Method for preparing 2,4-D choline amine salt

A choline and water preparation technology, which is applied in the preparation of 2,4-D amine salts and the preparation of herbicides, can solve the problems of easy crystallization, increased packaging and transportation costs, etc., and achieves low volatility and reduced packaging. and transportation costs, the effect of increasing usability

Active Publication Date: 2011-09-14
SHANDONG WEIFANG RAINBOW CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although 2,4-D amine saline solution is an environmentally friendly dosage form, high-concentration water formulations are prone to crystallization. Although low-concentration water formulations do not crystallize, it increases the cost of packaging and transportation. affect its use to a certain extent
However, as far as we know, there are no reports about the preparation method of 2,4-D choline solution and the original drug.

Method used

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  • Method for preparing 2,4-D choline amine salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 100.0g choline aqueous solution (50% choline content), 95.1g 2,4-D original drug (96% content), and 135.8g water into a 1L reactor equipped with a stirring, cooling and vacuum distillation device. To make it react, control the pH value of the reaction system at 8.0~10.0, heat is released during the reaction, the reaction temperature quickly rises to 50℃, continue to stir and react at a constant temperature of 50~55℃ for 45min, you can get 720g / L 2, 4-D Choline Water Agent.

Embodiment 2-6

[0022] Prepare the 2,4-D choline aqueous solution according to the operation steps in Example 1, and other conditions remain unchanged, the choline content used, the 2,4-D addition amount, the water addition amount, the pH value of the reaction system, the reaction time and The temperature is shown in Table 1 below.

[0023]

Embodiment 7

[0025] The 2,4-D choline aqueous solution obtained in Example 1 was placed in a 1L reactor equipped with a stirring, cooling and reduced-pressure distillation device for concentration. The reactor was heated by a water bath heating method and the reactor was pumped. Vacuum to make the relative pressure -0.01MPa, the reaction liquid starts to boil when the temperature of the water bath is 50 ℃, for better concentration, continue to increase the temperature of the water bath, and keep it at 70 ~ 85 ℃ for concentration, until the distillation When the mass of the effluent is 49.6g, the vacuum is stopped and the temperature begins to drop. When the temperature drops to 18.0℃, add 0.017g of 2,4-D choline nucleus, then crystals will be precipitated soon, continue to lower the temperature under stirring, stirring for 10min, stop cooling when the temperature drops to -5℃ , And subjected to suction filtration to obtain 133.8g wet product of 2,4-D choline, 147.5g mother liquor, after dry...

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Abstract

The invention discloses a method for preparing 2,4-D choline aqueous solution, which comprises the following step of: reacting choline aqueous solution with a 2,4-D technical in an alkaline environment by using water as a medium to obtain the 2,4-D choline aqueous solution, wherein the reaction temperature is between 50 and 60 DEG C. The 2,4-D choline aqueous solution and a 2,4-D choline technical can be prepared by the method. The obtained 2,4-D choline is environment-friendly, has high stability, low volatility, light peculiar smell and a wider application range, is difficult to crystallizeand easy to operate and mix, hardly diffuses and drifts, and is a good substitute of a 2,4-D salt herbicide. The preparation process is simple, wastewater is not generated, distillate and mother liquid can be recycled for preparing the 2,4-D choline aqueous solution, and high environment friendliness is achieved.

Description

Technical field [0001] The invention relates to a method for preparing 2,4-D amine salt, in particular to a method for preparing 2,4-D amine salt using 2,4-D original medicine and choline as raw materials, and belongs to a method for preparing herbicides Technical field. Background technique [0002] 2,4-D belongs to the chlorinated phenoxyacetic acid herbicide and can also be used as a plant growth regulator. The pure product of 2,4-D is white crystals with very low solubility in water, and is easily soluble in organic solvents such as ethanol and benzene, but its sodium and ammonium salts are extremely soluble in water. The main dosage form of 2,4-D is its ester emulsifiable concentrate and its amine salt aqueous solution. Due to the greater impact of emulsifiable concentrates on the environment, the proportion of this formulation in pesticide formulations is decreasing year by year. Although 2,4-D amine salt water is an environmentally friendly formulation, high-concentrati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C219/06C07C213/02C07C213/10A01N39/04A01P13/00
Inventor 孙国庆侯永生姚红霞邹宗加
Owner SHANDONG WEIFANG RAINBOW CHEM
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