Study On Synthesis Technogy Of TATB Without Chlorine And Its Application

TATB is a kind of commonly used single-compound insensitive explosives with the excellent performance.Now,the traditional method for preparing TATB is the route from sym-trichlorobenzene,by which chlorine impurities is indispensable with products,that has a bad influence on the thermal stability of the products,molding and strength of explosive column,metal projectile,et al.In recent years,in order to solve the problem of chlorine impurities,the new synthetic routes by using chlorine-free raw materials instead of sym-trichlorobenzene have become a hot research topic.In this thesis,recent reviews aiming at the developments of large batch for the manufacture of TATB are summerized,and the process route and enlarge effects of 1,3,5-triamino-2,4,6-trinitrobenzene with chlorine-free were discussed for solving problems of the high sensitivity of intermediates and the use of high pressure reaction equipment in the technological process and products in chlorine and so on.Preparation technology of TATB with laboratory scale was studied,by using phloroglucinol as raw material,through low temperature nitrification with mixed acid,alkylation with triethoxymethane and catalytic amination reaction,and the total yield is higher than 80%.Moreover,choosing 18-crown-6 ether as the phase transfer catalyst and ammonia liquor as the aminating agent,the atmospheric amination reaction with the yield of 96%was studied,which is matching the high-pressure amination reaction.Further more,via the studying of the apparent kinetics of the atmospheric amination reaction,the pseudo first order reaction kinetics model was established,and the apparent activation energy(Ea)was obtained with 12.312 kJ mol-1 by rate constants under different temperature.So,the extraction mechanism was got.On the basis of laboratory scale research,the amplification effect was studied by expanding the scale of loading of phloroglucinol from 2.52 g to 100 g,500g and 10kg,and finally the reaction conditions for a batch with 10kg TATB was made.The study shows that changing of nitration material liquid ratio can effectively eliminate the amplification effect during the enlarge from small experiment to 1 kg scale,and the amplification effect is almost 1 during the enlarge from 1 kg scale to 10 kg scale with the total yield of 82%and the purity of 98%.Then the material balance in the process was calculated.In order to effectively reduce the orientation degree of TATB crystal in the process of compression moulding,so as to improve the problem of the anisotropy of TATB based PBX expansion and poor stability,nearly spherical granular TATB was prepared by adding the modifier and seeds in the recrystallization.Determination of particle size distribution by laser particle size instrument(LPS)and observing of microstructure by scanning electron micr oscopy(SEM),so that TATB crystal with the average particle size obout 20μm and the shape of spheroidization was proved.TATB/HMX coating explosive was prepared by solvent evaporation method with estane-5703 as binder.TATB/HMX coating explosive prepared under the optimum process conditions was characterized by scanning electron microscopy,X-ray diffraction spectroscopy and X-ray photoelectron spectroscopy,and the result showed that the compact TATB/HMX coating explosive was got and the crystal phase with no change.And sensitivity test showed that impact sensitivity and friction sensitivity of TATB/HMX composites decreased to 0%.