CN108419799A - A kind of preparation method of 2,4 dichlorophenoxyacetic acid emulsifiable concentrate - Google Patents
A kind of preparation method of 2,4 dichlorophenoxyacetic acid emulsifiable concentrate Download PDFInfo
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- CN108419799A CN108419799A CN201710076666.9A CN201710076666A CN108419799A CN 108419799 A CN108419799 A CN 108419799A CN 201710076666 A CN201710076666 A CN 201710076666A CN 108419799 A CN108419799 A CN 108419799A
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- preparation
- emulsifier
- dichlorphenoxyacetic
- halogenated acetic
- acids ester
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N39/00—Biocides, pest repellants or attractants, or plant growth regulators containing aryloxy- or arylthio-aliphatic or cycloaliphatic compounds, containing the group or, e.g. phenoxyethylamine, phenylthio-acetonitrile, phenoxyacetone
- A01N39/02—Aryloxy-carboxylic acids; Derivatives thereof
- A01N39/04—Aryloxy-acetic acids; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/30—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group
- C07C67/31—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group by introduction of functional groups containing oxygen only in singly bound form
Abstract
The present invention relates to technical field of organic synthesis, and the present invention provides a kind of preparation methods of 2,4 dichlorphenoxyacetic acid emulsifiable concentrates, include the following steps：A) halogenated acetic acids ester and 2 after the mixing of 4 dichloro phenates, carries out condensation reaction, layered, obtains 2,4 dichlorphenoxyacetic acid esters；B) described 2,4 dichlorphenoxyacetic acid esters are mixed with solvent and emulsifier, obtains 2,4 dichlorphenoxyacetic acid missible oil.The present invention directly synthesizes 2,4 dichlorphenoxyacetic acid esters, 2,4 dichlorphenoxyacetic acid emulsifiable concentrates is prepared again, reaction production capacity is improved in this way, it is easy to operate and high with product yield, product is stablized, and exhaust gas and dust effectively controls and missible oil product substitutes the advantages such as pulvis good drug efficacy.
Description
Technical field
The present invention relates to technical field of organic synthesis, more particularly, to the preparation of one kind 2,4- dichlorphenoxyacetic acid emulsifiable concentrates
Method.
Background technology
2,4- dichlorphenoxyacetic acid class compounds are a kind of very important compounds, are that usage history is longest in the world
Organic synthesis herbicide kind, is still being widely used now.Wherein, 2,4- dichlorphenoxyacetic acids ester referred to as 2,4-D esters or 2,4-d
Ester；It is in missible oil to be prepared, and the main dosage form as herbicide is used in global range.
The preparation method of 2,4 dichlorophenoxyacetic acid esters missible oil disclosed in the prior art is mainly：2,4 dichloro benzene oxygen second
Acid synthesis 2,4- Dichlorophenoxy acid esters, adds auxiliary agent, solvent is configured to missible oil.2,4 dichlorophenoxyacetic acid esters missible oil is first
2,4- dichlorphenoxyacetic acids, acid and alcohol production ester are synthesized, then missible oil is prepared by ester, there are tedious process, complicated for operation, production capacity
Low, product yield is low, and exhaust gas and dust is difficult to control problem.Also, obtained missible oil product substitutes existing 2,4- Dichlorophenoxies
Acetic acid powder product exists and easily causes product bonding, be not easy to disperse to suspend in water, or blocks nozzle, is led in sprayer
Cause precipitation phenomena such as, cause to spray it is irregular, easily make crop locally generate poisoning main problem.
Invention content
In view of this, the technical problem to be solved in the present invention is to provide the system of one kind 2,4- dichlorphenoxyacetic acid emulsifiable concentrates
2,4- dichlorphenoxyacetic acid emulsifiable concentrates are prepared in Preparation Method, preparation method provided by the invention, and product is stablized, high income, and
It is high to react production capacity, it is easy to operate, it can effectively control the good drug efficacy of exhaust gas and dust and missible oil product.
The present invention provides the preparation methods of one kind 2,4- dichlorphenoxyacetic acid emulsifiable concentrates, include the following steps：
A) halogenated acetic acids ester and 2 after the mixing of 4- dichloro phenates, carries out condensation reaction, layered, obtains 2,4- Dichlorophenoxies
Acetic acid esters；
B) described 2,4- dichlorphenoxyacetic acid esters are mixed with solvent and emulsifier, obtains 2,4- dichlorphenoxyacetic acid breasts
Oil.
Preferably, the halogenated acetic acids ester is prepared by the following method：Alcohol and halogenated acetic acids carry out esterification, obtain halogenated
Acetic acid esters.
Preferably, 2, the 4- dichloros phenates is prepared by the following method：2,4- Dichlorophenols are reacted with alkali, obtain 2,4- dichloros
Phenates.
Preferably, it is carried out under the conditions of reaction existing for phase transfer catalyst in the step a).
Preferably, the halogenated acetic acids ester is selected from one or more of chloracetate, bromacetate and Alkyl Iodoacetates, institute
It states 2,4- dichloro phenates and is selected from 2,4- sodium dichlorophenol indophenols, 2,4- Dichlorophenols potassium, 2,4- Dichlorophenols calcium, 2,4- Dichlorophenols magnesium, 2,4- bis-
One or more of chlorophenol zinc and 2,4- Dichlorophenol aluminium.
Preferably, 2, the 4- dichloros phenates is selected from 2,4- sodium dichlorophenol indophenols or 2,4- Dichlorophenol potassium.
Preferably, the reaction temperature of the step a) is 70~200 DEG C；Reaction time is 1~7h.
Preferably, the molar ratio of the halogenated acetic acids ester and 2,4- dichloro phenates is (0.9~1.1)：(0.9~1.1).
Preferably, 2, the 4- dichlorphenoxyacetic acids ester and the mass ratio of solvent and emulsifier are (1~90)：(5~85)：
(5~12).
Preferably, the solvent is one or more in dimethylbenzene, solvent naphtha and vegetable oil；The emulsifier includes
First emulsifier and the second emulsifier, first emulsifier is in calcium dodecyl benzene sulfonate and neopelex
Any one or two kinds；Second emulsifier is selected from phenethyl phenol polyoxyethylene poly-oxygen propylene aether, phenethyl phenol polyoxy second
Alkene ether, phenethyl phenol polyethenoxy ether, nonyl phenol bring up Polyoxyalkylene ethers, Ben-zylphenol Polyoxyethyl Ether, fatty alcohol polyoxyethylene ether and
Any one or more in castor oil polyoxyethylene ether.
Compared with prior art, the present invention provides the preparation methods of one kind 2,4- dichlorphenoxyacetic acid emulsifiable concentrates, including
Following steps：A) halogenated acetic acids ester and 2 after the mixing of 4- dichloro phenates, carries out condensation reaction, layered, obtains 2,4- dichloro-benzenes
Fluoroacetic acid ester；B) described 2,4- dichlorphenoxyacetic acid esters are mixed with solvent and emulsifier, obtains 2,4- dichlorphenoxyacetic acid breasts
Oil.The present invention directly synthesizes 2,4- dichlorphenoxyacetic acids ester, 2,4- dichlorphenoxyacetic acid emulsifiable concentrates is prepared again, improves in this way
Reaction production capacity, easy to operate and high with product yield, product is stablized, and exhaust gas and dust effectively controls and missible oil product
Substitute the advantages such as pulvis good drug efficacy.
Description of the drawings
Fig. 1 is the flow sheet of 2,4 dichlorophenoxyacetic acid ester provided by the embodiments of the present application；
Fig. 2 is missible oil preparation process figure provided in an embodiment of the present invention.
Specific implementation mode
The present invention provides the preparation methods of one kind 2,4- dichlorphenoxyacetic acid emulsifiable concentrates, include the following steps：
A) halogenated acetic acids ester and 2 after the mixing of 4- dichloro phenates, carries out condensation reaction, layered, obtains 2,4- Dichlorophenoxies
Acetic acid esters；
B) described 2,4- dichlorphenoxyacetic acid esters are mixed with solvent and emulsifier, obtains 2,4- dichlorphenoxyacetic acid breasts
Oil.
Preparation method provided by the invention is directly synthesized to the production that esters arrive missible oil finished product again, can overcome in the prior art
Existing reaction production capacity is low, and complicated for operation, product yield is low, and product is unstable, not easy to control, pulvis drug effect difference of exhaust gas and dust etc.
Problem.
Halogenated acetic acids ester is prepared in the embodiment of the present invention first, prepares by the following method：Alcohol and halogenated acetic acids carry out ester
Change reaction, obtains halogenated acetic acids ester.Preferably, the esterification that alcohol and halogenated acetic acids are dehydrated by 3~5 grades of overflows, obtains
Halogenated acetic acids ester.Wherein, the alcohol can be methanol and other monohydric alcohols.Every grade of esterification can be dehydrated de- at 80~180 DEG C
It is molten, next stage esterification is then entered by overflow.Wherein, every grade of residence time can be controlled in 0.1h~2.0h.In this hair
In some bright embodiments, the esterification has 4 grades.
In the present invention, the preparation method of the halogenated acetic acids ester is preferably specially：By the monohydric alcohol of C2 or more and halogenated
Acetic acid continuous esterification obtains halogenated acetic acids ester.The monohydric alcohol and halogenated acetic acids of more preferably specific C2 or more is in catalyst
Under the action of be mixed, halogenated acetic acids ester is obtained by the reaction in continuous dehydration.The present invention for the stirring concrete mode not into
Row limits, agitating mode well known to those skilled in the art.
The monohydric alcohol of C2 the or more more than monohydric alcohol of C2 or more of the present invention namely two carbon atoms；Preferably C2
The monohydric alcohol of~C20；The more preferably monohydric alcohol of C2~C10；The most preferably monohydric alcohol of C3~C9.The halogenated acetic acids is preferred
Selected from one or more of monoxone, bromoacetic acid and iodoacetic acid；The alcohol and the catalyst of halogenated acetic acids reaction are preferably selected from
The concentrated sulfuric acid, toluene and butyl titanate.Wherein, the molar ratio of the monohydric alcohol of the C2 or more and halogenated acetic acids be preferably (1~
1.5):1；More preferably (1~1.2):1；Most preferably (1~1.1):1；The additive amount of the catalyst be preferably 1wt ‰~
1wt%.
In embodiments of the present invention, the halogenated acetic acids ester in chloracetate, bromacetate and Alkyl Iodoacetates one
Kind is several, preferably chloracetate or bromacetate.
The halogenated acetic acids ester intermediate stability that the present invention is preferably prepared is good, and byproduct of reaction is few, high income；In turn
Yield and purity subsequently to prepare provide good condition.
In addition, 2,4- dichloro phenates can be prepared in the embodiment of the present invention, such as 2,4- Dichlorophenols are reacted with alkali, obtain 2,4-
Dichloro phenates.It is preferred that being specially：2,4- Dichlorophenols are reacted with aqueous slkali in 70~95 DEG C, obtain 2,4- dichloro phenates.The alkali
The alkaline substance solutions such as sodium hydroxide, potassium hydroxide or solid may be used；The molar ratio of the 2,4- Dichlorophenols and alkali is 1:1
~1:1.5.
In an embodiment of the present invention, 2, the 4- dichloros phenates is selected from 2,4- sodium dichlorophenol indophenols, 2,4- Dichlorophenols potassium, 2,4-
Dichlorophenol calcium, 2,4- Dichlorophenols magnesium, 2,4- Dichlorophenols zinc and 2, one or more of 4- Dichlorophenol aluminium, preferably 2,4- dichloros
Phenol sodium or 2,4- Dichlorophenol potassium.
The present invention use oil phase halogenated acetic acids ester and 2,4- dichloro phenates, preferably phase transfer catalyst act under, instead
2,4- dichlorphenoxyacetic acid esters should be prepared, advantageously reduce and hydrolyze by-product in entire reaction process, accelerate reaction speed, carry
High conversion and yield reduce the wastewater flow rate of generation.
In the present invention, the phase transfer catalyst preferably is selected from one in polyethers, crown ether, quaternary ammonium salt, tertiary amine and quaternary phosphonium salt
Kind is several, more preferably quaternary ammonium salt, crown ether, tertiary amine or quaternary phosphonium salt.The crown ether such as cyclic crown ether；In the preferred reality of the present invention
It applies in example, the phase transfer catalyst is tetrabutylammonium bromide, 18 crown ethers, triethylamine or tetrabutyl phosphonium bromide phosphine.Wherein, the phase
The dosage of transfer catalyst is the 0.1%~5% of 2,4 dichlorophenoxyacetic acid ester quality.
The embodiment of the present invention is by the halogenated acetic acids ester and 2, after the mixing of 4- dichloro phenate solutions, carries out condensation reaction, warp
Layering, obtains 2,4- dichlorphenoxyacetic acid esters.In a preferred embodiment of the invention, by 3~5 grades of continuous condensation reactions, divide
2,4 dichlorophenoxyacetic acid ester is obtained after layer.
Wherein, the molar ratio of the halogenated acetic acids ester and 2,4- dichloro phenates can be (0.9~1.1)：(0.9~1.1).Contracting
The temperature for closing reaction is preferably 70~200 DEG C, more preferably 80~100 DEG C.In an embodiment of the present invention, by 2,4- Dichlorophenols
Salting liquid is mixed with the halogenated acetic acids ester that esterification obtains, and carries out level-one condensation reaction, then enters next stage condensation by overflow
Reaction, is finally layered, obtains 2,4- dichlorphenoxyacetic acid esters.Wherein, every grade of residence time can be controlled in 0.1h~2.0h at this
In some embodiments of invention, the condensation reaction has 4 grades.It is described to be layered as technological means well known to those skilled in the art,
The present invention is not particularly limited, if separation time can be 0.1h~2.0h.
The present invention can intermittently carry out above-mentioned operation；And it is preferred that being reacted by continuous esterification, continuous condensating, preparation
Obtain 2,4 dichlorophenoxyacetic acid ester.Some embodiments of the invention produce to obtain the detailed process of 2,4 dichlorophenoxyacetic acid ester such as
Shown in Fig. 1, Fig. 1 is the flow sheet of 2,4- dichlorphenoxyacetic acids ester provided by the embodiments of the present application.That is, the embodiment of the present invention
In, halogenated acetic acids and alcohol pass through level-one esterifying kettle, two level esterifying kettle, three-level esterifying kettle, the multistage of level Four esterifying kettle and are esterified successively
Reaction, is continuously available 2,4- dichlorphenoxyacetic acid esters；2,4- Dichlorophenols are reacted with alkali in and in kettle, obtain 2,4- Dichlorophenols
Salt；2,4- dichlorphenoxyacetic acid esters and 2 pass through level-one contractingization kettle, two level contractingization kettle, three-level successively after the mixing of 4- dichloro phenates
The multistage condensation reaction of contractingization kettle, level Four contractingization kettle obtains 2,4-d esters, can be placed in storage tank after layering kettle layering, spare.
Referring to Fig. 2, Fig. 2 is missible oil preparation process figure provided in an embodiment of the present invention.Obtain 2,4 dichloro benzene oxygen second
After acid esters, 2, the 4- dichlorphenoxyacetic acids ester is mixed with solvent and emulsifier in preparing kettle, preferably through filtering, is obtained
2,4 dichlorophenoxyacetic acid missible oil.
In the present invention, the solvent can be dimethylbenzene, polar solvent, solvent naphtha, one or more in vegetable oil etc..
The emulsifier preferably includes the first emulsifier (emulsifier 1) and the second emulsifier (emulsifier 2), and first emulsifier is optional
From any one or two kinds in calcium dodecyl benzene sulfonate and neopelex；Second emulsifier can be selected from benzene
Ethyl phenol polyoxyethylene poly-oxygen propylene aether, phenethyl phenol polyethenoxy ether, phenethyl phenol polyethenoxy ether, nonyl phenol bring up polyoxy alkene
Ether, Ben-zylphenol Polyoxyethyl Ether, any one or more in fatty alcohol polyoxyethylene ether and castor oil polyoxyethylene ether.It is described
The ratio of 2,4- dichlorphenoxyacetic acid esters and the mixing of solvent and emulsifier, different content mass ratioes is different, can only be 2,4- bis-
Chlorophenoxyacetic acid ester mass fraction 1%-90%, emulsifier mass fraction 5%-12%, solvent quality score 5%-85%.
Wherein, described to be mixed into technical means commonly used by such a person skilled in the art.Layering institute can be used in the embodiment of the present invention
The substance obtained, is added solvent, emulsifier for mixing, and heating and heat preservation obtains 2,4- dichlorphenoxyacetic acid emulsifiable concentrate finished products by press filtration.
Ranging from 25 DEG C~60 DEG C, preferably 30~50 DEG C of the holding temperature.
In conclusion 2,4- Dichlorophenoxy second is prepared by directly synthesizing 2,4- dichlorphenoxyacetic acid esters in the present invention
Acid esters missible oil improves reaction production capacity, easy to operate, and high with product yield, and product is stablized, and exhaust gas and dust is effectively controlled
System and missible oil product substitute the advantages such as pulvis good drug efficacy, are conducive to apply.
In order to further illustrate the present invention, with reference to embodiments to 2,4- dichlorphenoxyacetic acids ester provided by the invention breast
The preparation method of oil is described in detail.
Embodiment 1
2000kg butanol, 950kg (10kmol) monoxones and the 1kg concentrated sulfuric acids input level-one esterifying kettle are mixed, 80
DEG C precipitation is dehydrated 1h, then sequentially enters two, three-level esterifying kettle by overflow, feed rate 3000kg/h, and every grade when stopping
Between control in 1h, obtain butyl chloroacetate.
By 2,4 dichloro phenol 1640kg (10kmo1), the sodium hydrate aqueous solution 1250kg of mass fraction 32%
(10kmol) is mixed, and is warming up to 70 DEG C, obtains 2,4- sodium dichlorophenol indophenol solution.
2, the 4- sodium dichlorophenol indophenols solution is put into and is esterified obtained butyl chloroacetate and is mixed into level-one condensation kettle, 80
After DEG C stirring 0.5h, then sequentially enter two by overflow, three, level Four condensation kettle, feed rate 3000kg/h, every grade of stop
Time control enters layering kettle in 0.5h, then condensation gained reaction solution, separates 2, the 4- dichloros that upper layer obtains water white transparency
Phenoxy acetic acid butyl ester 2772kg, content 98.5%, yield 98.6%.
Gained ester is put into and is prepared in kettle, solvent xylene 210kg is added, 132kg emulsifiers 10 two are added in stirring
Alkyl benzene calcium sulfonate；2 nonyl phenol of 160kg emulsifiers is added and brings up Polyoxyalkylene ethers, by heating and heat preservation, press filtration obtains 3264kg 2,
4- dichlorobenzene oxygen butyl acetate 1000g/L missible oil, up-to-standard, yield 99.69%.
Embodiment 2
2000kg ethyl alcohol, 1400kg (10kmol) bromoacetic acids and the 1kg concentrated sulfuric acids are mixed, 100 DEG C of precipitation dehydrations
0.8h, then sequentially enters two, three-level esterifying kettle, feed rate 2500kg/h by overflow, and every grade of residence time control exists
0.8h obtains bromoacetate.
By 2,4 dichloro phenol 1640kg (10kmo1), the potassium hydroxide aqueous solution 1122kg of mass fraction 50%
(10kmol) is mixed, and is warming up to 70 DEG C, obtains 2,4- Dichlorophenol potassium solutions.
The obtained bromoacetate of 2,4- Dichlorophenols potassium solution input esterification is mixed into level-one condensation kettle, 90 DEG C
After stirring 0.5h, then sequentially enter two by overflow, three, level Four condensation kettle, feed rate 2000kg/h, every grade when stopping
Between control in 0.5h, then condensation reaction solution enters layering kettle, separates 2, the 4- Dichlorophenoxy second that upper layer obtains water white transparency
Acetoacetic ester 2772kg, content 98.3%, yield 98.4%.
Gained ester is put into and is prepared in kettle, solvent naphtha 150#220kg is added, 125kg emulsifiers 10 two are added in stirring
Alkyl benzene calcium sulfonate；2 castor oil polyoxyethylene ether of 157kg emulsifiers is added, by heating and heat preservation, press filtration obtains 3265kg 2,
4- dichlorphenoxyacetic acid ethyl ester 1000g/L missible oil, up-to-standard, yield 99.7%.
Embodiment 3
2000kg methanol, 950kg (10kmol) monoxones and the 1kg concentrated sulfuric acids input level-one esterifying kettle are mixed, 80
DEG C precipitation is dehydrated 0.3h, then sequentially enter two by overflow, three, level Four esterifying kettle, feed rate 3000kg/h, every grade is stopped
It stays time control in 0.3h, obtains methyl chloroacetate.
By 2,4 dichloro phenol 1640kg (10kmo1), the sodium hydrate aqueous solution 1250kg of mass fraction 32%
(10kmol) is mixed, and is warming up to 70 DEG C, obtains 2,4- sodium dichlorophenol indophenol solution.
2, the 4- sodium dichlorophenol indophenols solution is put into and is esterified obtained methyl chloroacetate and is mixed into level-one condensation kettle, 80
After DEG C stirring 0.5h, then sequentially enter two by overflow, three, level Four condensation kettle, feed rate 2000kg/h, every grade of stop
Time control enters layering kettle in 0.5h, then condensation gained reaction solution, separates 2, the 4- dichloros that upper layer obtains water white transparency
Phenoxy acetic acid butyl ester 2772kg, content 98.5%, yield 98.6%.
Gained ester is put into and is prepared in kettle, solvent methyl oleate 210kg is added, 132kg emulsifiers 10 are added in stirring
Dialkyl benzene sulfonic acids calcium；2 phenethyl phenol polyoxyethylene poly-oxygen propylene aether of 160kg emulsifiers is added, by heating and heat preservation, press filtration obtains
To 3264kg 2,4- dichlorphenoxyacetic acid methyl esters 1000g/L missible oil, up-to-standard, yield 99.69%.
As seen from the above embodiment, the present invention directly synthesizes 2,4- dichlorphenoxyacetic acids ester, 2,4- dichloros is prepared again
Phenoxy acetic acid emulsifiable concentrate；Qualified product, yield is 98% or more.Show that the present invention improves reaction production capacity, it is easy to operate,
And high with product yield, product is stablized, exhaust gas and dust effectively control and missible oil product to substitute pulvis good drug efficacy etc. excellent
Gesture.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. one kind 2, the preparation method of 4- dichlorphenoxyacetic acid emulsifiable concentrates, include the following steps：
A) halogenated acetic acids ester and 2 after the mixing of 4- dichloro phenates, carries out condensation reaction, layered, obtains 2,4- dichlorphenoxyacetic acids
Ester；
B) described 2,4- dichlorphenoxyacetic acid esters are mixed with solvent and emulsifier, obtains 2,4- dichlorphenoxyacetic acid missible oil.
2. preparation method according to claim 1, which is characterized in that the halogenated acetic acids ester is prepared by the following method：Alcohol
Esterification is carried out with halogenated acetic acids, obtains halogenated acetic acids ester.
3. preparation method according to claim 1, which is characterized in that 2, the 4- dichloros phenates is prepared by the following method：
2,4- Dichlorophenols are reacted with alkali, obtain 2,4- dichloro phenates.
4. preparation method according to claim 1, which is characterized in that reaction is deposited in phase transfer catalyst in the step a)
It carries out under the conditions.
5. preparation method according to claim 1, which is characterized in that the halogenated acetic acids ester is selected from chloracetate, bromine second
One or more of acid esters and Alkyl Iodoacetates, 2, the 4- dichloros phenates are selected from 2,4- sodium dichlorophenol indophenols, 2,4- Dichlorophenols potassium, 2,
One or more of 4- Dichlorophenols calcium, 2,4- Dichlorophenols magnesium, 2,4- Dichlorophenols zinc and 2,4- Dichlorophenol aluminium.
6. preparation method according to claim 5, which is characterized in that 2, the 4- dichloros phenates is selected from 2,4- sodium dichlorophenol indophenols
Or 2,4- Dichlorophenol potassium.
7. preparation method according to claim 1, which is characterized in that the reaction temperature of the step a) is 70~200 DEG C；
Reaction time is 1~7h.
8. preparation method according to claim 1, which is characterized in that the halogenated acetic acids ester and 2,4- dichloro phenates rubs
You are than being (0.9~1.1)：(0.9~1.1).
9. preparation method according to claim 1, which is characterized in that 2, the 4- dichlorphenoxyacetic acids ester and solvent and breast
The mass ratio of agent is (1~90)：(5~85)：(5~12).
10. preparation method according to claim 1, which is characterized in that the solvent is selected from dimethylbenzene, solvent naphtha and plant
It is one or more in oil；The emulsifier includes the first emulsifier and the second emulsifier, and first emulsifier is selected from 12
Any one in alkyl benzene calcium sulfonate and neopelex or two kinds；Second emulsifier is poly- selected from phenethyl phenol
Ethylene oxide polyethenoxy ether, phenethyl phenol polyethenoxy ether, phenethyl phenol polyethenoxy ether, nonyl phenol bring up Polyoxyalkylene ethers, benzyl
Phenol polyethenoxy ether, any one or more in fatty alcohol polyoxyethylene ether and castor oil polyoxyethylene ether.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110946138A (en) * | 2018-09-26 | 2020-04-03 | 江苏七洲绿色化工股份有限公司 | Trifluralin missible oil and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106242971A (en) * | 2016-08-04 | 2016-12-21 | 山东省化工研究院 | A kind of chloracetate synthesis in water technology and the new method of preparation 2,4 D esters thereof |
-
2017
- 2017-02-13 CN CN201710076666.9A patent/CN108419799A/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106242971A (en) * | 2016-08-04 | 2016-12-21 | 山东省化工研究院 | A kind of chloracetate synthesis in water technology and the new method of preparation 2,4 D esters thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110946138A (en) * | 2018-09-26 | 2020-04-03 | 江苏七洲绿色化工股份有限公司 | Trifluralin missible oil and preparation method thereof |
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Application publication date: 20180821 |