关键词: 黑索今, 直接法, 合成, 吸附, 分离, 副产物

Abstract: In order to improve the preparation of RDX through nitrolysis of hexamethylenetetramine by concentrated nitric acid，the byproducts in wastewater after nitrolysis were studied. The byproducts were first absorbed through reticular macroporous resin GDX-102，and then eluted by a mixture of methyl chloride and acetonitrile with a （molar or volume） ratio of 90：10. Last，the byproducts were concentrated and separated in thin layer chromatography （TLC），the developing solvent of which was acetone/methylene chloride/petroleum ether with a （molar or volume） ratio of 1∶3∶6. IR，NMR，MS，and elemental analysis were used to characterize the products obtained，which were recognized as 1,3,5-trinitro-1,3,5-triazapentane and 1,5-dinitro-acyloxy-2,4-dinitro-2,4-azapentane. The nitrolysis reaction of hexamethylenetetramine by concentrated nitric acid was extremely complicated and so many byproducts were produced in this process. The results indicated that nitric acid first transformed hexamethylenetetramine into its dinitrate. The intermediate products of DPT and the precursor of RDX was then formed by rapid nitration of dinitrate，and the main product RDX and little HMX were generated gradually. With the proceeding of reaction and increasing system oxidability，ring compounds were destroyed and broke into straight-chain compounds，such as 1,3,5-trinitro-1,3,5-triazapentane and 1,5-dinitro-acyloxy-2,4-dinitro-2,4- azapentane .

Key words: RDX, direct method, synthesis, adsorption, separation, byproduct