Ciba-geigy Corporation

Other

Richard B Lund

Glenn W Brown

Gottfried Seifert

Sebastian Staubli

Willy Regenass

John G Lee

Josef H Wieland

Milo C Pass

Larry W Bass

Wesley W McConnell

Sam G Ladd

Martin Buerli

2-(stilbyl-4')-(naphtho-1',2':4,5)-1,2,3-triazole-2'-sulfonic acid is obtained by diazotizing p-aminostilbene sulfonic acid, coupling the resulting diazonium salt with Tobias acid and then oxidizing the resulting monoazo sodium salt to close the ring and form the naphthotriazolyl moiety, and, more particularly, by performing the ring-closure oxidation step in a solution of the monoazo compound in a mixture of 2-butoxyethanol and water with pressurized air by contacting said solution in the presence of a copper salt catalyst at temperatures in the range 105.degree.-160.degree. C. and at pressures in the range 10-80 psig, for a time sufficient to effect ring-closure.

Manufacturing process for a naphthotriazole stilbene fluorescent agent

A gun support mechanism is provided which includes buttstock supporting means mounted on a support surface and forestock supporting means mounted on said support surface. The buttstock and forestock supporting means include adjustment means whereby the gun may be positioned at a selected distance from the support surface. The supporting means further include base members which may be affixed to the support surface and support members which are operatively engageable with the base members through the use of lugs or similar expedients. At least one of the supporting means include gripping means for releasably gripping the buttstock or the forestock, respectively, of the gun. The invention is readily adaptable to support objects other than guns.

Removable, adjustable gun support

The present invention relates to an improved process for the preparation of 4,4'-dinitrostilbene-2,2'-disulfonic acid and its salts.

Process for the preparation of 4,4'dinitrostilbene-2,2'-disulfonic acid

A process for the preparation of 4-nitrotoluene-2-sulfonic acid by sulfonating 4-nitrotoluene with oleum or liquid SO.sub.3 is described. The sulfonation is carried out continuously with oleum of at least 50% concentration or liquid 100% SO.sub.3 while keeping the conversion of 4-nitro-toluene in the reaction mixture at .gtoreq.90% during the entire reaction course. The process is inherently non-polluting, and provides the product in high yield and low sulfuric acid content in a form usable for 4,4'-dinitrostilbene-2,2'-disulfonic acid production without further purification.

Process for the production of 4-nitrotoluene-2-sulfonic acid

A process for preparing bis-diaminostilbene dilsulfonic acid from bis-dinitrostilbene disulfonic acid by an improved Bechamp reduction process is disclosed. The process involves reduction with metallic iron in an acidic medium consisting of 0.033 to 0.27% of acetic acid and 0.38 to 0.76% of sulfuric acid in water at an oxidation-reduction potential (iron/thalamide electrode) in the range 140 to 270 millivolts.

Bechamp reduction of DNS to DAS using H.sub.2 SO.sub.4 and trace of HOAc

A process for the preparation of sulfonated aromatic amines is disclosed based upon starting with the corresponding amine reacted with sulfuric acid in the presence of a sufficient excess of sulfuric acid to act as the reaction solvent. The sulfuric acid excess in the case of sulfanilic acid, the most common of these sulfonated amines and exemplified herein is an aniline:sulfuric acid ratio in the range 1:2.0 to 1:2.5. The reaction, with recycling of the excess acid, provides substantially 100% yield of high quality sulfonated aromatic amine with effectively no effluent but the product.

Production of sulfonated amines

An improved process for the production of 2-stilbylnaphthotriazole optical bleaches which involves diazotizing aminostilbene 2-sulfonic acids, coupling the thus formed diazonium salt with naphthylamino-sulfonic acid to form the stilbylnaphthyl monoazo salt by adding the naphthylamino-sulfonic acid to the diazonium salt from the diazotization, neutralized to a pH in the range of 6-8, in the presence of 2-butoxyethanol, oxidizing said monoazo salt to form the 2-stilbylnaphthotriazole compounds with air in an aqueous alkaline medium containing butoxyethanol and isolating and recovering said 2-stilbylnaphotriazole optical bleaches as their sodium salts.

Process for the production of 2-stilbylnaphthotriazole optical bleaches

A process is described for purifying the bacteriostat 2,4,4'-trichloro-2'-hydroxydiphenylether prepared by the diazotization of 2,4,4'-trichloro-2'-aminodiphenylether from the 2,4,8-trichlorodibenzofuran and associated nonphenolics which form. A selective solvent extraction for these non-phenolics consisting of tetrachlorethylene is used after neutralization of the hydrolyzed diazo product.

Purification of 2,4,4'-trichloro-2'-hydroxydiphenylether solvent

An improved synthesis of the bacteriostat 2,4,4'-trichloro-2'-hydroxydiphenylether is disclosed wherein the hydrolysis after diazotization is carried out at 175.degree.-180.degree. C. to increase the yield and reaction rate. The hydrolyzed product is distilled after neutralization to remove the major portion of undesirable colored products and phenolics. The distillate is then extracted with tetrachlorethylene to separate the product from non-phenolic by-products including the 25-28% 2,4,8-trichlorodibenzofuran which are present. The final product of the process then meets F.D.A. and commercial standards for use in soaps and cosmetics.

Process for the production and purification of

This invention relates to the manufacture of dicyanopiperazine. More particularly, it relates to inexpensive, ecologically desirable procedures based on the controlled reaction of piperazine with a cyanogen halide in water.

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Jackson, AL, United States of America

Richard B Lund