A new technology for the production of highly concentrated aqueous formaldehyde was developed by oxidizing methylal. Whereas the oxidation of methanol yields 1 mol of water per 1 mol of formaldehyde, methylal oxidation produces only 1 mol of water for every 3 mol of formaldehyde. Thus, the output from methylal oxidation is more than 70% formaldehyde compared with 55% from methanol oxidation. For this purpose, basic research for methylal synthesis was tried and the world's first commercial production of methylal was accomplished. Using this methylal, the world's first technology of methylal oxidation for manufacturing highly concentrated aqueous formaldehyde was established by development of a new methylal oxidation catalyst composed of iron, molybdenum, and a third component. This highly concentrated aqueous formaldehyde is then fed to the acetal homopolymer and copolymer plant whose combined capacity is 35,000 tons/years. © 1993 John Wiley & Sons, Inc.