Aqua-mesophase　pitch　(AMP)　was　prepared　from　the　oxidation　of　medium　coal　tar　pitch　with　a　mixture　of　concentrated　sulfuric　acid　and　nitric　acid,　and　then　pitch-based　carbon　nanospheres　were　prepared　by　using　carbon　sol-gel　method　in　water-in-oil　emulsion　formed　by　silicone　and　AMP.　AMP,　carbon　primary　powders　and　carbon　nanospheres　were　characterized　by　FT-IR,　TG,　TEM　and　X-ray　diffraction　analysis.　The　results　show　that　nitration,　oxidation　and　sulfonation　reaction　happen　during　the　preparation　of　AMP.　Nitro,　hydroxyl,　carboxyl　and　sulfonic　functional　groups　are　removed　during　the　carbonizing　process　of　carbon　nanospheres　preparation.　Water　removal,　functional　groups　decomposition　and　carbon　skeleton　rearrangement　are　main　three　stages　during　carbon　primary　powders　pyrolysis.　The　diameter　of　most　carbon　nanospheres　which　presented　disorganized　layer　graphite　structure　is　about　50　nm.　Moreover　the　sphericity　and　d002of　nanospheres　are　95.9%　and　0.348　0　nm,　respectively.