Abstract: The present invention discloses a preparation method of a polycarboxylate superplasticizer with carbon dioxide, comprising the following steps: (1) preparing a polycarboxylate superplasticizer prepolymer: performing an oxidation-reduction radical polymerization of an unsaturated macromonomer, an unsaturated phenol derivative, a reducing agent, an initiator and a chain transfer agent with different proportions under a nitrogen atmosphere to obtain a novel polycarboxylate superplasticizer prepolymer with different molecular weight; adjusting the pH by adding an alkali; (2) preparing a polycarboxylate superplasticizer: performing a Koble-Schmitt reaction between the polycarboxylate superplasticizer prepolymer and a carbon dioxide for a certain time to obtain the polycarboxylate superplasticizer.