EP4612361A1 - Arrangement and method in white liquor oxidation - Google Patents
Arrangement and method in white liquor oxidationInfo
- Publication number
- EP4612361A1 EP4612361A1 EP23800884.1A EP23800884A EP4612361A1 EP 4612361 A1 EP4612361 A1 EP 4612361A1 EP 23800884 A EP23800884 A EP 23800884A EP 4612361 A1 EP4612361 A1 EP 4612361A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- detector
- process flow
- white liquor
- amount
- wavelength range
- 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.)
- Pending
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
- D21C9/1068—Bleaching ; Apparatus therefor with O2
-
- 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
- D21C11/00—Regeneration of pulp liquors or effluent waste waters
- D21C11/0057—Oxidation of liquors, e.g. in order to reduce the losses of sulfur compounds, followed by evaporation or combustion if the liquor in question is a black liquor
-
- 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
- D21C3/00—Pulping cellulose-containing materials
- D21C3/02—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes
-
- 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
-
- 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
- D21C9/1026—Other features in bleaching processes
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/02—Details
- G01J3/10—Arrangements of light sources specially adapted for spectrometry or colorimetry
- G01J3/108—Arrangements of light sources specially adapted for spectrometry or colorimetry for measurement in the infrared range
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
Definitions
- the present disclosure relates to oxidation of white liquor in wood processing industry, and more particularly to an arrangement and a method in white liquor oxidation.
- oxidation of white liquor has been used since the commercialization of oxygen delignification, also known as oxygen bleaching.
- white liquor as an alkali source in oxygen bleaching has required oxidizing various sulphur forms to sulphates in an external vessel. This is done because if non-oxidized sulphurs are taken into the bleaching reactor, the oxygen atmosphere in the reactor would react to oxidize the non-oxidized sulphurs, which would consume the oxygen to undesired reactions and liberate heat, and thereby make temperature control in the reactor difficult.
- An object of the present disclosure is to provide a new arrangement and method in white liquor oxidation.
- the disclosure is based on the idea of determining an amount of at least one substance in the process flow by means of spectroscopy and use it for controlling white liquor oxidation process.
- the measurement is made using spectroscopy and online from the process flow without a need for taking samples and taking samples to a laboratory for detailed analysis.
- An advantage of the disclosure is that the measurements can be accurate and real time.
- the feedback time may be reduced considerably, and the process control improved.
- Figure 1 illustrates schematically some features related to a white liquor oxidation process according to an example
- Figure 2 illustrates an arrangement in white liquor oxidation
- Figure 3 illustrates a method in white liquor oxidation.
- the disclosure relates to an arrangement and a method in white liquor oxidation.
- Figure 1 illustrates schematically some features related to a white liquor oxidation process 100 according to an example. Different ways of implementing white liquor oxidation process are known, and it is known that related arrangements and details may vary. Therefore, these different examples are not discussed here in more detail and only one arbitrary example is disclosed in Figure 1 to illustrate some features and concepts.
- oxidation of white liquor is widely used in connection with oxygen delignification, also known as oxygen bleaching.
- oxygen delignification also known as oxygen bleaching.
- white liquor as an alkali source in oxygen bleaching precludes that various sulphur forms, usually mostly sodium sulphide, are oxidized to sulphates in an external vessel 110. This is important, because if non-oxidized sodium sulphide is taken into a bleaching reactor, oxygen atmosphere in the reactor would oxidize the Na2S, which in turn would liberate heat and thereby make the temperature control in the reactor difficult.
- thiosulphate causes cellulose degradation, and it is also corrosive to many of bleaching reactor materials, whereby the amount of thiosulphate should be kept as low as possible in oxidized white liquor (OWL).
- Figure 2 illustrates an arrangement in white liquor oxidation.
- An arrangement 1 in white liquor oxidation in other words an arrangement in connection with white liquor oxidation, such as the arrangement 1 in white liquor oxidation of Figure 2, comprises a detector 2 arranged inside an oxidized white liquor process flow, in other words inside a white liquor oxidation process flow, and configured to measure at least one characteristic of the process flow by means of spectroscopy.
- This enables providing an inline measurement, in other words a measurement directly from the process flow by a detector 2 provided in the process flow, which is a real time measurement, as compared to samples taken to a laboratory for measurements.
- the arrangement 1 in white liquor oxidation also comprises a controller 3 connected to the detector 2 to receive measurement data from the detector 2.
- the controller 3 is also configured to determine an amount of at least one substance in the process flow based on the measurement data.
- the controller 3 is further configured to control the white liquor oxidation process based on the determined amount of the at least one substance.
- the controller 3 may comprise a control system of the arrangement 1 or a part of a control system of the arrangement 1 .
- the controller 3 may comprise a control unit and/or a regulator.
- the detector 2 may comprise an infrared spectrometer. More particularly, infrared spectrometer may be used to measure the concentration of compounds, for instance in one or more measurement points of the process, using infrared spectroscopy. According to an embodiment, the detector 2 more particularly may comprise a Fourier Transform Infrared (FTIR) Spectroscopy spectrometer.
- FTIR Fourier Transform Infrared
- FTIR Fourier-transform infrared spectroscopy
- An advantage of such embodiments is that an FTIR spectrometer can simultaneously collect high-resolution spectral data over a wide spectral range. FTIR spectrometers are known as such and are, thus, not explained here in more detail.
- Detectors 2 based on spectroscopy typically have a wavelength range, within which the detector 2 can be used and/or is configured to be used.
- the detector 2 may be configured to use the whole wavelength range of the detector 2, when making the measurements disclosed in this description and accompanying claims and figures.
- the detector 2 may be a spectrometer configured to use midinfrared wavelength range in the measurement.
- the detector 2 may be a spectrometer configured to use a wavelength range of 400-4000 cm 1 .
- the detector 2 may be a spectrometer configured to use a wavelength range of 648 - 4000 cm 1 .
- the detector 2 may be a spectrometer configured to use a wavelength range of 800 - 1220 cm 1 , and according to a further embodiment, the detector 2 may be a spectrometer configured to use a wavelength range of 1000 - 1168 cm 1 . In some embodiments, it may be beneficial to use a wider range of wavelengths. This may be true for instance in embodiments, in which multiple characteristics of the process flow, for instance amount, such as concentrations, of multiple substances a measured.
- the strongest correlations for sulphur forms, such as sulphite, sulphate and thiosulphate may be found within the wavelength range of 800 - 1220 cm 1 or 1000 - 1168 cm 1 ., for example, whereby it may be beneficial to use one of these ranges.
- the detector 2 may be arranged inside the oxidized white liquor process flow by mounting the detector to a line and/or a vessel of the process flow. According to an embodiment, the detector 2 may be arranged to the line and/or vessel of the process flow by means of a mounting flange, directly to the line or vessel and/or in another manner suitable for the type of the detector 2 in question.
- a vessel may comprise any type of a vessel, container, receptacle or similar suitable for receiving the material or process flow in question.
- the amount of at least one substance in the process flow may comprise at least one of the following: an amount of sulphite in the process flow material, an amount of sulphate in the process flow material and an amount of thiosulphate in the process flow material.
- the amount of at least one substance in the process flow may comprise the amount of sulphite, sulphate and thiosulphate in the process flow material measured by means of spectroscopy.
- the controller 3 may be configured to adjust at least one of the white liquor and oxygen process flow in the white liquor oxidation process based on the determined amount of at least one substance in the process flow to ensure sufficient oxidization of the oxidized white liquor for the purpose of oxygen bleaching.
- the oxidized white liquor may comprise at least one of the following: partly oxidized white liquor and totally oxidized white liquor (TOWL).
- the process flow in which the amount of at least one substance is measured, comprises oxidized white liquor, more particularly totally or partly oxidized white liquor.
- the controller 3 may be further configured to adjust process temperature in the white liquor oxidation process to an optimal reaction temperature based on the determined amount of at least one substance in the process flow to ensure sufficient oxidization of the white liquor for the purpose of oxygen bleaching.
- process temperature may be adjusted to improve oxygen solubility and to optimize oxygen consumption to desired reactions. Oxidation reactions are exothermic, whereby lowering the temperature may enhance at least some of the oxidation reactions. The process temperature may also affect the delays in the oxidation reactions.
- Figure 3 illustrates a method in white liquor oxidation.
- a method in white liquor oxidation may comprise the steps of: measuring 31 by a detector 2 arranged inside an oxidized white liquor process flow at least one characteristic of the process flow by means of spectroscopy; receiving 33 in a controller 3 connected to the detector 2 measurement data from the detector 2; determining 35 by the controller 3 an amount of at least one substance in the process flow based on the measurement data received from the detector; and controlling 37 the white liquor oxidation process based on the determined amount of the at least one substance.
- the method in white liquor oxidation may be implemented using an arrangement in white liquor oxidation according to an embodiment or a combination of embodiments disclosed in this description and/or accompanying claims and drawings.
- the detector 2 may be arranged inside the oxidized white liquor process flow by mounting the detector to a line or a vessel of the process flow.
- the amount of at least one substance in the process flow may comprise at least one of the following: an amount of sulphite in the process flow material, an amount of sulphate in the process flow material and an amount of thiosulphate in the process flow material.
- the method further comprise adjusting by the controller at least one of the white liquor and oxygen process flow in the white liquor oxidation process based on the determined amount of at least one substance in the process flow to ensure sufficient oxidization of the white liquor for the purpose of oxygen bleaching.
- An advantage of the disclosure is that measuring and controlling quality of oxidized white liquor using on-line spectroscopy, preferably an FTIR measurement system, enables fulfilling required quality aspects in a more economical manner than in the known solutions.
- Measuring the quality of oxidized white liquor may, then, comprise measuring the content of sulphite, sulphate, and thiosulphate ions in the process flow. These measurements also enable adjusting both white liquor and oxygen process flows on-line in an effective and efficient manner.
Landscapes
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- General Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Inorganic Chemistry (AREA)
- Paper (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FI20225977A FI132034B1 (en) | 2022-11-02 | 2022-11-02 | SYSTEM AND METHOD FOR WHITE LIQUEFY OXIDATION |
| PCT/FI2023/050601 WO2024094924A1 (en) | 2022-11-02 | 2023-10-27 | Arrangement and method in white liquor oxidation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| EP4612361A1 true EP4612361A1 (en) | 2025-09-10 |
Family
ID=88695648
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP23800884.1A Pending EP4612361A1 (en) | 2022-11-02 | 2023-10-27 | Arrangement and method in white liquor oxidation |
Country Status (5)
| Country | Link |
|---|---|
| EP (1) | EP4612361A1 (en) |
| CN (1) | CN120129776A (en) |
| CL (1) | CL2025001251A1 (en) |
| FI (1) | FI132034B1 (en) |
| WO (1) | WO2024094924A1 (en) |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020053640A1 (en) * | 1998-11-12 | 2002-05-09 | Michael Kester | Determination of ionic species concentration by near infrared spectroscopy |
| US7390669B2 (en) * | 2000-02-24 | 2008-06-24 | Georgia Tech Research Corporation | Simultaneous and rapid determination of multiple component concentrations in a Kraft liquor process stream |
| WO2007006150A1 (en) * | 2005-07-13 | 2007-01-18 | Fpinnovations | Method for quantitative determination of individual polysulphide species in oxidized white liquors by means of raman spectroscopy |
-
2022
- 2022-11-02 FI FI20225977A patent/FI132034B1/en active
-
2023
- 2023-10-27 WO PCT/FI2023/050601 patent/WO2024094924A1/en not_active Ceased
- 2023-10-27 EP EP23800884.1A patent/EP4612361A1/en active Pending
- 2023-10-27 CN CN202380075492.8A patent/CN120129776A/en active Pending
-
2025
- 2025-04-25 CL CL2025001251A patent/CL2025001251A1/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| FI132034B1 (en) | 2026-04-29 |
| FI20225977A1 (en) | 2024-05-03 |
| WO2024094924A1 (en) | 2024-05-10 |
| CN120129776A (en) | 2025-06-10 |
| CL2025001251A1 (en) | 2025-06-06 |
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Legal Events
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