Occidental Chemical Corporation

Hooker Chemicals & Plastics Corporation

Harry E Buckholtz

Arun C Bose

David Y Tang

Mary K Cocoman

Tilak V Bommaraju

Mohan Singh Saran

George T Miller

Karl W Seper

Joseph S Wisnouskas

John C Graham

Joseph J Moritz

Mohamed W Hisham

Edward J Colman

David A Flautt

Frederick C Leitert

Disclosed is a process for producing phosphorous trichloride, phosphorous pentachloride, or phosphorous tribromide by reacting phosphine gas with chlorine gas or bromine gas, in a mixture with hydrogen gas. The phosphine is dried and the reaction is performed at a temperature up to about 250&deg; C. The phosphorous trichloride or phosphorous tribromide product can be reacted with oxygen to form phosphorous oxychloride or phosphorous oxybromide, respectively.

Process for making phosphorus halides and oxyhalides

Disclosed is a method of making an alkali metal alcoholate by performing the reaction ##STR1## where M is sodium or potassium, ROH is methanol, ethanol, propanol, or butanol, and D.C. is direct current. The process can be used to make sodium methylate in a modified Hybinette cell having a separator in between a cathode compartment and an anode compartment. The cell is filled with methanol and a solution of sodium chloride in methanol is added to the cathode compartment. When direct current is passed between the cathode and the anode, a solution of sodium methylate in methanol collects in the anode compartment. The solution of sodium methylate can be continuously removed and cooled to separate any sodium chloride in it which can be recycled back to the cathode compartment. Alternatively, the sodium chloride can be added to the anode compartment while an inert salt is added to the cathode compartment. The process can also be performed in a three-compartment cell.

Method of making alkali metal alcoholates

Disclosed is a method of making phosphorous acid or hypophosphorous acid by reacting hydrogen chloride with a sodium phosphite or a sodium hypophosphite, respectively, in the presence of water to precipitate sodium chloride crystals and form the acid. The acid is separated from the sodium chloride crystals and can be passed through an anion exchange column that is preferably loaded with phosphite or hypophosphite ions, respectively, to remove residual chloride ions.

Zero discharge process for manufacturing of phosphorous acid and

Halophthalic anhydrides are prepared by the liquid phase reaction of a brominating agent with halogen substituted hexa- or tetra-hydrophthalic anhydrides.

Process for the preparation of halophthalic anhydrides

A process for the preparation of a halophthalic anhydride, such as chlorophthalic anhydride, comprising the liquid phase reaction of bromine with a halogen substituted hexa- or tetra-hydrophthalic anhydride to produce halophthalic anhydride and gaseous HBr, and reacting the gaseous HBr with chlorine to regenerate bromine.

Disclosed is a method of making a eutectic mixture of copper and tricopper phosphide by reacting elemental copper with phosphine. The elemental copper is heated to a temperature above about 714.degree. C. and the liquid eutectic mixture runs off of the cooper as it is formed, exposing more copper for reaction. The liquid eutectic mixture can be used as a source of copper and phosphorus in making metal alloys.

Method of making eutectic mixture of copper and tricopper phosphide

Disclosed is a method of making hexametaphosphates by reacting sodium tripolyphosphate, tetrasodium pyrophosphate, or trisodium phosphate with phosphoric acid, forming a molten glass of said mixture, and chilling said molten glass to form a solid.

Production of hexametaphosphates from other phosphates

Disclosed is a method of preventing fluids in the ground from rising around an oil well pipe by filling the space around the pipe with an oil well completion fluid comprising water, about 50 to about 65% by weight, based on total fluid weight, of dipotassium phosphate, and at least about 10 ppm hexavalent chromium. The fluid can be prepared by neutralizing wet process phosphoric acid with potassium hydroxide to a pH of less than 12 and filtering off any solids. Also disclosed is an oil well employing the completion fluid.

Oil well and method using completion fluid

Disclosed is a method of making potassium tripolyphosphate by loading an ion exchange resin with either potassium or hydrogen ions and passing an aqueous solution of sodium tripolyphosphate through the resin so that the sodium ions of the sodium tripolyphosphate are exchanged with the ions loaded onto the resin, forming either potassium tripolyphosphate or tripolyphosphoric acid, respectively. The tripolyphosphoric acid is reacted with potassium hydroxide to form potassium tripolyphosphate. When the ion exchange resin becomes exhausted it is regenerated using a potassium-containing ionic solution, forming a sodium ion containing stream. The sodium ion containing stream is reacted with a phosphoric acid to form a stream of sodium phosphates.

Zero discharge process for preparing potassium tripolyphosphate

The process disclosed in this invention takes the waste solids, gases, and water from a phosphorus pentasulfide manufacturing facility and hydrolyzes the phosphorus pentasulfide by heating. The phosphorus portion is converted to a soluble phosphate and the sulfur portion to a mixture of sulfide, sulfite and sulfate. The soluble fraction is then treated with a calcium hydroxide solution precipitating the phosphate and sulfates which are removed. The gaseous portion of the hydrolysis is fed to a catalytic oxidizer which converts the sulfides to sulfur, which is removed and the gas, free of sulfur containing species, is exhausted to the atmosphere. The filtrate from the precipitation reaction can be recycled to the plant, or may be chlorinated and discharged.

Phosphorus pentasulfide waste water treatment

Thianthrene compounds are prepared by adding sulfur monochloride to an excess of a benzene compound in the presence of aluminum chloride, and reacting to form a thianthrene compound as an insoluble aluminum chloride complex; slurrying the complex in an inert organic liquid; treating the slurry with a Lewis base, such as ammonia to free the thianthrene compound from the complex.

Process for the manufacture of substituted thianthrene based products

In the process for the nuclear chlorination of alkylbenzenes, such as toluene, in the presence of a para-directing catalyst system comprising a substantially iron-free Lewis acid catalyst and thianthrene compound co-catalyst, wherein the reaction mixture is in contact with iron or an alloy thereof, the para-directing effect of the catalyst system is improved by the addition of an amide.

Process for the chlorination of toluene

Thianthrene is prepared by adding sulfur monochloride to an excess of benzene in the presence of aluminum chloride, and reacting at a temperature of 60.degree. to 80.degree. C to form thianthrene as an insoluble thianthrene-aluminum chloride complex; separating the complex by filtration, slurrying the complex in an inert organic liquid; treating the slurry with a Lewis base, such as ammonia to free the thianthrene from the complex and recovering a relatively high purity thianthrene product.

Process for the manufacture of thianthrene

Thianthrene in monochlorotoluene, is reacted with excess chlorine in the presence of a Lewis acid catalyst, to yield a mixture of chlorothianthrenes, the major component of which is 2,3,7,8-tetrachlorothianthrene. Recrystallization of the chlorothianthrene mixture from a suitable solvent, such as tetrahydrofuran yields 2,3,7,8-tetrachlorothianthrene of greater than 90 percent purity.

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Lewiston, NY, United States of America

Harry E Buckholtz