EP1831599A2 - Nouveau procede de production de liquides contenant une dose d'ozone sous pression - Google Patents

Nouveau procede de production de liquides contenant une dose d'ozone sous pression

Info

Publication number
EP1831599A2
EP1831599A2 EP05856242A EP05856242A EP1831599A2 EP 1831599 A2 EP1831599 A2 EP 1831599A2 EP 05856242 A EP05856242 A EP 05856242A EP 05856242 A EP05856242 A EP 05856242A EP 1831599 A2 EP1831599 A2 EP 1831599A2
Authority
EP
European Patent Office
Prior art keywords
pressurization
ozone
vessel
gas
pressurized
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Withdrawn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
EP05856242A
Other languages
German (de)
English (en)
Inventor
Steven A. Fisher
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.)
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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
Priority claimed from US11/145,137 external-priority patent/US20050268646A1/en
Application filed by Air Liquide SA, LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude filed Critical Air Liquide SA
Publication of EP1831599A2 publication Critical patent/EP1831599A2/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C5/00—Methods or apparatus for filling containers with liquefied, solidified, or compressed gases under pressures
    • F17C5/06—Methods or apparatus for filling containers with liquefied, solidified, or compressed gases under pressures for filling with compressed gases
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23B—PRESERVATION OF FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES; CHEMICAL RIPENING OF FRUIT OR VEGETABLES
    • A23B2/00—Preservation of foods or foodstuffs, in general
    • A23B2/70—Preservation of foods or foodstuffs, in general by treatment with chemicals
    • A23B2/704—Preservation of foods or foodstuffs, in general by treatment with chemicals in the form of gases, e.g. fumigation; Compositions or apparatus therefor
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23B—PRESERVATION OF FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES; CHEMICAL RIPENING OF FRUIT OR VEGETABLES
    • A23B2/00—Preservation of foods or foodstuffs, in general
    • A23B2/70—Preservation of foods or foodstuffs, in general by treatment with chemicals
    • A23B2/725—Preservation of foods or foodstuffs, in general by treatment with chemicals in the form of liquids or solids
    • A23B2/788—Inorganic compounds
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C9/00—Methods or apparatus for discharging liquefied or solidified gases from vessels not under pressure
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2205/00—Vessel construction, in particular mounting arrangements, attachments or identifications means
    • F17C2205/01—Mounting arrangements
    • F17C2205/0123—Mounting arrangements characterised by number of vessels
    • F17C2205/013—Two or more vessels
    • F17C2205/0134—Two or more vessels characterised by the presence of fluid connection between vessels
    • F17C2205/0138—Two or more vessels characterised by the presence of fluid connection between vessels bundled in series
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2221/00—Handled fluid, in particular type of fluid
    • F17C2221/01—Pure fluids
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2223/00—Handled fluid before transfer, i.e. state of fluid when stored in the vessel or before transfer from the vessel
    • F17C2223/01—Handled fluid before transfer, i.e. state of fluid when stored in the vessel or before transfer from the vessel characterised by the phase
    • F17C2223/0107—Single phase
    • F17C2223/0123—Single phase gaseous, e.g. CNG, GNC
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2223/00—Handled fluid before transfer, i.e. state of fluid when stored in the vessel or before transfer from the vessel
    • F17C2223/03—Handled fluid before transfer, i.e. state of fluid when stored in the vessel or before transfer from the vessel characterised by the pressure level
    • F17C2223/033—Small pressure, e.g. for liquefied gas
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2223/00—Handled fluid before transfer, i.e. state of fluid when stored in the vessel or before transfer from the vessel
    • F17C2223/04—Handled fluid before transfer, i.e. state of fluid when stored in the vessel or before transfer from the vessel characterised by other properties of handled fluid before transfer
    • F17C2223/042—Localisation of the removal point
    • F17C2223/043—Localisation of the removal point in the gas
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2225/00—Handled fluid after transfer, i.e. state of fluid after transfer from the vessel
    • F17C2225/01—Handled fluid after transfer, i.e. state of fluid after transfer from the vessel characterised by the phase
    • F17C2225/0107—Single phase
    • F17C2225/0123—Single phase gaseous, e.g. CNG, GNC
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2225/00—Handled fluid after transfer, i.e. state of fluid after transfer from the vessel
    • F17C2225/03—Handled fluid after transfer, i.e. state of fluid after transfer from the vessel characterised by the pressure level
    • F17C2225/035—High pressure, i.e. between 10 and 80 bars
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2227/00—Transfer of fluids, i.e. method or means for transferring the fluid; Heat exchange with the fluid
    • F17C2227/01—Propulsion of the fluid
    • F17C2227/0128—Propulsion of the fluid with pumps or compressors
    • F17C2227/0171—Arrangement
    • F17C2227/0178—Arrangement in the vessel
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2227/00—Transfer of fluids, i.e. method or means for transferring the fluid; Heat exchange with the fluid
    • F17C2227/01—Propulsion of the fluid
    • F17C2227/0192—Propulsion of the fluid by using a working fluid
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2265/00—Effects achieved by gas storage or gas handling
    • F17C2265/02—Mixing fluids
    • F17C2265/025—Mixing fluids different fluids
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2270/00—Applications
    • F17C2270/05—Applications for industrial use

Definitions

  • Treating and sanitation of food, equipment, pharmaceutical products, and even water to reduce undesirable biological microorganisms is important to the protection of public health.
  • food can be damaged by microbes, spores, insects, and other similar sources.
  • economic losses of food and labor due to damage from such sources is more than $100 billion.
  • food items are preserved using a variety of methods, including refrigeration, fumigation with toxic chemicals, irradiation, biological control, heat exposure, and controlled atmosphere storage (a fruit industry technique that involves modifying the concentration of gases naturally present in the air).
  • Effective sanitation of food or other items depends on the combination of what is to be sanitized and the sanitation process type. Not all of the currently available technologies can deliver an effective reduction of microorganisms and at the same time prevent product or environmental degradation. It is well known in the art to cool products, such as foods, during processing with some type of refrigerant to slow down the growth of unwanted microbes and enzymatic reactions in foods. For instance, the shelf life and quality of food products are improved by processing, transporting, and storing under refrigerated conditions.
  • Cooling agents such as water ice, dry ice, carbon dioxide, or nitrogen
  • Cooling agents are liquid or solid agents that can be used as an expendable refrigerant.
  • liquids such as nitrogen, are used to cool and inert the atmosphere during food processing or storage.
  • Biocidal agents are used to sanitize equipment, provide antiseptic environments, treat water, and sanitize foods.
  • the reaction of biocidal agents with microbial cell structures is often irreversible; therefore the cells either become attenuated or die.
  • ozone One biocidal agent commonly used in the industry is ozone.
  • ozone is very unstable, and therefore, must be produced at the location of consumption. Production of ozone requires specialized equipment and involves safety issues due to handling of the equipment and feedstock, such as pure oxygen. After the ozone is produced, it must be delivered in some form to the target item as a sanitizer. Ozone is often dissolved or absorbed in water as a mechanism to deliver the unstable ozone to a target item.
  • Ozone is often dissolved or absorbed in water as a mechanism to deliver the unstable ozone to a target item.
  • ozone has poor solubility in water. Mixtures of ozone and water typically contain less than about 20 ppm by weight (ppmwt) ozone. As a result, large quantities of water relative to the ozone are required if water is used as a delivery agent. Furthermore, because of the large quantities of water required, the ozone and water cannot be pre-mixed and transported to site. Thus,
  • Ozone generating equipment known in the art typically produces an ozone- containing gas stream at fairly low pressures. These ozone generators are typically limited to producing a stream with a pressure of less than about 25 psig.
  • Conventional mechanical compression cannot be used to compress ozone because the unstable ozone molecule is destroyed in conventional compressors.
  • Oil-lubricated or water ring compression can be used to compress a stream containing ozone up to 150 psig; however, these compressors inherently contaminate the ozone stream with oil or water respectively.
  • the prior art fails to provide a method to compress the ozone to pressures above about 25 psig without contaminating the ozone stream with some level of oil or water. Furthermore, the prior art fails to provide any method to successfully compress an ozone stream to pressures of greater than about 150 psig without destroying the ozone.
  • the current invention fulfills the need to provide a process to pressurize an ozone-containing stream without destroying the ozone or contaminating the ozone-containing stream with oil or water. It is desirable to be able to provide a pressurized ozone-containing stream that is substantially free of oil and moisture. It is also desirable to the ozone-containing stream at pressures above 150 psig. It further desirable to pressurize ozone and feed it into a liquid, so that it is absorbed under pressure into the liquid.
  • the current invention pressurizes ozone by feeding an ozone- containing source to an ozone pressurization system to establish a first pressure followed by pressurizing the ozone pressurization system.
  • the ozone pressurization system is pressurized by feeding a pressurization gas to the ozone pressurization system to raise the pressure to the second pressure and form a pressurized ozone-containing gas.
  • the pressurized ozone- containing gas is then withdrawn from the ozone pressurization system. This method pressurizes the ozone-containing stream without contaminating the stream with oil or water.
  • the ozone pressurization system comprises a pressurization vessel, the pressurization gas is fed into the lower portion of the pressurization vessel, and the pressurized ozone-containing gas is withdrawn from the upper portion of the pressurization vessel.
  • the pressurization system comprises a first pressurization vessel and a last pressurization vessel. In this embodiment, the pressurization vessels are fluidly connected in series and the pressurizing gas is fed exclusively to the first pressurization vessel.
  • the current inventive method also provides a method to produce an ozonated liquid by feeding an ozone-containing gas from the ozone source to an ozone pressurization system to establish a first pressure, pressurizing the ozone pressurization system by feeding a pressurization gas into the system; thus, raising the pressure of the ozone-containing gas to a second pressure and forming a pressurized ozone-containing gas.
  • This method also places a liquefied dry gas in an expansion vessel, and sparges the pressurized ozone- containing gas through the liquefied dry gas to form an ozonated liquefied dry gas, which is withdrawn from the expansion vessel.
  • Figure 1 is a schematic of an embodiment of the current invention for pressurizing ozone
  • Figure 2 is a schematic of another embodiment of the current invention for pressurizing ozone
  • Figure 3 is a schematic of yet another embodiment of the current invention for pressurizing ozone
  • Figure 4 is a schematic of still another embodiment of the current invention for pressurizing ozone
  • - Figure 5 is a schematic of an embodiment for pressurizing ozone and producing an ozonated liquefied gas according to the current invention
  • Figure 6 is a graph showing the concentrations of ozone in a liquefied gas attained by the current method of the current invention.
  • the current invention provides a method of pressurizing an ozone- containing stream without destroying the ozone or contaminating the ozone- containing stream with oil or water. Furthermore, the method forms an ozonated liquefied dry gas by bubbling the pressurized ozone-containing stream through a reservoir of liquefied dry gas.
  • the current invention pressurizes ozone by feeding an ozone- containing source to an ozone pressurization system to establish a first pressure followed by pressurizing the ozone pressurization system.
  • the ozone pressurization system is pressurized by feeding a pressurization gas to the ozone pressurization system to raise the pressure to the second pressure and form a pressurized ozone-containing gas.
  • the pressurized ozone- containing gas is then withdrawn from the ozone pressurization system.
  • the pressurization gas is a dry gas.
  • One preferred dry gas is CO2.
  • the method pressurizes the ozone-containing stream without contaminating the stream with oil or water.
  • the method preferable pressurizes the ozone-containing stream to a pressure that is greater than about 150 psig. Furthermore, the method can pressurize the ozone-containing stream from a pressure of less than about 50 psig to a pressure that is preferably greater than about 150 psig and even more preferably greater than about 200 psig.
  • the ozone pressurization system comprises a pressurization vessel, the pressurization gas is fed into the lower portion of the pressurization vessel, and the pressurized ozone-containing gas is withdrawn from the upper portion of the pressurization vessel.
  • the pressurization system comprises a first pressurization vessel and a last pressurization vessel.
  • the pressurization vessels are fluidly connected in series and the pressurizing gas is fed exclusively to the first pressurization vessel.
  • the pressurized gas mixture is withdrawn from the first pressurization vessel and fed to the last pressurization vessel, while the pressurized ozone-containing gas is withdrawn from the last pressurization vessel.
  • the pressurization gas is fed into a lower portion of the first pressurization vessel while the pressurized gas mixture is withdrawn from an upper portion of that first pressurization vessel.
  • the pressurized gas mixture is then fed into a lower portion of the last pressurization vessel and the pressurized ozone-containing gas is finally withdrawn from an upper portion of the last pressurization vessel.
  • the pressurization system comprises a number of pressurization vessels in series and includes the steps of withdrawing a pressurized gas mixture from the first pressurization vessel, feeding the pressurized gas mixture to a successive pressurization vessel, and transferring the pressurized gas mixture from the successive pressurization vessel to the last pressurization vessel.
  • This embodiment like those above withdraws the pressurized ozone-containing gas from the last pressurization vessel.
  • One further embodiment of this method feeds the pressurization gas into a lower portion of the first pressurization vessel, withdraws the pressurized gas is from an upper portion of the first pressurization vessel, feeds the pressurized gas mixture into a lower portion of the successive pressurization vessel, withdraws that pressurized gas from an upper portion of the successive pressurization vessel, and ultimately transfers the pressurized gas mixture into a lower portion of the last pressurization vessel.
  • the current inventive method also provides an ozonated liquid by feeding an ozone-containing gas from the ozone source to an ozone pressurization system to establish a first pressure, pressurizing the ozone pressurization system by feeding a pressurization gas into the system thus raising the pressure of the ozone-containing gas to a second pressure and forming a pressurized ozone-containing gas.
  • the method also places a liquefied dry gas in an expansion vessel, and sparges the pressurized ozone- containing gas through the liquefied dry gas to form an ozonated liquefied dry gas, which is withdrawn from the expansion vessel.
  • This method may further include steps of withdrawing a vent gas from the expansion tank and recycling the vent gas to a liquefied dry gas storage vessel.
  • the sparging occurs substantially continuously.
  • one embodiment of the current method provides an ozone-containing gas 102 from an ozone source 104.
  • Ozone can be generated in commercially available ozone generator known to one of ordinary skill in the art.
  • the ozone generation unit preferably uses a pure oxygen feed, to form the ozone-containing gas 102, which preferably contains about 6 to about 13 wt% ozone in oxygen, and more preferably about 9 to about 11 wt% ozone.
  • the ozone pressurization system 106 is purged with the ozone-containing gas 102 to establish a concentration of ozone in the entire ozone pressurization system 106.
  • the ozone pressurization system 106 is pressurized with the ozone-containing gas 102 to set an initial pressure, for instance about 5 to about 25 psig, in the entire ozone pressurization system 106.
  • an initial pressure for instance about 5 to about 25 psig
  • the entire ozone pressurization system 106 is then isolated from the ozone generator.
  • the ozone-containing gas 102 is pressurized in an ozone pressurization system 106 to form a pressurized ozone-containing gas 108.
  • the ozone-containing gas 102 is fed to the ozone pressurization system 106 to establish a concentration of ozone-containing gas throughout the ozone pressurization system 106 at first pressure in the ozone pressurization system 106.
  • the first pressure is preferably less than about 100 psig, more preferably less than about 50 psig and even more preferably less than about 30 psig.
  • a pressurization gas 110 is fed to the ozone pressurization system 106 to raise the pressure in the ozone pressurization system 106 to a second pressure.
  • the pressurization gas 110 enters the ozone pressurization system 106, the ozone-containing gas in the ozone pressurization system 106 is compressed. It is believed that if the density of the pressurization gas 110 and the ozone-containing gas 102 is substantially different, the gases stratify in the tanks and mixing is minimal. The final result is a compressed ozone-containing feed mixture typically containing close to, but somewhat lower concentration of ozone in oxygen that the ozone-containing gas 102 in the upper portion of any vessels in the ozone pressurization system 106.
  • the pressurization gas 110 feed to the ozone pressurization system 106 is stopped when the desired second pressure is reached.
  • the pressurized ozone-containing gas 108 is then withdrawn from the ozone pressurization system 106.
  • the ozone pressurization system 106 preferably comprises at least one pressurization vessel 112.
  • the pressurization gas 110 is preferably fed to a lower portion of the pressurization vessel 112 and more preferably fed to the bottom portion of the pressurization vessel 112.
  • the pressurized ozone- containing gas 108 is preferably removed from an upper portion of the pressurization vessel 112 and more preferably removed from the top of the pressurization vessel 112.
  • the pressurization gas 110 is fed at a slow flow rate to the pressurization system 106 in order to minimize the mixing for the ozone-containing gas 102 and the pressurization gas 110. It is preferable to maintain laminar flow rates in the pressurization vessel 112.
  • the pressurization gas 110 is fed to the pressurization vessel to raise the pressure in the ozone pressurization system 106 to a second pressure of greater than about 100 psig, more preferably greater than about 150 psig, and even more preferably greater than about 200 psig. Then, the pressurized ozone-containing gas 108 can be withdrawn from the ozone pressurization system 106. Using this method, it is feasible to pressurize an ozone-containing stream to pressures of greater than about 500 psig and even greater than about 1 ,000 psig without destroying the ozone. Furthermore, a substantial portion of the ozone (O3) remains relatively undiluted. Still further, the resulting pressurized ozone-containing gas 108 is substantially free of oil, water, or other undesirable contaminants. In one preferred embodiment, the pressurized ozone-containing gas 108 contains less than about
  • 0.05 wt% water preferably contains less than about 200 ppm wt water, and more preferably less than about 20 ppm wt water.
  • One preferred pressurization gas 110 is a dry gas.
  • the dry gas can be any suitable non-aqueous gas, but is preferably a liquefied gas, particularly a liquefied gas with a high gas density compared to the ozone-containing gas 102.
  • the dry gas preferably contains less than 0.05 wt% water, and more preferably containing less than 20 ppm wt water.
  • the pressurization gas 110 is preferably a dry gas that is stored as a liquid, such as CO 2 .
  • the liquefied dry gas is removed from the liquid storage vessel and expanded to form the pressurization gas 110.
  • One preferred embodiment uses a pressurization gas 110 that has a gas density that is higher that the gas density of the ozone-containing gas 102.
  • This pressurization gas 110 is preferably cold after expansion to provide a pressurization gas at the highest gas density possible for that gas.
  • the pressurization gas is preferably less than about 2O 0 C after expansion, and more preferably less than about 10 0 C after expansion.
  • the concentration of ozone in the pressurized ozone-containing gas 108 is at least about 70% of the concentration of ozone in the ozone- containing gas 102, more preferably at least 80% of the concentration of ozone in the ozone-containing gas 102, and even more preferably at least about 90% of the concentration of ozone in the ozone-containing gas 102.
  • a continuous flow of pressurized ozone gas 110 is supplied by using a plurality of ozone pressurization systems 106 operated in a "round robin" to maximize the use of the ozone generator and minimize the waste of pressurization gas 110 by cross-tying (not shown) the sets of ozone pressurization systems 106.
  • one embodiment of the current method utilizes an ozone pressurization system 106 that comprises a plurality of pressurization vessels, which comprise at least a first pressurization vessel 202 and a last pressurization vessel 204.
  • An upper portion of the first pressurization vessel 202 and a lower portion of the last pressurization vessel 204 are connected by a fluid connection means 206.
  • the fluid connection means can be any type or combination of pipe, conduit, vessel, valve, orifice, chamber, or other flow passage that allows a pressurized gas mixture to flow from one vessel to another.
  • One preferred fluid connection means 206 has at least part of the means that is smaller in diameter than the first pressurization vessel 202 or the last pressurization vessel 204.
  • a pressurized gas mixture is withdrawn (or pushed) from the upper portion of the first pressurization vessel 202 and fed into a lower portion of the last pressurization vessel 204 as the pressurization gas 110 is fed into the lower portion of the first pressurization vessel 202.
  • the first pressurization vessel 202 will be completely filled with a gas mixture that primarily comprises the pressurization gas 110. Having a plurality of pressurization vessels helps prevent the pressurization gas 110 from mixing with the ozone-containing gas 102.
  • the compressed ozone-containing gas 110 is withdrawn from the last pressurization vessel 204.
  • the last pressurization vessel 204 is preferably isolated from any upstream pressurization vessels to prevent unwanted dilution of the pressurized ozone mixture.
  • the pressure from the last pressurization vessel 204 is allowed to drop as the ozone-containing gas 110 is fed to the process.
  • one embodiment of the current method uses a plurality of pressurization vessels comprising more than two pressurization vessels fluidly connected in series.
  • the ozone-containing gas 102 is first fed to fill the plurality of pressurization vessels with the ozone-containing gas 102 at a first pressure.
  • the pressurization gas 110 is fed into a first pressurization vessel 202 in the series of pressurization vessels and the pressurized ozone-containing gas 108 flows out of a last pressurization vessel 204 in the series of pressurization vessels.
  • the embodiment of Figure 3 uses an ozone pressurization system that comprises a first pressurization vessel 202, a successive pressurization vessel 303, and a last pressurization vessel 204.
  • a pressurized gas mixture is withdrawn from the first pressurization vessel 202 and fed to the successive pressurization vessel.
  • the pressurized gas mixture then flows from the successive pressurization vessel to the last pressurization vessel 204.
  • the pressurized ozone- containing gas 108 is then withdrawn from the last pressurization vessel 204 after the ozone pressurization system 106 reaches a second pressure.
  • the pressurization gas is fed into a lower portion of the first pressurization vessel 202.
  • a pressurized gas mixture is withdrawn from an upper portion of the first pressurization vessel 202 and fed into a lower portion of the successive pressurization vessel 302 via a first conduit 304.
  • the pressurized gas is then withdrawn from an upper portion of the successive pressurization vessel 302 and transferred into a lower portion of the last pressurization vessel 204 via a second conduit 306.
  • the pressurized ozone-containing gas 108 is withdrawn from the upper portion of the last pressurization vessel 204 after the ozone pressurization system 106 reaches a second pressure.
  • the ozone pressurization system 106 comprises a first pressurization vessel 202, at least two successive pressurization vessels 402, 404, and a last pressurization vessel 204, all fluidly connected in series.
  • the ozone-containing gas 102 is first fed to fill all of the pressurization vessels 202, 204, 402, 404 with the ozone-containing gas 102 at a first pressure.
  • the pressurization gas 110 is fed into a first pressurization vessel 202 and the pressurized ozone-containing gas 108 flows out of a last pressurization vessel 204.
  • a pressurized gas mixture is withdrawn from the first pressurization vessel 202 and fed to the successive pressurization vessels 402 and 404 in series via a plurality of gas transfer conduits 406, 408, 410.
  • the pressurized gas mixture then flows from the successive pressurization vessels 402 and 404 to the last pressurization vessel 204.
  • the pressurized ozone-containing gas 108 is then withdrawn from the last pressurization vessel 204 after the ozone pressurization system 106 reaches a second pressure.
  • the incoming gases flow into the lower portions of the respective vessels and the outgoing gases exit the upper portions of the respective vessels.
  • a continuous supply of pressurized ozone feed is supplied.
  • the pressurization vessels upstream of the last pressurization vessel 204 are replenished with ozone-containing gas 102.
  • the tanks upstream of the last pressurization vessel 204 are vented of their pressure, purged, re-filled with the ozone-containing gas 102, and re-pressurized as described above.
  • This new batch of pressurized gas may then be released into the last pressurization vessel 204. This re-filling gives a slightly more dilute ozone mixture.
  • a more efficient arrangement consists of several sets of tanks, operated in a "round robin" to maximize the use of the ozone generator, capture all pressurized ozone that does not reach the last pressurization vessel 204, and minimize the waste of pressurization gas 110 by allowing the sets of tanks to be cross-tied.
  • the current inventive method also provides an ozonated liquefied dry gas 502 by transferring a liquefied dry gas 504 to an expansion vessel 506 and sparging the pressurized ozone-containing gas 110 through the liquefied dry gas to form the ozonated liquefied dry gas 502.
  • the liquefied dry gas 504 is stored in a liquefied dry gas storage vessel 508 at a pressure suitable to maintain the dry gas in liquid form.
  • the liquefied dry gas 504 is transferred to the expansion vessel 506 where the pressure is somewhat less than the pressure in the liquefied dry gas storage vessel 508.
  • the ozone pressurization system 106 pressurizes an ozone-containing gas 102 as described in the previous embodiments to form a pressurized ozone-containing gas 110 at a second pressure, which is above the pressure in the expansion vessel 506.
  • the second pressure is preferably at least about 50 psig above the pressure in the expansion vessel 506, and more preferably at least about 100 psig above the pressure in the expansion vessel 506.
  • the pressurized ozone-containing gas 110 is then sparged through the liquefied dry gas in the expansion vessel 506 to form the ozonated liquefied dry gas 502.
  • the ozonated liquefied dry gas is withdrawn from the expansion vessel 506 after sufficient sparging to assure the liquid contains a desired amount of ozone.
  • the expansion vessel 506 is substantially filled with the liquefied dry gas 504 and then the pressurized ozone-containing gas 110 is sparged through the liquid on a batch basis. In other embodiments, there is a continuous flow of liquefied dry gas 504 into the expansion vessel 506 and the pressurized ozone-containing gas 110 is sparged continuously through the liquid.
  • This method may further include steps of withdrawing a vent gas 510 from the expansion tank. In some embodiments, the vent gas 510 is fed to a recovery system 512 for recovery and recycling of the vent gas back to the liquefied dry gas storage vessel
  • one embodiment of the current invention uses CO 2 as the liquefied dry gas.
  • the pressure in the liquefied dry gas storage vessel 508 is about 200 to about 400 psig.
  • the liquefied dry gas 504 is transferred to the expansion vessel 506 where the pressure is preferably about 100 to about 200 psig, more preferably about 150 to 200 psig, and even more preferably about 200 to about 300 psig.
  • the ozone pressurization system 106 provides the pressurized ozone-containing gas 110 at a second pressure, which is above the pressure in the expansion vessel 506, preferably at least about 50 psig above the pressure in the expansion vessel 506, and more preferably at least about 100 psig above the pressure in the expansion vessel 506.
  • the ozonated liquefied dry gas is withdrawn from the expansion vessel 506 after sufficient sparging to assure the liquid CO 2 contains a desired amount of ozone.
  • an ozonated liquid CO2 can be supplied containing at least about 200 ppm wt ozone, and more preferably greater than about 250 ppm wt ozone.
  • the current method provides an ozonated liquid with a much higher concentration of ozone that the prior art methods of saturating water with ozone.
  • Another embodiment of the dry gas pressurization method described above is used to dose other liquids, including aqueous and dry (non-aqueous) liquids.
  • the dry gas compression method is used to ozonate a liquid, where the liquid is at pressures greater than about 150 psig.
  • a liquid is placed into a pressure vessel where the pressure is greater than about 150 (or is raised to above this pressure), preferably great than about 200 psig, and more preferably greater than about 300 psig.
  • the ozone pressurization system provides the pressurized ozone- containing gas at a second pressure, which is above the pressure in the pressure vessel, preferably at least about 50 psig above the pressure in the expansion vessel, and more preferably at least about 100 psig above the pressure in the expansion vessel.
  • the ozonated liquid is withdrawn from the pressure vessel after sufficient sparging to assure the liquid contains a desired amount of ozone.
  • any liquid which one skilled in the art wishes to saturate with ozone can be substituted for the liquefied dry gas of the current invention in the method.
  • the current invention may be used in a variety of processes for processing food, or non-food items. Therefore, the spirit and scope of the appended claims should not be limited to the description of the preferred versions contained herein.

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  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Chemical & Material Sciences (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Food Preservation Except Freezing, Refrigeration, And Drying (AREA)

Abstract

La présente invention se rapporte à des procédés de traitement et de purification d'aliments et d'autres objets ciblés, qui font appel à l'ozone, et à un procédé permettant d'obtenir un liquide renfermant une dose d'ozone sous pression. Le liquide à l'ozone selon l'invention est particulièrement utile pour traiter des aliments, des dispositifs de stockage d'aliments et des dispositifs de transport d'aliments, ainsi que pour traiter de l'eau ou d'autres objets cibles. L'invention concerne un procédé permettant de mettre sous pression un flux contenant de l'ozone sans détruire l'ozone ou contaminer le flux avec de l'huile ou de l'eau. Le flux contenant de l'ozone sous pression sert ensuite à dose un liquide, qui servira à son tour à purifier ou traiter un objet cible.
EP05856242A 2004-12-21 2005-12-19 Nouveau procede de production de liquides contenant une dose d'ozone sous pression Withdrawn EP1831599A2 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US63802004P 2004-12-21 2004-12-21
US11/145,137 US20050268646A1 (en) 2002-08-20 2005-06-03 Novel biological treating agent
US11/281,996 US20060168999A1 (en) 2002-08-20 2005-11-17 Novel method of dosing liquids with pressurized ozone
PCT/IB2005/003819 WO2006085135A2 (fr) 2004-12-21 2005-12-19 Nouveau procede de production de liquides contenant une dose d'ozone sous pression

Publications (1)

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EP1831599A2 true EP1831599A2 (fr) 2007-09-12

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US (1) US20060168999A1 (fr)
EP (1) EP1831599A2 (fr)
AU (1) AU2005326948A1 (fr)
CA (1) CA2591869A1 (fr)
WO (1) WO2006085135A2 (fr)

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GB2516959B (en) * 2013-08-08 2018-01-10 Intelligent Energy Ltd Gas filling apparatus and method
US10688450B2 (en) * 2016-07-14 2020-06-23 Espresso Amore System and method for gas impregnation of a liquid
CN110382944B (zh) * 2017-03-30 2021-10-01 全耐塑料高级创新研究公司 氢气存储系统
US20220395002A1 (en) * 2021-06-09 2022-12-15 Jo{hacek over (z)}ef Stefan Institute Method for deactivation of aflatoxins

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AU2005326948A1 (en) 2006-08-17
WO2006085135A2 (fr) 2006-08-17
US20060168999A1 (en) 2006-08-03
CA2591869A1 (fr) 2006-08-17
WO2006085135A3 (fr) 2007-03-15

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