Preparation method of 2-nitro-4-methylsulfonylbenzoic acid

A technology of methylsulfonylbenzoic acid and methylsulfonyltoluene is applied in the field of preparation of 2-nitro-4-methylsulfonylbenzoic acid, and can solve the problems of small amount of three wastes, high production cost, large amount of three wastes and the like

Active Publication Date: 2020-10-23
JIANGSU FENGSHAN GROUP
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] The object of the present invention is to provide a kind of preparation method of 2-nitro-4-thiamphenicol benzoic acid, solve the three wastes amount that exists in the preparation technology of intermediate 2-nitro-4-thiamphenicol benzoic acid big, select In order to solve the problems of poor performance and high production cost, based on the nitric acid oxidation scheme, a green, environmentally friendly and safe preparation scheme was developed, which realized the mechanical application of waste acid and solvent in the two-step reaction. After repeated application, the waste acid produced can be The reduction is more than 90%, which improves the safety of the reaction, the process is safe and environmentally friendly, and the amount of three wastes is small, which is suitable for industrial production

Method used

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  • Preparation method of 2-nitro-4-methylsulfonylbenzoic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] 1) Nitrification reaction

[0045]First drop 1000kg of dichloromethane into the dissolution kettle, then drop into 170kg (1.0kmol) p-thiamphenicol toluene, stir, dissolve, and set aside; add 613kg (5kmol) of sulfuric acid with a mass fraction of 90wt% to the mixing acid kettle, and start the circulating water temperature control 20-30°C, slowly add 101.9kg (1.1kmol) of nitric acid dropwise, control the temperature at 20-50°C during the dropwise addition, and then cool down to 20-30°C for later use.

[0046] Simultaneously and continuously pump p-thiamphenyltoluene dichloromethane solution and sulfuric acid-nitric acid mixed acid solution into the tubular reactor, control the flow of the two solutions, keep the reaction temperature at 20-30°C, and receive the output material until nitration treatment Still, sampling detection p-thymphenyltoluene content is less than 0.5%, and the reaction ends.

[0047] The nitration treatment tank that receives the reaction discharge i...

Embodiment 2

[0057] 1) Nitrification reaction

[0058] First put 1600kg of dichloroethane into the dissolution kettle, then drop into 170kg (1.0kmol) p-thiamphenicol toluene, stir, dissolve, and set aside; add 871kg (8kmol) of sulfuric acid with a mass fraction of 90wt% to the mixed acid kettle, and open the circulating water control Temperature 10~20 ℃, slowly drop nitric acid 139kg (1.5kmol), control temperature 20~50 ℃ during dropwise, then cool down to 20~30 ℃ standby, the sulfuric acid that described mass fraction is 90wt% is the nitration treatment still. Apply sulfuric acid out.

[0059] Simultaneously and continuously pump p-thiamphenyltoluene dichloromethane solution and sulfuric acid-nitric acid mixed acid solution into the tubular reactor, control the flow of the two solutions, keep the reaction temperature at 10-20°C, and control the feed and output of the reactor. The material speed, the total material time is 2 hours, the output material is received into the nitration treatm...

Embodiment 3

[0069] 1) Nitrification reaction

[0070] First put 1200kg of chloroform into the dissolution kettle, then put in 170kg (1.0kmol) of p-thiamphenicol toluene, stir, dissolve, and set aside; add 80% sulfuric acid 735kg (6kmol) to the mixing acid kettle, and turn on the circulating water to control the temperature at 20-30°C , slowly add 92.6kg (1.0kmol) of nitric acid dropwise, control the temperature at 20-50°C during the dropwise addition, and then cool down to 20-30°C for later use;

[0071] Simultaneously and continuously pump p-thiamphenyltoluene dichloromethane solution and sulfuric acid-nitric acid mixed acid solution into the tubular reactor, control the flow of the two solutions, keep the reaction temperature at 20-30°C, and control the feed and output of the reactor. The material speed, the total material time is 3 hours, the output material is received into the nitration treatment tank, and when the content of p-thymphenyltoluene is less than 1%, the sample is qualifi...

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Abstract

The invention relates to a preparation method of 2-nitro-4-methylsulfonylbenzoic acid. Based on a nitric acid oxidation scheme, p-methylsulfonyltoluene is dissolved into a chloroalkane solvent, nitricacid is dropwise added into sulfuric acid with the mass fraction of 80-90wt%, a chloroalkane solution of p-methylsulfonyltoluene and a mixed acid solution are simultaneously and continuously added into a reaction system for a nitration reaction, the sulfuric acid is repeatedly used after the nitration reaction material liquid is treated, the sulfuric acid can be used both in the nitration reaction and the oxidation reaction, the sulfuric acid in the oxidation reaction can be repeatedly used, the total molar yield of the 2-nitro-4-methylsulfonylbenzoic acid can achieve more than 90%, and the content is more than 99%. By means of the method, the amount of waste acid in production of 2-nitro-4-methylsulfonylbenzoic acid can be reduced by 90% or above, the use amount of vanadium pentoxide isreduced by 90% or above, three wastes are greatly reduced, the process is safe and environmentally friendly, the amount of the three wastes is small, and the method is suitable for industrial large-scale production.

Description

technical field [0001] The invention belongs to the field of preparation of herbicide intermediates, in particular to a preparation method of 2-nitro-4-thiamphenicol benzoic acid. Background technique [0002] p-Hydroxyphenylpyruvate Dioxygenase (HPPD) is a key enzyme in the biosynthetic pathway of plastoquinone and tocopherol necessary for normal plant growth, and can catalyze the biochemical process from tyrosine to plastoquinone in plants , HPPD is currently one of the most important herbicide targets. [0003] Mesotrione can inhibit hydroxyphenylpyruvate dioxygenase (HPPD) and ultimately affect the biosynthesis of carotenoids. Absorbed by the root, and conduct to the top and base in the xylem and phloem, and distribute throughout the plant. The selectivity of mesoflurale stems from the difference in its metabolism in crops and weeds. In crops, it is metabolized as 4- Hydroxyl derivatives may also be absorbed by crops slower than weeds. After weeds are treated, the leav...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C315/04C07C317/14C07C317/44
CPCC07C315/04C07C317/14C07C317/44
Inventor 陈宝明韦自强孔禄张磊刘华珍姚金莉王海洋殷平殷凤山
Owner JIANGSU FENGSHAN GROUP
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