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(12) United States Patent (10) Patent No.: US 6,270,722 B1

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(12) United States Patent (10) Patent No.: US 6,270,722 B1 USOO6270722B1 (12) United States Patent (10) Patent No.: US 6,270,722 B1 Yang et all e 45) Date of Patent:e Aug. 7, 2001 (54) STABILIZED BROMINE SOLUTIONS, (56) References Cited METHOD OF MANUFACTURE AND USES THEREOF FOR BOFOULING CONTROL U.S. PATENT DOCUMENTS 3,328.294 6/1967 Self et al.. (75) Inventors: Shunong Yang; William F. McCoy, 3,558,503 1/1971 Goodenough et al.. both of Naperville; Eric J. Allain, 3,767,586 10/1973 Rutkiewic et al.. Aurora; Eric R. Myers, Aurora; 5,683,654 11/1997 Dalmier et al.. Anthony W. Dalmier, Aurora, all of IL 5,795,487 8/1998 Dalmier et al.. (US) 6,007,726 * 12/1999 Yang et al. ........................ 422/37 X 6,015,782 1/2000 Petri et al. ........................... 510/379 (73) Assignee: Nalco Chemical Company, Naperville, 6,110,387 * 8/2000 Choudhury et al. ................. 210/752 IL (US) FOREIGN PATENT DOCUMENTS (*) Notice: Subject to any disclaimer, the term of this WO 97/20909 6/1997 (WO). patent is extended or adjusted under 35 WO 97/43392 11/1997 (WO). U.S.C. 154(b) by 0 days. * cited by examiner Primary Examiner Elizabeth McKane (21) Appl. No.: 09/283,122 (74) Attorney, Agent, or Firm-Kelly L. Cummings; (22) Filed: Mar. 31, 1999 Thomas M. Breininger (51) Int. Cl." ................................ A61L 2/16; C01B 709; (57) ABSTRACT D06L 3/06 Stabilized bromine Solutions are prepared by combining a (52) U.S. Cl. ..................................... 422/37; 422/6; 8/107; bromine Source and a Stabilizer to form a mixture, adding an 8/137; 162/1; 423/500; 252/187.2 oxidizer to the mixture, and then adding, an alkaline Source (58) Field of Search .................................... 422/37, 6, 14; to adjust the pH of the mixture to at least 13. 8/107, 137; 162/1, 4; 423/500, 504; 252/1872, 380 30 Claims, No Drawings US 6,270,722 B1 1 2 STABILIZED BROMINE SOLUTIONS, DETAILED DESCRIPTION OF THE METHOD OF MANUFACTURE AND USES INVENTION THEREOF FOR BOFOULING CONTROL The present invention is directed to a method of making FIELD OF THE INVENTION Stabilized bromine Solutions. In accordance with this 5 invention, a bromine Source and a Stabilizer are combined to This invention relates generally to water treatment and, form a mixture, an oxidizer is next added to the mixture and more particularly, to Stabilized bromine Solutions, method of then an alkaline Source is added to adjust the pH of the manufacture and uses thereof for biofouling control. mixture to at least 13. BACKGROUND OF THE INVENTION The bromine sources which may be used in the practice of Sodium hypochlorite has been widely used in a variety of the present invention include hydrobromic acid, bromine industrial and recreational water Systems to control biofoul chloride, elemental bromine and alkali or alkaline earth ing. However, Sodium hypochlorite is unstable and must be metal bromides, Such as Sodium bromide, potassium bro provided in a stabilized form. There are several methods mide and lithium bromide. known in the art for Stabilizing hypochlorite (See, e.g., U.S. 15 The stabilizers which may be employed in this invention Pat. Nos. 3,328.294 and 3,767,586). have the chemical formula R-NH-R, wherein R and R' Bromine is preferred over chlorine for use in water are selected from the group consisting of R CO, RSO, R treatment because of its lower volatility and better perfor CF, RCHF, H, OH and PO(OH), and R is an alkyl group mance at high pH and amine environments. However, like or an aromatic group. Suitable Stabilizers include Saccharin, Sodium hypochlorite, Sodium hypobromite is unstable in urea, thiourea, creatine, cyanuric acids, alkyl hydantoins, typical Storage conditions and must therefore also be pro monoethanolamine, diethanolamine, organic Sulfonamides, vided in a stabilized form. U.S. Pat. Nos. 5,683,654 and biuret, Sulfamic acid, organic Sulfamates and melamine. 5,795,487, as well as the references disclosed therein, teach Sulfamic acid is the most preferred stabilizer. various methods for stabilizing sodium hypobromite. The The oxidizers which may be used include chlorine gas, 654 and 487 patents disclose batch methods which utilize 25 hypochlorous acid, hypochlorite Salt, chlorite, chlorate, Sodium hypochlorite and Sodium bromide as Starting elemental bromine, bromine chloride, hydrogen peroxide, materials, followed by the addition of a stabilizer. WO perSulfate, permanganate and peracetic acid. It is believed 97/20909 similarly discloses a process which includes a that other peroxy compounds can also be used in accordance hypobromite formation step followed by a bromine stabili with this invention. Zation Step. However, a disadvantage associated with this The alkaline Source is preferably an alkali or alkaline technique is that unstabilized hypobromite is formed in a earth metal hydroxide. Suitable alkaline Sources include Separate Step at a high concentration and pH. It is known that Sodium hydroxide, lithium hydroxide, potassium hydroxide, unstabilized hypobromite degrades quickly under Such con magnesium hydroxide and calcium hydroxide. ditions to form bromate, a non-biocidal compound that is It is preferred that the molar ratio between the bromine very toxic and a Suspected carcinogen. 35 Source and the stabilizer be in the range of about 0.2 to 5. In addition, WO 97/43392 discloses a process that first The molar ratio between the bromine source and the oxidizer forms Stabilized chlorine compounds and then converts them should preferably be in the range of about 0.5 to 2. to stabilized bromine compounds. However, this type of The method of the present invention is maintained at a process is limiting because only hypochlorite-releasing 40 temperature of less than 80 F., and preferably in the range compounds can be used as the oxidizing Source. of about 40 to 70° F. The pH of the mixture during the Therefore, because the demand for stabilized bromine oxidizer addition should be kept below about 7. The present Solutions is expected to increase in the future due to its invention can be carried out as either a batch or continuous advantages over chlorine, there is a need for other cost proceSS. effective methods of manufacturing stabilized bromine 45 The stabilized bromine solutions which are prepared in which can use a wider range of oxidants and produce a accordance with this invention may be used in a wide variety higher Strength product at higher yield. of commercial applications. These applications include, but Accordingly, it would be desirable to provide a method of are not limited to, the use of the stabilized bromine Solution: making a Stabilized bromine Solution which can be carried (1) as the bleaching agent in a method for the laundering of out as a batch or continuous process and which can produce 50 Soiled garments in which the Soiled garments are washed in a higher Strength product at higher yield. It would also be an aqueous media containing a detergent and a bleaching desirable to develop a method of making a Stabilized bro agent; (2) as the oxidizing agent in a method for the mine solution which is flexible and allows a variety of manufacture of cellulosic materials in which cellulosic fibers oxidizers to be utilized. are bleached; (3) as the oxidizing and biocidal agent in a 55 method for the control of biofouling in a recreational water SUMMARY OF THE INVENTION System in which an oxidizing and biocidal agent is added to The stabilized bromine solutions of the present invention control biofouling; (4) as the oxidizing and biocidal agent in are prepared by combining a bromine Source and a Stabilizer a method for the control of biofouling on a hard surface in to form a mixture, adding an oxidizer to the mixture, and which an oxidizing and biocidal agent is applied to the then adding an alkaline Source to adjust the pH of the 60 Surface to control biofouling on the Surface; (5) in a method mixture to at least 13. for the control of biofouling occurring on the Surfaces of The inventive method is economically appealing because equipment in contact with produced oil field waters; and (6) it can be carried out as a batch or continuous proceSS and in a method for controlling biofouling in an aqueous System. because it produces a high-strength Stabilized bromine Solu In another embodiment, the invention is a method of tion at higher yield. The method of preparation is also 65 preventing biofouling on the Surfaces of equipment in con flexible and allows for the utilization of a variety of oxidiz tact with an industrial water System. The method comprises CS. adding an effective biofouling controlling amount of a US 6,270,722 B1 3 4 stabilized bromine solution to the water system, wherein the also Suggested that the product was mostly oxidizing bro Solution is prepared by combining a bromine Source and a mine compounds (~98%). Stabilizer to form a mixture, adding an oxidizer to the mixture, and then adding an alkaline Source to adjust the pH Example 2 of the mixture to at least 13. The Same process performed above in Example 1 was The types of industrial water systems in which the stabi used to make a higher concentration product using industrial lized bromine Solution may be used to prevent biofouling grade Sodium hypochlorite in a lab Scale. include, but are not limited to, cooling water Systems, The product was prepared by: Sweetwater Systems, gas Scrubber Systems, air washer Systems, evaporative condensers, pasteurizers, produce Sani a. mixing 20.5 grams of a 45% sodium bromide solution tizer Streams, fire protection water Systems and heat with 8.70 grams of solid sulfamic acid in a 200 ml flask and then immersing the flask in an ice-water bath to eXchanger tubes.
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