CN103497094B - A kind of preparation method of anisic aldehyde - Google Patents
A kind of preparation method of anisic aldehyde Download PDFInfo
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- CN103497094B CN103497094B CN201310428640.8A CN201310428640A CN103497094B CN 103497094 B CN103497094 B CN 103497094B CN 201310428640 A CN201310428640 A CN 201310428640A CN 103497094 B CN103497094 B CN 103497094B
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- anisic aldehyde
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/27—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
- C07C45/28—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation of CHx-moieties
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/32—Preparation of ethers by isomerisation
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Abstract
The invention discloses the preparation method of a kind of anisic aldehyde, purpose is to provide the preparation method of a kind of new anisic aldehyde, to reduce the production cost of anisic aldehyde, reducing pollution to environment, the method comprises the steps: isomery, frozen centrifugation, aoxidizes, is centrifuged, washes, neutralizes.The present invention, by chavicol methyl ether step such as isomerization, centrifugal, oxidation under catalyst existence condition, makes the electronics in chavicol methyl ether molecule reset, and foreign body generates the trans-anethole needed.Trans-anethole carries out oxidation reaction under the acid condition of manganese dioxide, ketone be converted into aldehyde, finally obtain anisic aldehyde.The present invention, using chavicol methyl ether as raw material, prepares the purification content of chavicol methyl ether up to more than 97%, exceeds about 13% than the purification content of traditional handicraft.The present invention can significantly improve the yield of anisic aldehyde, is more easily purified, it is possible to meeting industrialization large-scale production, and the corrosion to equipment is little, the pollution to environment is few.
Description
Technical field
The present invention relates to production of flavor field, the preparation method of a kind of anisic aldehyde.
Background technology
The chemical name of anisic aldehyde is P-methoxybenzal-dehyde, and it has relatively broad application.Its tool
Having lasting Fructus Crataegi fragrance, fragrance is tempting, thus is widely used in preparing sweet floral type, Fructus Crataegi odor type and Flos Caryophylli
The multiple essence such as odor type, and food, saccharide and the preparation of beverage class essence；In terms of medicine, it is to prepare
The important intermediate of the medicine (such as medicines such as hydroxybenzyl penicillium sp rope, Porphyrin-Based Sensitizer) that anti-dimension is biological；?
In electroplating industry, it can be as the excellent brightener of non-cyanogen galvanization DE additive；At agriculture field, Fructus Anisi Stellati
Fragrant aldehyde can be as insecticide, insecticide additive, biological growth inhibitor etc..Owing to anisic aldehyde has excellence
Performance, thus be widely used.
At present, the method for domestic synthesis anisic aldehyde mainly has three kinds.First method is isoesdragol oxygen
Change method, the method is owing to being limited by natural resources, and cost price is higher, seldom uses.The second be with
Methyl phenyl ethers anisole (sodium dichromate) is the oxidizing process (i.e. Sommelet reaction method) of raw material, and the method can produce a large amount of acid
Property waste water, causes seriously corroded to equipment.The third is cresol synthetic method, and it is serious that the method exists three-waste pollution,
The problem that yield is the highest.
Therefore, at present in the urgent need to the preparation method of a kind of new anisic aldehyde, to reduce anisic aldehyde
Production cost, reduces the pollution to environment.
Summary of the invention
The goal of the invention of the present invention is: for the problem of above-mentioned existence, it is provided that the system of a kind of anisic aldehyde
Preparation Method.The present invention, with chavicol methyl ether as raw material, by providing a kind of new technological process, successfully prepares Fructus Anisi Stellati
Fragrant aldehyde.The present invention can significantly improve the production yield of anisic aldehyde, simplification of flowsheet, shortens the production cycle,
Reduce production cost.The present invention is little to the corrosion of equipment, it is thus possible to the service life of extension device, is conducive to
The industrialization of anisic aldehyde, large-scale production.
To achieve these goals, the present invention adopts the following technical scheme that
The preparation method of a kind of anisic aldehyde, comprises the steps:
(1) isomery: chavicol methyl ether is put into isomery pot, then adds potassium hydroxide in isomery pot, control isomery pot
Interior temperature is 175-185 DEG C, reacts 3-5h, after reaction terminates, stops heating isomery pot, obtains fennel
Brain；
(2) frozen centrifugation: trans-anethole step 1 obtained carries out freezing at subzero less than 20 DEG C, simultaneously at freezing bar
Under part, trans-anethole is centrifuged, obtains high-purity trans-anethole；
(3) oxidation: high-purity trans-anethole step 2 obtained is put in reactor, and adds dilute sulfur in reactor
Acid, MnO2, the temperature controlled in reactor is 80-110 DEG C, reacts 2-6h, obtains anisic aldehyde crude product；
(4) centrifugal, washing: anisic aldehyde crude product is put into centrifuge and is centrifuged separating, after centrifugation again
Wash with saline；
(5) neutralize: the anisic aldehyde crude product sodium bicarbonate water after washing is carried out secondary washing, makes anisic aldehyde thick
The pH value of product is alkalescence, obtains product.
In described step 1, the quality of the potassium hydroxide of addition is the 3%-10% of chavicol methyl ether quality；
In described step 3, the ratio of weight and number adding component is as follows: 1000 parts of high-purity trans-anetholes, 100-300 part are dilute
Sulphuric acid, 200-500 part MnO2Catalyst；
In described step 4, saline is mixed with water by chloride, and chloride accounts for the 2%-10% of brine quality, chlorine
Compound is the one in sodium chloride, potassium chloride；
In described step 5, in sodium bicarbonate water, the mass percent of solute is 2-20%.
In described step 1, raw material natural grass estragole is put in rectifying column, purifies, rectifying column
Bottom temperature is 150-170 DEG C, and the temperature of tower top is 110-130 DEG C, the chavicol methyl ether after being purified；
Chavicol methyl ether after purifying puts into isomery pot, then adds potassium hydroxide in isomery pot, controls in isomery pot
Temperature is 175-185 DEG C, reacts 3-5h, after reaction terminates, stops heating isomery pot, obtains trans-anethole.
In described step 1, raw material natural grass estragole is put in rectifying column, purifies, rectifying column
Bottom temperature is 155-165 DEG C, and the temperature of tower top is 115-125 DEG C, the chavicol methyl ether after being purified.
In described step 1, the quality of the potassium hydroxide of addition is the 5% of chavicol methyl ether quality.
In described step 1, chavicol methyl ether is put into isomery pot, then in isomery pot, adds potassium hydroxide,
The temperature controlled in isomery pot is 180 DEG C, reacts 4h, after reaction terminates, stops heating isomery pot,
Obtain trans-anethole.
In described step 2, the brain that returns step 1 obtained carries out freezing at subzero 20 DEG C, simultaneously in freezing
Under the conditions of, it being centrifuged returning brain, centrifugation time is 10-60min, obtains high-purity trans-anethole.
In described step 3, high-purity trans-anethole step 2 obtained is put in reactor, and to reactor
Interior addition dilute sulfuric acid, MnO2, the temperature controlled in reactor is 100 DEG C, reacts 4h, obtains anisic aldehyde thick
Product；
The ratio of weight and number adding component is as follows: 1000 parts of high-purity trans-anetholes, 200 parts of dilute sulfuric acids, 300 parts of MnO2
Catalyst.
In described step 5, the anisic aldehyde crude product sodium bicarbonate water after washing is carried out secondary washing, makes
The pH value of anisic aldehyde crude product is 7.5-8.5.
In described step 5, the anisic aldehyde crude product sodium bicarbonate water after washing is carried out secondary washing, makes
The pH value of anisic aldehyde crude product is 8.
In described step 5, in sodium bicarbonate water, the mass percent of solute is 5%.
In described step 5, the anisic aldehyde crude product sodium bicarbonate water after washing is carried out secondary washing, makes
The pH value of anisic aldehyde crude product is alkalescence, obtains product, then product is sent into purification in rectifying column, rectifying column
Bottom temperature be 155 DEG C-165 DEG C, tower top temperature is 115 DEG C-125 DEG C, purify obtain high purity product.
The molecular structural formula of chavicol methyl ether is as follows:
If allyl aldehyde can be become after allyl double bonds therein oxidation, be not target product.
Applicant is found by analysis, and chavicol methyl ether, after certain isomerization reaction, obtains this isomers of trans-anethole,
After the oxidized double bond of trans-anethole, anisic aldehyde will be obtained, wherein, when the selection of catalyst, reaction temperature, reaction
Between, heating control, prepared by important for anisic aldehyde.
The preparation method of the present invention include isomery, frozen centrifugation, aoxidize, be centrifuged, wash, the step such as neutralization
Suddenly.Owing to the chavicol methyl ether purity in the place of production is generally about 50%, therefore can first raw material natural grass estragole be carried out
Purify.The condition that chavicol methyl ether purifies is the harshest, and raw material natural grass estragole is put in rectifying column by the present invention, enters
Row purifies, and the bottom temperature of rectifying column is 150-170 DEG C, and the temperature of tower top is 110-130 DEG C, is purified
After chavicol methyl ether.Through purifying, the purity of the 50% raw material natural grass estragole that purity is can be made significantly to be carried
Height, up to 98%.
Then chavicol methyl ether is carried out isomery process, isomerization reaction quickly will depend on smoothly catalyst and
The selection of reaction condition, for the present invention, the catalyst of employing, reaction temperature, response time during isomery
Isomerization reaction had material impact.This step can make chavicol methyl ether chain rupture become trans-anethole, after measured:
Using the present invention, the conversion ratio of isomery reaches more than 98%, after stopped reaction, it is possible to obtain the trans-anethole of about 95%.
Again trans-anethole is carried out frozen centrifugation, by trans-anethole being carried out below-20 DEG C freezing, and in freezing
Under the conditions of, trans-anethole is centrifuged, available high-purity trans-anethole.Further, trans-anethole is carried out cold at-20 DEG C
Freeze.Anisaldehyde belongs to thermal sensitivity spice, if temperature is too high, it may occur that neutralize reaction or polyreaction, thus must
Must strict control condition.The present invention carries out frozen centrifugation to trans-anethole, it is possible to obtain the trans-anethole of 99.9%.
Again high-purity trans-anethole is carried out oxidation processes, obtain anisic aldehyde crude product.Aoxidize organic compound double
The reaction of key oxidation scission is the response type that a class is unique, its product depend on the structure of matter, solvent species and
Reaction temperature.In the present invention, in oxidation reaction, the catalyst of use, solvent, reaction temperature, time are to finally
Product there is material impact, it directly determines the trans-anethole conversion to anisic aldehyde.
The most again anisic aldehyde crude product is centrifuged, washes and neutralizes.By thick for the anisic aldehyde after washing
Product sodium bicarbonate water carries out secondary washing, and the pH value making anisic aldehyde crude product is alkalescence, obtains product.Enter one
Step, the pH value making anisic aldehyde crude product is 7.5-8.5；Further, the pH value making anisic aldehyde crude product is
8.Applicant finds through research, and in the basic conditions, anisic aldehyde is not susceptible to polyreaction, thus selects
Secondary washing is carried out with sodium bicarbonate water.Further, purify in the product obtained is sent into rectifying column, rectifying column
Bottom temperature is 155 DEG C-165 DEG C, and tower top temperature is 115 DEG C-125 DEG C, and it is more than 99% that purification obtains purity
Product.
Dilute sulfuric acid refers to the sulphuric acid of concentration less than 70%, the wherein mass fraction of the solute sulfur less than 70%
Acid.In the present invention, the concentration of the dilute sulfuric acid of employing can be 3%-70%.The quality hundred of solute in sodium bicarbonate water
Proportion by subtraction is 5% to refer to, in sodium bicarbonate water, sodium bicarbonate accounts for the 5% of sodium bicarbonate water gross mass.In step 1,
Raw material natural grass estragole is put in rectifying column, purifies, the chavicol methyl ether after being purified, the tower of rectifying column
Still temperature is 150-170 DEG C, and the temperature of tower top is 110-130 DEG C, and rectifying column adds with can use conduction oil
Heat, the temperature of conduction oil is 180 DEG C-200 DEG C.
In the present invention, only produce a small amount of waste water, effectively reduce the discharge capacity of waste water, it is only necessary to waste water
Carry out precipitating, neutralisation treatment, after reaching discharge standard, can discharge, effectively reduce the intractability of waste water.
Applicant by with other unit cooperation, obtained the present invention.The present invention is being catalyzed by chavicol methyl ether
Under agent potassium hydroxide existence condition, the step such as isomerization, centrifugal, oxidation, makes the electronics in chavicol methyl ether molecule occur
Resetting, foreign body generates the trans-anethole needed.Trans-anethole carries out oxidation reaction under the acid condition of manganese dioxide, by ketone
It is converted into aldehyde, finally obtains anisic aldehyde.The present invention contains using chavicol methyl ether as raw material, the purification preparing chavicol methyl ether
Amount, up to more than 97%, exceeds about 13% than the purification content of traditional handicraft.The present invention can significantly improve
The yield of anisic aldehyde, is more easily purified, it is possible to meet industrialization large-scale production, and the corrosion to equipment is little,
Pollution to environment is few.The price of anisic aldehyde is more than 2 times of trans-anethole, thus the employing present invention can be notable
Improve value-added content of product.
Detailed description of the invention
All features disclosed in this specification, or disclosed all methods or during step, except
Beyond mutually exclusive feature and/or step, all can combine by any way.
Any feature disclosed in this specification, unless specifically stated otherwise, all can by other equivalence or there is class
Replaced like the alternative features of purpose.I.e., unless specifically stated otherwise, each feature is a series of equivalence or class
Like an example in feature.
Embodiment 1
Being put in rectifying column by the raw material natural grass estragole that purity is 50%, purify, the bottom temperature of rectifying column is
160 DEG C, the temperature of tower top is 120 DEG C, the chavicol methyl ether after being purified, and its purity is about 98%.
Chavicol methyl ether after purifying puts into isomery pot, then adds catalyst potassium hydroxide in isomery pot,
The temperature controlled in isomery pot is 180 DEG C, reacts 4h, after reaction terminates, stops heating isomery pot,
Obtain trans-anethole.Wherein, the 5% of the quality of the chavicol methyl ether after the quality of the potassium hydroxide of addition is purification.
Trans-anethole is carried out freezing at subzero less than 20 DEG C, the most under freezing conditions, trans-anethole is centrifuged,
Centrifugation time is 20min, obtains high-purity trans-anethole.
1000kg high-purity trans-anethole is put in reactor, and in reactor add 200kg dilute sulfuric acid,
300kgMnO2, the temperature controlled in reactor is 100 DEG C, reacts 4h, obtains anisic aldehyde crude product.Dilute sulfuric acid
Concentration be 20%.
Anisic aldehyde crude product is put into centrifuge be centrifuged separating, carry out with saline again after centrifugation
Washing.Wherein, saline be mass percent be the sodium chloride solution of 5%.
The sodium bicarbonate water that anisic aldehyde crude product Solute mass percentage ratio is 5% after washing is carried out secondary
Washing, the pH value making anisic aldehyde crude product is 8.0, obtains product.
Purifying in product is sent into rectifying column again, the bottom temperature of rectifying column is 160 DEG C, and tower top temperature is
120 DEG C, purify and obtain the high purity product that purity is 98-99%.
Embodiment 2
Being put in rectifying column by raw material natural grass estragole, purify, the bottom temperature of rectifying column is 150 DEG C, tower top
Temperature be 110 DEG C, the chavicol methyl ether after being purified.
Chavicol methyl ether after purifying puts into isomery pot, then adds potassium hydroxide in isomery pot, controls different
Temperature in structure pot is 185 DEG C, reacts 3h, after reaction terminates, stops heating isomery pot, obtains trans-anethole.
Wherein, the 3% of the quality of the chavicol methyl ether after the quality of the potassium hydroxide of addition is purification.
Trans-anethole is carried out below-20 DEG C freezing, the most under freezing conditions, trans-anethole is centrifuged, from
The heart time is 50min, obtains high-purity trans-anethole.
1000kg high-purity trans-anethole is put in reactor, and in reactor add 100kg dilute sulfuric acid,
400kgMnO2, the temperature controlled in reactor is 100 DEG C, reacts 4h, obtains anisic aldehyde crude product, wherein,
The concentration of dilute sulfuric acid is 35%.
Anisic aldehyde crude product is put into centrifuge be centrifuged separating, carry out with saline again after centrifugation
Washing.Wherein, saline be mass percent be the sodium chloride solution of 3%.
The sodium bicarbonate water that anisic aldehyde crude product Solute mass percentage ratio is 6% after washing is carried out secondary
Washing, the pH value making anisic aldehyde crude product is alkalescence, obtains product.
Purifying in product is sent into rectifying column again, the bottom temperature of rectifying column is 155 DEG C, and tower top temperature is
115 DEG C, purify and obtain high purity product.
Embodiment 3
Being put in rectifying column by raw material natural grass estragole, purify, the bottom temperature of rectifying column is 155 DEG C, tower top
Temperature be 115 DEG C, the chavicol methyl ether after being purified.
Chavicol methyl ether after purifying puts into isomery pot, then adds potassium hydroxide in isomery pot, controls different
Temperature in structure pot is 175 DEG C, reacts 5h, after reaction terminates, stops heating isomery pot, obtains trans-anethole.
Wherein, the 8% of the quality of the chavicol methyl ether after the quality of the potassium hydroxide of addition is purification.
Trans-anethole is carried out below-25 DEG C freezing, the most under freezing conditions, trans-anethole is centrifuged, from
The heart time is 15min, obtains high-purity trans-anethole.
1000kg high-purity trans-anethole is put in reactor, and in reactor add 300kg dilute sulfuric acid,
250kgMnO2, the temperature controlled in reactor is 105 DEG C, reacts 3h, obtains anisic aldehyde crude product.
Anisic aldehyde crude product is put into centrifuge be centrifuged separating, carry out with saline again after centrifugation
Washing.Wherein, saline be mass percent be the sodium chloride solution of 7%.
Anisic aldehyde crude product sodium bicarbonate water after washing is carried out secondary washing, makes anisic aldehyde crude product
PH value is alkalescence, obtains product.In sodium bicarbonate water, the mass percent of sodium bicarbonate is 10%.
Purifying in product is sent into rectifying column again, the bottom temperature of rectifying column is 160 DEG C, and tower top temperature is
120 DEG C, purify and obtain the high purity product that purity is 98-99%.
Embodiment 4
Being put in rectifying column by raw material natural grass estragole, purify, the bottom temperature of rectifying column is 165 DEG C, tower top
Temperature be 125 DEG C, the chavicol methyl ether after being purified.
Chavicol methyl ether after purifying puts into isomery pot, then adds potassium hydroxide in isomery pot, controls different
Temperature in structure pot is 180 DEG C, reacts 4.5h, after reaction terminates, stops heating isomery pot, obtains fennel
Brain.Wherein, the 7% of the quality of the chavicol methyl ether after the quality of the potassium hydroxide of addition is purification.
Trans-anethole is carried out below-22 DEG C freezing, the most under freezing conditions, trans-anethole is centrifuged, from
The heart time is 20min, obtains high-purity trans-anethole.
1000kg high-purity trans-anethole is put in reactor, and in reactor add 200kg dilute sulfuric acid,
200kgMnO2, the temperature controlled in reactor is 100 DEG C, reacts 5h, obtains anisic aldehyde crude product.
Anisic aldehyde crude product is put into centrifuge be centrifuged separating, carry out with saline again after centrifugation
Washing.Wherein, saline be mass percent be the Klorvess Liquid of 5%.
The sodium bicarbonate water that anisic aldehyde crude product Solute mass percentage ratio is 15% after washing is carried out secondary
Washing, the pH value making anisic aldehyde crude product is alkalescence, obtains product.
Purifying in product is sent into rectifying column again, the bottom temperature of rectifying column is 165 DEG C, and tower top temperature is
125 DEG C, purify and obtain high purity product.
Embodiment 5
Being put in rectifying column by raw material natural grass estragole, purify, the bottom temperature of rectifying column is 160 DEG C, tower top
Temperature be 120 DEG C, the chavicol methyl ether after being purified.
Chavicol methyl ether after purifying puts into isomery pot, then adds potassium hydroxide in isomery pot, controls different
Temperature in structure pot is 180 DEG C, reacts 4h, after reaction terminates, stops heating isomery pot, obtains trans-anethole.
Wherein, the 6% of the quality of the chavicol methyl ether after the quality of the potassium hydroxide of addition is purification.
Trans-anethole is carried out below-20 DEG C freezing, the most under freezing conditions, trans-anethole is centrifuged, from
The heart time is 40min, obtains high-purity trans-anethole.
1000kg high-purity trans-anethole is put in reactor, and in reactor add 250kg dilute sulfuric acid,
350kgMnO2, the temperature controlled in reactor is 105 DEG C, reacts 4.5h, obtains anisic aldehyde crude product.
Anisic aldehyde crude product is put into centrifuge be centrifuged separating, carry out with saline again after centrifugation
Washing.Wherein, saline be mass percent be the Klorvess Liquid of 3%.
The sodium bicarbonate water that anisic aldehyde crude product Solute mass percentage ratio is 3% after washing is carried out secondary
Washing, the pH value making anisic aldehyde crude product is alkalescence, obtains product.
Purifying in product is sent into rectifying column again, the bottom temperature of rectifying column is 160 DEG C, and tower top temperature is
120 DEG C, purify and obtain high purity product.
The invention is not limited in aforesaid detailed description of the invention.The present invention expands to any in this specification
The new feature of middle disclosure or any new combination, and disclose arbitrary new method or the step of process or any
New combination.
Claims (7)
1. the preparation method of an anisic aldehyde, it is characterised in that comprise the steps:
(1) isomery: the chavicol methyl ether after purifying puts into isomery pot, then adds potassium hydroxide in isomery pot, and the temperature controlled in isomery pot is 175-185 DEG C, reacts 3-5h, after reaction terminates, stops heating isomery pot, obtains trans-anethole；
(2) frozen centrifugation: trans-anethole step 1 obtained carries out freezing at subzero less than 20 DEG C, the most under freezing conditions, is centrifuged trans-anethole, obtains centrifugal trans-anethole；
(3) oxidation: centrifugal trans-anethole step 2 obtained is put in reactor, and in reactor, add dilute sulfuric acid, MnO2, the temperature controlled in reactor is 80-110 DEG C, reacts 2-6h, obtains anisic aldehyde crude product；
(4) centrifugal, washing: anisic aldehyde crude product is put into centrifuge and is centrifuged separating, wash with saline again after centrifugation；
(5) neutralize: the anisic aldehyde crude product sodium bicarbonate water after washing is carried out secondary washing, and the pH value making anisic aldehyde crude product is alkalescence, obtains product；
In described step 1, the quality of the potassium hydroxide of addition is the 3%-10% of chavicol methyl ether quality；
In described step 3, the ratio of weight and number adding component is as follows: 1000 parts of centrifugal trans-anetholes, 100-300 part dilute sulfuric acid, 200-500 part MnO2Catalyst；
In described step 4, saline is mixed with water by chloride, and chloride accounts for the 2%-10% of brine quality, and chloride is the one in sodium chloride, potassium chloride；
In described step 5, in sodium bicarbonate water, the mass percent of solute is 2-20%；
Being put in rectifying column by raw material natural grass estragole, purify, the bottom temperature of rectifying column is 150-170 DEG C, and the temperature of tower top is 110-130 DEG C, the chavicol methyl ether after being purified；
In described step 5, anisic aldehyde crude product sodium bicarbonate water after washing is carried out secondary washing, the pH value making anisic aldehyde crude product is 7.5-8.5, obtain product, purify in product is sent into rectifying column again, the bottom temperature of rectifying column is 155 DEG C-165 DEG C, and tower top temperature is 115 DEG C-125 DEG C, purifies and obtains centrifuge product.
The preparation method of anisic aldehyde the most according to claim 1, it is characterised in that in described step 1, being put in rectifying column by raw material natural grass estragole, purify, the bottom temperature of rectifying column is 155-165 DEG C, the temperature of tower top is 115-125 DEG C, the chavicol methyl ether after being purified.
The preparation method of anisic aldehyde the most according to claim 1, it is characterised in that in described step 1, the quality of the potassium hydroxide of addition is the 5% of chavicol methyl ether quality.
The preparation method of anisic aldehyde the most according to claim 1, it is characterized in that, in described step 1, chavicol methyl ether being put into isomery pot, then adds potassium hydroxide in isomery pot, the temperature controlled in isomery pot is 180 DEG C, reaction 4h, after reaction terminates, stop isomery pot is heated, obtain trans-anethole.
The preparation method of anisic aldehyde the most according to claim 1, it is characterised in that in described step 2, trans-anethole step 1 obtained carries out freezing at subzero 20 DEG C, the most under freezing conditions, is centrifuged trans-anethole, centrifugation time is 10-60min, obtains centrifugal trans-anethole.
6. according to the preparation method of the anisic aldehyde described in any one of claim 1-5, it is characterised in that in described step 3, centrifugal trans-anethole step 2 obtained is put in reactor, and adds dilute sulfuric acid, MnO in reactor2, the temperature controlled in reactor is 100 DEG C, reacts 4h, obtains anisic aldehyde crude product；
The ratio of weight and number adding component is as follows: 1000 parts of centrifugal trans-anetholes, 200 parts of dilute sulfuric acids, 300 parts of MnO2Catalyst.
The preparation method of anisic aldehyde the most according to claim 1, it is characterised in that in described step 5, carries out secondary washing by the anisic aldehyde crude product sodium bicarbonate water after washing, and the pH value making anisic aldehyde crude product is 8.
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