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filingDate 1972-03-23-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationDate 1975-11-19-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber GB-1414478-A
titleOfInvention Phosphorylation of alkylated phenols
abstract 1414478 Phosphorylation of alkylated phenols ALBRIGHT & WILSON Ltd 22 March 1973 [23 March 1972] 13668/72 Heading C2P [Also in Division C5] Triaryl phosphate mixtures, triaryl phosphite mixtures and triaryl dichlorophosphoranetrioate mixtures are prepared by: (1) reacting a phosphorylating agent (e.g. POCl 3 , POBr 3 , P 2 O 5 , H 3 PO 4 , PCl 3 , PCl 5 ) with a composition of phenols recycled from stage 4, optionally in the presence of an additional composition of phenols, the total molar proportion of phenols to atoms of phosphorus in the phosphorylating agent being less than 3 : 1; (2) reacting the product of stage 1 with a feedstock phenol composition obtained by alkylation (including cycloalkylation) of phenol or a mixture of phenols comprising a major molar proportion of phenols having less than three alkyl carbon atoms, with a C 3-16 alkylating agent, the amount of feedstock being such that the total molar ratio of phenols in stages 1 and 2 to phosphorus atoms is at least 3 : 1; (3) separating unreacted phenols from the obtained desired product mixture; and (4) recycling the unreacted phenols to stage 1. The process may be effected batchwise, continuously or semicontinuously at 15‹- 300‹ C. in the presence of a catalyst, e.g. AlCl 3 , MgCl 2 or an alkyl titanate. In the products, preferably 20-85 mole. per cent of the aryl moieties have one or more C 3-12 alkyl or cycloalkyl substituents, e.g. isopropyl, sec-butyl or cyclohexyl. When the product comprises triaryl phosphites or triaryl dichlorophosphoranetrioates, these may be converted to triaryl phosphates by oxidation or hydrolysis respectively. The optional additional phenol composition for stage 1 may be the same or different from the feedstock composition for stage 2. Specified components of these and of the recycle composition are: o-, m- and p-isopropylphenol; 2,3-, 2,4-, 2,5- and 2,6-diisopropyl-phenol and 2,4,6- triisopropylphenol. The separation of stage 3 may be effected by distillation whereafter the triaryl products may be purified by low-pressure distillation, treatment with aqueous alkali, and/or treatment with an oxidizing agent to remove oxidizable impurities.
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Total number of triples: 40.