Abstract:mono-trimethylolpropane trimaleates(TMPTM) and methacrylic acid(MAA) were employed to produce linear-hyperbranched block copolymers. Reactivity ratios of monomers indicated block copolymerization occured between TMPTM and MAA and produced linear-hyperbranched block copolymers, the indication was then confirmed by NMR, law of lg[η]-lgMw and branching factor g’. Furthermore, DSC revealed the Tg of LHBP is 209.98℃, TGA showed two-stage degradation occurred during heating-up from 50℃ to 600℃,first stage at 206.38℃(decarboxylization) and second at 429.57℃(backbone degradation).