Preparation method and production system for 2,4-dichlorophenoxyacetate missible oil

A technology of dichlorophenoxyacetate and production system, applied in the preparation of carboxylate, botanical equipment and method, preparation of organic compounds, etc., can solve uneven spraying, crop phytotoxicity, low product yield, etc. To achieve the effect of effective control of waste gas and dust, improvement of reaction capacity and high product yield

Inactive Publication Date: 2018-08-21
SHANDONG RUNBO BIOTECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the synthesis of 2,4-dichlorophenoxyacetate and the preparation of emulsifiable concentrate are batch reactions, which have problems such as low production capacity, low product yield, and difficult control of exhaust gas and dust.
Moreover, the obtained emulsifiable concentrate product replaces the existing 2,4-dichloro powder, and it is easy to cause product sticking, be difficult to disperse and suspend in water, or block the nozzle, cause precipitation in the sprayer, etc., resulting in uneven spraying and easy The main problems that cause local phytotoxicity of crops

Method used

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  • Preparation method and production system for 2,4-dichlorophenoxyacetate missible oil

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preparation example Construction

[0028] The invention provides a kind of preparation method of 2,4-dichlorophenoxyacetate emulsifiable concentrate, comprises the steps:

[0029] A) Alcohol and halogenated acetic acid undergo the esterification reaction of 3-5 stages of overflow dehydration to obtain halogenated acetate;

[0030] B) After the haloacetate is mixed with 2,4-dichlorophenoxylate, 2,4-dichlorophenoxyacetate is obtained through 3-5 stages of continuous condensation reaction and layered;

[0031] C) mixing the 2,4-dichlorophenoxyacetic acid ester with a solvent and an emulsifier to obtain 2,4-dichlorophenoxyacetic acid emulsifiable concentrate.

[0032] The preparation method provided by the invention can overcome the problems of low reaction production capacity, complicated operation, low product yield, unstable product, difficult control of exhaust gas and dust, poor efficacy of powder and the like caused by batch reaction in the prior art.

[0033] In the embodiment of the present invention, the ...

Embodiment 1

[0069] Put 2000kg of butanol, 950kg (10kmol) of chloroacetic acid and 1kg of concentrated sulfuric acid into the primary esterification tank, mix and stir, desolventize and dehydrate at 80°C for 1 hour, and then enter the secondary and tertiary esterification tanks through overflow in sequence, and the feeding rate is 3000kg / h, and the residence time of each stage is controlled at 1h to obtain butyl chloroacetate.

[0070] 1640kg (10kmol) of 2,4-dichlorophenol and 1250kg (10kmol) of sodium hydroxide aqueous solution with a mass fraction of 32% were mixed and stirred, and the temperature was raised to 70°C to obtain sodium 2,4-dichlorophenate solution.

[0071] Put the 2,4-dichlorophenate sodium solution into the first-stage condensation kettle and mix it with the butyl chloroacetate obtained by esterification, stir at 80°C for 0.5h, and then enter the second, third, and fourth-stage condensation kettles through overflow , the feed rate is 3000kg / h, and the residence time of e...

Embodiment 2

[0074] Mix and stir 2000kg ethanol, 1400kg (10kmol) bromoacetic acid and 1kg concentrated sulfuric acid, desolventize and dehydrate at 100°C for 0.8h, and then enter the second and third stage esterification kettles through the overflow, the feed rate is 2500kg / h, and each stage stays The time was controlled at 0.8h to obtain ethyl bromoacetate.

[0075] 1640kg (10kmol) of 2,4-dichlorophenol and 1122kg (10kmol) of potassium hydroxide aqueous solution with a mass fraction of 50% were mixed and stirred, and the temperature was raised to 70°C to obtain potassium 2,4-dichlorophenolate solution.

[0076] Put the 2,4-dichlorophenate potassium solution into the ethyl bromoacetate obtained by esterification and mix it into the first-stage condensation kettle, stir at 90°C for 0.5h, and then enter the second, third, and fourth-stage condensation kettles in turn through overflow, The feed rate is 2000kg / h, and the residence time of each stage is controlled at 0.5h. Then the condensation...

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Abstract

The invention provides a preparation method and production system for 2,4-dichlorophenoxyacetate missible oil. The preparation method comprises the following steps: A) subjecting alcohol and halogenated acetic acid to an esterification reaction with three to five stages of overflow dehydration so as to obtain halogenated acetate; B) mixing halogenated acetate with 2,4-dichlorophenolate, and carrying out three to five stages of continuous condensation reaction and layering so as to obtain dichlorophenoxyacetate; and C) mixing 2,4-dichlorophenoxyacetate with a solvent and an emulsifier so as toobtain the 2,4-dichlorophenoxyacetate missible oil. The production system mainly comprises a multistage esterification device, a multistage condensation device, a layering device and a missible oil preparation device. According to the invention, the 2,4-dichlorophenoxyacetate missible oil is prepared by using a specific continuous method, so reaction capacity is improved; the preparation method issimple in operation, high in product yield, stable in product quality and capable of effectively controlling exhaust gas and dust; and in replacement of powder, the prepared missible oil has the advantages of good drug effect, etc.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of 2,4-dichlorophenoxyacetate emulsifiable concentrate and a production system thereof. Background technique [0002] 2,4-Dichlorophenoxyacetic acid compounds are a very important class of compounds. They are the longest-used organic synthetic herbicides in the world and are still widely used. Among them, 2,4-dichlorophenoxyacetate is referred to as 2,4-D ester or 2,4-d ester; it is prepared as an emulsifiable concentrate, which is used as the main dosage form of herbicides worldwide. [0003] The preparation method of the 2,4-dichlorophenoxyacetic acid ester emulsifiable concentrate disclosed in the prior art is mainly: 2,4-dichlorophenoxyacetic acid is synthesized into 2,4-dichlorophenoxyacetic acid ester, and then adding additives and solvents Formulated as a cream. Among them, the synthesis of 2,4-dichlorophenoxyacetate and the preparation of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/31C07C69/712A01N25/04A01N39/04A01P13/00
CPCA01N25/04A01N39/04C07C67/08C07C67/31C07C69/63C07C69/712
Inventor 孙国庆侯永生李遵亮赵广理陈桂元
Owner SHANDONG RUNBO BIOTECH CO LTD
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