Abstract: A high efficiency process for producing hydroxy-diphosphonic acid derivatives of higher carboxylic acids comprising a first step of mixing a tri-valent phosphorous compound with the higher carboxylic acid in a molar ratio in the range of 13:12 to 18:12, and subsequently heating the reaction mixture to a temperature of 80.degree. to 110.degree. C. for about 3 to 20 hours.In one embodiment, a subsequent solvolysis step is employed wherein the product resulting from the heating step is heated with a solvent having a hydroxyl function.