EP0490978A1 - Acide chlorique de grande purete - Google Patents

Acide chlorique de grande purete

Info

Publication number
EP0490978A1
EP0490978A1 EP90914002A EP90914002A EP0490978A1 EP 0490978 A1 EP0490978 A1 EP 0490978A1 EP 90914002 A EP90914002 A EP 90914002A EP 90914002 A EP90914002 A EP 90914002A EP 0490978 A1 EP0490978 A1 EP 0490978A1
Authority
EP
European Patent Office
Prior art keywords
chloric acid
solution
weight
percent
aqueous
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP90914002A
Other languages
German (de)
English (en)
Other versions
EP0490978A4 (en
Inventor
Budd L. Duncan
George W. Geren
Donald R. Leonard
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Olin Corp
Original Assignee
Olin Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Olin Corp filed Critical Olin Corp
Publication of EP0490978A1 publication Critical patent/EP0490978A1/fr
Publication of EP0490978A4 publication Critical patent/EP0490978A4/en
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B11/00—Oxides or oxyacids of halogens; Salts thereof
    • C01B11/12—Chloric acid

Definitions

  • Chloric acid can be used in the formation of chlorine dioxide, a commercial bleaching and sanitizing agent.
  • Chloric acid is a known compound which has been made in laboratory preparations by the reaction of barium chlorate with sulfuric acid to precipitate barium sulfate and produce a dilute aqueous solution of chloric acid which was concentrated by evaporation of water under partial vacuum.
  • sodium chlorate is reacted with an acid such as
  • Schlumberger teaches a process for producing chloric acid of high purity by passing an aqueous solution containing from 0.2 gram mole to 11 gram moles per liter of an alkali metal chlorate such as sodium chlorate through a selected cationic exchange resin at a temperature from 5o to 40o C.
  • the proces produces an aqueous solution containing from 0.2 gram mole to about 4.0 gram moles of HClO 3 .
  • chlorous acid [HCIO 2 ] is stated to be an intermediate in the formation.
  • Decomposition of HOCl by both mechanisms is said to increase with concentration, temperature and exposure to light and are pH dependent.
  • the first reaction mechanism is said to be accelerated by
  • Chloric acid however, up to the present time, has not been commercially produced or available commercially because of the high manufacturing costs and/or the undesired
  • chloric acid can be produced efficiently at substantially reduced production costs using a process which can be operated commercially.
  • the chloric acid solutions produced are of high purity and are stable at ambient conditions.
  • a process for producing chloric acid which comprises converting an aqueous solution of hypochlorous acid containing at least 20 percent by weight of HOCl at a temperature in the range of from about 10° to about 120 oC. to a reaction mixture
  • the novel process of the present invention employs as the starting material a concentrated solution of high purity hypochlorous acid, HOCl.
  • One method of producing high purity concentrated HOCl solutions is that in which gaseous mixtures, having high concentrations of hypochlorous acid vapors and chlorine monoxide gas and controlled amounts of water vapor are produced, for example, by the process described by J. P. Brennan et al in U.S. Patent No. 4,147,761, which is
  • the gaseous mixture is then converted to a concentrated hypochlorous acid solution as described in WO 90/05111 published May 17, 1990 by J. K. Melton, et. al. which is incorporated in its entirety by reference.
  • the concentrated hypochlorous acid solution employed as a reactant contains at least 20 percent by weight of HOCl.
  • Preferred solutions are those having concentrations in the range of from about 30 to about 60, and more preferably from about 40 to about 55 percent by weight of HOCl.
  • the solution is substantially free of ionic impurities such as chloride ions and alkali metal ions and has low concentrations of dissolved chlorine.
  • concentrations of the chloride ion are preferably less than about 50 parts per million and the alkali metal ion concentration is preferably less than about 50 parts per million.
  • the dissolved chlorine concentration in the hypochlorous acid solution is normally less than about 2 percent, and preferably less than about 1 percent by weight.
  • the concentrated hypochlorous acid is converted to chloric acid in any suitable manner and because the
  • hypochlorous acid reagent is of high purity, the conversion is believed to produce chloric acid according to the following reactions:
  • conversion of the concentrated hypochlorous acid to chloric acid takes place in an open vessel. Under these conditions the gaseous by-products are released as formed, for example, to a scrubbing apparatus containing an alkaline solution.
  • Suitable temperatures are those, for example, in the range of from about 10 to about 120o at autogenous pressures.
  • the conversion times are directly related to the temperature, however, as the conversion temperature increases, the yield of chloric acid is reduced. Therefore the hypochlorous acid conversion, where the by-product gases are released or
  • a dilute aqueous solution of chloric acid is produced which is may be further concentrated.
  • the chloric acid is produced by heating the hypochlorous acid solution at elevated temperature
  • the concentrated hypochlorous acid solution may be heated at temperatures in the range of from about 40 to about 120, preferably in the range of from about 50 to about 110 oC, and more preferably in the range of from about 60 to about 100oC.
  • chloric acid solution produced by the process of the invention is dilute, i.e. less than about 10 percent by weight of HCIO 3 , the chloric acid solution is further
  • any residual hypochlorous acid is converted to chloric acid product.
  • Concentration is suitably accomplished by heating the chloric acid solution at temperatures above about 40oC, for example at temperatures in the range of from about 40 to about 120 oC, preferably at from about 70 to about 120 oC. and more preferably at from about 95 to about 120 oC.
  • the chloric acid solutions may also be concentrated by vacuum distillation. Any suitable vacuum pressures may be used such as those in the range of from about 0.01 to about 100 mm Hg. pressure
  • the highly pure chloric acid solutions which are produced by the novel process of the present invention contain at least about 10 percent, for example 12 percent or greater, by weight of HClO 3 . Concentrated solutions up to about 45% by weight of HClO 3 may be produced. Preferred chloric acid solutions are those having from about 15% to about 40%, and more preferably 18% to about 35% by weight of HClO 3 .
  • the highly pure concentrated solutions produced i.e. those above about 30% by weight of HClO 3 , are surprisingly stable and can be stored safely without significant decomposition for extended periods of time.
  • hypochlorous acid containing 30% by weight of HOCl was added to a large open vessel at ambient temperature and pressure.
  • the solution was analyzed
  • a solution containing 22.8% by weight of HClO 3 produced by the process of the invention was further concentrated by heating at 95oC in an open vessel.
  • the chloric acid product recovered contained 43.34% by weight of HClO 3 .
  • Hypochlorous acid (44%, 600 g.) was heated in an open vessel at 95o for 1 hour.
  • the product solution contained 6.3% HOCl and 5.5% HClO 3 (yield 29%).
  • the product solution may be further concentrated by evaporation of water, for example, by the method of Example 1.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

Procédé de fabrication d'acide chlorique consistant à convertir une solution aqueuse d'acide hypochloreux contenant au moins 20 pour cent en poids de HOCl à une température comprise entre environ 10 et 120 °C, en un mélange réactionnel comprenant une solution aqueuse diluée d'acide chlorique et de sous-produits gazeux tout en enlevant en permanence les sous-produits gazeux afin de produire une solution d'acide chlorique qui contient au moins environ 10 pour cent en poids de HClO3. L'utilisation du nouveau procédé a permis de constater que l'acide chlorique peut être produit efficacement à des frais de fabrication sensiblement réduits grâce à un procédé qui peut être exploité à l'échelle industrielle. En outre, les solutions d'acide chlorique sont produites en des concentrations élevées et à une grande pureté, et sont sensiblement dépourvues d'impuretés telles que les ions de métaux alcalins, les ions chlorure, et les ions de sulfate.
EP19900914002 1989-09-05 1990-09-04 High purity chloric acid Withdrawn EP0490978A4 (en)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US40327989A 1989-09-05 1989-09-05
US403279 1989-09-05
US55228290A 1990-07-13 1990-07-13
US552282 1990-07-13

Publications (2)

Publication Number Publication Date
EP0490978A1 true EP0490978A1 (fr) 1992-06-24
EP0490978A4 EP0490978A4 (en) 1992-08-12

Family

ID=27018232

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19900914002 Withdrawn EP0490978A4 (en) 1989-09-05 1990-09-04 High purity chloric acid

Country Status (5)

Country Link
EP (1) EP0490978A4 (fr)
JP (1) JPH05500201A (fr)
AU (1) AU6435790A (fr)
FI (1) FI920376A0 (fr)
WO (1) WO1991003421A1 (fr)

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2347151A (en) * 1940-04-30 1944-04-18 Shell Dev Production of hypohalous acid solutions
GB984378A (en) * 1962-10-24 1965-02-24 Murgatroyds Salt & Chem Improvements in or relating to sodium hypochlorite production

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
No further relevant documents disclosed *
See also references of WO9103421A1 *

Also Published As

Publication number Publication date
JPH05500201A (ja) 1993-01-21
FI920376A0 (fi) 1992-01-28
AU6435790A (en) 1991-04-08
EP0490978A4 (en) 1992-08-12
WO1991003421A1 (fr) 1991-03-21

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