JPH05500201A

JPH05500201A - High purity chloric acid

Info

Publication number: JPH05500201A
Application number: JP2513031A
Authority: JP
Inventors: ダンカン，バッド　エル．; ゲレン，ジョージ，ダブリュ．; レオナード，ドナルド，アール．
Original assignee: オリンコーポレイション
Priority date: 1989-09-05
Filing date: 1990-09-04
Publication date: 1993-01-21
Also published as: AU6435790A; FI920376A7; WO1991003421A1; EP0490978A4; FI920376A0; EP0490978A1

Abstract

(57)【要約】本公報は電子出願前の出願データであるため要約のデータは記録されません。 (57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

【発明の詳細な説明】本出願は１９８９年９月５日に出願した米国出願番号第４０３，２７９号の部分継続出願である。[Detailed description of the invention] This application is part of U.S. Application No. 403,279, filed September 5, 1989. This is a continuation application.

本発明は塩素酸、ＨＣｌＯｓの製造に関する。塩素酸は二酸化塩素、商業用漂白剤及び商業用消毒剤の生成に用いることができる。The present invention relates to the production of chloric acid, HClOs. Chloric acid is chlorine dioxide, commercial bleach It can be used to produce disinfectants and commercial disinfectants.

従来技術の説明塩素酸は既知化合物であり、実験室調製では、塩素酸バリウムを硫酸で反応させて硫酸バリウムを沈殿させ、塩素酸の希薄水溶液（不完全真空下で水分を蒸発させて濃縮させる）を製造することによって作られてきた。他の方法では、塩素酸ナトリウムを塩酸又は硫酸のような酸で反応させ、塩素酸の水溶液（不純物として硫酸塩又は塩化物のイオンを含む）を製造する。更に、二酸化塩素の商業的製造法では中間体として塩素酸が生成される。Description of prior art Chloric acid is a known compound, and laboratory preparation involves reacting barium chlorate with sulfuric acid. Barium sulfate was precipitated using a dilute aqueous solution of chloric acid (water was evaporated under partial vacuum). It has been made by manufacturing (concentration). In other methods, chloric acid Sodium is reacted with an acid such as hydrochloric acid or sulfuric acid, and an aqueous solution of chloric acid (as an impurity) containing sulfate or chloride ions). Additionally, commercial production of chlorine dioxide The manufacturing method produces chloric acid as an intermediate.

１９７４年５月１４日、Ａ、Ａ、ジュランバーガー（Ｓｃｈｌｕｍｂｅｒｇｅｒ）に付与された米国特許第３，８１０゜９６９号明細書から、塩素酸ナトリウムのようなアルカリ金属の塩素酸塩を１リットル当り０．２〜１１グラムモル含む水溶液を、５〜４０°Ｃの温度で選択陽イオン交ルから約４．０グラムモルのＨＣ１０ｓを含む水溶液が製造される。May 14, 1974, A. Schlumberger ), from U.S. Pat. No. 3,810°969, issued to Contains 0.2 to 11 gmol per liter of alkali metal chlorates such as The aqueous solution is prepared from a selective cation exchanger at a temperature of 5 to 40°C with approximately 4.0 gmol of H An aqueous solution containing C10s is produced.

カーク・オス？　−（Ｋｉｒｋ−Ｏｔｈｍｅｒ　）　：　ｒＥｎｃｙｃｌｏｐｅｄｉａｏｆ　ｃｈｅｍｉｃａｌ　Ｔｅｃｈｎｏｌｏｇｙ　Ｊ第３版、第５巻、５８７ページから、次亜塩素酸の希薄溶液（１モル）の分解は２通りで生じることが分かる：ＭＯＣＩ２ＨＯＣ１→２　ＨＣｌ　＋ＯＩ　＝＝＝２　Ｃｌ　＊　＋Ｏｘ　＋　２　Ｈｔ　Ｏ（１）第２機構にあっては、亜塩素酸（ＨＣ１０ｘ　）はその生成における中間体であると述べられている。両機構によるＨＯＣＩの分解は、濃度、温度及び光照射と共に増大し、ｐＨに依存していると述べられている。第１反応機構は触媒によって加速され、第２反応機構は塩化物のイオンのような電解室の圧力によって有利になると述べられている。しかし、その参考文献から、次亜塩素酸の濃縮溶液の分解に関しては何も知ることかできない。Kirk Os? -(Kirk-Othmer): rEncyclope Diaof chemical Technology J 3rd edition, Volume 5, 5 From page 87, the decomposition of a dilute solution (1 mol) of hypochlorous acid occurs in two ways. You can see: MOCI 2HOC1→2 HCl + OI ===2 Cl * +Ox + 2 Ht In the O(1) second mechanism, chlorous acid (HC10x) plays a role in its formation. It is stated that it is an intermediate. The decomposition of HOCI by both mechanisms is dependent on concentration, temperature and It is said that it increases with light irradiation and is dependent on pH. The first reaction mechanism is Accelerated by the catalyst, the second reaction mechanism is that chloride ions, such as This is said to be advantageous. However, from that reference, hypochlorous acid Nothing can be known about the decomposition of concentrated solutions.

しかし、塩素酸は今日まで商業的に生産されなかった又は商業的に利用できなかった。その理由は、製造費が高くかつこれらの反応によって製造されるＨ　Ｃ１０ｍ溶液中に好ましくない不純物が存在するということ、又はそのいずれかである。However, to date, chloric acid has not been commercially produced or commercially available. It was. The reason for this is that the production cost is high and the HCl produced by these reactions The presence of undesirable impurities in the 0m solution, or Ru.

発明の概要現在、塩素酸は、商業的に操作可能な方法を用いて実質的に低減製造費で効率的に製造することができるということが分かってきた。更に、製造された塩素酸の溶液は高純度であり、周囲条件で安定である。Summary of the invention Currently, chloric acid is produced efficiently with substantially reduced manufacturing costs using commercially operable methods. It has become clear that it can be manufactured in Furthermore, the produced chloric acid The solution is of high purity and stable at ambient conditions.

本発明によると、約１０〜約１２０℃の範囲の温度で、を、塩素酸の希薄水溶液と気体副生物とからなる反応混合物に転換させ、かつ該気体副生物を連続的に除去してＨＣｌ０．を約１０重量％又はそれ以上含む塩素酸溶液を製造することからなる塩素酸の製造方法が提供される。According to the present invention, a dilute aqueous solution of chloric acid is prepared at a temperature in the range of about 10 to about 120°C. and a gaseous by-product, and the gaseous by-product is continuously removed. Remove HCl0. to produce a chloric acid solution containing about 10% by weight or more of A method for producing chloric acid is provided.

発明の詳細な説明本発明の新しい方法では、出発物質として高純度次亜塩素酸、ＨＯＣＩの濃縮溶液を使用する。高純度の濃縮ＨＯＣ１溶液を製造する１つの方法は、高濃度次亜塩素酸の蒸気と、−酸化塩素ガスと、制御量の水蒸気とを含む気体混合物を、例えば、米国特許第４．１４７．７６１号明細書でＪ、Ｐ、ブレナン（Ｂｒｅｎｎａｎ　）等が述べている方法（その全体の内容を参照する）によって製造する方法である。ついで、１９９０年５月１７日発行のＷＯ９０１０５１１１号明細書でＪ、に、　メルトン（Ｍｅｌｔｏｎ）等が述へているような次亜塩素酸の濃縮溶液（その全体の内容を参照）に前記気体混合物を転換させる。Detailed description of the invention The new method of the invention uses high purity hypochlorous acid as the starting material, a concentrated solution of HOCI. Use liquid. One method for producing concentrated HOC1 solutions with high purity is For example, a gas mixture containing chloric acid vapor, -chlorine oxide gas and a controlled amount of water vapor is For example, in U.S. Pat. No. 4,147,761, J.P. Manufactured by the method described by (refer to the entire contents) It is the law. Next, the specification of WO90105111 issued on May 17, 1990 Concentration of hypochlorous acid as described by Melton et al. Converting the gas mixture into a solution (see its entire contents).

反応物として用いる次亜塩素酸の濃縮溶液には、ＨＯＣＩが少なくとも２０重量％含まれる。好ましい溶液はＨＯＣ１が約３０重量％から約６０重量％の範囲の濃度のものであり、更に好ましくは、約４０重量％から約５５重量％の濃度のものである。その溶液には、塩化物のイオンおよびアルカリ金属イオンのようなイオン不れる。例えば、塩化物のイオンの濃度は、好ましくは約５０　ｐｐｍ未満であり、アルカリ金属イオンの濃度は、好ましくは約５０　ｐｐｍ未満である。The concentrated solution of hypochlorous acid used as a reactant contains at least 20% by weight of HOCI. %included. Preferred solutions have HOC1 in the range of about 30% to about 60% by weight. concentration, more preferably from about 40% to about 55% by weight. It is. The solution contains ions such as chloride ions and alkali metal ions. It doesn't turn on. For example, the concentration of chloride ions is preferably less than about 50 ppm. and the concentration of alkali metal ions is preferably less than about 50 ppm.

次亜塩素酸溶液中の溶存塩素濃度は、通常、約２重量％未満であり、好ましくは約１重量％未満である。The dissolved chlorine concentration in the hypochlorous acid solution is typically less than about 2% by weight, preferably Less than about 1% by weight.

その濃縮次亜塩素酸は適切な方法によって塩素酸に転換する。そして、次亜塩素酸試薬は高純度であるために、次の反応によって転換し、塩素酸が生じるものと考えられる。The concentrated hypochlorous acid is converted to chloric acid by a suitable method. And hypochlorite Since the acid reagent is highly pure, it is assumed that it will be converted in the following reaction to produce chloric acid. Conceivable.

３ＨＯＣ１→ＨＣｌ０．　＋２ＨＣ１（１）２ＨＯＣ１＋２ＨＣ１→２ＣＩ！　＋２Ｈｚ　Ｏ（２）５ＨＯＣ１→ＨＣｌＯｓ　＋２Ｃ１，＋２Ｈ，Ｏｆ３）本発明の方法の１つの具体例では、濃縮次亜塩素酸の塩素酸への転換は開放容器中で行う。これらの条件下で、生成する気体副生物は、例えば、アルカリ溶液を含む気体洗浄装置へ放気す＝、適温は、例えば、自然圧において約ｌＯ〜約１２０° Ｃの範囲である。転換時間は転換温度に直接関係するが、転換温度が増大するにつれて、塩素酸の収率は減少する。従って、次亜塩素酸の転換は、製造し、その水溶液は更に濃縮することかできる。3HOC1→HCl0. +2HC1(1)2HOC1+2HC1→2CI!　 +2Hz O(2)5HOC1→HClOs +2C1,+2H,Of3) Main source In one embodiment of the disclosed method, the conversion of concentrated hypochlorous acid to chloric acid is performed in an open vessel. conduct. Under these conditions, the gaseous by-products that form include, for example, alkaline solutions. The appropriate temperature for releasing air to the gas cleaning device is, for example, about 10 to about 120 degrees at natural pressure. It is in the range of C. Conversion time is directly related to conversion temperature, but as conversion temperature increases As a result, the yield of chloric acid decreases. Therefore, the conversion of hypochlorous acid The aqueous solution can be further concentrated.

好ましい具体例では、次亜塩素酸溶液を高温で加熱することにより塩素酸を製造すると共に、反応時間中、反応混合物と接触して生成する気体副生物を保持する。このことは、例えば、自然圧下で、密封容器内でその方法を実行することによって達成することができる。そして、そこでは塩素酸の収率が実質的に増加する。例えば、約４０〜約Ｉ２０°Ｃの範囲の温度で、好ましくは約−５０〜約１１Ｏ℃の範囲で、更に好ましくは約６０〜約１００゛Ｃの範囲で、次亜塩素酸の濃縮溶液を加熱する。In a preferred embodiment, chloric acid is produced by heating a hypochlorous acid solution at high temperature. and retain gaseous by-products formed on contact with the reaction mixture during the reaction period. . This can be done, for example, by carrying out the method in a sealed container under natural pressure. can be achieved. And there the yield of chloric acid increases substantially . For example, at a temperature in the range of about 40 to about I20°C, preferably about -50 to about 11 The concentration of hypochlorous acid is in the range of 0°C, more preferably in the range of about 60 to about 100°C. Heat the condensation solution.

本発明の方法で製造した塩素酸溶液が希薄、すなわち、約１０重量９６未満のＨＣｌ０．である場合は、蒸発により水分の一部を除去することにより、その塩素酸溶液を更に濃縮する。蒸発している間、残留次亜塩素酸はすべて塩素酸生成物に転換する。濃縮は、約４０°Ｃ以上の温度で、例えば、約４０〜約１２０°Ｃの範囲の温度で、好ましくは約７０〜約１２０°Ｃの範囲で、更に好ましくは約９５〜約１２０℃の範囲で、その塩素酸溶液を加熱することによって適切に達成させる。The chloric acid solution prepared by the method of the present invention is dilute, i.e., less than about 10% by weight H Cl0. If so, remove some of the water by evaporation to remove the chlorine Further concentrate the acid solution. During evaporation, all residual hypochlorous acid is converted into chloric acid products Convert to Concentration is carried out at a temperature of about 40°C or higher, for example from about 40°C to about 120°C. preferably in the range of about 70 to about 120°C, more preferably in the range of about Suitably achieved by heating the chloric acid solution in the range of 95 to about 120°C. let

その塩素酸溶液は、真空蒸留によって濃縮するとともてきる。圧約０，０１〜約１００ｎｕ＋＋Ｈｇの範囲のような、いかなる適切な真空圧も使用することかできる。The chloric acid solution is concentrated by vacuum distillation. Pressure approx. 0.01 to approx. by using any suitable vacuum pressure, such as in the range of 100 nu++ Hg. Wear.

本発明の新しい方法によって製造される高純度塩素酸溶液には、ＨＣｌＯｓが少なくとも約１０重量％、例えば、約１２重量％又はそれ以上含まれる。ＨＣＩ　Ｏ２’約４５重量％までの濃縮溶液を製造することができる。好ましい塩素酸溶液は、ＨＣｌＯｓ約１５〜約４０重量％を含む溶液、そして更に好ましくは、約１８〜約３５重量％を含む溶液である。製造した高純度の濃縮溶液、すなわち、ＨＣｌＯｓ約３０重量％以上の溶液は、非常に安定であり、長期間、有意な分解はせず安全に貯蔵することができる。The high purity chloric acid solution produced by the new method of the present invention contains less HClOs. At least about 10% by weight, such as about 12% or more. HCI Concentrated solutions of up to about 45% O2' by weight can be produced. Preferred chloric acid solution The liquid is a solution containing about 15 to about 40% by weight HClOs, and more preferably about 18 to about 35% by weight. The produced high purity concentrated solution, i.e. Solutions of HClOs above about 30% by weight are very stable and do not undergo significant decomposition over long periods of time. It can be safely stored without any damage.

本発明の新しい方法を、更に次の例によって説明するが、その例に限定されるものではない。部及び百分率はすべて、別に表示しない限り重量による。The new method of the invention will be further illustrated by, but not limited to, the following example. It's not. All parts and percentages are by weight unless otherwise indicated.

例　１ＨＯＣｌ　３０重量％を含む次亜塩素酸溶液を、周囲温度及び周囲圧力の下で、大型開放容器に加えた。その溶液を定期的に分析し、反応によって、ＭＣｌ０゜６．０重量％、ＨＯＣｌ　５．３重量％及びＨＣｌ０．１重量％を含む溶液を製造したとき、その溶液を３０°Ｃて加熱し、ＨＣｌ０２　７．８重量％、ＨＯＣ１０，６重量％及びＨＣｌ０．１重量％を含む溶液を製造した。この塩素酸溶液かＨＣ１０３を２０．０３重量％、ＨＯＣＩ又はＨＣＩを０．１重量％未満含む溶液になるまで、２０〜２４°Ｃ１約０．ｌｍｍＨｇの真空蒸留にＨＯＣＩ　４１重量％を含む次亜塩素酸の濃縮溶液を、例１で使用した大型開放容器に入れ、室温で２４時間放置した。次いで、その溶液を２５°Ｃで真空蒸発によって濃縮し、ＨＣｌ０１　２３．５重量％を含む塩素酸溶液を製造した。分析結果は次の通りである。Example 1 A hypochlorous acid solution containing 30% by weight of HOCl under ambient temperature and pressure, Added to large open container. The solution is periodically analyzed and the reaction shows that MCl0° A solution containing 6.0% by weight, 5.3% by weight of HOCl and 0.1% by weight of HCl was prepared. When prepared, the solution was heated to 30°C and 7.8% by weight of HClO2, HOC A solution containing 10.6% by weight and 0.1% by weight of HCl was prepared. This chloric acid solution Contains 20.03% by weight of HC103 and less than 0.1% by weight of HOCI or HCI Heat at 20-24°C until it becomes a solution, about 0. HOCI 4 for vacuum distillation of lmmHg A concentrated solution of hypochlorous acid containing 1% by weight was placed in the large open container used in Example 1; It was left at room temperature for 24 hours. The solution was then concentrated by vacuum evaporation at 25 °C. A chloric acid solution containing 23.5% by weight of HCl01 was prepared. The analysis results are as follows That's right.

表　工初　期　２４時間後　濃縮後重量％ＨＣｌＯｓ　Ｌ４．３１　２３．５１ＨＯＣＩ　４１　０．８０　０．１２ＨＣＩ　ＢＤＬ”　ＢＤＬ” ０検出限界未満例　３ＨＯＣＩ　４’０．５４重量％を含む次亜塩素酸の濃縮溶液（６００ｇ）を密閉反応器に注ぎ、５５°Ｃて加熱した。生成気体をアルカリ気体洗浄装置へ送った。反応の後、ＨＣＩｃｅｓ　Ｉ　１．　９１％、ＨＯＣｌ　４．９２％及びＨＣｌ０．１％を含む溶液（４５４，８ｇ）を製造した。ＨＯＣＩに基づ＜ＨＣｌＯ３の収率は７１％であった。反応溶液及び気体洗浄装置の溶液（１１２４，７ｇ）の分析結果は次の通りである。Front work Initial stage: 24 hours later, after concentration weight% HClOs L4.31 23.51 HOCI 41 0.80 0.12 HCI　BDL”　BDL” 0 below detection limit Example 3 HOCI 4' Concentrated solution (600g) of hypochlorous acid containing 0.54% by weight is sealed Pour into reactor and heat to 55°C. The generated gas was sent to the alkaline gas cleaning device. . After the reaction, HCIces I1. 91%, HOCl 4.92% and HC A solution (454.8 g) containing 10.1% was prepared. Based on HOCI<HClO The yield of 3 was 71%. Reaction solution and gas cleaning device solution (1124.7g ) analysis results are as follows.

表　■ 初期溶液　）１０Ｃ１転換後　アルカリ気体洗浄重量％　装置ＨＯＣＩ　４０．５４　４．９２ＨＣ１０３０，２９１１，９１ＨＣＩ　Ｏ，１２０，１ＮａＯＣ１１０，９３Ｎａ　Ｃ１０ｓ　０．６９ＮａＣ１１０，０７例　４ＨＯＣＩ　４０．５４重量％を含む次亜塩素酸の濃縮溶液（６００ｇ）を、例３で使用した密閉反応器中で９５°Ｃの温度で加熱した。ＨＯＣＩに基づ＜ＨＣｌ０ｓ（４４５，５ｇ）の収率は８１９６であった。分析結果を下表■に示す。Table ■ Initial solution) After 10C1 conversion Alkaline gas cleaning weight % device HOCI 40.54 4.92 HC1030,2911,91 HCI　O,120,1 NaOC110,93 Na C10s 0.69 NaC110,07 Example 4 A concentrated solution (600 g) of hypochlorous acid containing 40.54% by weight of HOCI was added to Example 3. The mixture was heated at a temperature of 95°C in a closed reactor used in . Based on HOCI<HCl The yield of 0s (445.5 g) was 8196. The analysis results are shown in Table ■ below.

表　■ 初期溶液　ＨＯＣ１転換後重量％ＨＯＣ１４０，８９２，４５ＨＣ１０ｘ　１．０４　１３．７４ＨＣＩ　Ｏ，５４０，２２例　５本発明の方法によって製造した、ＨＣｌ０ｘ　２２．ｓ重量％を含む溶液を、開放容器中で９５°Ｃで加熱することにより更に濃縮した。回収した塩素酸の生成物には、ＨＣｌＯｓ　４３．３４重量％が含まれていた。Table ■ Initial solution after HOC1 conversion weight% HOC140,892,45 HC10x 1.04 13.74 HCI　O,540,22 Example 5 HCl0x produced by the method of the present invention 22. A solution containing s wt % is opened. It was further concentrated by heating at 95°C in a release vessel. Generation of recovered chloric acid The material contained 43.34% by weight of HClOs.

例　６ＨＣｌ０２　１５重量％を含む溶液を大気圧下、１０２〜１０４°Ｃで煮沸することにより、２８重量％まで濃縮した。その塩素酸の回収率は９７．２％であった。濃縮に要した総時間は４５分間であり、その内の１３分間は初めの溶液を加熱して煮沸させるのに必要とした。塩素又は二酸化塩素か放出している形跡は全く観察されなＨＣｌ０２を３０重量％及び３７．８７重量％含む塩素酸溶液を、本発明の方法で製造した。Example 6 A solution containing 15% by weight of HCl02 is boiled at 102-104°C under atmospheric pressure. By this, it was concentrated to 28% by weight. The recovery rate of chloric acid was 97.2%. Ta. The total time required for concentration was 45 minutes, of which 13 minutes were spent adding the initial solution. It was necessary to heat it to a boil. There is no evidence of chlorine or chlorine dioxide being released. A chloric acid solution containing 30% by weight and 37.87% by weight of HCl02, which was not observed in Produced by the method of the present invention.

各溶液の分取（１０００ｍｌ）を開放容器に入れ、３０°Ｃ及び４０°Ｃて貯蔵した。貯蔵期間中、周期的にその溶液のＨＣｌ０．ｌ１１度を、滴定分析によって分析した。その結果を下表■に示す。Aliquots (1000 ml) of each solution were placed in open containers and stored at 30°C and 40°C. did. During the storage period, the solution was periodically diluted with HCl0. 11 degrees by titration analysis. It was analyzed. The results are shown in Table ■ below.

表　■ ３０°Ｃ及び４０°ＣにおけるＨＣＩ　Ｏ２溶液の安定性３０．０１　０　３０．０１２９．７９　３　２９．７８２９．９９　６　２９．８７３０．０１　１４　３０．０３３０．６８　２６　３０．４５３０．３７　４４　３０．４２３０．３４　６４　３０．０７３０．５４　８１　３０．４６例８３７．８７　０　３７．８７３７．７８　３　３７．８７３７．８４　６　３８．０１３８．１３　１４　３８．４０３８．５８　２６　３８．５１３８．２７　４４　３８．７０３７．８９　６４　３８．７３３８．３０　８１　４０．１２３９．２７　１２１　４０．９３例　９次亜塩素酸（４４％、６００　ｇ）を開放容器中で９５°Ｃで１時間加熱した。Table ■ Stability of HCI O2 solution at 30°C and 40°C 30.01 0 30 ．． 01 29.79 3 29.78 29.99 6 29.87 30.01 14 30.03 30.68 26 30.45 30.37 44 30.42 30.34 64 30.07 30.54 81 30.46 Example 8 37.87 0 37.87 37.78 3 37.87 37.84 6 38.01 38.13 14 38.40 38.58 26 38.51 38.27 44 38.70 37.89 64 38.73 38.30 81 40.12 39.27 121 40.93 Example 9 Hypochlorous acid (44%, 600 g) was heated in an open vessel at 95°C for 1 hour.

生成溶液には、ＨＯＣ１６，３％及びＨＣｌ０３　５．５％が含まれていた（収率２９％）。生成溶液は、例えば例１の方法によって水分を蒸発させ、更に濃縮することができる。The resulting solution contained 16.3% HOC and 5.5% HCl03 (yield rate 29%). The resulting solution is further concentrated by evaporating water, for example by the method of Example 1. can do.

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Claims

[Claims]

1. Contains at least 20% by weight HOCl at a temperature in the range of about 10 to about 120°C Transferring an aqueous solution of hypochlorous acid to a reaction mixture consisting of an aqueous solution of chloric acid and a gaseous by-product. and continuously remove the gaseous by-products to reduce HClO3 to about 10% by weight or less. A method for producing an aqueous chloric acid solution characterized by producing an aqueous chloric acid solution containing at least Law.

2. Claim 1, wherein the aqueous solution of hypochlorous acid comprises from about 20 to about 60% by weight HOCl. Method described.

3. 12. The aqueous solution of chloric acid is concentrated at a temperature in the range of about 40 to about 120<0>C. The method described in 1.

4. The method of claim 1, wherein the dilute aqueous solution of chloric acid is concentrated by vacuum distillation. .

5. 5. The method of claim 4, wherein the conversion temperature ranges from about 25 to about 70<0>C.

6. An aqueous solution of hypochlorous acid containing at least 20% by weight of HOCl is heated above ambient temperature. heating at a low temperature to form a reaction mixture consisting of an aqueous chloric acid solution and a gaseous by-product. , the gaseous byproduct is kept in contact with the chloric acid solution, and about 10% by weight HClO3 is added. or more. Production method.

7. 12. The hypochlorous acid solution is heated to a temperature in the range of about 40 to about 120C. The method described in 6.

8. 7. The hypochlorous acid solution comprises from about 20 to about 60% by weight HOCl. the method of.

9. 4. The hypochlorous acid solution is heated to a temperature in the range of about 50 to about 110C. 8. The method described in 8.

10. 7. The hypochlorous acid solution comprises from about 30 to about 55% by weight HOCl. How to put it on.

11. The hypochlorous acid solution is heated at a temperature in the range of about 60 to about 100°C. The method according to item 10.

12. 7. The method of claim 6, wherein the aqueous chloric acid solution is further concentrated by evaporation.

13. evaporating the aqueous chloric acid solution at a temperature in the range of about 70 to about 120°C; The method according to claim 12.

14. 13. The method of claim 12, wherein the aqueous chloric acid solution is concentrated by vacuum distillation. .

15. evaporating the aqueous chloric acid solution at a temperature in the range of about 95 to about 120°C; The method according to claim 14.

16. Claim wherein the aqueous chloric acid solution comprises about 12% or more by weight HClO3. The method described in Section 1.

17. the aqueous chloric acid solution produced comprises about 15 to about 40% by weight HClO2; The method according to claim 3.

18. 6. The chloric acid solution comprises about 12% or more by weight HClO3. Method described.

19. the aqueous chloric acid solution produced comprises about 15 to about 40% by weight HClO3; The method according to claim 10.