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US5152915.Pdf |||||||||||||| USOO5152915A United States Patent (19) 11 Patent Number: 5,152,915 Ralston, Jr. et al. (45) Date of Patent: Oct. 6, 1992 54 RECOVERY OF DICHLORINE MONOXIDE FROM HYPOCHLOROUSACD OTHER PUBLICATIONS SOLUTIONS Noyes, et al., J. American Chem. Soc. 44, 1630-1637 (75) Inventors: Richard W. Ralston, Jr., Cleveland; Mar. 16, 1922. Budd L. Duncan, Athens; Ronald L. Kirk-Othmer, Encycl. of Chem. Tech. 3rd Ed., vol. 8, Dotson, Cleveland, all of Tenn. pp. 116-119, 123, 124, CR 1979. Primary Examiner-Michael Lewis 73 Assignee: Olin Corporation, Cheshire, Conn. Assistant Examiner-Valerie Lund (21) Appl. No.: 753,560 Attorney, Agent, or Firm-Allen A. Meyer, Jr.; Paul 22 Filed: Sep. 3, 1991 Weinstein 5ll Int. Cl. .............................................. C01B 11/04 57) ABSTRACT 52 U.S. Cl. ...... ... 252/186.36: 423/462; A process for producing dichlorine monoxide which 55/71 includes: feeding an aqueous solution of hypochlorous (58) Field of Search ............... 423/466, 462, 473, 474, acid containing at least 20% by weight of HOCl to a 423/500; 62/11; 252/187.21, 186.36; 55/71 reaction vessel; maintaining the temperature of the aqueous solution of hypochlorous acid in the range of 56) References Cited from about - 10 to about +40° C.; passing an inert gas U.S. PATENT DOCUMENTS through the aqueous solution of hypochlorous acid to Re. 31,348 8/1983 Wejtowicz et al. .. ... 42.3/474 produce a gaseous mixture comprising dichlorine mon 4,32,795 3/1982 Brandt et al. ........................... 62/ oxide, chlorine and inert gas; an contacting the gaseous mixture with dry ice to provide a solid phase of dry ice FOREIGN PATENT DOCUMENTS and dichlorine monoxide. 1560614 2/1969 France .................................... 62/11 WO9065 5/1990 World Int. Prop. O. ... 42.3/473 9 Claims, No Drawings 5,152,915 1. 2 b) maintaining the temperature of the aqueous solu RECOVERY OF DICHLORINE MONOXDE FROM tion of hypochlorous acid in the range of from HYPOCHLOROUS ACID SOLUTIONS about -10 to about - 40 C., c) passing an inert gas through the aqueous solution BACKGROUND OF THE INVENTION 5 of hypochlorous acid to produce a gaseous mixture comprising dichlorine monoxide, chlorine and 1, Field of the Invention inert gas, This invention relates to a process for the production d) liquefying the gaseous mixture at a temperature of dichlorine monoxide. More particularly, the inven below about -20° C. to produce a liquid contain tion is concerned with a process for recovering dichlo 10 rine monoxide from hypochlorous acid solutions. ing dichlorine monoxide and chlorine, and Dichlorine monoxide, Cl2O, has been found to be an e) separating the chlorine from the dichlorine monox effective reagent for the bleaching of wood pulp and ide. textiles. Dichlorine monoxide has been made in the DETAILED DESCRIPTION OF THE laboratory by the reaction of chlorine with mercury 15 INVENTION oxide, HgC). On an industrial or commercial scale, di The novel process of the present invention employs chlorine monoxide has been prepared by reacting chlo as one reactant a concentrated solution of high purity rine with sodium carbonate (soda ash) or sodium bicar hypochlorous acid, HOCl. The method of producing bonate in the presence of controlled amounts of water. high purity concentrated HOC solutions is that in An example of this approach is found in U.S. Pat. No. 20 which-gaseous mixtures, having high concentrations of 3,914,397, issued Oct. 21, 1975 to W. A. Mueller. In this hypochlorous acid vapors and chlorine monoxide gas, process, dry gaseous chlorine in the presence of a moist and controlled amounts of water vapor, are produced, dilutant gas such as air oxygen or nitrogen is reacted for example, by the process described by J. P. Brennan with alkali metal carbonates or bicarbonates in the form et al in U.S. Pat. No. 4,147,761. The gaseous mixture is of dry solids having reactive open structure forms and 25 then converted to a concentrated hypochlorous acid specified surfaces areas. The process is carried out at a solution as described in WO 90/05111 Published May temperature in the range of -20° C. to +30 C, while 17, 1990 by J. K. Melton, et. al. Each of these publica maintaining the pH at 9.5 or higher. tions is incorporated in its entirety by reference. Gaseous dichlorine monoxide has also been prepared 30 The concentrated hypochlorous acid solution em by treating concentrated solutions of hypochlorous acid ployed as a reactant contains concentrations in the with anhydrous calcium nitrate. In U.S. Reissue Pat. range of from about 35 to about 60, and more preferably No. 31,348, issued Aug. 16, 1983 to J. A. Wojtowicz et from about 40 to about 55 percent by weight of HOCl. al, gaseous chlorine is passed rapidly across the surface The solution is substantially free of ionic impurities of an agitated aqueous solution of sodium hydroxide at 35 such as chloride ions and alkali metal ions and has low a reduced temperature. A gaseous mixture of hypochlo concentrations of dissolved chlorine. For example, con rous acid, chlorine monoxide and unreacted chlorine is centrations of the chloride ion are preferably less than produced which, if dried over anhydrous calcium ni about 50 parts per million and the alkali metal ion con trate, produces dichlorine monoxide. centration is preferably less than about 50 parts per A slow current of air was passed through a dilute million. The dissolved chlorine concentration in the solution of hypochlorous acid (0.2715 N, 1.4% by wt.), hypochlorous acid solution is normally less than about 3 through calcium nitrate to absorb water vapor, and percent, and preferably less than about 1 percent by through sodium hydroxide to absorb dichlorine monox weight. These highly pure, concentrated solutions of ide in a study on the ionization of hypochlorous acid by hypochlorous acid are also highly acidic, having a pH W. A. Noyes and T. A. Wilson (J. Amer. Chem. Soc. 45 of less than about 2, for example, in the range of from 44, 1630-1637, 1922). Moles of dichlorine monoxide in about 1 to about 1.75. the range of 0.0025 to 0.0114 were collected. In the novel process of the present invention an inert These methods produce mixtures of dichlorine mon gas such as air, nitrogen, argon, carbon dioxide or mix oxide and chlorine. However the presence of chlorine is tures thereof are passed through the concentrated hypo 50 chlorous acid solution. During the stripping of dichlo undesirable in many applications of dichlorine monox rine monoxide, the hypochlorous acid solution is main ide. tained at a temperature in the range of from about - 10 Further, these methods have not produced dichlorine to about --40, and preferably from about 0 to about monoxide in high concentrations and volumes which 10 C. A gaseous mixture of dichlorine monoxide, chlo could economically be used in commercial applications. 55 rine, inert gas, water vapor and having traces of oxygen Thus there is a need for a process for producing gase and hypochlorous acid vapor is produced. To remove ous dichlorine monoxide substantially free of chlorine. any water vapor which may be present, the gaseous In addition, there is a need for a process for producing mixture is preferably dried. Suitable drying methods efficiently in amounts and concentrations for commer include, for example, contacting the gaseous mixture cial applications. with a drying agent or chilling the gaseous mixture and/or passing the gaseous mixture through a molecu SUMMARY OF THE INVENTION lar sieve. Drying agents which may be employed in These and other advantages are accomplished in a clude calcium sulfate, calcium nitrate, sodium sulfate, process for producing dichlorine monoxide which com magnesium perchlorate, perfluorosulfonic acid resins prises: 65 and mixtures thereof. a) feeding an aqueous solution of hypochlorous acid The dried gaseous mixture of chlorine, dichlorine containing at least 20% by weight of HOCl to a monoxide and inert gas is then liquefied, for example, by reaction vessel, cooling to a temperature below about -20° C., and 5,152,915 3 4. preferably in the range of from about -25 to about TABLE 1 -80 C. Gaseous Mixture Stripped from HOCl Solution A liquefied mixture of chlorine and dichlorine mon (Balance nitrogen) oxide is recovered in a collection unit at a temperature Mass. Spec. Analysis at or below -25 C. Time N2 Fow C12O CI2 HOCl O2 H2O The dichlorine monoxide is separated from the chlo Lapsed Temp C. ml/min % % % % % rine. Separation of the dichlorine monoxide from the O - 4 0.5 2.28 7.30 0.25 0.63 1.42 3 -5 1.0 2.52 6.60 0.26 0.64 1.42 chlorine may be accomplished by any suitable method s O 1.0 2.77 5.75 0.28 0.62. 1.42 including, for example, distillation, freezing or dissolu 10 13 3 1.0 3.00. 4.00 0.30 0.62 1.42 tion in selected solvents. Suitable solvents include per 9 4. 1.0 3.37 4.00 0.30 0.63 .42 23 4 1.0 3.57 3.75 0.32 0.64 1.42 fluoro- and chlorofluoroalkanes such as methane or 28 4 1.0 3.81 3.74 0.34 0.66 .42 ethane, i.e. carbon tetrachloride. In one embodiment, 36 6 1.0 3.99 3.74 0.36 0.67 1.59 the liquified mixture is fed to a distillation column and 41 8 1.0 4.07 3.78 0.36 0.68 1.59 the temperature of the mixture raised to a temperature 15 46 11 1.0 4.14 3.78 0.37 0.69 1.63 above the boiling point of chlorine and below the boil ing point of the dichlorine monoxide.
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