Ethyl Corporation

Albemarle Corporation

R Woodrow Wilson, Jr

Robert M Moore, Jr

Kryn G Ihrman

James E Torres

Olan W Mitchell

Gary D Focht

Kim R Smith

Dennis J Malfer

Gerald M Sulzer

Dustin H Thomas

Marshall B Nelson

Y-d Mark Chen

Rebecca F Smith

George A Daniels

Alfred P Anderson

Mayur P Shah

J Francis Steadman

J Keitt Hane

Sharon B McGee

The process involves (a) continuously forming bromine chloride from separate feed streams of bromine and chlorine by maintaining said streams under automatic feed rate control whereby the streams are continuously proportioned to come together in equimolar amounts to form bromine chloride; (b) continuously forming an aqueous product having an active bromine content of at least 100,000 ppm (wt/wt), a pH of at least 7, and an atom ratio of nitrogen to active bromine greater than 0.93:1 by continuously feeding into mixing apparatus separate feed streams of (1) bromine chloride formed in (a), and (2) an aqueous solution of alkali metal salt of sulfamic acid, under automatic feed rate control whereby the feed streams are continuously proportioned to come together in amounts that produce an aqueous product having an active bromine content of at least 100,000 ppm (wt/wt), a pH of at least 7, and an atom ratio of nitrogen to active bromine from (1) and (2) greater than 0.93:1; and, (c) withdrawing said aqueous product from said mixing apparatus at a rate sufficient to enable the continuous feeding in (a) and (b) to be maintained.

Continuous processes for preparing concentrated aqueous liquid biocidal composition

The process involves (a) continuously forming bromine chloride from separate feed streams of bromine and chlorine by maintaining said streams under automatic feed rate control whereby the streams are continuously proportioned to come together to form bromine chloride; (b) continuously forming an aqueous product having an active bromine content of at least 100,000 ppm (wt/wt), a pH of at least 7, and an atom ratio of nitrogen to active bromine greater than 0.93:1 by continuously or intermittently feeding into mixing apparatus separate feed streams of (1) bromine chloride formed in (a), and (2) an aqueous solution of alkali metal salt of sulfamic acid, under automatic feed rate control.

Processes for preparing concentrated aqueous liquid biocidal compositions

A concentrated liquid biocide composition is produced by a continuous process. The process comprises continuously feeding into mixing apparatus (i) bromine chloride and (ii) an aqueous solution of alkali metal salt of sulfamic acid. These are proportioned to produce an aqueous product having an active bromine content of at least 100,000 ppm (wt/wt), and an atom ratio of nitrogen to active bromine from (i) and (ii) greater than 0.93:1. The desired product is withdrawn from the mixing apparatus at a rate sufficient to enable the continuous feeding to be maintained. Thus, the withdrawal of the product can be continuous or intermittent, depending upon the type of mixing apparatus being used.

Concentrated aqueous bromine solutions and their preparation

A concentrated liquid biocide composition is produced by a process which comprises continuously or intermittently feeding (i) bromine chloride into mixing apparatus where the bromine chloride contacts (ii) an aqueous solution of alkali metal salt of sulfamic acid. An aqueous product is produced having an active bromine content of at least 100,000 ppm (wt/wt), and an atom ratio of nitrogen to active bromine from (i) and (ii) greater than 0.93:1. The desired product can be withdrawn from the mixing apparatus continuously or intermittently.

A highly pure, white, solid amine oxide is prepared in high yield with minimal decomposition of the solvent by (A) reacting a tert-amine with a 15-20% stoichiometric excess of concentrated hydrogen peroxide at 50.degree.-55.degree. C. in the presence of controlled amounts of carbon dioxide and ethyl acetate until the reaction mixture contains 35-45 % by weight of ethyl acetate and less than 0.8% by weight of unreacted amine, (B) catalytically decomposing residual hydrogen peroxide, (C) separating the reaction mixture from the decomposition catalyst, (D) cooling the reaction mixture to 0.degree. C. to form a slurry, (E) centrifuging the slurry to separate the amine oxide, and (F) vacuum drying the amine oxide at ambient temperature--the reaction mixture being diluted to an amine oxide content of 25-30% by weight with additional ethyl acetate or a mixture thereof with a co-solvent, such as a low-boiling n-alkane, after the completion of Step A and prior to the beginning of Step D.

Process for preparing solid amine oxides

Production of alkyl substituted aromatic diamines by reacting triethlyaluminum with an aromatic diamine and a chloride ion source in the presence of an olefin is disclosed. The alkyl substituted aromatic diamines are useful as chain extenders in polyurethane processes.

Process for alkylation of aromatic diamines

Production of alkyl substituted aromatic diamines by reacting triethylaluminum with an aromatic diamine and a chloride ion source in the presence of an olefin is disclosed. The alkyl substituted aromatic diamines are useful as chain extenders in polyurethane processes.

Contaminants in spent nitric-sulfuric nitration acid can be removed by mixing the spent acid with urea and heating to 75.degree.-150.degree. C. Off-gas from the spent acid/urea reaction is passed through a Group IB, VB, VIB or VIII metal containing catalyst to decompose nitrous oxides and the so-treated off-gas is contacted with spent acid, denitrated spent acid, or fresh sulfuric acid, and optionally air (i.e. oxygen), to absorb oxides of nitrogen. The spent acid scrubbing fluid is then subjected to the same process for removing contaminants.

Spent acid purification process

A process for making an alkali metal alkoxide (e.g. sodium alkoxide) of a halogen-substituted alcohol (e.g. fluorine-substituted alcohols) by dispersing an alkali metal (e.g. sodium) in a cycloalkane (e.g. cyclohexane) containing a phenol (e.g. o-allylphenol) and adding the resultant dispersion to an ether (e.g. THF) solution of a halogen-substituted alcohol. The resultant alkali metal haloalkoxide solution contains phenoxides and can be reacted with a phosphonitrilic chloride polymer to introduce haloalkoxide and phenoxide substituents.

Polyphosphazene process

A process for making an alkali metal alkoxide (e.g. sodium alkoxide) of a halogen-substituted alcohol (e.g. fluorine-substituted alcohols) by dispersing an alkali metal (e.g. sodium) in a cycloalkane (e.g. cyclohexane) and adding the resultant dispersion to an ether (e.g. THF) solution of a halogen-substituted alcohol. The resultant alkali metal haloalkoxide solution can be reacted with a phosphonitrilic chloride polymer to introduce haloalkoxide substituents.

An improved process for the preparation of O,O-dialkyl phosphorochloridothioates in which distillation to recover substantially pure product is carried out in presence of a solubilizing or suspending agent, for example, liquid hydrocarbons, particularly aromatics having at least 10 carbon atoms which have good sulfur solubility, higher boiling point than the product and are inexpensive; specifically, naphthalenes are useful.

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Baton Rouge, LA, United States of America

R Woodrow Wilson, Jr