Polycarboxylate　superplasticizer　(PCE)　prepared　by　free　radical　copolymerization　of　different　monomers　in　aqueous　solution　has　the　advantages　of　high　efficiency,　stability　and　safety　and　convenience,　which　is　the　mainstream　process　of　PCE　production　at　present.　However,　the　problem　with　free　radical　copolymerization　is　that　the　composition　and　structure　of　the　synthesized　polymers　deviate　significantly　from　the　design　values.　Based　on　the　reactivity　rate　of　comonomers　obtained　from　the　experiment,　and　with　the　aim　of　preparing　PCE　copolymers　with　uniform　and　stable　composition,　this　paper　investigated　a　new　process　for　the　precise　control　of　monomer　conversion　rate　change　and　polymer　composition　during　copolymerization　by　combining　theoretical　calculations　and　experimental　measurements.　Gel　permeation　chromatography　(HPLC)　and　high　performance　liquid　chromatography　(HPLC)　were　used　to　study　and　compare　the　formation　process　and　structural　characteristics　of　PCE　copolymers　synthesized　by　precise　controlled　feeding　process　(CFP)　and　one-　time　feeding　process　(OFP)　and　continuous　dropping　process　(CDP),　including　the　molecular　weight　of　polymers,　distribution　of　monomer　sequence　structures,　and　conversion　rate　of　macromonomers.　The　results　show　that　the　composition　and　structure　of　PCE　copolymers　synthesized　by　OFP　and　CDP　fluctuate　greatly　with　the　polymerization　process,　which　deviate　from　the　target　design　values.　The　average　acid/ether　ratio　of　PCE　copolymers　synthesized　by　CFP　is　close　to　the　design　value　(4.0),　and　the　acid/ether　ratio　fluctuates　slightly　above　and　below　the　design　value　(2.70~4.77)　during　each　time　period.　The　performance　of　PCE　copolymers　synthesized　by　different　processes　shows　that　the　PCE　copolymers　prepared　by　CFP　have　better　dispersing　property　and　flow　retention　ability　at　the　same　raw　material　ratio.　©　2023　Sichuan　University.　All　rights　reserved.