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Herbicide dimethylamine salt and preparation method thereof

A technology of dimethylamine salt and herbicide, which is applied in the field of herbicide dimethylamine salt and its preparation, can solve the problems of difficult removal of water, unfriendly environment, long process time, etc. It is easy to control the end point of the reaction, The effect of convenient separation and purification and safe physical properties

Pending Publication Date: 2020-08-18
上海希康默化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, most of the phenoxycarboxylic acid herbicides and benzoic acid herbicides on the market are in the form of emulsifiable concentrate formulations, and the herbicides in the form of emulsifiable concentrates have a long residual time on plants, are easy to drift, are not friendly to the environment, and are used improperly. It will cause phytotoxicity, human and animal poisoning accidents and other disadvantages; compared with sodium salt, ammonium salt has a wider application temperature and high safety. The amine salt water and water-soluble granules of formic acid herbicides all belong to environment-friendly dosage forms, but the water can not be equipped with high-concentration dosage forms due to the influence of solubility; the U.S. patent describes a dry water-soluble salt composition and Its manufacturing method has high energy consumption requirements. In order to reduce the decomposition of salt products, complex equipment is required to remove water at low temperature; in the preparation method of 2,4-D amine salt and its water-soluble granules in the patent of Runfeng Chemical Both describe the use of water as a solvent, crystallization and centrifugation after dehydration under reduced pressure to prepare amine salts. This method uses direct dehydration under reduced pressure. Because the amine salts are unstable at high temperatures, it is difficult to remove water, and it is very difficult to filter. Now In the existing technology, the traditional method of direct heating, stirring and mixing, and natural water discharge under normal pressure is adopted. This process mode requires high heating temperature, long process time, and high energy consumption. Make certain components of the product volatilize and deteriorate; in the patent of Niufarm Co., Ltd. of Australia and the patent of Runfeng Chemical, anhydrous dimethylamine is used to form a salt in an organic solvent to make a soluble salt, but anhydrous dimethylamine is inconvenient to use , and the use of anhydrous dimethylamine is less safe than aqueous dimethylamine

Method used

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  • Herbicide dimethylamine salt and preparation method thereof
  • Herbicide dimethylamine salt and preparation method thereof
  • Herbicide dimethylamine salt and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Get the herbicide, place it in a four-necked flask equipped with a pH meter, add an organic solvent to dissolve it, drop the temperature to 30°C, add 40% dimethylamine solution dropwise, and keep the temperature for 1 hour after the dropwise addition. The holding temperature is 50°C, the pH value is controlled at 9, and the pH value is maintained for 1 hour;

[0025] (2) Use the reflux dehydration technology under negative pressure, control the vacuum degree at -0.086~-0.088MPa, raise the dehydration temperature to 55~60°C, until no water comes out, then lower the temperature to 45°C, precipitate crystals, stir for 1 hour, Then lower the temperature to 25° C., filter, collect the precipitate, and dry at 50° C. to obtain the dimethylamine salt.

[0026] The raw material adopted in the present embodiment comprises herbicide, dimethylamine aqueous solution and organic solvent; Herbicide is 2,4-dichlorophenoxyacetic acid, and organic solvent is toluene, and the mol rati...

Embodiment 2

[0028] (1) Get the herbicide, place it in a four-necked flask equipped with a pH meter, add an organic solvent to dissolve it, drop the temperature to 30°C, add 40% dimethylamine solution dropwise, and keep the temperature for 1 hour after the dropwise addition. The holding temperature is 50°C, the pH value is controlled at 9, and the pH value is maintained for 1 hour;

[0029] (2) Use the reflux dehydration technology under negative pressure, control the vacuum degree at -0.086~-0.088MPa, raise the dehydration temperature to 60°C until no water comes out, then cool down to 45°C, precipitate crystals, stir for 1 hour, and then cool down Centrifuge at 25°C, collect the precipitate, and dry at 50°C to obtain the dimethylamine salt.

[0030] The raw material adopted in the present embodiment comprises herbicide, dimethylamine aqueous solution and organic solvent; Herbicide is 2,4-dichlorophenoxypropionic acid, and organic solvent is toluene, and the mol ratio of herbicide and dim...

Embodiment 3

[0032] (1) Get the herbicide, place it in a four-necked flask equipped with a pH meter, add an organic solvent to dissolve it, drop the temperature to 30°C, add 40% dimethylamine solution dropwise, and keep the temperature for 1 hour after the dropwise addition. The holding temperature is 50°C, the pH value is controlled at 9, and the pH value is maintained for 1 hour;

[0033] (2) Use the reflux dehydration technology under negative pressure, control the vacuum degree at -0.086~0.088MPa, raise the dehydration temperature to 60°C until no water comes out, then cool down to 45°C, precipitate crystals, stir for 1 hour, and then cool down to Centrifuge at 25°C, collect the precipitate, and dry at 50°C to obtain the dimethylamine salt.

[0034] The raw materials adopted in this embodiment include herbicide, dimethylamine aqueous solution and organic solvent; : 1.07; The weight ratio of described herbicide and organic solvent is 1:3.

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Abstract

The invention discloses a herbicide dimethylamine salt and a preparation method thereof, the herbicide dimethylamine salt comprises at least one phenoxy carboxylic acid herbicide or benzoic acid herbicide in an organic solvent, a dimethylamine aqueous solution is dropwise added and reacts to form a salt, reflux dehydration is carried out under negative pressure, cooling amine salt is precipitatedin the solvent, and the dimethylamine salt is obtained by collecting a precipitate and drying the precipitate; wherein the dimethylamine salt is mainly prepared from the following raw materials: phenoxy carboxylic acid herbicides or benzoic acid herbicides, a dimethylamine aqueous solution and an organic solvent. Compared with the prior art, the solid amine salt is prepared from phenoxy carboxylicacid or benzoic acid herbicides and dimethylamine aqueous solution, and the method has the advantages that the process is simple, the yield is high, the solvent can be used indiscriminately, and theobtained amine salt is good in solubility in water and high in solution stability.

Description

technical field [0001] The invention relates to the technical field of pesticide herbicides, in particular to a herbicide dimethylamine salt and a preparation method thereof. Background technique [0002] At present, there are many kinds of herbicides on the market, and phenoxycarboxylic acid herbicides and benzoic acid herbicides have the advantages of low price, fast weeding speed, wide weeding spectrum, and no residue; they are widely used; in recent years, pesticides The mainstream direction of field research is high-efficiency, low-toxicity, low-residue pesticides and formulations. [0003] At present, most of the phenoxycarboxylic acid herbicides and benzoic acid herbicides on the market are in the form of emulsifiable concentrate formulations, and the herbicides in the form of emulsifiable concentrates have a long residual time on plants, are easy to drift, are not friendly to the environment, and are used improperly. It will cause phytotoxicity, human and animal poi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C51/42C07C51/43C07C59/70C07C59/68C07C59/64C07C209/00C07C209/86C07C211/04
CPCC07C51/412C07C51/42C07C51/43C07C59/70C07C59/68C07C59/64C07C209/00C07C209/86C07C211/04
Inventor 岳晟
Owner 上海希康默化工有限公司
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