Fmc Corporation

Joseph H Finley

John H Blumbergs

Burton M Baum

Gaylen R Brubaker

Hsiang P Liao

Clifford A Erickson

Fui-Tseng H Lee

Charles V Juelke

Richard R Severns

Robert M Zakotnik

Jared S Sproul

Lewis L Hammermeister

Michael J McCarthy

Fred Richard Scholer

Richard E Hall

Charles W Lutz

Michael L Pinsky

Harry M Smith

Monte L Uhrig

Norman C Parsons

Terry W Willis

John M Polkowski

Unreacted phosphorus and heavy metals, such as arsenic and antimony, are removed in environmentally acceptable form from the non-aqueous still bottoms residue resulting from the production of PCl.sub.3, by reacting the residue with an excess of calcium hydroxide in the form of an aqueous lime slurry and separating the reaction product into a precipitate and a filtrate. The reaction with lime slurry may be preceded by hydrolysis with water. The precipitate passes the Toxicity Characteristic Leaching Procedure (TCLP) test and the filtrate contains less than 5 ppm of the heavy metals, thus permitting disposal by landfill and sewering, respectively, under EPA regulations.

Process for removing phosphorus and heavy metals from phosphorus

Compacted shapes of phosphatic material, suitable as a charge for a phosphorus furnace, are produced by compacting a mixture of calcined phosphate fines and phosphoric acid. The compacted shapes are conveniently produced on a roll briquetting press.

Phosphate feed material for phosphorus electric furnaces and production

Nodule fines, formed by abrasion of an electric furnace feed material of phosphate shale nodules, are utilized by mixing a recycle stream of the nodule fines with fresh phosphate in the presence of phosphoric acid prior to forming the shale into nodules. The phosphoric acid prevents loss in mechanical strength of the nodule caused by admixture with the nodule fines.

Phosphate feed material for phosphorus electric furnace

Phosphorus values in the raffinate from wet acid purification and nodule fines from an electric phosphorus furnace are recovered as elemental phosphorus by forming briquettes with a bed of the raffinate and nodule fines, curing the briquettes and feeding the cured briquettes plus the requisite coke and silica fluxing agent into an electric phosphorus furnace.

Utilization of phosphourus containing by-products

Formcoke is produced by introducing feedstocks of calcined coal particles, bituminous binder, an aqueous carbohydrate and phosphoric acid into a mixing zone. The resulting mixture is compacted into shapes, such as briquettes, which are then cured in an oxygen-containing atmosphere and optionally heated to coking temperatures.

Formcoke having modified bituminous binder

Formcoke is produced by separately introducing feedstocks of calcined coal particles, bituminous binder and a carbohydrate, preferably an aqueous sugar, into a mixing zone. The resulting mixture is compacted into shapes, such as briquettes, which are then cured in an oxygen-containing atmosphere and optionally heated to coking temperatures.

A mixed phenyl/mesityl phosphate ester composition that is useful as a fire retardant additive, having a phosphorus content of from about 8.2% to about 8.4% is prepared by reacting with agitation at about 120.degree. C. to 130.degree. C. distilled still bottom phenols with phosphorus oxychloride in the presence of a Friedel-Crafts catalyst to form a reaction product containing a substantial quantity of monoaryl phosphodichloridate and diaryl phosphochloridate. This reaction product is then further reacted at an elevated temperature with sufficient phenol to form a triaryl phosphate ester mixture. The mixed phenyl/mesityl phosphate ester so obtained remains a liquid at room temperature over a substantial period of time.

Mixed phenyl/mesityl phosphate ester composition

Mixed phosphoric acid ester compositions containing less than 4 weight percent of a triaryl phosphate, from about 10 to about 20 weight percent of an aryl dialkyl phosphate and from about 65 to about 80 weight percent of an alkyl diaryl phosphate are prepared by heating a monohydric alcohol or alkoxy alcohol with a triaryl phosphate, such as triphenyl phosphate, in the presence of a catalytic amount of an alkali metal phenoxide, for example, potassium phenoxide. The mixed phosphoric acid ester composition may be separated from by-products of the reaction by distillation.

Process for the manufacture of alkyl diaryl phosphate esters

Mixed phosphoric acid ester compositions containing less than 4 weight percent of a triaryl phosphate, from about 10 to about 20 weight percent of an aryl dialkyl phosphate and from about 65 to about 80 weight percent of an alkyl diaryl phosphate are prepared by heating a monohydric alcohol with aqueous sodium hydroxide to form the sodium alkoxide, distilling off the water as an alcohol azeotrope and reacting the alcohol sodium alkoxide with a triphenyl phenol. The mixed phosphoric acid ester composition may be separated from by-products of the reaction by distillation.

Process for the manufacture of mixed phosphoric acid ester compositions

Mixed phosphoric acid ester compositions containing by weight less than 4% of a triaryl phosphate; from about 30% to about 35% of an aryl dialkoxyalkyl phosphate and from about 60% to about 65% of an alkoxyalkyl diaryl phosphate are prepared by heating an alkoxy alcohol with aqueous sodium hydroxide to form the sodium alkoxide, distilling off the water as an alkoxy alcohol azeotrope and reacting the alkoxy alcohol sodium alkoxide with a triphenyl phenol. The mixed phosphoric acid ester composition may be separated from by-products of the reaction by distillation.

A process for the production of alkoxyalkyl triorganic phosphates utilizing a continuous process for the manufacture of alkoxyalkyl alkoxides comprising treating an alkoxyalkanol with a sodium borohydride for 20 minutes to 4 hours reacting the treated alkoxyalkanol continuously with an alkali metal hydroxide to form an alkali metal alkoxide. A large excess of alcohol is employed. The alkoxide is phosphorylated to form a trialkoxyalkyl phosphate. The alkoxidation reaction and the phosphorylation reaction are both conducted in a non-oxidizing atmosphere. The crude product is then refined by conventional means.

Production of alkoxyalkyl phosphate esters

Allylic esters of tetrachlorophthalic acid are formed using allylic alcohol both as a reactant and a solvent. In the first step, the alcohol and a base are reacted with tetrachlorophthalic anhydride to form the half-ester sodium salt. In the second step, the sodium salt is reacted with allylic halide to form the diester which crystallizes from solution. The excess solvent may be treated to recover the raw materials or recycled.

Process for making allylic esters of tetrachlorophthalic acid

Allylic esters of tetrabromophthalic acid are formed using allylic alcohol both as a reactant and a solvent. In the first step, the alcohol and a base are reacted with tetrabromophthalic anhydride to form the half-ester sodium salt. In the second step, the half-ester sodium salt is reacted with allylic halide to form the diester which crystallizes from solution. The excess solvent may be treated to recover the raw materials or recycled.

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Metuchen, NJ, United States of America

Joseph H Finley