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Novel preparation method of insensitive explosive TATB

A new type of explosive technology, which is applied in the field of new preparation of insensitive explosive TATB, can solve the problems of expensive raw materials, harsh step conditions, and high overall cost, and achieve the effect of mature synthesis process, simple synthesis route, and reduced economic cost

Active Publication Date: 2020-11-27
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Abstract
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  • Claims
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AI Technical Summary

Problems solved by technology

Method (3) uses 4-nitroaniline as a raw material, first introduces nitro groups at the 2 and 4 sites, and then uses 2,4,6-trinitroaniline as an important intermediate, with the help of 4-amino-1, 2-triazole completes the C-amination reaction. However, in the last step of the reaction, the price of 4-amino-1,2-triazole used is very high. The reaction requires dimethyl sulfoxide as a solvent and sodium methoxide (CH 3 ONa) to maintain a strong alkaline environment, overall, the overall cost of the process is higher than other options
[0005] The synthetic schemes related to TATB mainly have three common defects: (1) the price of raw materials used is quite expensive, so that the economic cost of existing synthetic routes remains high, and it is urgent to find cheaper alternative synthetic routes; (2) each route There are some problems of harsh conditions in some steps, and the difficulty of implementation is relatively high, which leads to the extremely high difficulty of large-scale production of ATB; (3) in the existing synthetic route, the conversion rate of some steps is low, and many by-products remain in the final product , reducing the quality of the final product
[0006] Considering that the synthesis of TATB is relatively difficult at present, and many deficiencies in the synthesis route, a technical problem that needs to be urgently solved by those skilled in the art is: to provide a simple, efficient, safe, low-pollution and low-cost method to prepare TATB

Method used

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  • Novel preparation method of insensitive explosive TATB
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  • Novel preparation method of insensitive explosive TATB

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Step 1: Preparation of 2,4,6-triacetamidotoluene.

[0059] The reduction reaction and the in-situ acylation reaction are combined in the same system: take 2,4,6-trinitrotoluene I (TNT, 3.4g, 0.015mol, 1eq) and dissolve it in ethyl acetate (30ml) / acetic anhydride ( 25ml, 0.25mol, 17eq) in the mixed solution, obtain TNT solution, drop into Pd / C catalyst (5wt%, 0.3g), transfer in the high-pressure stirred reactor, vacuumize the high-pressure stirred reactor, fill with nitrogen, repeat Finally, vacuumize to ensure that there is no air residue, and continue to feed hydrogen for high-pressure (0.6MPa) reduction reaction and in-situ N-acetylation reaction at room temperature. The reaction lasts for 4 hours. After the reaction, a deep red solution and Pd / C Catalyst, the post-treatment steps are: after filtering out the Pd / C catalyst (the specific process is: first filter the reaction solution after the reaction, then wash the filter residue with 70°C preheated absolute ethanol ...

Embodiment 2

[0098] Step 1: Preparation of 2,4,6-triacetamidotoluene.

[0099]The reduction reaction and the in-situ acylation reaction are carried out in two systems: take 2,4,6-trinitrotoluene I (TNT, 6.8g, 0.03mol, 1eq) and dissolve it in methanol (50ml) to obtain a TNT solution, and put it into Pd / C catalyst (5wt%, 0.5g), transferred to the high-pressure stirred reactor, vacuumize the high-pressure stirred reactor, fill with nitrogen, repeat several times, finally vacuumize to ensure that there is no air residue, fill with hydrogen to make the pressure gauge display When the pressure reaches 0.8MPa, carry out the high-pressure hydrogenation reaction at room temperature. During the period, when the reading on the pressure gauge drops to 0.2MPa, the reaction is temporarily stopped, and the hydrogen gas is introduced to make the pressure rise to 0.8MPa. The aeration operation is repeated 4 to 5 times in total. Continued for 3 hours, after the end of the reaction, a reddish-brown solution ...

Embodiment 3

[0112] Step 1: Preparation of 2,4,6-triacetamidotoluene.

[0113] Dissolve 2,4,6-trinitrotoluene (TNT, 3.4g, 0.015mol, 1eq) in acetonitrile (25ml) to obtain a TNT solution, put into Pd / C catalyst (5wt%, 0.5g), transfer to 250ml round bottom In the flask, use a hydrogen balloon to supplement hydrogen to carry out a hydrogenation reaction under normal pressure (0.1MPa) at room temperature. The reaction lasts for 12 hours. After the reaction, a reddish-brown solution (ie 2,4,6-triaminotoluene) and Pd / C Catalyst, after filtering out the Pd / C catalyst, add acetic anhydride (10ml, 0.1mol, 6.5eq) dropwise into the solution, the reaction time is 0.5h, the reaction temperature is 25°C, a lot of white solids are precipitated, and white solids are obtained by filtration The powdery solid was washed with ethyl acetate for 3-5 times, and dried in a vacuum oven at 60°C to obtain 2,4,6-triacetamidotoluene (5.2 g, yield 65.7%).

[0114] In the embodiment of the present invention 3, the proto...

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Abstract

The invention provides a novel preparation method of an insensitive explosive TATB. The method comprises the following steps: 1, with 2,4,6-trinitrotoluene as a raw material, subjecting 2,4,6-trinitrotoluene to reacting with hydrogen and acetic anhydride in sequence to obtain 2,4,6-triacetylaminotoluene; 2, subjecting the obtained 2,4,6-triacetylaminotoluene o oxidation and a decarboxylation reaction to obtain 1,3,5-triacetylaminobenzene; and 3, carrying out nitrification and hydrolysis reactions on the obtained 1,3,5-triacetylaminobenzene to obtain 2,4,6-trinitro-1,3,5-triaminobenzene. According to the invention, the raw material used in the preparation method is the cheap 2,4,6-trinitrotoluene, and used reactants or catalysts are commonly used products in the chemical industry, so the preparation method has characteristics of low cost and usage of simple and easily available raw materials. In addition, the preparation method also has the characteristics of short synthesis steps, simple operation of each step, high yield, high reaction rate, easy separation and collection of intermediate and final products and the like, and is beneficial for realization of mass production of TATB.

Description

technical field [0001] The invention relates to the fields of chemical industry and materials, and mainly relates to a novel preparation method of an insensitive explosive TATB. Background technique [0002] 1,3,5-Triamino-2,4,6-trinitrobenzene (TATB) is an insensitive explosive, which is a bright yellow powdery solid at room temperature. TATB is a powerful explosive, slightly stronger than RDX, far stronger than the common explosive 2,4,6-trinitrotoluene (TNT). Although it has excellent explosive performance, TATB is extremely insensitive to vibration, flame and impact, and has good thermal stability and impact stability. According to observations, TATB can exist stably for a long time at an extremely high temperature of at least 250°C . The insensitive nature of TATB makes it the preferred explosive for safe application under extreme conditions. TATB is an insensitive high explosive (IHS) approved by the US Department of Energy and is widely used in nuclear bombs and pol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/50C07C211/52
CPCC07C209/50C07C231/02C07C231/12C07C233/43C07C211/52
Inventor 黄木华罗贤升邓汉林贾琼付浩熹彭山青柴春鹏
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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