polymerization, increasing yield, and avoiding high temperature contact

Inactive Publication Date: 2015-01-07
GUANGXI FORESTRY RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problem existing in the prior art is that a large amount of alkaline waste liquid is discharged during production, which is heated and refluxed under normal pressure, which easily produces side reactions such as oxidation polymerization, and the volatilization of raw materials and products causes waste of resources and organic pollution of the air

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] An example of the method that safrole of the present invention is converted into isosafrole, comprises the steps:

[0024] Take 1t of sassafras oil, properties: light yellow or yellowish brown liquid; it has a clove-like aroma, relative density is 1.030-1.050, and refractive index is 1.530-1.540. Main ingredients: 77.8% safrole, 1.5% α-terpineol, 1.6% linalool, 5.3% pinene, 2.3% camphor.

[0025] Add the safrole raw material to the reactor, stir and add 10kg NaOH / γ-Al 2 o 3 Composition catalyst, the composition catalyst by weight ratio is NaOH:γ-Al 2 o 3 =1:3~5, control the reaction temperature at 110-125°C, keep the pressure at 0.08-0.1MPa, and react for 1-2h to obtain crude isosafrole. Cool down, and when the temperature in the reactor drops to 50-60°C, discharge the crude isosafrole into the pickling tank. Adding hydrochloric acid with a concentration of 10% under stirring, adjusting the pH to 7-8, standing for stratification, the upper layer is crude isosafrole...

Embodiment 2

[0027] Another example of the method that safrole of the present invention is converted into isosafrole may further comprise the steps:

[0028] Take 1t of cinnamon oil, properties: light yellow to yellowish brown liquid; with clove-like aroma, relative density 1.030-1.050, refractive index 1.530-1.540. Main ingredients: 90.5% safrole, 1.5% α-terpineol, 0.6% linalool, 3.1% pinene, 2.3% camphor.

[0029] Put the safrole raw material into the reactor, stir and add 10kg of NaOH / CaO composition catalyst, the composition catalyst is NaOH:CaO=1:3-5 by weight. Control the reaction temperature at 110-125° C., keep the pressure at 0.08-0.1 MPa, and react for 1-2 hours to obtain crude isosafrole. Cool down, and when the temperature in the reactor drops to 50-60°C, discharge the crude isosafrole into the pickling tank. Adding hydrochloric acid with a concentration of 15% under stirring, adjusting the pH to 7-8, standing for stratification, the upper layer is crude isosafrole, and the l...

Embodiment 3

[0031] Another example of the method that safrole of the present invention is converted into isosafrole may further comprise the steps:

[0032] Take 1t of sassafras oil, properties: light yellow to yellowish brown liquid; it has a clove-like aroma, relative density is 1.030-1.050, and refractive index is 1.530-1.540. Main ingredients: 84.5% safrole, 3.5% α-terpineol, 1.6% linalool, 4.3% pinene, 2.4% camphor.

[0033]Put the safrole raw material into the reactor, stir and add 8kg of 5% NaOH solution, control the reaction temperature at 110-125°C, keep the pressure at 0.08-0.1MPa, and react for 1-2h to obtain crude isosafrole . Cool down, and when the temperature in the reactor drops to 50-60°C, discharge the crude isosafrole into the pickling tank. Adding sulfuric acid with a concentration of 20% under stirring, adjusting the pH to 7-8, standing for stratification, the upper layer is crude isosafrole, and the lower layer is saline waste water. Wash the above oil layer with ...

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Abstract

The invention discloses a method for converting safrole into iso-safrole. The method comprises the following steps: performing isomerization reaction on the safrole and a NaOH-containing basic catalyst under the condition of pressurization to generate the iso-safrole, wherein the basic catalyst is NaOH / gamma-Al2O3 or NaOH / CaO, the addition amount is 1-5 percent of the weight of the safrole, the NaOH-containing basic catalyst can be a NaOH solution of which the mass percentage concentration is 5-60%, and the use amount is 0.2-0.8% of the weight of the safrole; performing neutralization, washing, vacuum rectification and the like on the isomerized coarse iso-safrole to obtain high-purity iso-safrole of which the purity is more than 99.8 percent. The method has the advantages that the reaction time is short, the use amount of alkali is small, long-time high-temperature contact between the alkali and air is avoided, side reactions such as oxidative polymerization are reduced, and the yield of the iso-safrole is improved.

Description

technical field [0001] The invention relates to the technical field of processing natural flavors and fragrances, in particular to a method for converting safrole into isosafrole. Background technique [0002] Sassafras oil is an important natural fragrance, which exists in the essential oils of more than 70 kinds of plants, such as sassafras, cinnamon, rock laurel, cinnamon, and cinnamon. Wherein the content of safrole is 60-95% in sassafras oil, 88-95% in cinnamon leaf oil, and 97-98% in rock laurel oil. Safrole is mainly used as a raw material to synthesize a series of synthetic spices such as jasmonal, neojasmonal, piperonyl acetone, and jasmonil. The first step of synthesizing jasmonal from safrole is to isomerize the allyl group in the structural formula of safrole to propenyl group, even if the isomerization reaction of safrole occurs, isosafrole is produced Olein. The isomerization methods of safrole mainly include carbonyl iron isomerization method and potassium ...

Claims

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Application Information

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IPC IPC(8): C07D317/50
CPCC07D317/50
Inventor 孟中磊陆顺忠李秋庭高首娜关继华黎贵卿邱米杨漓杨素华苏骊华党中广李绍勇
Owner GUANGXI FORESTRY RES INST
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