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Method for preparing TNT (Trinitrotoluene) by taking nitrotoluene as raw material through one-step method

A technology of nitrotoluene and o-nitrotoluene, applied in the field of one-step preparation of TNT, which can solve the problems of factory equipment corrosion, unstable operation, oxidation side reactions, etc., and achieve the effect of reducing environmental pollution

Inactive Publication Date: 2018-10-26
ZHONGBEI UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With the continuous progress of society, the shortcomings of production technology widely used in industry have become increasingly prominent, mainly as follows: produce asymmetric TNT (2,4,5-, 2,3,4-, 2,3,6-, 2,3,5- and 3,4,5-trinitrotoluene), while also producing large amounts of pollutants such as nitrogen oxides (NO x ) and tetranitromethane (TNM), for example, using traditional manufacturing methods, every 100 kg of TNT produced will produce 0.5% TNM, these pollutants need to be removed to prevent them from damaging the environment and causing harm to the environment; strong acid Extensive use has caused serious harm to the environment, and it has been unable to meet the sustainable development of the environment and economy; in industrial production, it has caused serious corrosion to factory equipment; the rapid heat release in the reaction process has caused unstable operation, and it is easy to produce Explosions and other safety accidents occur during the process; when the nitric acid is excessive, oxidation side reactions are prone to occur, resulting in the decomposition of explosives and a decrease in yield; there is no nitrification regioselectivity, a large amount of unnecessary organic isomers are produced, resulting in a large waste of resources; a large amount of waste Acid emissions, raising disposal costs

Method used

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  • Method for preparing TNT (Trinitrotoluene) by taking nitrotoluene as raw material through one-step method
  • Method for preparing TNT (Trinitrotoluene) by taking nitrotoluene as raw material through one-step method
  • Method for preparing TNT (Trinitrotoluene) by taking nitrotoluene as raw material through one-step method

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Experimental program
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Effect test

Embodiment 1

[0045] Embodiment 1: the method for synthesizing TNT by one-step method

[0046]This embodiment has investigated the influence of reaction time on TNT yield:

[0047] Take 0.05 mol of p-nitrotoluene, 0.15 mol of nitric acid, and 0.5 mol of sulfuric acid, and the reaction temperature is 120°C. The reaction time is 3h, 4h, 5h, 6h, 7h, 8h respectively. The effect of reaction time on the product is shown in Table 1. As can be seen from Table 1, the yield of the product TNT increases first and then remains unchanged with the prolongation of time, and it is the best when the reaction is 4h.

[0048] The influence of table 1 reaction time on TNT yield

[0049]

[0050] Optimization of reaction time: take 0.05mol of p-nitrotoluene, HNO 3 :H 2 SO 4 =3:10, 0.15mol of nitric acid, 0.5mol of sulfuric acid, the reaction temperature is 120 degrees. The reaction time is 3h, 4h, 5h, 6h, 7h, 8h respectively. The product in 3h was a mixture (the reaction was not completed), and the o...

Embodiment 2

[0051] Embodiment 2: the method for synthesizing TNT by one-step method

[0052] This embodiment has investigated the influence of temperature of reaction on TNT yield

[0053] Take 0.05mol of p-nitrotoluene, HNO 3 :H 2 SO 4 =1:3.5, 0.15mol of nitric acid, 0.5mol of sulfuric acid, the reaction time is 4h. The reaction temperatures were 100°C, 110°C, 120°C, 130°C, and 140°C, respectively.

[0054] The influence of reaction temperature on product TNT is as follows figure 1 . Depend on figure 1 It can be seen that the product yield first increases and then decreases, and the product yield is the highest at 110 °C.

[0055] Optimization of reaction temperature: take 0.05mol of p-nitrotoluene, HNO 3 :H 2 SO 4 =1:3.5, 0.15mol of nitric acid, 0.5mol of sulfuric acid, the reaction time is 4h. The reaction temperatures were 100°C, 110°C, 120°C, 130°C, and 140°C, respectively. The yields were 90.8%, 92.2%, 89%, 89%, and 86%, respectively.

Embodiment 3

[0056] Embodiment 3: the method for one-step synthetic TNT

[0057] This embodiment has investigated the influence of nitric acid and the concentrated sulfuric acid mol ratio on TNT yield

[0058] Take 0.05mol of o-nitrotoluene, the reaction time is 4h, and the reaction temperature is 110°C. The ratio (molar ratio) of nitric acid to sulfuric acid is 1:2.5, 1:3, 1:3.5, 1:4 respectively. Product yield n(NA): n(SA) changes as figure 2 shown. from figure 2 It can be seen that the yield of the target product first increases and then decreases with the increase of concentrated sulfuric acid, and reaches the maximum when n(NA):n(SA)=1:3.5.

[0059] The optimization of the mixed acid ratio of nitric acid and sulfur in the reaction: take 0.05 mol of o-nitrotoluene, the reaction time is 4 hours, and the reaction temperature is 110 degrees. The ratio of nitric acid to sulfuric acid is 1:2.5, 1:3, 1:3.5, 1:4 respectively. The yields were 87%, 89%, 92.2%, and 89%, respectively.

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Abstract

The invention discloses a method for preparing TNT (Trinitrotoluene) by taking nitrotoluene as a raw material through a one-step method. According to the method disclosed by the invention, p-nitrotoluene or o-nitrotoluene is used as the raw material and a mixed system of fuming HNO3 / concentrated H2SO4 is used as a nitrating agent, and 2,4,6-trinitrotoluene TNT is prepared through one-step nitrification reaction; the 2,4,6-trinitrotoluene TNT is subjected to structure characterization by adopting a melting point, thin-layer chromatography, mass spectrometry and liquid chromatography. Influences, caused by a ratio, a feeding manner and a dosage of the mixed system of the fuming HNO3 / concentrated H2SO4, to the yield of a product are explored and reaction conditions are optimized. The TNT is synthesized by taking the nitrotoluene as the raw material through one-step nitrification, so that environment pollution caused by the fact that a lot of waste acid and red water are generated is avoided, and energy source and power consumption caused by reaction steps and nitrification equipment are reduced.

Description

technical field [0001] The invention relates to a method for preparing TNT by using nitrotoluene as a raw material in one-step method, belonging to the technical field of explosive preparation. Background technique [0002] 2,4,6-Trinitrotoluene (TNT) is a high explosive first synthesized in 1863. It is produced in large quantities by nitration of toluene with nitric acid mixed acid. At present, most of the TNT produced at home and abroad use toluene as raw material, and carry out three-stage nitration process with nitric-sulfur mixed acid, using nine nitration machines, that is, toluene is nitrated into mononitrotoluene (MNT) in one-stage nitration, and one-stage nitration Nitrotoluene includes: o-nitrotoluene, p-nitrotoluene and m-nitrotoluene; MNT is nitrated into dinitrotoluene (DNT) in the second-stage nitration; DNT is nitrated into trinitrotoluene (TNT) in the third-stage nitration ). In a nutshell, toluene is mixed with fuming nitric acid and concentrated sulfuric...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/08C07C205/06
CPCC07C201/08C07C205/06
Inventor 李永祥王景奇陈军王建龙柴笑笑李敏方克雄曹端林赵林秀陈丽珍
Owner ZHONGBEI UNIV
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