The coupling reaction of formaldehyde (FA) and methyl formate (MF) with solid sodium bisulfate catalyst was investigated in an autoclave. The effects of reaction temperature，reactants ratio

catalyst dosage and reaction time on the yields of methyl glycolate (MG) and methyl methoxy acetate (MMAc) were examined. Under optimal reaction conditions：formaldehyde 1. 08 mol，methyl formate 1. 66 mol，sodium bisulfate 0. 24 mol， reaction temperature 160℃，reaction time 4 h，the overall yield of MG and MMAc was 42. 15％. The catalyst could be easily recovered and reused

and had very good activity and stability. The reaction process was confirmed and the performance of sodium bisulfate catalyst was also compared with other acid catalysts. The catalytic activity of sodium bisulfate catalyst was higher than others.