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Preparation method and application of composition of 2,4-dichlorophenoxyacetic acid and 2,4-dichlorophenoxyacetate

A technology of dichlorophenoxyacetate and dichlorophenoxyacetic acid, applied in the field of phenoxycarboxylate synthesis, can solve problems such as incomplete reaction, instability, poor product quality and the like

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

AI Technical Summary

Problems solved by technology

However, both processes are reacted with phenoxide and chloroacetate, not only the reaction is not complete, the product quality is poor, but also the situation of instability when used in preparation products usually occurs, which seriously affects the production of 2,4-dichlorophenoxy Production and Application of Acetic Acid

Method used

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  • Preparation method and application of composition of 2,4-dichlorophenoxyacetic acid and 2,4-dichlorophenoxyacetate
  • Preparation method and application of composition of 2,4-dichlorophenoxyacetic acid and 2,4-dichlorophenoxyacetate
  • Preparation method and application of composition of 2,4-dichlorophenoxyacetic acid and 2,4-dichlorophenoxyacetate

Examples

Experimental program
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Effect test

Embodiment 1

[0094] Combine 123g (1mol) of ethyl chloroacetate and 186g (1mol) of 2,4-dichlorophenate sodium, heat and stir for 3 hours, filter off the sodium chloride solid generated by the reaction, and ethanol is stripped from the filtrate to obtain 2,4-dichlorobenzene Ethyl oxyacetate, add 0.5g concentrated sulfuric acid, keep stirring at 80°C for 2h, crystallize at 10°C for 1h, filter, and dry the filter cake to obtain 2,4-dichlorophenoxyacetic acid and 2,4-dichlorophenoxyacetic acid Ester composition 230g.

[0095] The composition prepared in Example 1 of the present invention was prepared into a suspoemulsion.

[0096]The preparation method specifically includes the following steps: combining 2,4-dichlorophenoxyacetic acid and 2,4-dichlorophenoxyacetic ester, an emulsifier, a wetting and dispersing agent, a defoamer, a thickening stabilizer, The antifreeze agent and water are uniformly sheared and mixed at high speed, and ball milled in a ball mill for 2 to 3 hours, so that the par...

Embodiment 2

[0099] Combine 151g (1mol) butyl chloroacetate and 186g (1mol) of 2,4-dichlorophenate sodium, heat and stir for 3h, filter off the sodium chloride solid generated by the reaction, and remove butanol from the filtrate to obtain 2,4-dichlorophenate Butyl phenoxyacetate, add 0.3g p-toluenesulfonic acid, keep stirring at 120°C for 2h, crystallize at 10°C for 1h, filter, and dry the filter cake to obtain 2,4-dichlorophenoxyacetic acid and 2,4-dichlorobenzene Oxyacetate composition 228g.

[0100] The composition prepared in Example 2 of the present invention was prepared into a suspoemulsion.

[0101] The formula is: 2,4-dichlorophenoxyacetic acid and 2,4-dichlorophenoxyacetic ester composition 42%, calcium dodecylbenzenesulfonate 1%, phenylethylphenol polyoxyethylene polyoxypropylene Ether 2%, naphthalenesulfonic acid formaldehyde condensate sodium salt 3%, polycarboxylate sodium salt 1%, calcium lignosulfonate 1%, ethylene glycol 5%, silicone compounds 0.5%, magnesium aluminum si...

Embodiment 3

[0103] Combine 210g (1mol) of butyl bromoacetate and 186g (1mol) of 2,4-dichlorophenate sodium, heat and stir for 3 hours, filter off the solid sodium bromide generated by the reaction, and remove butanol from the filtrate to obtain 2,4-dichlorophenate Butyl phenoxyacetate, add 0.3g acetic acid, keep stirring at 120°C for 2h, crystallize at 10°C for 1h, filter, and dry the filter cake to obtain 2,4-dichlorophenoxyacetic acid and 2,4-dichlorophenoxyacetic acid Ester composition 236g.

[0104] The composition prepared in Example 3 of the present invention was used for suspoemulsion.

[0105] The formula is: 2,4-dichlorophenoxyacetic acid and 2,4-dichlorophenoxyacetic ester composition 26%, phenethylphenol polyoxyethylene ether 1%, castor oil polyoxyethylene ether 2%, naphthalene Sulfonic acid formaldehyde condensate sodium salt 1%, polycarboxylate sodium salt 3%, calcium lignosulfonate 1%, ethylene glycol 5%, silicone compounds 0.3%, magnesium aluminum silicate 0.14%, xanthan g...

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Abstract

The invention provides a preparation method for a composition of 2,4-dichlorophenoxyacetic acid and 2,4-dichlorophenoxyacetate. The preparation method comprises the following steps: reacting halogenated acetate with 2,4-dichlorophenate so as to obtain 2,4-dichlorophenoxyacetate; and directionally hydrolyzing 2,4-dichlorophenoxyacetate prepared in the previous step to obtain the composition of 2,4-dichlorophenoxyacetic acid and 2,4-dichlorophenoxyacetate. According to the invention, a process route is adjusted and creative improvement is made from the foundation; halogenated acetate reacts with2,4-dichlorophenate so as to prepare 2,4-dichlorophenoxyacetate, and directional hydrolysis is carried out so as to obtain the composition of 2,4-dichlorophenoxyacetic acid and 2,4-dichlorophenoxyacetate. The composition of 2,4-dichlorophenoxyacetic acid and 2,4-dichlorophenoxyacetate of the invention has excellent quality, high stability and good drug effect.

Description

technical field [0001] The invention belongs to the technical field of synthesis of phenoxycarboxylates, in particular to a preparation method and application of a composition of 2,4-dichlorophenoxyacetic acid and 2,4-dichlorophenoxyacetic acid ester. Background technique [0002] 2,4-dichlorophenoxyacetic acid, also known as 2,4-D, (2,4-dichlorophenoxy)acetic acid or 2,4-D acid, etc., the molecular formula is C 8 h 6 Cl 2 o 3 , with a melting point of 140.5°C and a boiling point of 160°C, white diamond-shaped crystal, soluble in most organic solvents such as alcohol, ether or ketone, and almost insoluble in water. [0003] 2,4-Dichlorophenoxyacetic acid compounds are a very important class of compounds. They are the longest-used organically synthesized herbicides in the world and are still widely used. They are mainly used in agriculture as herbicides or Plant growth agent is used, in the field of analysis, for the determination of carbon and hydrogen standards in organ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A01N39/04A01P13/00A01P21/00C07C51/09C07C59/70
CPCA01N39/04C07C51/09A01N2300/00C07C59/70
Inventor 孙国庆侯永生张全赵广理陈桂元
Owner SHANDONG RUNBO BIOTECH CO LTD
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