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Preparation method of chlorophenoxycarboxylic acid herbicide

A technology of chlorophenoxycarboxylic acid and chlorophenoxycarboxylic acid ester, which is applied in the direction of carboxylate/lactone preparation, herbicides and algicides, botany equipment and methods, etc., and can solve the problems affecting chlorophenoxycarboxylic acid The production and application of similar compounds, difficult recovery of catalysts, high processing costs, etc., achieve the effects of easy separation, thorough reaction, and increased reaction rate

Inactive Publication Date: 2018-12-07
SHANDONG RUNBO BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned processes all have the problems of a lot of waste water and waste salt, difficult recovery of catalysts, high treatment costs, and great pressure on environmental protection, which seriously affect the production and application of chlorophenoxycarboxylic acid compounds

Method used

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  • Preparation method of chlorophenoxycarboxylic acid herbicide
  • Preparation method of chlorophenoxycarboxylic acid herbicide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Mix and stir 100g of methyl 2,4-dichlorophenoxyacetate with a mass fraction of 99%, 100g of 30% hydrochloric acid, and 5g of p-toluenesulfonic acid, raise the temperature to 120°C, react for 2 hours, let stand to separate layers, and separate the water phase Applying the same method to the next batch, the temperature of the oil phase was lowered to obtain solid 2,4-dichlorophenoxyacetic acid, which was dried to obtain 93.1 g of 2,4-dichlorophenoxyacetic acid with a purity of 99.6% and a yield of 99.6%.

Embodiment 2

[0039] Mix 100g of methyl 2-methyl-4-chlorophenoxyacetate with a mass fraction of 99%, 120g of 30% hydrochloric acid, and 8g of dodecylbenzenesulfonic acid, mix and stir, heat up to 150°C, react for 1.5h, and stand to separate layers , the water phase was separated and applied to the next batch, the oil phase was cooled to obtain 2-methyl-4-chlorophenoxyacetic acid solid, and dried to obtain 92.3g of 2-methyl-4-chlorophenoxyacetic acid with a purity of 99.3%. Rate 99.0%.

Embodiment 3

[0041] Mix and stir 100g of methyl 2,4-dichlorophenoxyacetate with a mass fraction of 99%, 150g of 30% hydrochloric acid, and 10g of dodecylbenzenesulfonic acid, heat up to 160°C, react for 1.0h, and let the The water phase was separated and applied to the next batch, and the oil phase was cooled to obtain solid 2,4-dichlorophenoxyacetic acid, which was dried to obtain 93.0 g of 2,4-dichlorophenoxyacetic acid with a purity of 99.7% and a yield of 99.6%.

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Abstract

The invention provides a preparation method of a chlorophenoxycarboxylic acid herbicide, wherein the preparation method includes the following steps: A) carrying out hydrolysis reaction of chlorophenoxycarboxylic ester under the action of hydrochloric acid, wherein the reaction system contains a surfactant; B) after the reaction is finished, dividing the system into an oil phase and a water phase,and cooling and crystallizing the oil phase, to obtain chlorophenoxycarboxylic acid. Hydrochloric acid is chosen as an acid catalyst and is used in combination with the surfactant; in the reaction process, the raw material and the catalyst are fully contacted, the reaction rate is increased, the reaction time is shortened, and the reaction is more thorough; after the reaction is finished, the oilphase and the water phase are stratified to facilitate the separation of the product and the catalyst. Excess hydrochloric acid can be evaporated and recycled, water-washing water can be recycled, nowaste salt or waste water exists, the energy consumption is low, and the preparation method is economic and environmentally friendly.

Description

technical field [0001] The invention relates to the technical field of herbicide preparation, in particular to a preparation method of chlorophenoxycarboxylic acid herbicides. Background technique [0002] Chlorophenoxy carboxylic acid compounds have a large market demand, but there are many defects in the preparation process. The synthesis method of chlorophenoxy carboxylic acid compounds disclosed in the prior art mainly adopts the Williamson condensation method, and the production process can be specifically divided into There are two types: first condensation and then chlorination and first chlorination and then condensation. However, both processes generate chlorophenoxycarboxylate, and finally acidify with hydrochloric acid to obtain chlorophenoxycarboxylic acid. The above-mentioned processes all have the problems of a lot of waste water and waste salt, difficult recovery of catalysts, high treatment costs, and great pressure on environmental protection, which serious...

Claims

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Application Information

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IPC IPC(8): C07C51/09C07C59/70A01N39/04A01P13/00
Inventor 孙国庆侯永生张国中迟志龙胡义山
Owner SHANDONG RUNBO BIOTECH CO LTD
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