Abstract: In order to develop green production process for chlorine dioxide and glyoxylic acid.A new technology that chlorine dioxide and glyoxylic acid were produced simultaneously in sulfuric acid by reducing chloric acid with glyoxal was creatively designed and tested.Yields of chlorine dioxide and glyoxylic acid were 85.6% and 78.6% respectively,under the optimized process conditions as follows:n(chloric acid)∶n(glyoxal)∶n(sulfuric acid)=2.5∶1∶1,reaction temperature was 45 ℃,reaction pressure was -0.07 MPa,and reaction time was 8 h.New technology has good process security and stability,non-polluting and could greatly reduce the production cost of chlorine dioxide and glyoxylic acid.