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A controlled cross—linking polymerization system comprising of inter- and intramolecular reactions was designed and soluble intramolecularly cross-linking macromolecule (ICM) was synthesized from polyvinyl butyral(PVB) and 4,4’-diphenylmethane diisocyanante(MDI). Transmission Electron Microscopy (TEM) photographs show a special structure and chain propagation process of ICM. Pre-ICM, the globule with a well-defined and stable shape, is formed in the early stage of the polymerization, and then Pre-ICMs connect each other to form ICMs.