Albemarle Corporation

Ethyl Corporation

Albermarle Corporation

Albemarie Corporation

Robert M Moore, Jr

Christopher J Nalepa

R Woodrow Wilson, Jr

Joseph W Roos

James E Torres

Gary D Focht

Bonnie G McKinnie

David R Brackenridge

Lawrence H Shepherd, Jr

Robert L Davis

Alvin E Harkins, Jr

Burnell Lee

William E Moehle

Edgar E Spielman, Jr

Michael G McKenna

Clarinda M Whitton

Described are highly concentrated liquid biocidal solutions formed in water from (a) specified bromine sources (e.g., BrCl or mixtures of BrCl and Br) and (b) alkali metal salt of sulfamic acid and/or sulfamic acid and alkali metal base, wherein the solution contains &#x3e;160,000 ppm of active bromine. Solutions of this type have been found to have greater stability than a commercially-available solution made from the same components containing 148,600 ppm of active bromine. Also described are new, water-soluble, solid state biocidal products formed by removing the water from solutions made in water from (a) and (b) irrespective of the initial concentration of active bromine. Removal of water can be accomplished by flashing or distillation at reduced pressure or preferably by spray drying. Such solid state products are typically in the form of powders or small particles, but can be compacted into larger forms preferably with the aid of one or more suitable binding agents.

Active bromine containing biocidal compositions and their preparation

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 compositions

A process of producing a concentrated liquid biocide formulation is described. Mixed together are (a) bromine and (b) an aqueous solution of alkali metal salt of sulfamic acid having a pH of at least about 12, in amounts such that (i) the active bromine content of the solution is at least about 100,000 ppm (wt/wt), and (ii) the atom ratio of nitrogen to active bromine from (a) and (b) is greater than 1. A continuous process for producing the concentrated liquid biocide composition is provided. This process comprises continuously feeding into mixing apparatus (i) bromine and (ii) an aqueous solution of alkali metal salt of sulfamic acid; the desired product is withdrawn from the mixing apparatus at a rate sufficient to enable the continuous feeding to be maintained. Also described are methods for disinfecting surfaces and for sanitizing bodies of water using a single-feed, bromine-based biocide. These methods use concentrated liquid biocide compositions comprising biocidally active bromine as the biocide.

Preparation of concentrated aqueous bromine solutions and biocidal applications thereof

Described is a process of producing a concentrated liquid biocide formulation. Mixed together are (a) bromine chloride or bromine and (b) an aqueous solution of alkali metal salt of sulfamic acid having a pH of at least about 7, in amounts such that (i) the active bromine content of the solution is at least about 100,000 ppm (wt/wt), and (ii) the atom ratio of nitrogen to active bromine from (a) and (b) is greater than 1 when bromine is used and is greater than 0.93 when bromine chloride is used. Use of bromine chloride as the source of the active bromine in the process is preferred because in the resulting aqueous compositions, all of the bromine of the bromine chloride is made available as active bromine in solution. In other words, the chlorine of the bromine chloride is converted in the process to dissolved alkali metal chloride salt, thereby liberating all of the bromine in the biocidal composition as active bromine capable of providing biocidal activity.

Concentrated aqueous bromine solutions and their preparation

The production process comprises A) forming an acidic aqueous solution comprising alkali metal cations, bromide anions, and sulfamate anions; B) feeding into said aqueous solution a source of alkali metal cations and chlorine-containing bromide oxidant proportioned to keep the resultant aqueous medium acidic and to form an acidic product solution containing at least about 5 wt % of active bromine, and C) raising the pH of the aqueous product solution with water-soluble base to at least about 10.

Production of concentrated biocidal solutions

Concentrated aqueous bromine solutions and their preparation and use

The production process comprises A) forming an acidic aqueous solution comprising alkali metal cations, bromide anions, and sulfamate anions; B) feeding into said aqueous solution a source of alkali metal cations and chlorine-containing bromide oxidant proportioned to keep the resultant aqueous medium acidic and to form an acidic product solution containing at least about 5 wt % of active bromine; and C) raising the pH of the aqueous product solution with water-soluble base to at least about 10.

Concentrated liquid biocide compositions are produced by: A) feeding (a) bromine atoms and chlorine atoms in the form of (i) one or more of BrCl, (ii) Br , and (iii) Cl into (b) water containing sulfamate anions, or feeding each of (a) and (b) into a reaction vessel, such that the numerical ratio of the total number of bromine atoms fed to the total number of chlorine atoms fed is in the range of about 0.7:1 to about 1.7:1; and B) providing enough alkali metal base in the mixture being formed in A) to keep the pH of such mixture in the range of about 7-11 during all or substantially all of the time feeding in A) is occurring, the amounts of (a) and (b) used being amounts that form an active-bromine-containing solution in which (i) the active bromine content is 50,000 ppm or more, and (ii) the atom ratio of nitrogen to active bromine originating from (a) and (b) is greater than about 0.93; and wherein if any sulfate is present in the solution as formed, the molar ratio of sulfate to sulfamate in the solution is less than about 0.2.

Described is a process of producing a concentrated liquid biocide formulation. Mixed together are (a) bromine chloride or bromine and (b) an aqueous solution of alkali metal salt of sulfamic acid having a pH of at least about 7, in amounts such that (i) the active bromine content of the solution is at least about 100,000 ppm (wt/wt), and (ii) the atom ratio of nitrogen to active bromine from (a) and (b) is greater than 1 when bromine is used and is greater than 0.93 when bromine chloride is used. Use of bromine chloride as the source of the active bromine in the process is preferred because in the resulting aqueous compositions, all of the bromine of the bromine chloride is made available as active bromine in solution. In other words, the chlorine of the bromine chloride is converted in the process to dissolved alkali metal chloride salt, thereby liberating all of the bromine as the active bromine content of the biocidal composition.

The production process comprises A) forming acidic aqueous solution comprising alkali metal cations, bromide anions, and sulfamate anions; B) feeding into said aqueous solution a source of alkali metal cations and chlorine-containing bromide oxidant proportioned to keep the resultant aqueous medium acidic and to form an acidic product solution containing at least about 5 wt % of active bromine; and C) raising the pH of the aqueous product solution with water-soluble base to at least about 10.

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.

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Baton Rouge, LA, United States of America

Robert M Moore, Jr