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A kind of bendazone decolorization and purification method

A purification method and technology of bentazon, applied in the field of fine chemical production technology, can solve problems such as instability of water preparations, and achieve great competitive advantages and good quality of original drugs and water preparations.

Active Publication Date: 2018-10-23
盐城联合伟业化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The product obtained by this method contains more impurities, the product is yellow or brown, and the content is less than 95%, and the prepared liquid is unstable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Taking isatoic anhydride as a raw material, first in the dichloroethane solvent system, go through reactions such as amide synthesis, sulfonation synthesis, and ring-closure synthesis, and then carry out the following steps:

[0030] The first step is to finish washing the organic phase after the closed-loop synthesis, prepare the organic phase into the extraction kettle and slowly add alkali to adjust pH=7~8, stop adding alkali, stir for half an hour and re-measure pH=7~8, stop stirring and let stand ;

[0031] The second step, treat the first step solution standing and stratification: the upper stratum caustic soda solution is transferred to the decolorizing still, and the bentazon content in the caustic soda solution is measured by sampling, and activated carbon is added according to the bentazon weight wherein the amount is the bentazone. 15% of the loose weight, then heat up to 80-90 ° C, and keep the temperature for 2 hours;

[0032] In the third step, the materi...

Embodiment 2

[0036] Taking isatoic anhydride as a raw material, first in the dichloroethane solvent system, go through reactions such as amide synthesis, sulfonation synthesis, and ring-closure synthesis, and then carry out the following steps:

[0037] The first step is to finish washing the organic phase after the closed-loop synthesis, prepare the organic phase into the extraction kettle and slowly add alkali to adjust pH=8 to 9, stop adding alkali, stir for half an hour and re-measure pH=8 to 9, stop stirring and let stand ;

[0038] The second step, treat the first step solution standing and stratification: the upper stratum caustic soda solution is transferred to the decolorizing still, and the bentazon content in the caustic soda solution is measured by sampling, and activated carbon is added according to the bentazon weight wherein the amount is the bentazone. 10% of the loose weight, then heat up to 70-80°C, and keep the temperature for 2 hours;

[0039] In the third step, the ma...

Embodiment 3

[0043] Taking isatoic anhydride as a raw material, first in the dichloroethane solvent system, go through reactions such as amide synthesis, sulfonation synthesis, and ring-closure synthesis, and then carry out the following steps:

[0044] The first step is to finish washing the organic phase after the closed-loop synthesis, prepare the organic phase into the extraction kettle and slowly add alkali to adjust pH=9~10, stop adding alkali, stir for half an hour and re-measure pH=9~10, stop stirring and let stand ;

[0045] The second step, treat the first step solution standing and stratification: the upper stratum caustic soda solution is transferred to the decolorizing still, and the bentazon content in the caustic soda solution is measured by sampling, and activated carbon is added according to the bentazon weight wherein the amount is the bentazone. 15% of the loose weight, then heat up to 80-90 ° C, and keep the temperature for 2 hours;

[0046] In the third step, the mate...

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PUM

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Abstract

The invention relates to a bentazone decolouring and purifying method. The method comprises the following steps: alkali extraction, including taking isatoic anhydride as a raw material, performing synthetic reactions, such as amidation, sulfonation and loop closure, in a dichloroethane solvent system, and carrying out washing and alkali addition for extraction to obtain an alkali-extracted liquid; decolouring, including, transferring the alkali-extracted liquid to a decolouring kettle, adding a certain amount of activated carbon according to the bentazone content, raising the temperature to 40-95 DEG C, and performing heat preservation for 1-5 h; filtration, including after the heat preservation is over, transferring the obtained material to a cooling kettle, performing fast stirring, leading brine in for cooling, performing plate filtration, allowing the obtained filtered liquid to pass an acidification kettle, and then blowing the plate to dry; acidification, including raising the temperature of the filtered liquid in the acidification kettle to 30-70 DEG C, slowly dropwise adding inorganic acid to the filtered liquid till the pH is less than 4, and allowing a great amount of bentazone to precipitate; and drying, including putting the precipitated material in a centrifugal machine for direct spin-drying, and then drying bentazone in a vacuum condition with the temperature in a range of 60-100 DEG C to obtain the final product. Through the method, a white bentazone primary drug is obtained.

Description

technical field [0001] The invention relates to the technical field of fine chemical production technology, in particular to a method for decolorizing and purifying bendazone. Background technique [0002] Bentazone is a widely used low-toxicity herbicide. Its mode of action and mechanism are mainly realized by sodium salt of bentazone: contact-killing selective post-emergence weed control, used for stem and leaf treatment at seedling stage, through leaf contact. kick in. When used in dry fields, it is first transmitted to the chloroplast through foliar infiltration to inhibit photosynthesis. Used in paddy fields, it can penetrate through the leaves and absorb through the roots, and transmit to the stems and leaves, which strongly hinders the photosynthesis and water metabolism of weeds, causing nutrient starvation, causing physiological dysfunction and death. The active ingredients are metabolized to weakly active glycoconjugates and detoxified in resistant crops, which a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D285/16
CPCC07D285/16
Inventor 张海飞陆红健
Owner 盐城联合伟业化工有限公司
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