Using water separation technique,acrylic acid (AA) and polyethylene glycol (PEG) 1000,of which the ratio was 1.5,were esterified and the optimum esterification ratio of 90% could be reached under the condition of 110 ℃×3 h.Using polyoxyethylene acrylate macro-monomer (PA) prepared in the esterification,AA and sodium methylacryl sulfonate (MAS) as monomers,a copolymer which could be used as superplasticizer was prepared by free radical co-polymerization in n(PA):n(AA):n(MAS) of 1:7:3.When the synthesis condition was 80 ℃× 5 h,the optimal dosage of initiator was 3.0%-4.0%,the fluidity of cement paste with the samples could reach 270 mm.By analyzing the effect of the content of residual small molecule sulfonic monomer on the properties of sample,n(MAS)/n(PA) was controlled in a range of 2.5-3.8.