Method of comprehensively use of chloronitrobenzene mixture by fluoro-reaction

A technology of monochloronitrobenzene and chloronitrobenzene, which is applied in the field of comprehensive utilization of o-, m-, and p-chloronitrobenzene mixtures, can solve the problems of many steps and poor utilization of resources, and achieve simple operation Effect

Active Publication Date: 2013-05-08
浙江省常山长盛化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN101289396 discloses a method for separating and utilizing mixed components of o-, m-, and p-nitrochlorobenzene. The method adopts a three-step reaction: (1) chlorination, (2) fluorination, (3) chlorination, so that the components Realized separation, and obtained the product with high added value, its shortcoming is that there are many steps, and the m-nitrochlorobenzene of high added value can't be fully separated, only as general monochloronitrobenzene is used, uses resources are not well utilized

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 158 grams (1 mole) of a chloronitrobenzene mixture, 15.8 grams of catalyst tetrabutylammonium bromide, and 157 grams (2.7 moles) of anhydrous potassium fluoride into the reaction flask, heat to 200 ° C, react for 5 hours, and filter Solids such as potassium chloride were removed, and 63.5 grams of p-fluoronitrobenzene and 12.7 grams of o-fluoronitrobenzene were separated through rectification in a rectification tower, with a total yield of 90%. The residue was recrystallized from toluene to obtain 60 g of m-chloronitrobenzene with a recovery rate of 95% and a purity of ≥99.5%.

Embodiment 2

[0021] Add 158 grams (1 mole) of a chloronitrobenzene mixture, 1.58 grams of catalyst tetrabutylammonium bromide, and 157 grams (2.7 moles) of anhydrous potassium fluoride into the reaction flask, heat to 150 ° C, react for 15 hours, and filter Solids such as potassium chloride were removed, and 65 grams of p-fluoronitrobenzene and 13 grams of o-fluoronitrobenzene were separated through rectification in a rectification tower, with a total yield of 92%. The residue was recrystallized from toluene to obtain 60 g of m-chloronitrobenzene with a recovery rate of 95% and a purity of ≥99.5%.

Embodiment 3

[0023] Add 158 grams (1 mole) of a chloronitrobenzene mixture, 158 grams of catalyst calix[6]arene, and 476 grams (8.2 moles) of anhydrous potassium fluoride into the reaction flask, heat to 150°C, react for 5 hours, and remove by filtration Potassium chloride and other solids were rectified by a rectification tower to separate 67 grams of p-fluoronitrobenzene and 13.4 grams of o-fluoronitrobenzene, with a total yield of 95%. The residue was recrystallized from toluene to obtain 60 g of m-chloronitrobenzene with a recovery rate of 95% and a purity of ≥99.5%.

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Abstract

The invention discloses a method of comprehensively use of chloronitrobenzene mixture by fluoro-reaction, comprising steps of: generating a mixture mainly composed of parachloronitrobenzene, o-chloronitrobenzene and m-chloronitrobenzene in process of parachloronitrobenzene, o-chloronitrobenzene by chlorobenzene nitration method; removing low-boiling-point substances by evaporation; then adding anhydrous potassium fluoride and catalyst to the mixture for fluoro-reaction at 150 DEG. C to 250 DEG. C; after reaction, filtering to remove potassium chloride, after rectifying to acquire parachloronitrobenzene, o-chloronitrobenzene, the residual portion via recrystallization acquires m-chloronitrobenzene; the catalyst is quaternary ammonium salt or calixarene; charge rate of chloronitrobenzene mixture and mixture is 1:0.01 to 1. The method of the invention is simple to operate, in scale and changes waste material into things of value, which realizes zero discharge. The method is characterizedin sustainable development, energy saving, consumption reduction and environmentally friendly property.

Description

(1) Technical field [0001] The invention relates to a method for comprehensively utilizing the mixture of o-, m- and p-chloronitrobenzene by utilizing fluorination reaction. (2) Background technology [0002] In the production of p-chloronitrobenzene and o-chloronitrobenzene by the nitration of monochlorobenzene in China, a large amount of mixture is produced, and its main components are about 40% of m-chloronitrobenzene, about 50% of p-chloronitrobenzene, and o-chloronitrobenzene. Nitrobenzene about 10%. In order to meet the requirements of environmental protection and achieve the purpose of energy saving and emission reduction, how to rationally utilize these industrial production residues of p- and o-nitrochlorobenzene to separate and produce high value-added downstream products is a technical issue worth studying. CN101289396 discloses a method for separating and utilizing mixed components of o-, m-, and p-nitrochlorobenzene. The method adopts a three-step reaction: (1)...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C205/12C07C201/12B01J31/02
Inventor 周智慧陈生荣沈志良裴文
Owner 浙江省常山长盛化工有限公司
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