Thiokol Corporation

Ventron Corporation

Robert C Wade

Lawrence J Guilbault

Nuno M Rei

Benjamin C Hui

Supported alkali metal borohydride reagents are prepared by contacting high surface area solid support material with a solution of alkali metal borohydride in an anhydrous aprotic solvent so as to form a coating and then removing the solvent to leave a residual coating that is predominantly composed of alkali metal borohydride on the surface of the support material. Supported reagents containing for example, greater than 10 wt. % of a thin alkali metal borohydride coating, based upon total weight coating and support material, are advantageously prepared by the procedure of the invention.

Preparation of supported alkali metal borohydride reagents

Alkali metal borohydride concentrates are prepared by dry blending alkali metal borohydride powder with a dry non-reactive plastic resin, melting and extruding the blended mixture to form an encapsulated alkali metal borohydride concentrate, and then chopping the extrusion into pellets. The pellet concentrate may then be blended into other materials.

Alkali metal borohydride concentrate

Alkali metal borohydride concentrates are prepared by dry blending alkali metal borohydride power with a dry non-reactive plastic resin, melting and extruding the blended mixture to form an encapsulated alkali metal borohydride concentrate, and then chopping the extrusion into pellets. The pellet concentrate may then be blended into other materials.

Quaternary ammonium hydroxides are prepared by the electrolysis of quaternary ammonium halides in electrolytic cells having the anode and cathode separated by a cation exchange membrane.

Electrolytic method for producing quaternary ammonium hydroxides

Concentrates containing from 0.5% to 20% by weight of an alkali metal borohydride, balance essentially inert dry resinous polymer are added to plastics in amounts effective to reduce traces impurities and thereby result in improved heat and light stability.

Alkali metal borohydride concentrate useful as a stability improver

A process for the preparation of compounds of the formula RBH.sub.3 CN wherein R is an alkali metal, a quaternary ammonium radical or a phosphonium radical wherein a compound of the formula RCN is treated with a stoichiometric amount or slightly less than a stoichiometric amount of a BH.sub.3 donor is described. The final products are useful as hydrolysis stable reductants and as synthetic intermediates.

Synthesis of NaBH.sub.3 CN and related compounds

The invention provides aqueous solutions of (1) the reaction product of anhydrous trimethyl borate with titanium tetrachloride and (2) polyvinyl alcohol, preferably not exceeding about 0.5 weight percent of each. These solutions have a pH of about 1 but when ammonium hydroxide is added the pH may be raised to about 10 without precipitation of titanium or gelation of the polyvinyl alcohol. When the pH of the above solutions is adjusted to between about 2 and about 10, the solutions are photosensitive. When these solutions are in a confined zone, sunlight or actinic radiation in the range between ultraviolet light and the lower wavelengths of the visible spectrum causes oxygen from the air above the solutions to be consumed until it is all gone. Then, reduction of the colorless dissolved Ti(IV) compound to the dark blue Ti(III) state occurs without precipitation of the Ti(III) product or reoxidation to Ti(IV). The blue Ti(III) solution is quickly reoxidized by reexposure to air. Similar photosensitive solutions are formed with polyvinyl alcohol and other Ti(IV) compounds, such as (1) the tetravalent titanium compound conforming substantially to the formula Cl.sub.2 Ti(OR).sub.2 where R is H, CH.sub.3, C.sub.2, H.sub.5, C.sub.3 H.sub.7 or C.sub.4 H.sub.9 ; (2) titanyl sulfate, and (3) titanyl chloride. The polyvinyl alcohol may be replaced by other complexing agents, such as N-hydroxyethylenediaminetriacetic acid, diethanolglycine, glucoheptanoic acid, arabonic acid, glusonic acid, galactonic acid, saccharic acid, mucic acid, and the sodium and ammonium salts of these compounds.

Photosensitive redox solutions

The invention provides aqueous solutions of (1) the reaction product of anhydrous trimethyl borate with titanium tetrachloride and (2) polyvinyl alcohol, preferably not exceeding about 0.5 weight percent of each. These solutions have a pH of about 1, but when ammonium hydroxide is added, the pH may be raised to about 10 without precipitation of titanium or gelation of the polyvinyl alcohol. When the pH of the above solutions is adjusted to between about 2 and about 10, the solutions are photosensitive. When these solutions are in a confined zone, sunlight or actinic radiation in the range between ultraviolet light and the lower wavelengths of the visible spectrum causes oxygen from the air above the solutions to be consumed until it is all gone. Then, reduction of the colorless dissolved Ti(IV) compound to the dark blue Ti(III) state occurs without precipitation of the Ti(III) product or reoxidation to Ti(IV). The blue Ti(III) solution is quickly reoxidized by reexposure to air. Similar photosensitive solutions are formed with polyvinyl alcohol and other Ti(IV) compounds, such as (1) the tetravalent titanium compound conforming substantially to the formula Cl.sub.2 Ti(OR).sub.2 where R is H, CH.sub.3, C.sub.2 H.sub.5, C.sub.3 H.sub.7 or C.sub.4 H.sub.9 ; (2) titanyl sulfate, and (3) titanyl chloride. The polyvinyl alcohol may be replaced by other complexing agents, such as N-hydroxyethylenediaminetriacetic acid, diethanolglycine, glucoheptanoic acid, arabonic acid, gluconic acid, galactonic acid, saccharic acid, mucic acid, and the sodium and ammonium salts of these compounds.

This invention relates to stabilized aqueous solutions of sodium borohydride containing soluble zinc in the form of sodium zincate. They may contain from about 35 to about 46.9 percent sodium hydroxide and from about 9.35 to about 12.9 percent sodium borohydride and 0.5 to 3 percent zinc which is preferentially added as zinc oxide and reacted with the sodium hydroxide present in the solution to form sodium zincate. These solutions may be used to react with sodium bisulfite to form solutions of sodium hydrosulfite in excellent yield. Such hydrosulfite solutions do not form trace amounts of hydrogen sulfide and do not darken or corrode copper based paper machine wires in contrast to hydrosulfite solutions which contain no soluble zinc.

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Ipswich, MA, United States of America

Robert C Wade