绿色、安全、低成本、高质量制备氧化石墨烯（GO）是GO及石墨烯相关研究和应用的基础。本论文围绕电化学氧化法制备氧化石墨烯（EGO）展开了系统研究，目的是实现电化学法可控、宏量制备EGO，同时探究连续化和低成本的EGO工业化制备方案。本论文主要内容如下：（1）电化学插层-氧化两步设计能够显著提高EGO的氧化度，预插层处理对于电化学法高质量制备EGO必不可少。基于两步电化学法，我们提出了限制空间电化学氧化制备EGO工艺，通过保证插层石墨纸的结构完整性和氧化反应充分进行，限制空间制备能够提高EGO的氧化度（C/O = 2.38），达到化学氧化法制备的GO的同等氧化水平。通过对电化学参数和浸液速度的调整，可以实现EGO氧化度的有效控制。（2）限制空间电化学氧化制备工艺可应用于EGO的放大制备，实现了千克级别的EGO宏量制备，产率达到153%。基于此，我们推算出该工艺的产能为0.37 t/m2/y，建设百吨级EGO工业化生产线所需厂房仅千平方米。（3）插层-氧化两步电化学法中参与第二步氧化反应的石墨层间化合物不限于连续的插层石墨纸，通过对泥状插层石墨进行纸化塑型再电化学氧化，制备的EGO同样具有高氧化度（C/O = 2.68），达到了典型化学氧化法的水平，同时制备的EGO单层率达到了93.3%。通过对泥状插层石墨纸进行连续塑型及电化学氧化，可实现EGO的连续化制备。（4）鳞片石墨价格低廉，是最佳的GO工业化生产原料，采用非连续状的鳞片石墨作为EGO制备的石墨原料，通过电化学插层可以制备出1阶插层鳞片石墨，并在限制空间的条件下进行电化学氧化反应，制备的EGO具有较高的氧化度（C/O = 5.2）。基于电化学氧化泥状石墨层间化合物制备EGO的方案易实现EGO的连续化、低成本制备，对规模化生产EGO具有重要意义。

The green, safe, low cost and high quality preparation of graphene oxide (GO) is the basis of GO and its related research and applications. In this paper, a systematic study was conducted on the preparation of graphene oxide (EGO) by electrochemical method, with the purpose of realizing the controllable preparation of EGO and exploring the continuous and low-cost industrial fabrication scheme of EGO. The main contents of this thesis are as follows:(1) The two-step electrolysis design of intercalation and oxidation can significantly improve the oxidation degree of EGO, and pre-intercalation treatment is essential for high-quality electrochemical preparation of EGO. Based on this two-step electrochemical method, we further proposed the space-confined electrolysis process for EGO preparation. By ensuring the structural integrity of graphite intercalation compound paper (GICP) and sufficient oxidation reaction, the space-confined preparation can improve the oxidation degree (C/O = 2.38) of EGO and reach the same oxidation level as that by the chemical oxidation method. By adjusting the electrolytic parameters and leaching speed, the controllable preparation of EGO with different oxidation degrees can be achieved.(2) The space-confined electrolysis preparation technology can be applied to the mass fabrication of EGO. Through this process, we obtained the kilogram level of EGO, and the yield reached 153%. It is estimated that the production capacity of the space-confined electrolysis fabrication technology is 0.37 t/m2/y, and the industrial production of 100 tons of EGO can be realized with a workshop of 1,000 square meters.(3) The graphite interlayer compounds (GICs) participating in the second-step oxidation reaction in the two-step electrochemical method of intercalation and oxidation are not limited to the continuous GICpaper. Through the electrolytic oxidation of formed anode by shaping mud-like GICs the prepared EGO also has a high oxidation degree (C/O = 2.68), reaching the level of GO by typical chemical oxidation. At the same time, the mono-layer ratio of EGO was 93.3%. The continuous preparation of EGO can be realized easily by continuous electrolysis of the formed anode from mud GICs. (4) Flake graphite has low price and is the best raw material for GO industrial production. Discontinuous flake graphite was directly used as the raw material for EGO farbrication, and the first-order GICs can be prepared by electrochemical intercalation. Then EGO was prepared through the space-confined electrolytic oxidation reaction, and the EGO has a high oxidation degree (C/O = 5.2). This EGO fabrication process is of great significance for large-scale EGO production.