GB822887A - Calcium trimethylolphenate - Google Patents

Abstract

The invention comprises calcium 2 : 4 : 6-trimethylolphenate which may be prepared by reacting calcium phenate, substantially free of phenol, with a least a stoichiometric amount of formaldehyde at 20-70 DEG C. It is possible to prepare the calcium phenate in situ from phenol and calcium oxide or hydroxide and the preferred conditions are to heat a mixture containing at least 3 mols. of formaldehyde per mol. of phenol and not more than 2 mols. of phenol per mol. of calcium oxide or hydroxide at 25-55 DEG C. The product may be precipitated by adding to the reaction mixture a water-soluble solvent in which the product is insoluble such as methanol, ethanol, isopropanol, acetone, methyl ethyl ketone, ethylene glycol, diethylene glycol, ethylene glycol diethyl ether, p diethylene glycol diethyl ether, ethylene glycol dibutyl ether, dioxan, morpholine or alkylene polyamines. The reaction time may range from about 5 to 25 hours, depending on the temperature. The formaldehyde used may be in anhydrous form, in polymerized form e.g. paraldehyde or as an aqueous solution e.g. formalin, the presence of water is not found to be detrimental to the reaction although an excess may make difficult the recovery of the product. In Examples: (1) 1 mol. calcium oxide is added to a cooled mixture of 2 mols. phenol, 4 mols. 37% formalin and 3 mols. paraldehyde such that the temperature does not exceed 35 DEG C.; water is added and the solution allowed to stand for 16 hours at 25-30 DEG C.; it is poured into a 2 : 1 mixture of acetone and isopropanol and the precipitated product collected and dried; (2) a similar reaction is carried out on a larger scale using 10 mols. phenol, 30 mols. formaldehyde and 5 mols. calcium oxide; 2 : 4 : 6-trimethylolphenol and sodium 2 : 4 : 6-trimethylolphenate monohydrate are prepared from this product. Specification 822,886 and U.S.A. Specification 2,579,329 are referred to.