Preparation method for 2,4-dichlorophenoxyacetate missible oil

A technology of dichlorophenoxyacetate and haloacetate, applied in the field of preparation of 2,4-dichlorophenoxyacetate emulsifiable concentrate, which can solve uneven spraying, complicated operation, low product yield, etc. problems, to achieve effective control of exhaust gas and dust, increase reaction capacity, and high product yield

Inactive Publication Date: 2018-08-21
SHANDONG RUNBO BIOTECH CO LTD
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

2,4-Dichlorophenoxyacetic ester EC is first synthesized 2,4-dichlorophenoxyacetic acid, acid and alcohol to produce ester, and then the ester is used to prepare EC, which has cumbersome procedures, complicated operation, low production capacity and low product yield. Low, the exhaust gas dust is not easy to control
Moreover, the obtained emulsifiable concentrate product replaces the existing 2,4-dichlorophenoxyacetic acid powder product, which is easy to cause product bonding, is not easy to disperse and suspend in water, or blocks the nozzle, and causes precipitation in the sprayer, etc., resulting in poor spraying. The main problem is that it is easy to cause local phytotoxicity of crops

Method used

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  • Preparation method for 2,4-dichlorophenoxyacetate missible oil
  • Preparation method for 2,4-dichlorophenoxyacetate missible oil

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preparation example Construction

[0020] The invention provides a kind of preparation method of 2,4-dichlorophenoxyacetate emulsifiable concentrate, comprises the steps:

[0021] a) After the haloacetate is mixed with 2,4-dichlorophenoxylate, condensation reaction is carried out, and 2,4-dichlorophenoxyacetate is obtained through layering;

[0022] b) mixing the 2,4-dichlorophenoxyacetic acid ester with a solvent and an emulsifier to obtain 2,4-dichlorophenoxyacetic acid emulsifiable concentrate.

[0023] The preparation method provided by the invention is directly synthesized to esters and then to the production of emulsifiable concentrate products, which can overcome the low reaction capacity, complicated operation, low product yield, unstable product, difficult control of waste gas and dust, and powder drug efficacy in the prior art. Bad question.

[0024] In the embodiment of the present invention, firstly, a haloacetate is prepared by the following method: an alcohol and a haloacetic acid are subjected t...

Embodiment 1

[0042] 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.

[0043] 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.

[0044] 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

[0047] 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.

[0048] 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.

[0049] 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 for 2,4-dichlorophenoxyacetate missible oil, belonging to the technical field of organic synthesis. The preparation method comprises the following steps: a)reacting halogenated acetate with 2,4-dichlorophenolate and then carrying out a condensation reaction and layering successively so as to obtain 2,4-dichlorophenoxyacetate; and b) mixing 2,4-dichlorophenoxyacetate with a solvent and an emulsifier so as to obtain the 2,4-dichlorophenoxyacetate missible oil. According to the invention, 2,4-dichlorophenoxyacetate is directly synthesized and then the2,4-dichlorophenoxyacetate missible oil is prepared, so reaction capacity is improved; the preparation method is simple 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. 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. 2,4-Dichlorophenoxyacetic ester EC is first synthesized 2,4-dichlorophenoxyacetic acid, acid and alcohol to pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A01N39/04A01N25/04A01P13/00C07C69/712C07C67/31
CPCA01N25/04A01N39/04C07C67/31A01N2300/00C07C69/712
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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