# US 5,707,546 A · Generation and storage of chlorine dioxide in a non-aqueous medium

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- Number: US 5,707,546 A
- Document ID: US5707546A
- Status: Granted
- Kind: A
- Application number: 08/416,153
- Filed: 1995-04-04
- Granted: 1998-01-13
- Earliest claimed: 1991-06-17
- Assignees: Rio Linda Chemical Co., Inc.
- Inventors: Anthony R. Pitochelli
- Web page: https://patentgrep.com/patent/US5707546A

## CPC

- C01B 11/022: {Chlorine dioxide (ClO2)}
- C01B 11/024: {from chlorites}
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}

## Abstract

A method of preparing and storing a stable solution of chlorine dioxide in a non-aqueous, water-immiscible liquid. An aqueous solution of chlorine dioxide is vigorously mixed with a non-aqueous, water immiscible liquid and, in a single extraction, the chlorine dioxide is extracted into the non-aqueous liquid. The aqueous and non-aqueous phases are separated and the chlorine dioxide containing non-aqueous liquid is stored in a closed light-free environment. In an alternate embodiment, gaseous chlorine dioxide is introduced into the non-aqueous, water-immiscible liquid. Concentrations of 2,000 mg to 17,000 mg chlorine dioxide per liter are obtained. The chlorine dioxide in the non-aqueous liquid is stabilized for at least one month. A highly purified aqueous solution of chlorine dioxide is prepared by mixing the non-aqueous solution of chlorine dioxide with water and extracting chlorine dioxide into the water.

## Claims

### Claim 1

A method of preparing and storing for subsequent use, a stable solution of chlorine dioxide in a non-aqueous, water-immiscible hydrocarbon liquid comprising the steps of preparing chlorine dioxide in an aqueous solution, adding a non-aqueous water-immiscible hydrocarbon liquid to the aqueous solution and agitating the mixture vigorously to extract a concentration of chlorine dioxide into the non-aqueous water-immiscible hydrocarbon liquid in an amount sufficient to form a concentration of chlorine dioxide ranging from 1,822 to 17,200 mg/l in said liquid, allowing the mixture to separate into a non-aqueous water-immiscible hydrocarbon phase containing chlorine dioxide and an aqueous phase, placing the separated non-aqueous water-immiscible hydrocarbon phase containing said chlorine dioxide in a closed, opaque container, with the container providing a light-free environment to stabilize the chlorine dioxide for a period of at least one month of storage.

### Claim 2 (depends on 1)

The method of claim 1, wherein the container containing said chlorine dioxide is stored at a temperature of approximately 4.degree. C.

### Claim 3 (depends on 1)

The method of claim 1, wherein the volume of non-aqueous, water-immiscible hydrocarbon liquid to the volume of the water ranges from approximately 0.8 to 4.0 times the volume of the water.

### Claim 4 (depends on 1)

The method of claim 1, wherein a single extraction is performed, with the single extraction being sufficient to efficiently extract an amount of the chlorine dioxide into the non-aqueous liquid effective for sterilizing and disinfecting.

### Claim 5 (depends on 1)

The method of claim 1, wherein the non-aqueous, water immiscible hydrocarbon liquid is an aliphatic hydrocarbon.

### Claim 6 (depends on 1)

The method of claim 1, wherein a concentration of chlorine dioxide dissolved in the non-aqueous water-immiscible hydrocarbon liquid and stored at ambient temperature retains at least one-half of its original concentration.

### Claim 7

A method of preparing chlorine dioxide in a non-aqueous water-immiscible hydrocarbon liquid comprising the steps of dissolving chlorine in a non-aqueous water-immiscible hydrocarbon liquid, the non-aqueous water-immiscible hydrocarbon liquid being substantially non-reactive with chlorine and substantially non-reactive with chlorine dioxide; providing an aqueous solution of about 0.5% to 25% by weight of chlorite; mixing and agitating the non-aqueous water-immiscible hydrocarbon liquid and the aqueous solution wherein the chlorine and the chlorite react to form chlorine dioxide; with 2,000 mg to 17,000 mg chlorine dioxide per liter being extracted into and dissolved in the non-aqueous water-immiscible hydrocarbon liquid and being isolated therein; separating the aqueous solution from the non-aqueous water-immiscible hydrocarbon liquid, with the chlorine dioxide in the non-aqueous water-immiscible hydrocarbon liquid being of high purity, substantially free of chlorite and chlorine, and storage stable for at least one month.

### Claim 8 (depends on 7)

The method of claim 7 wherein the non-aqueous water-immiscible hydrocarbon liquid containing chlorine dioxide is stored in a closed container in a substantially light-free environment.

### Claim 9 (depends on 8)

The method of claim 8 wherein the non-aqueous water-immiscible hydrocarbon liquid containing chlorine dioxide is stored in a refrigerated environment wherein the concentration, after one month, remains at approximately 90% of the initial concentration.

### Claim 10

A method for disinfecting and sterilizing a surface comprising the steps of dissolving by an extraction process about 2,000 mg to 17,000 mg of chlorine dioxide per liter of non-aqueous, water-immiscible hydrocarbon liquid to provide a concentrated solution, said concentrated solution stable for at least one month when stored in a light-free environment, diluting the concentrated solution with an additional volume of the non-aqueous water-immiscible hydrocarbon liquid to provide a concentration of chlorine dioxide sufficient to disinfect and sterilize and applying said diluted solution of chlorine dioxide to the surface to be disinfected and sterilized.

### Claim 11 (depends on 10)

The method of claim 10, wherein the amount of chlorine dioxide in the diluted solution is approximately 0.5 to 50 ppm.

### Claim 12

A method of preparing a highly purified aqueous solution of chlorine dioxide free from salts, acid, and chlorine, comprising the steps of preparing an aqueous solution of chlorine dioxide, adding a non-aqueous water-immiscible hydrocarbon liquid to the aqueous solution of chlorine dioxide thereby forming an aqueous phase and a non-aqueous water-immiscible liquid hydrocarbon phase, the non-aqueous water-immiscible hydrocarbon liquid being substantially non-reactive with chlorine dioxide; agitating the liquid phases, the chlorine dioxide being extracted into and dissolved in the non-aqueous water-immiscible liquid hydrocarbon phase; separating the non-aqueous water-immiscible liquid hydrocarbon phase from the aqueous phase thereby obtaining a non-aqueous water-immiscible liquid hydrocarbon containing chlorine dioxide; mixing the non-aqueous, water-immiscible hydrocarbon liquid containing chlorine dioxide with a volume of water; agitating the water and the non-aqueous, water-immiscible hydrocarbon liquid containing chlorine dioxide, wherein a first portion of the chlorine dioxide is dissolved in the water and a second portion of the chlorine dioxide is dissolved in the non-aqueous water-immiscible hydrocarbon liquid, and separating the water from the non-aqueous, water-immiscible hydrocarbon liquid thereby obtaining the aqueous solution of chlorine dioxide having a high purity free of salts, acid and chlorine.

### Claim 13

A method of preparing, storing, and using a stable solution of chlorine dioxide comprising the steps of:
dissolving chlorine dioxide in a non-aqueous water-immiscible hydrocarbon liquid at a concentration of 1,822 to 17,200 mg/l in said liquid by an extraction process, said liquid being substantially non-reactive with chlorine dioxide;
placing the non-aqueous water-immiscible hydrocarbon liquid containing the chlorine dioxide in a closed container, the container being made of a material which prevents the transmission of light therethrough;
storing the closed container with the non-aqueous water-immiscible hydrocarbon liquid containing the chlorine dioxide therein for at least one month;
shipping the non-aqueous water-immiscible hydrocarbon liquid containing the chlorine dioxide in the closed container to a work site;
opening the closed container at the work site and diluting said liquid with a non-aqueous water-immiscible hydrocarbon liquid to a concentration of 0.5 ppm to 17,000 ppm, wherein said concentration is effective for sterilizing and disinfecting.
