EP1478803A2 - Method for ozone treatment of a liquid phase containing solid particles - Google Patents
Method for ozone treatment of a liquid phase containing solid particlesInfo
- Publication number
- EP1478803A2 EP1478803A2 EP03718869A EP03718869A EP1478803A2 EP 1478803 A2 EP1478803 A2 EP 1478803A2 EP 03718869 A EP03718869 A EP 03718869A EP 03718869 A EP03718869 A EP 03718869A EP 1478803 A2 EP1478803 A2 EP 1478803A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- contactor
- liquid phase
- ozone
- solid particles
- containing solid
- 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- Withdrawn
Links
Classifications
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/10—Bleaching ; Apparatus therefor
- D21C9/147—Bleaching ; Apparatus therefor with oxygen or its allotropic modifications
- D21C9/153—Bleaching ; Apparatus therefor with oxygen or its allotropic modifications with ozone
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/26—Nature of the water, waste water, sewage or sludge to be treated from the processing of plants or parts thereof
- C02F2103/28—Nature of the water, waste water, sewage or sludge to be treated from the processing of plants or parts thereof from the paper or cellulose industry
Definitions
- the invention relates to a process for ozonating a liquid phase containing solid particles. It relates more particularly to a process for ozonating paper pulps.
- Ozone is increasingly used in the treatment of paper pulp both virgin and from old paper to be recycled.
- ozonation steps are introduced in the processes for manufacturing virgin paper pulps, in particular for the bleaching of these paper pulps.
- Ozonation stages are also implemented in the waste paper treatment processes with a view to their recycling, for their bleaching, their defluorescence, their deinking, and the elimination of the microorganisms and enzymes brought in by the waste paper.
- Both virgin and recycled paper pulp can be likened to a liquid phase containing solid particles, the solid particles being disintegrated paper.
- a pulp ozonization process is known in which the pulp is ozonated while it has a solids concentration of between about 25 to 40% by weight relative to the total weight of the pulp.
- mixers known in the stationery profession are used under the name of "dynamic mixer” which are in practice centrifugal pumps.
- the reaction takes place here under pressure and the residence time is approximately a few seconds.
- the paper fiber is also subject to significant mechanical stresses which can deteriorate it.
- the reaction taking place under pressure it is necessary in this process to compress the ozone. Compressors are expensive to purchase and require significant maintenance.
- Ozone is also used in many other areas of the industry to ozonate solids in a liquid phase. The same problems then arise.
- the invention aims to overcome the drawbacks of the ozonation processes of the prior art by proposing a process for ozonization of a paste comparable to a liquid phase containing solid particles which makes it possible to limit the mechanical stresses exerted on the paste, to obtain a homogeneous ozonation of the dough and to reduce and even eliminate the stage of compression of the ozone.
- the invention provides a process for ozonating a liquid phase containing solid particles by contacting with gaseous ozone, characterized in that it is implemented in a two-phase tubular contactor of the type gas-liquid operating in a co-current of liquid and gas and in that the liquid phase containing solid particles is introduced into the contactor at a solid concentration of between 0.5 and 5% by weight relative to the total weight of the liquid phase containing solid particles.
- the liquid phase containing solid particles is introduced into the contactor at a solid concentration of between 0.5 and 3% by weight relative to the total weight of the liquid phase containing solid particles.
- the ozone is introduced into the contactor in the form of a gaseous air-ozone or oxygen-ozone mixture.
- the ozone is introduced into the contactor in the form of a gas mixture containing between 50 and 200 g of ozone per m 3 of gas mixture.
- the ozone or the gaseous mixture is preferably introduced into the contactor at a speed greater than 0.5 m / s and less than or equal to 10 m / s.
- the contactor is implemented in wave mode.
- the contactor is implemented in plug mode.
- the ozone or the gaseous mixture is introduced into the contactor at a speed of between 0.5 and 2 m / s and the liquid phase containing solid particles is introduced into the contactor at a speed of between 0.5 and 2 m / s.
- the tubular contactor is a horizontal tubular stainless steel contactor having an internal diameter and a length allowing, given the pulp flow rate, to obtain the rates of introduction of the liquid phase and of the 'ozone or gas mixture between 0.5 and 2 m / s.
- FIG. 1 schematically shows a sectional view of a two-phase tubular contactor of the gas-liquid type operating in segregated regime
- FIG. 2 schematically represents a sectional view of a two-phase tubular contactor of the gas-liquid type operating in regime wave
- FIG. 3 schematically represents a sectional view of a two-phase tubular contactor of the gas-liquid type operating in plug mode
- FIG. 4 shows schematically a sectional view of a two-phase tubular contactor of the gas-liquid type operating in dispersed bubble regime.
- ozone allows it to react quickly to most of the major functions of organic chemistry, and in particular to all the unsaturated benzene or phenolic groups often present, especially in waste paper.
- ozone destroys microorganisms such as bacteria, fungi, yeasts, as well as enzymes like the catalase enzyme often present, especially in waste paper.
- Ozone therefore finds a particular application during the manufacture of paper pulps, whether these are virgin or old paper to be recycled.
- ozone can be used in many pulp manufacturing processes to whiten pulps, remove dyes, optical brighteners, adhesives and inks, as well as to sanitize the circuits of the facilities in which one puts implements the manufacturing processes.
- the ozonation processes in particular pulp, whether these are virgin or from old paper, take place at a solids concentration of between 8 and 40 g of solids per 100 g of dough.
- paper pulps can be assimilated to a liquid medium, in general an aqueous medium, in which solid particles, in particular of wood fibers, are in suspension, during the ozonation reaction, we are then in the case of a mixture which can be assimilated to a two-phase mixture: a gas phase and a liquid phase containing solid particles.
- a mixture which can be assimilated to a two-phase mixture a gas phase and a liquid phase containing solid particles.
- the chemical reaction of ozonation of solids being rapid, it is necessary to have a very rapid rate of dissolution of the gas in said liquid phase containing solid particles so that the ozone reacts rapidly with all of the solid particles and that the reaction is not limited by the rate of dissolution of ozone.
- the terms “low consistency paper pulp” designate a paper pulp and by extension a liquid-solids mixture, the concentration of solid particles of which is between 0.5 and 5% by weight relative to the total weight of the liquid / solid mixture.
- concentration of solid particles of the paste will be determined by the passage of the paste from a Newtonian behavior to a non-Newtonian behavior; this value depends on the type of wood.
- very low consistency pulp denote pulp and by extension a mixture liquid-solids, the concentration of solid particles of which is approximately 1% by weight relative to the total weight of the liquid-solid mixture.
- the ozonation process of the invention is therefore characterized in that it is implemented in a two-phase tubular contactor of the gas-liquid type and in that the liquid phase containing solid particles at low or very low is introduced consistency.
- the tubular contactor for implementing the method of the invention can be a horizontal or vertical tubular contactor, or of any intermediate inclination, operating cocurrently with the liquid phase containing solid particles.
- the gas can be introduced by a simple pipe or by a more sophisticated system, for example a static mixer.
- the rate of dissolution of ozone in the liquid phase containing solid particles is a function of the gas-liquid mass transfer coefficients, the aim here is to obtain a good gas-paste emulsion.
- the reactor will operate in segregated mode, in wave mode, in plug mode or in dispersed bubble mode.
- FIG. 1 represents a diagrammatic section of a horizontal tubular contactor T operating in segregated regime in which the gas phase is denoted 1 and the liquid phase containing solid particles is denoted 3.
- the interfacial area is represented by the contact surface between the gas phase 1 and the liquid phase 3.
- This contact surface 2 when the tubular contactor is in segregated mode, as shown in FIG. 1, can be assimilated to a flat surface.
- the interfacial area corresponding to the contact surface 2 is less important than in the cases represented in FIGS. 2 to 4 which will be discussed below. For this reason, the ozone dissolution rate is less favorable.
- Such a segregated regime is obtained when the respective rates of introduction of the gas phase and of the liquid phase are less than 0.5 m / s.
- the contact surface between the gas phase and the liquid phase containing solid particles is improved when, the contactor T operates in wave regimes, as shown in FIG. 2.
- the contact surface denoted 2 ′ between the gas phase 1 and the liquid phase containing solid particles 3, forms waves.
- the contact surface is increased in this area. The dissolution of the gas therefore takes place more quickly in this case than in the case shown in FIG. 1, that is to say in a segregated regime.
- the gas phase 1 therefore has a contact surface denoted 2 "high with the liquid phase 3 when the contactor operates in such a plug regime.
- the contactor T operates in wave mode or in plug mode when the respective introduction speeds of the gas phase and the liquid phase containing solid particles are between 1 and 2 m / s.
- the contactor is in a dispersed bubble flow regime, as shown in FIG. 4.
- the liquid phase 3 forms bubbles which are dispersed in the gas phase 1 and the contact surface 2 ' "between the gas phase 1 and the liquid phase containing solid particles 3 is very high.
- Such a dispersed bubble regime is obtained for respective rates of introduction of the gas and of the liquid phase containing solid particles greater than 2 m / s and which can range up to 10 m / s.
- the ozonation process of the invention can be implemented in the contactor T operating in segregated mode, in wave mode, in plug mode or in bubble mode dispersed, it will preferably be implemented in wave mode or in plug mode, that is to say with gas introduction speeds between 0.5 and 2 m / s and introduction speeds of the liquid phase containing solid particles between 0.5 and 2 m / s.
- the introduction speeds mentioned above and in what follows are the speeds obtained when the contactor T is empty.
- the gas introduction rate will be calculated as a function of the internal section of the contactor used so as to obtain a gas introduction speed of between 0.5 and 2 m / s when the contactor does not contain any phase. liquid containing solid particles.
- the speed of introduction of the liquid phase containing solid particles will be calculated according to its rate of introduction into the empty contactor and according to the internal section of the contactor.
- a gaseous mixture containing ozone and a carrier gas such as for example air or oxygen at high concentrations of ozone.
- Ozone is very reactive, and the quantities of ozone required are generally low; for example, in the case of paper pulps, they are less than 20 kg / t of pulp. Thus, it has been determined that an ozone-air gas mixture containing between 50 and 200 g of ozone per m 3 of gas mixture is entirely suitable.
- a horizontal stainless steel tubular contactor having an internal diameter of 4.5 cm and a length of 100 m is used.
- the contactor is supplied with a virgin pulp having a consistency of 2.5%.
- the flow rate of the paper pulp is calculated so as to obtain pulp speeds (in the empty contactor) of between 1 and 2 m / s.
- the same speeds are used for the gas mixture consisting of a mixture of air and ozone having an ozone content of 100 g / m 3 of mixture. Under these conditions, the pressure drops are 2 to 3 bars.
- the ozone transfer capacity is then 1.5 to 3 kg / t of pulp for a residence time of the order of one minute.
- the pressure drops from 2 to 3 bars are low enough to be compatible with existing ozone compression systems, and even without a compressor, if the ozonator accepts a slight overpressure. Installation is therefore inexpensive and easy to use.
- the method of the invention may be applied to the ozonation of all other phases comparable to a liquid phase containing solid particles and in particular papers to be recycled, as long as the solid content does not exceed
- tubular contactor has been described as being of stainless steel, it may be of any other material compatible with wet ozone.
- tubular contactor has been described as having an internal diameter of 4.5 cm and a length of 100 m, its dimensions may be different, the main thing being that its dimensions allow the dough to remain in the contactor for the time necessary for the completion of the ozonization reaction, taking into account the feed rate of the dough into the contactor.
- gas mixture is generally an air-ozone or oxygen-ozone mixture
- any other gas or gas mixture which does not react with ozone may be used as carrier gas
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Paper (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
Description
Claims
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR0202023A FR2836163B1 (en) | 2002-02-18 | 2002-02-18 | PROCESS FOR OZONATION OF A LIQUID PHASE CONTAINING SOLID PARTICLES |
FR0202023 | 2002-02-18 | ||
PCT/FR2003/000462 WO2003070648A2 (en) | 2002-02-18 | 2003-02-12 | Method for ozone treatment of a liquid phase containing solid particles |
Publications (1)
Publication Number | Publication Date |
---|---|
EP1478803A2 true EP1478803A2 (en) | 2004-11-24 |
Family
ID=27636269
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP03718869A Withdrawn EP1478803A2 (en) | 2002-02-18 | 2003-02-12 | Method for ozone treatment of a liquid phase containing solid particles |
Country Status (7)
Country | Link |
---|---|
US (1) | US20050109475A1 (en) |
EP (1) | EP1478803A2 (en) |
JP (1) | JP2005517831A (en) |
AU (1) | AU2003222908A1 (en) |
CA (1) | CA2475684A1 (en) |
FR (1) | FR2836163B1 (en) |
WO (1) | WO2003070648A2 (en) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2836162B1 (en) * | 2002-02-18 | 2004-05-07 | Air Liquide | PROCESS FOR TREATING WASTE PAPER WITH OZONE |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2257327A1 (en) * | 1974-01-10 | 1975-08-08 | Commissariat Energie Atomique | Liq-gas exchange process for water treatment - using ozonised air bubbles to strike interface in con-current flow |
FR2662616B1 (en) * | 1990-05-31 | 1994-07-08 | Anjou Rech | INSTALLATION FOR THE TREATMENT OF LIQUID FLOWS WITH SINGLE-PHASE CONTACTOR, AND RECIRCULATOR-DEGASSER DEVICE FOR SUCH AN INSTALLATION. |
US5405497A (en) * | 1990-08-28 | 1995-04-11 | Kamyr, Inc. | Method of chemically reacting a liquid with a gas in a vortex |
FR2705333B1 (en) * | 1993-05-18 | 1995-08-04 | Omnium Traitement Valorisa | Process and installation for the purification of an aqueous effluent by oxidation on an adsorbent support. |
US6454871B1 (en) * | 1997-06-23 | 2002-09-24 | Princeton Trade & Technology, Inc. | Method of cleaning passageways using a mixed phase flow of gas and a liquid |
US6773547B2 (en) * | 1998-05-08 | 2004-08-10 | American Air Liquide, Inc. | Process for the bleaching of low consistency pulp using high partial pressure ozone |
FR2826309B1 (en) * | 2001-06-22 | 2003-10-31 | Goemar Lab Sa | TREATMENT OF LIGNOCELLULOSIC SUBSTRATES WITH OZONE |
-
2002
- 2002-02-18 FR FR0202023A patent/FR2836163B1/en not_active Expired - Fee Related
-
2003
- 2003-02-12 JP JP2003569564A patent/JP2005517831A/en active Pending
- 2003-02-12 CA CA002475684A patent/CA2475684A1/en not_active Abandoned
- 2003-02-12 WO PCT/FR2003/000462 patent/WO2003070648A2/en active Application Filing
- 2003-02-12 AU AU2003222908A patent/AU2003222908A1/en not_active Abandoned
- 2003-02-12 US US10/504,807 patent/US20050109475A1/en not_active Abandoned
- 2003-02-12 EP EP03718869A patent/EP1478803A2/en not_active Withdrawn
Non-Patent Citations (1)
Title |
---|
See references of WO03070648A2 * |
Also Published As
Publication number | Publication date |
---|---|
AU2003222908A8 (en) | 2003-09-09 |
AU2003222908A1 (en) | 2003-09-09 |
CA2475684A1 (en) | 2003-08-28 |
WO2003070648A2 (en) | 2003-08-28 |
US20050109475A1 (en) | 2005-05-26 |
WO2003070648A3 (en) | 2004-03-25 |
FR2836163B1 (en) | 2004-05-07 |
JP2005517831A (en) | 2005-06-16 |
FR2836163A1 (en) | 2003-08-22 |
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Legal Events
Date | Code | Title | Description |
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PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
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17P | Request for examination filed |
Effective date: 20040927 |
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Kind code of ref document: A2 Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IT LI LU MC NL PT SE SI SK TR |
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AX | Request for extension of the european patent |
Extension state: AL LT LV MK RO |
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RAP1 | Party data changed (applicant data changed or rights of an application transferred) |
Owner name: L'AIR LIQUIDE, SOCIETE ANONYME POUR L'ETUDE ET L'E |
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RAP1 | Party data changed (applicant data changed or rights of an application transferred) |
Owner name: L'AIR LIQUIDE, SOCIETE ANONYME POUR L'ETUDE ET L'E |
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17Q | First examination report despatched |
Effective date: 20091126 |
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STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: THE APPLICATION HAS BEEN WITHDRAWN |
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18W | Application withdrawn |
Effective date: 20100329 |