Poly(2-methoxy-5-(2′-ethylhexyloxy)- p -phenylenevinylene) (MEH-PPV) has been prepared by a liquid/solid two-phase reaction.The liquid phase is tetrahydrofuran containing 1,4-bis(chloromethyl)-2-methoxyl-5-(2′-ethylhexyloxy) benzene as the monomer and a certain amount of tetrabutylammonium bromide (TBAB) as phase transfer catalyst (PTC).The solid phase is potassium hydroxide particles with diameters smaller than 0 5 mm.Gelation was found in the polymerization processes.As a result,MEH-PPV is partly soluble because of its large molar mass.Soluble MEH-PPV was obtained by using bromomethylbenzene as retardant regent.The molar mass of soluble MEH-PPV was measured to be 6 4×10 4g/mol.The Structure of polymer was identified by IR,Raman,UV/vis and PL spectra.A thin compact film of MEH-PPV can be formed by spin-coating and it emit a yellow light.