Oxidation intercalation is one of the mainstream methods to prepare graphene oxide (GO) monolayer/multilayer materials. The key steps are oxidation agent and intercalation agent selection and process matching. The traditional process maily uses Hummers method which has problems such as large amount of nitrogen oxide emissions, significant environmental hazards and poor safety. In this paper, the research progress of graphene oxide prepared by oxidation intercalation in recent years was reviewed. The green oxidantion agent, intercalation agent research progress and corresponding process improvement and innovation were emphatically expounded. The reaction mechanism and application effect of different agents were systematically analyzed, aiming to find a green, low-cost and more suitable preparation method for industrial production.