Method for preparing 2, 4-dinitrochlorobenzene by green nitrification technology

A technology of dinitrochlorobenzene and p-chloronitrobenzene is applied in nitrification technology and 2 fields, can solve the problems of high water consumption and energy consumption, difficult process control, slow reaction speed and the like, and achieves low price, simple operation, high purity effect

Inactive Publication Date: 2017-09-05
WUHAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, domestically, chlorobenzene is mainly used as raw material and nitric acid mixed acid as nitrating agent to prepare 2,4-dinitrochlorobenzene. This method has the disadvantages of high water consumption and energy consumption, slow reaction speed, difficult process control, waste acid Disadvantages such as difficult to deal with

Method used

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  • Method for preparing 2, 4-dinitrochlorobenzene by green nitrification technology
  • Method for preparing 2, 4-dinitrochlorobenzene by green nitrification technology

Examples

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example 1

[0016] Prepare 0.1 g / ml of nitrogen pentoxide / nitric acid (1 gram of nitrogen pentoxide, 10 milliliters of nitric acid) solution in a 100 ml three-necked flask, slowly add 5 grams of p-chloronitrobenzene that have been weighed into the flask, After the addition was complete, the temperature of the water bath was raised to 40°C to start the reaction. Within 100 minutes of the reaction, first take a sample every 5 minutes, take 5 samples, then take a sample every 10 minutes, take 5 samples, and take 10 samples in total. The sample was pipetted for 0.1 minutes of the reaction solution, then 10 ml of ice water was added to terminate the reaction and 10 ml of dichloromethane was used as the extraction agent, neutralized with sodium bicarbonate solution, after separation, 1 ml was added to the organic phase The prepared toluene solution was used as an internal standard, and the concentration of p-chloronitrobenzene in the organic phase was quantitatively analyzed by chromatography u...

example 2

[0018] Prepare 0.1 g / ml of nitrogen pentoxide / nitric acid (1 gram of nitrogen pentoxide, 10 milliliters of nitric acid) solution in a 100 ml three-necked flask, slowly add 5 grams of p-chloronitrobenzene that have been weighed into the flask, After the addition, react at 20°C, 30°C, 40°C, 50°C, and 60°C for 80 minutes respectively, and finally use the internal standard curve method for chromatographic quantitative analysis of the amount of the product in the organic phase.

example 3

[0020] Prepare 0.1 g / ml, 0.2 g / ml, 0.3 g / ml, 0.4 g / ml, 0.6 g / ml, 0.8 g / ml of dinitrogen pentoxide / nitric acid solution (10 ml of nitric acid) in a 100 ml three-necked flask In the flask, 5 grams of p-chloronitrobenzene that had been weighed were slowly added into the flask. After the addition, they were reacted at 50° C. for 80 minutes, and finally the internal standard curve method was used for chromatographic quantitative analysis of the amount of the product in the organic phase.

[0021] By above 3 examples, draw nitrogen pentoxide / nitric acid nitration p-nitrochlorobenzene to prepare 2, the optimum reaction condition of 4-dinitrochlorobenzene is: when p-chloronitrobenzene is 5 grams, the reaction time For 70 minutes, the reaction temperature was 50°C, and the nitrogen pentoxide concentration was g / ml (3 grams of nitrogen pentoxide, 10 milliliters of nitric acid). At this moment, the productive rate of 2,4-dinitrochlorobenzene was 96.73%. , 100% pure.

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Abstract

The invention discloses a method for preparing 2, 4-dinitrochlorobenzene by green nitrification technology. Nitrogen pentoxide/nitric acid serves as a nitrification system, and parachloronitrobenzene serves as a raw material to prepare the 2, 4-dinitrochlorobenzene. When 5 grams of parachloronitrobenzene is used, reaction time is 70 minutes, reaction temperature is 50 DEG C, the concentration of the nitrogen pentoxide is 0.3 gram per milliliter (3 grams of nitrogen pentoxide and 10 milliliters of nitric acid), the yield of the 2, 4-dinitrochlorobenzene is 96.73%, and the purity of the 2, 4-dinitrochlorobenzene is 100%.

Description

technical field [0001] The invention relates to the technical fields of nitration technology and 2,4-dinitrochlorobenzene preparation, more specifically, the invention relates to a green nitration technology for preparing 2,4-dinitrochlorobenzene. Background technique [0002] Nitrification is a common organic unit reaction. At present, the widely used nitrating agents include nitric sulfur mixed acid, nitrate ester, metal nitrate and so on. The atomic economy of these processes is not high, and a large amount of waste acid and organic acid wastewater will be generated during the production process, resulting in serious environmental pollution. The preparation of 2,4-dinitrochlorobenzene is a curved nitration reaction. [0003] 2,4-Dinitrochlorobenzene is a light yellow crystal with a bitter almond flavor, insoluble in water, slightly soluble in organic solvents such as ethanol and benzene, and is an important fine chemical intermediate used in the synthesis of dyes, Raw ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/08C07C205/12
CPCC07C201/08C07C205/12
Inventor 胡衍甜严莉吕早生
Owner WUHAN UNIV OF SCI & TECH
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