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Method for producing civil dinitrotoluene

A dinitrotoluene and preparation technology technology, applied in the field of organic chemistry, can solve the problems of difficulty in controlling the isomerization ratio of dinitrotoluene products, increase the difficulty of waste acid treatment, and low product quality, and achieve maximum implementation value and Socioeconomic benefit, low production cost, and low nitrate content

Inactive Publication Date: 2008-08-20
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Like this, caused the sulfuric acid consumption to be big, and produced a large amount of waste acid that contains sulfuric acid concentration lower, strengthened the difficulty of waste acid treatment, produced a large amount of waste water, caused serious pollution to environment; The requirement of temperature is relatively harsh, the dinitrotoluene product isomerization ratio of production is difficult to control, and product quality is not high, and productive rate is generally not also high (yield rate is 85~90%)

Method used

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  • Method for producing civil dinitrotoluene

Examples

Experimental program
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Effect test

Embodiment 1

[0021] One-stage nitration: add 4mL of carbon tetrachloride and 4mL of toluene in turn into a 100mL pear-shaped flask, raise the temperature to 50°C and slowly add 1.8mL of fuming nitric acid dropwise, and react for 20min.

[0022] Two-stage nitration: Slowly add 7mL of concentrated sulfuric acid (concentration: 98%) dropwise, add 2.4mL of fuming nitric acid dropwise after heating up to 65°C, and continue stirring for 60min.

[0023] Post-reaction treatment: after the reaction, let stand to separate the layers, then separate the organic phase while it is hot, distill off the solvent carbon tetrachloride to precipitate the product DNT; Chloromethane precipitates the product DNT. The combined product DNT was first washed with a sodium carbonate solution of about 2.5% DNT mass until the pH value was 7-8, then washed 2 to 3 times with an appropriate amount of water, pre-dried at room temperature for one day, then vacuum-dried to constant weight, weighed and Take an appropriate am...

Embodiment 2

[0025] One stage nitration: Add 8mL of carbon tetrachloride and 4mL of toluene into a 100mL pear-shaped flask in sequence, and slowly add 1.8mL of fuming nitric acid and 7mL of concentrated sulfuric acid (concentration 98.2%) dropwise after heating up to 30°C. React for 30 minutes.

[0026] Two-stage nitration: After heating up to 65°C, add 2.4mL of fuming nitric acid dropwise, and continue stirring for 60min.

[0027] Post-reaction treatment: After the reaction is over, let stand to separate layers, then separate the organic phase while it is hot, and distill the organic phase to remove the solvent carbon tetrachloride to precipitate the product DNT; The solvent chloroform precipitates the product DNT. The combined product DNT was first washed with a sodium carbonate solution of about 3% DNT mass until the pH value was 7-8, then washed 2 to 3 times with an appropriate amount of water, pre-dried at room temperature for one day, then vacuum-dried to constant weight, weighed an...

Embodiment 3

[0029] One-stage nitration: add 8mL of carbon tetrachloride and 4mL of toluene into a 100mL pear-shaped flask in sequence, raise the temperature to 50°C and slowly add 1.8mL of fuming nitric acid dropwise, and react for 10min.

[0030] Two-stage nitration: Slowly add 7mL of concentrated sulfuric acid (98.2%) dropwise, after heating up to 65°C, add 2.4mL of fuming nitric acid dropwise, and continue stirring for 90min.

[0031] Post-reaction treatment: after the reaction, let stand to separate the layers, then separate the organic phase while it is hot, distill off the solvent carbon tetrachloride to precipitate the product DNT; Chloromethane precipitates the product DNT. The combined product DNT was first washed with 3.5% sodium carbonate solution of DNT mass until the pH value was 7-8, then washed 2 to 3 times with an appropriate amount of water, pre-dried at room temperature for one day, then vacuum-dried to constant weight, weighed and taken Appropriate amount of DNT for ga...

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Abstract

The invention provides a new technique for synthesized civil (DNT) with good quality, which regards toluene and nitric acid as raw materials, concentrated sulfuric acid as catalyst, and carbon tetrachloride with low boiling point as solvents; in certain conditions, the DNT is produced directly, the yield of the products can reach 96.4 percent, the purity is above 98 percent, and the quality of the products satisfies the first-rate standards, 2,4-DNT / 2,6-DNT is equal to 80 plus or minus 1 / 20 plus or minus 1, as organic solvent is introduced, little influence of temperature is caused towards the isomer ratio of products in reaction, and the conditions of nitration reaction are mild, the ratio of isomer produced is easy to be controlled, the density of waste liquid is high, and nitrate containing amount is low, which is beneficial for the concentration of waste liquid and the reduce of emission of waste water, primary nitrification and secondary nitrification are both carried on in the same reaction kettle, the technique is simple, the production cost is low, the requirement of environmental protection is satisfied, so the new technique for synthesized civil DNT with good quality has rather great implementary value and social economic benefits.

Description

technical field [0001] The invention belongs to the field of organic chemistry and relates to a preparation process of dinitrotoluene, in particular to a preparation process of civil standard dinitrotoluene (DNT). Background technique [0002] Toluene is a heavy tonnage product of the petrochemical industry with low price and abundant sources. The development of its downstream products has always been valued by the chemical and chemical industry. Through deep processing of toluene, many valuable chemical products can be produced, such as oxidation to produce benzyl alcohol, benzoic acid, chlorination to produce benzyl chloride, sulfonation to produce toluenesulfonic acid, nitration to produce 2-nitrotoluene, 3-nitrotoluene A series of important pharmaceutical intermediates such as methyl toluene and p-nitrotoluene can increase its added value many times and have considerable economic benefits. [0003] Among the downstream products of toluene, dinitrotoluene (DNT) is an imp...

Claims

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Application Information

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IPC IPC(8): C07C205/06C07C201/08
Inventor 魏太保陈靖张治仁冷艳丽张有明
Owner NORTHWEST NORMAL UNIVERSITY
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