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A kind of catalytic process of producing 2-nitro-4-thiamphenicol benzoic acid

A technology of methylsulfonyl benzoic acid and methylsulfonyl toluene is applied in the field of catalytic technology for producing 2-nitro-4-methylsulfonyl benzoic acid, and can solve the problems of low conversion rate, unsuitability for industrialized production, limited oxidizing ability, etc. question

Active Publication Date: 2016-08-24
SINOCHEM AGRO +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this type of method does not consume expensive chemical oxidants, does not produce waste gas and liquid, and is beneficial to environmental protection, it still has limited oxidation capacity and low conversion rate, and is not suitable for industrial production.

Method used

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  • A kind of catalytic process of producing 2-nitro-4-thiamphenicol benzoic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] The coconut shell gac of 15g is soaked in the phosphomolybdovanadic acid (H 6 PMo 9 V 3 o 40 ) solution, heated to reflux for 6 hours, filtered, washed with hot water until neutral, drained, dried at 110°C for 4 hours, and then activated at 280°C for 8 hours under nitrogen protection to obtain a loading capacity of 10%. (mass) H 6 PMo 9 V 3 o 40 / C Catalyst.

[0075] The experiment was carried out in a stirred reactor with a volume of 1000ml, 800ml of glacial acetic acid, 80g of water, 80g of 2-nitro-4-thiamphenicol toluene were added, and the H 6 PMo 9 V 3 o 40 / C catalyst 10g, manganese sulfate 6.5g, potassium iodide 0.5g, reaction temperature 200 ℃, pressure 25 atmospheres, air flow rate is 1L / min, after the reaction starts, take liquid samples every 0.5 hours and use liquid chromatography to analyze, react for 3 hours Finally, the conversion rate of 2-nitro-4-thiamphenicol toluene reached 92%, and the yield of 2-nitro-4-thiamphenicol benzoic acid reached ...

Embodiment 2

[0079] The preparation method of activated carbon-supported heteropolyacid catalyst is as in Example 1.

[0080]The experiment was carried out in a fixed-bed reactor with a height of 80 cm and an inner diameter of 3 cm, which contained 10-20 meshes of activated carbon-supported heteropolyacid catalysts. The gas-liquid two-phase flowed through the reactor from bottom to top, and the flow rate of the liquid was 5ml / min. The flow rate of air 500ml / min, in liquid feed, 2-nitro-4-thiamphenicol toluene 10% (weight), water 10% (weight), manganese 0.10% (weight), iodine 0.03% (weight), All the other is acetic acid, 210 ℃ of reaction temperature, pressure 25atm, liquid chromatographic analysis of reactor outlet liquid, 2-nitro-4-thiamphenicol toluene transformation rate reaches 81%, 2-nitro-4-thiamphenicol benzene The yield of formic acid reaches 80%.

Embodiment 3

[0082] 15g of coal-based activated carbon was immersed in 20% phosphotungstic acid (H 3 PW 12 o 40 ) solution, heated to reflux for 4 hours, filtered, washed with hot water until neutral, drained, dried at 110°C for 5 hours, and then activated at 300°C for 7 hours under nitrogen protection to obtain a loading capacity of 15%. (mass) H 3 PW 12 o 40 / C Catalyst.

[0083] The experiment was carried out in a stirred reactor with a volume of 1000ml, 800ml of glacial acetic acid, 80g of water, 80g of 2-nitro-4-thiamphenicol toluene were added, and the H 3 PW 12 o 40 / C catalyst 12g, cobalt acetate 1g, manganese acetate 2g, tetrabromoethane 0.4g, reaction temperature 210 ℃, pressure 30atm, air flow 1L / min, after the reaction starts, take liquid samples every 0.5h and use liquid chromatography to analyze, After reacting for 3 hours, the conversion rate of 2-nitro-4-thiamphenicol toluene reached 93%, and the yield of 2-nitro-4-thiamphenicol benzoic acid reached 92%.

[0084] T...

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Abstract

The invention relates to a method for producing 2-nitro-4-methylsulfonylbenzoic acid by adopting 2-nitro-4-methylsulfonyl methylbenzene. The method for producing the 2-nitro-4-methylsulfonylbenzoic acid comprises the steps of oxidizing 2-nitro-4-methylsulfonyl methylbenzene serving as a raw material into 2-nitro-4-methylsulfonylbenzoic acid in a gas-liquid-solid three-phase reaction system which is formed in a reactor at 4-70 atmospheric pressure at the temperature of 100-450 DEG C based on air (oxygen-rich air or oxygen) as an oxidant and aliphatic carboxylic acid as a solvent. The method for producing 2-nitro-4-methylsulfonylbenzoic acid can overcomes the defects of the existing 2-nitro-4-methylsulfonylbenzoic acid production method that massive waste gas and waste water are produced, corrosion is serious, selectivity is low and production cost is high, the selectivity is improved, pollution to the environment is reduced, and clean production of 2-nitro-4-methylsulfonylbenzoic acid is realized.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a catalytic process for producing 2-nitro-4-thiamphenicol benzoic acid. Background technique [0002] Mesotrione is a triketone herbicide developed by Zeneca Agrochemical Company. It is a special herbicide for corn fields. It has a wide herbicidal spectrum, high activity, strong miscibility, low toxicity, and is environmentally friendly. The following crops are safe and flexible to use. 2-nitro-4-thiamphenicol benzoic acid is an important intermediate in the synthesis of mesotrione, 2-nitro-4-thiamphenicol benzoic acid (NMSBA) is also known as o-nitro-p-thiamphenicol benzene Formic acid, 2-nitro-4-thiamphenicol benzoic acid or 4-thiamphenicol-2-nitrobenzoic acid, the English name is 2-Nitro-4-methylsulfonylbenzoic acid or O-Nitro-P-Methylsulfonyl Benzoic Acid. Molecular formula is C 8 h 7 NO 6 S, with a molecular weight of 245.21, is a white or light yellow crys...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C317/44C07C315/04B01J31/16
Inventor 龙湘犁李兆强杨春河李超杨志林程春生魏振云
Owner SINOCHEM AGRO
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