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WO2008144383A1 - Procédés pour détecter des contaminants organiques dans de la pâte et des fibres - Google Patents

Procédés pour détecter des contaminants organiques dans de la pâte et des fibres Download PDF

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Publication number
WO2008144383A1
WO2008144383A1 PCT/US2008/063693 US2008063693W WO2008144383A1 WO 2008144383 A1 WO2008144383 A1 WO 2008144383A1 US 2008063693 W US2008063693 W US 2008063693W WO 2008144383 A1 WO2008144383 A1 WO 2008144383A1
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WIPO (PCT)
Prior art keywords
organic contaminants
sample
fiber
pulp
hydrophobic dye
Prior art date
Application number
PCT/US2008/063693
Other languages
English (en)
Inventor
Robert A. Cooper
Christopher D. Perry
Stuart Johns
Original Assignee
Buckman Laboratories International, Inc.
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
Application filed by Buckman Laboratories International, Inc. filed Critical Buckman Laboratories International, Inc.
Priority to JP2010508570A priority Critical patent/JP2010529421A/ja
Priority to CN200880016268A priority patent/CN101680173A/zh
Priority to EP20080755527 priority patent/EP2145046A1/fr
Priority to CA 2685307 priority patent/CA2685307A1/fr
Priority to AU2008255038A priority patent/AU2008255038A1/en
Priority to MX2009011956A priority patent/MX2009011956A/es
Priority to BRPI0810276A priority patent/BRPI0810276A2/pt
Publication of WO2008144383A1 publication Critical patent/WO2008144383A1/fr

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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
    • D21C9/08—Removal of fats, resins, pitch or waxes; Chemical or physical purification, i.e. refining, of crude cellulose by removing non-cellulosic contaminants, optionally combined with bleaching
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/34—Paper
    • G01N33/343—Paper pulp
    • 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
    • D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
    • D21C5/02—Working-up waste paper
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/64—Paper recycling

Definitions

  • the present invention relates to pulp and fiber and more particularly relates to methods to detect and/or quantify organic contaminants, such as microstickies, present in pulp and fiber.
  • the first step in conventional recycling is to separate the paper into individual fibers with water to form a pulp slurry followed by removing ink and contaminants from the fibers by a combination of various process steps, such as screening, centrifugal cleaning, washing, flotation, and the like.
  • the screening and centrifugal cleaning step removes large contaminants, such as paperclips, staples, plastics, and the like.
  • the primary purpose of washing and flotation steps is to solubilize and/or suspend contaminants in the water and to remove the contaminants from the water.
  • Surfactants and caustic agents are added to facilitate the solubilization and separation of contaminants from the fibers. Once caustic agents are used, some yellowing of the fibers occurs which results in a need to bleach the fibers.
  • the fibers are blended with, typically, virgin fibers and then used in the papermaking process for which the fiber properties are suitable.
  • Recent developments in waste paper de-inking make use of enzymes to aid in the detachment and removal of inks from the fibers. These processes describe the use of particular types of enzymes to facilitate ink removal without the negative effects of caustic treatment on brightness along with the use of flotation to remove the agglomerated ink particles.
  • Stickies are generally adhesives, glues, hot melts, coatings, coating binders, ink residues, de-inking chemicals, wood resins, rosin, and unpulped wet strength resins that typically are present with the fiber to be recycled. These organic contaminants typically must be removed in substantial quantities so that they do not affect the subsequent processing steps. There is always a desire in the papermaking industry to develop new methods to remove such organic contaminants in more effective and environmentally friendly ways.
  • Stickies can be generally described as tacky, hydrophobic, pliable organic materials found in recycled paper systems. Stickies have a broad range of melting points and different degrees of tackiness dependent upon the composition of the stickies. Temperature, pH, concentration, size, and composition can affect the tackiness of stickies.
  • Recycled paper fibers contain many components that when repulped in recycle fiber plants become stickies. Recycled furnishes may have as many as a dozen different types of stickies, each having its own characteristics. Sources of stickies may include any of the following: adhesives, hot melts, coating binders, ink residues, deinking chemicals, wood resins, rosin, pitch, and wet strength resins.
  • the actual tacky deposits found on paper machines may be a combination of several of these organic contaminants as well as inorganic particles such as talc, clay, or calcium carbonate.
  • Stickies deposit on machine surfaces, fabrics, wires, felts, and rolls and lead to problems such as wet end breaks, pressroom breaks, dryer section breaks, holes, sheet defects, and high dirt counts. These deposits and associated problems lead to a significant amount of downtime yearly.
  • the cost of stickies has been estimated at over 500 million dollars annually in the U.S., when considering the cost of downtime, chemical costs, production losses, rejected materials, and customer complaints.
  • Mechanical methods include screening, cleaning, washing, floating, and disperging, with each method designed to remove a different size contaminant.
  • Screening typically removes larger or macro stickies (>0.004 inch or >100 microns).
  • Forward and reverse cleaners can be used. Based on density differences using centrifugal force, forward cleaners remove contaminants heavier than water and reverse cleaners remove particles lighter than water. This method removes more macro stickies than micro stickies.
  • Floating removes intermediate size stickies (50-300 microns), which are troublesome, because they're small enough to be accepted by screening and cleaning but too large to be removed by washing.
  • disperging the stock is thickened, passed through a device at high temperature, pressure, and shear, which breaks organic contaminants, including stickies, into smaller pieces.
  • Various chemical methods can be used. For instance, in pacification, additives like talc, clay, nonionic organic polymers, and other inorganic particles are used to render the stickies less tacky. In dispersion, dispersants, surfactants, and solvents are used to make stickies smaller. [00012] In fixation, the stickies are attached to the paper sheet by using a cationic water soluble polymer, which adds charge to the stickies. In disperse and fix, a dispersant is added first to reduce the size of the stickies and then a cationic polymer is used to fix the stickies onto the sheet.
  • Macrostickies are defined as stickies that are retained on a 0.10 mm (100 micron) screen plate (Heise, 1998). These contaminants which come from adhesives, coatings, binders, and other materials are incorporated into the furnish during the pulping process, and will deposit on forming fabrics, press felts, dryer fabrics, press section pick rolls, UhIe boxes, and calendar stacks (Douek, 1997). These materials remain tacky in the papermaking process, leading to the "stickies” label (Doshi, 1997). Once the materials are incorporated into the furnish, they are difficult to remove, since they are deformable in nature and are often close to the specific gravity of water.
  • a feature of the present invention is to provide methods to detect organic contaminants, e.g., microstickies, in pulp and fiber.
  • a further feature of the present invention is to provide methods to quantify organic contaminants present in pulp and fiber.
  • a further feature of the present invention is to provide methods to detect and/or quantify organic contaminants present in pulp and fiber on a real time basis.
  • An additional feature of the present invention is to provide a method to detect and/or quantify organic contaminants in pulp and fiber which provides an accurate reading and can be conducted at the papermill site.
  • the present invention relates, in part, to a method to detect organic contaminants in pulp and fiber.
  • the method includes obtaining a sample of the pulp and fiber and contacting the sample with at least one hydrophobic dye, such as a fluorescent hydrophobic dye or other excitable hydrophobic dye, wherein the hydrophobic dye stains the organic contaminants present in the sample.
  • the amount of organic contaminants can be measured by placing the sample under a microscope and contacting the sample with an appropriate energy source to excite the hydrophobic dye that may be present so that the organic contaminants are readily seen from amongst the pulp and fiber and other non-organic contaminant material. By doing so, the size of the contaminants, surface area of the contaminants, number of contaminants, and any other determination that can be made from observation can be determined.
  • the present invention further relates to organic contaminants in pulp and fiber with at least one hydrophobic dye that stains organic contaminants present in the pulp and fiber without staining the pulp and fiber.
  • Fig. 1 is a microphotograph showing organic contaminants that have been stained with a fluorescent dye and which are present amongst pulp and fiber which have not been stained.
  • Fig. 2 is a graph with plots of Krofta feed and accepts microstickies data measured in tests conducted in a paper production facility as described in the examples set forth hereinafter.
  • Fig. 3 is a graph with plots of paper machine (PM) headbox and PM Whitewater (WW) microstickies data measured in tests conducted in a paper production facility as described in the examples set forth hereinafter.
  • the present invention relates, in part, to methods to detect organic contaminants in pulp and fiber.
  • the present invention further relates to pulp and fiber containing organic contaminants, wherein the organic contaminants have been stained with at least one hydrophobic dye, and optionally wherein the pulp and fiber themselves have not been stained.
  • the present invention further relates to methods to quantify and/or otherwise analyze one or more characteristics of the organic contaminants present in pulp and fiber using one or more hydrophobic dyes.
  • examples of organic contaminants include what is known in the industry as "stickies” and include, but are not limited to, synthetic polymers resulting from adhesives and the like, glues, hot melts, coatings, coating binders, ink residues, de-inking chemicals, wood resins, rosin, and unpulped wet strength resins.
  • sticky include, but are not limited to, synthetic polymers resulting from adhesives and the like, glues, hot melts, coatings, coating binders, ink residues, de-inking chemicals, wood resins, rosin, and unpulped wet strength resins.
  • polymers e.g., thermoplastic(s) present, such as styrene butadiene rubber, vinyl acrylates, polyisoprene, polybutadiene, natural rubber, ethyl vinyl acetates, polyvinyl acetates, ethylvinyl alcohols, polyvinyl alcohols, styrene acrylates, and/or other synthetic type polymers.
  • microstickies are typically stickies having a particle size above 100 microns and microstickies are considered organic contaminant particles having a particle size of 100 microns or less (e.g., 10 microns to 100 microns).
  • the present invention is especially useful in detecting microstickies in pulp and fiber since, typically, microstickies can be effectively removed, as discussed above, using mechanical and/or chemical techniques. It would be quite beneficial to be able to detect and know information regarding the organic contaminants present in pulp and fiber, and especially microstickies, so as to assist a papermill in determining proper treatments, treatment levels, and/or whether treatment should be initiated or not based on the amount of microstickies present.
  • the present invention permits a papermill to be able to detect organic contaminants, especially microstickies, on a real time basis, thus permitting the papermill to tailor the treatment of microstickies based on real information, and/or to adjust treatment levels based on the amount of stickles present, which can save the papermill significant amounts of money, chemicals, and increase the efficiency of the papermill plant.
  • the present invention relates to a method to detect organic contaminants in pulp and fiber.
  • the method includes the step of obtaining a sample of the pulp and fiber and then contacting this sample with at least one hydrophobic dye, wherein the hydrophobic dye stains the organic contaminants present in the sample.
  • the hydrophobic dye does not stain the pulp and fiber present in the sample or at least does not significantly stain the pulp and fiber such that the staining of the organic contaminants is clearly distinguishable from the pulp and fiber.
  • the pulp and fiber can be any pulp and fiber that is used in a papermill.
  • the pulp and fiber can be virgin, recycled, or a blend of the two.
  • the fiber is typically cellulose fibers and more typically includes recycled fibers from one or a variety of paper products or fiber containing products, such as old corrugated containers (OCC), old newsprint (ONP), mixed office waste (MOW), or combinations thereof.
  • OCC old corrugated containers
  • OTP old newsprint
  • MOW mixed office waste
  • These types of paper containing products typically contain large amounts of organic contaminants which are present in the paper products. When these types of paper products are recycled, these organic contaminants are present along with the fibers formed during the pulping stage of a papermaking process. These organic contaminants, if not substantially removed, can severely interfere with subsequent stages in the papermaking process by affecting the quality of the resulting sheets of paper formed and/or affecting the machinery used to form the paper. Accordingly, the removal of such organic contaminants is important to the paper making process when such organic contaminants are present in fibers.
  • the sample of the pulp and fiber can be obtained at any stage (or multiple stages) of the papermaking process.
  • the sample can be obtained prior to any mechanical or chemical treatment to control organic contaminants.
  • the sample can be obtained during any mechanical or chemical treatment, after treatment, or at any other stage of the papermaking process. There is no limit as to where the sample can be taken from the papermaking process.
  • any amount of the pulp and fiber sample can be used, such as from about 10 to about 30 oven dried grams of fiber (if pulp slurry) or about 1 to about 200 grams water-based samples (i.e., whitewater/process water, UhIe box discharge, washer, press filtrates (low fiber containing samples)).
  • the size of the sample is not critical to the method of the present invention. In determining the amount or concentration of organic contaminants present, it would be helpful to know the amount of the sample being tested.
  • the sample is contacted with at least one hydrophobic dye.
  • the hydrophobic dye is preferably a fluorescent dye or a dye that is otherwise excitable such that is emits radiation which can be detected.
  • the hydrophobic dye is a fluorescent hydrophobic dye or a dye that emits visible radiation, but UV detectable or infrared detectable dyes can also be used.
  • hydrophobic dyes examples include, but are not limited to, the following: Quinoline Dye (Naphthalimide) (e.g., Morplas Fluorescent Yellow G Powder, syn: Solvent Yellow 43)); Anthraquinone (e.g., Morplas Red 46 Powder, syn: Solvent Red 168, and Morplas Blue 1003 Powder, syn: Solvent Blue 36); Coumarin (e.g., Navipal SWNR Powder, Fluorescent Brightener 140, and Ranipal SWNR Powder). Each of these are available from Sunbelt Corporation. Other examples include TRY 53 Tracer Yellow Dye and TRY-33 Tracer Yellow Dye Solution from Day-Glo Color Corporation.
  • Quinoline Dye Naphthalimide
  • Anthraquinone e.g., Morplas Red 46 Powder, syn: Solvent Red 168, and Morplas Blue 1003 Powder, syn: Solvent Blue 36
  • Coumarin e.g., Navipal SWNR Powder, Fluorescent Brightener 140, and Ranipal SW
  • hydrophobic dyes of the Sudan group can be used, such as Oil Red O, Sudan in, Sudan IV, or Sudan black B.
  • Oil Red O Sudan in, Sudan IV, or Sudan black B.
  • Nile Red which is a phenoxazone dye.
  • Other examples include dyes from Oreo and including the Orcoplast® group of dyes, which include fluorescent dyes.
  • Other dyes that can be used that are hydrophobic dyes include dyes from New Dragon Co., Ltd., which include fluorescent dyes.
  • Fluorescent dyes having an aminostyryl and quinolinium moieties can be used. These dyes are also known as fluorescent aminostyryl quinolinium dyes.
  • the amount of the hydrophobic dye used in the present invention can be any amount sufficient to stain the organic contaminants present in the pulp and fiber sample.
  • the dye is diluted or dissolved in an appropriate solvent, such as an organic solvent, like propylene glycol.
  • organic solvents include, but are not limited to, methylcarbitol, methylpyrrolidone, tetrahydrofuran, dipropylene glycol monoethyl ether, butanol, acetone, and alcohol.
  • Tetrahydrofuran can come as an acetic anhydride, and the butanol, alcohol, and acetone particularly may be in anhydrous form.
  • the hydrophobic dye is one which dissolves in an organic solvent for the preparation of the dispersion in an amount of at least 2 g/L, preferably 20 to 500 g/L at 25° C. from the viewpoint of efficiently containing the hydrophobic dye.
  • Suitable solvents can be selected based on their ability to solubilize the particular class of hydrophobic dyes of interest. It is preferable that their solubility characteristics are substantially similar.
  • the solvents can be acyl, aliphatic, cycloaliphatic, aromatic or heterocyclic hydrocarbons; the solvents may or may not have halogens, oxygen, sulfur, nitrogen, and/or phosphorous as either terminal groups or as integral parts of a ring or chain.
  • solvents such as toluene, xylene, hexane, pentane, acetone, DMSO, or methylene chloride can be used.
  • Chlorinated solvents, such as chloroform can be used.
  • one gram of dye can be combined with 100 mis of organic solvent, such as propylene glycol, to create an appropriate solution which then can be used in staining the organic contaminants present in the pulp and fiber sample.
  • the amount of dye that can be used is from about 100 ppm to about 1% by weight (or more) of dye which is present in solution with at least one organic solvent in an amount to achieve these concentration levels.
  • the dye can be present in a solvent in an amount of 1000 ppm to about 1% by weight of the overall solution containing the dye.
  • hydrophobic dye examples include oil-soluble dyes, disperse dyes and the like.
  • the oil-soluble dyes are not limited to specified ones, and include, for instance, CL Solvent Black 3, 7, 27, 29 and 34; CL Solvent Yellow 14, 16, 29, 56 and 82; CL Solvent Red 1, 3, 8, 18, 24, 27, 43, 51, 72 and 73; CI. Solvent Violet 3; CI. Solvent Blue 2, 11 and 70; CI. Solvent Green 3 and 7; C.I. Solvent Orange 2; C.I.
  • one or more fluorescent dyes can be used, such as squaraine, e.g., red dye which can be l,3-bis[(l,3-dihydro-l,3,3-trimethyl-2H-indol-2-ylidene)methyI]- 2,4-dihydroxy-cyc lobutenediylium, bis(inner salt) and an orange dye can be 2-(3,5- dimethylpyrrol-2-y])-4-(3,5-dimethyl-2H-pyrrol-2-ylidene)-3-hydroxy-2-cyclobuten-l-one.
  • the molar ratio between first and second dye can be from about 0 to 10,000.
  • Both dyes can be excited at the same absorption wavelength, e.g., ranging from ultraviolet to about 800 nm, and emit fluorescent light at two distinct, essentially non-overlapping wavelengths distant from each other by at least 10 nm, preferably 30 nm, and more preferably by at least 50 nm.
  • the emission peak of the dye #1 can be at 585 nm
  • the peak emission of dye #2 can be at 630 nm.
  • the squaric acid based fluorescent dyes can be synthesized by methods described in the literature. See, for example, Sprenger et al. Angew. Chem., 79, 581 (1967); Angew. Chem., 80, 541 (1968); and Maaks et al., Angew Chem. Intern. Edit., 5, 888 (1966). Briefly, one equivalent of squaric acid (1,2-dihydroxycyclobutenedione) is condensed with two equivalents of an active compound, such as a pyrrole, indoline, or aniline, and refluxed in a mixture of an alcohol and an aromatic solvent (such as benzene) under conditions that allow removal of water from the reaction mixture.
  • an active compound such as a pyrrole, indoline, or aniline
  • the resulting dye can be collected and purified by a number of standard methods, such as recrystallization, distillation, chromatography, etc. Additionally, unsymmetrically substituted squaric acid compounds can be synthesized by methods such as those described by Law et al., J. Org. Chem. 57, 3278, (1992). Specific methods of making such dyes are well known in the art and can be found for example in U.S. Pat. Nos. 5,795,981 ; 5,656,750; 5,492,795; 4,677,045; 5,237,498; and 5,354,873.
  • such dyes can contain functional groups capable of forming a stable fluorescent product with functional groups including activated esters, isothiocyanates, amines, hydrazines, halides, acids, azides, maleimides, alcohols, acrylamides, haloacetamides, phenols, thiols, acids, aldehydes and ketones.
  • functional groups capable of forming a stable fluorescent product with functional groups including activated esters, isothiocyanates, amines, hydrazines, halides, acids, azides, maleimides, alcohols, acrylamides, haloacetamides, phenols, thiols, acids, aldehydes and ketones.
  • Related dyes can be used, such as cyclobutenedione derivatives, substituted cephalosporin compounds, fluorinated squaraine compositions, symmetrical and unsymmetrical squaraines, alkylalkoxy squaraines, or squarylium compounds. Some of these dyes can fluoresce at near infrared as well as at infrared wavelengths that would effectively expand the range of emission spectra up to about 1,000 nm.
  • hydrophobic dyes such as phthalocyanines and naphthalocyanines can be also selected as operating at longer wavelengths.
  • Other classes of fluorochromes are equally suitable for use as dyes according to the present invention.
  • the present invention thus involves or Includes a pulp and fiber sample that contains organic contaminants wherein the organic contaminants are stained with at least one hydrophobic dye and preferably at least one hydrophobic fluorescent dye.
  • the amount of dye present in the staining can be based on the amounts previously provided.
  • a method for determining fluorescence in accordance with the present invention can involve the use of the fiber optic cytometer, for instance, as described in U.S. Pat. No. 4,564,598, the disclosure of which is incorporated herein in its entirety.
  • An optical fiber is used to define a relatively small volume from which fluorescent light can be received and counted.
  • the volume is related to the volume in which there is likely to be one or relatively few particles which produce predetermined fluctuations.
  • the fluorescence fluctuations are related to the presence of an analyte in a sample.
  • the fluctuations are observed over a period of time in a static mode or preferably by sampling a plurality of volumes in the sample.
  • the contacting of the sample with at least one hydrophobic dye can be done in any manner in which a dye is used to stain an object.
  • a dye for instance, an eyedropper can be used, a pipette can be used, a spray bottle can be used, a beaker can be used, and a titration apparatus can be used.
  • an eyedropper can be used, a pipette can be used, a spray bottle can be used, a beaker can be used, and a titration apparatus can be used.
  • a titration apparatus There are no limitations with respect to the manner in which one can contact the dye with the pulp and fiber sample.
  • the sample can then be analyzed for determining if organic contaminants are present, whether the organic contaminants are microstickies, and other characteristics of the organic contaminants, such as surface area, amount, and the like.
  • This analysis can be done, as an option, under a microscope or other detection device that permits detection of dyes. For instance, GFP
  • Illuminators can be used, stereo microscopes for GFP observation can be used, fluorescence spectrometers can be used, and motic cameras can be used. These are merely several examples.
  • a microscope can be used, wherein the microscope is either equipped with a fluorescent light or other means that will illuminate the dye if the dye is excitable such that analysis of the organic contaminants can easily be made.
  • this sample can be subjected to computer analysis wherein a program can be used to analyze the staining and a computer program can calculate various characteristics of this sample, such as the surface area of the organic contaminants, the amount of the organic contaminants, and the like.
  • the program can further inform the user of these characteristics, and the computer can further be programmed to determine the appropriate treatment that should be used to treat the organic contaminants based on this analysis.
  • the computer program can determine what chemical treatment should be used, the amount of chemical treatment, and/or the duration of the chemical treatment.
  • the method to detect organic contaminants can be done on a continual basis, on a semi-continual basis, on a batch basis, or whenever there is a need to detect organic contaminants is desired. Any type of systematic analysis can be conducted in order to effectively monitor the amount of organic contaminants present in the pulp and fiber.
  • a purpose of the method of the present invention is to stain the organic contaminants (i.e., stickies) so they can be easily detected/seen/observed amongst fibers, regardless of fiber size, shape, species, etc. (long/short/hard/soft).
  • polyvinyl acetate shows as "bright green” and styrene shows as "whiter-green.”
  • image analysis can be used to study the sample having the stained organic contaminants which can be done visually or with a computer program. By this image analysis, size distribution, the amount of contaminants, and the like can be used. Further, this information can be made available to the papermill or other user by on-line techniques, by e-mails, or other electronic means which can provide such information.
  • Example 1 A fresh 1% w/w solution of a D4 stain (Dupont #4 dye, from E.I. DuPont de Nemours & Co.) in tap water was prepared. To ensure the complete dissolution of the stain, the solution was heated to almost boiling. 0.1 g (0.1ml) of stock sample was placed into a test tube. 5 mis of D4 solution was added and the tube was put in hot, not boiling, water for 20 minutes. The contents of the test tube were poured onto a watch glass. A very small quantity of fibre and liquor was transferred onto a microscope slide. The slide was examined at x40, xlOO, x400 magnification.
  • each organic contaminant has a different color, thus permitting one to determine the amount of each contaminant, besides knowing the overall amount of stickies present. Also, there is a direct correlation between the number of particles seen under the microscope at 4Ox to 15Ox and the problem seen on a paper machine.
  • Example 2 A procedure for enumerating microstickies was experimentally studied in a field application (i.e., an actual paper producing facility). This paper producing facility uses recovered post consumer papers as a raw material to produce a commercial paper product. In the past, this particular location has experienced operational problems due to stickies deposition on the paper machine equipment. These operational "outbreaks" (i.e. off-quality sheet due to holes, defects/contamination, PM breaks, reduced production, downtime, etc.) are costly. Moreover, these stickies-related outbreaks were not predicted in the past.
  • Table 1 lists the excitation and emission wavelengths for the fluorescent tag/microstickies compound of these experiments.
  • the data was generated using a Perkin- Elmer 150 Fluorescence Spectrophotometer with a Xenon Power Supply.
  • microstickies in the PM headbox sample correlate with some significance to at least the following:
  • microstickies testing procedure is an indicator of potential problems. If there are high microstickies counts, there is at least a possibility that there could be an outbreak on the paper machine.
  • microstickies data indicates the high levels seen in the PM system were at the time that the outbreak occurred. • There appears to be a correlation between higher microstickies counts in the PM
  • the present invention does not rely on the use of a dye (to impart color), but instead relies on a UV light source used in combination with a fluorescent tag.
  • the tag reacts with the microstickies present in the sample (PVAc, SBR, etc).
  • the stickies/tag complex emits a strong optical fluorescent signal.
  • talc, clay, fibers, starch, etc. also absorb the fluorescent tag, the resulting optical signal emitting from these objects is considerably less intense than the signal emitting from the excited microstickies/dye complex. As a result, an operator/observer can easily view the microstickies. Ultimately, this technique diminishes false-positive recordings.
  • dye(s)/pigments are used to differentiate the microstickies from other materials in a given sample by "color" when viewed with a visible light source, then, in that instance, it is difficult to differentiate between the colored microstickies and all the other colored objects (background noise), which leads to false-positive readings.
  • this present invention focuses on the use of an alternative light source (UV) in combination with a fluorescent tag (which reacts specifically with microstickies).
  • UV alternative light source
  • the result of viewing the sample in a UV light source is the emission of a superior optical signal, thereby diminishing false-positive recordings. Consequently, the inventive test procedure is easier for the operator to use, with results that are more repeatable and potentially more useful as a predictor/barometer for stickies outbreaks in paper machine systems.
  • this example is only exemplary.
  • the present invention can be practiced using different forms of luminescence. Luminescence is "light', which is not generated from high temperatures alone. Non-limiting examples of luminescence in this regard include:
  • Example 3 Experimental evaluations were conducted on BULAB® 5453 bentonite (from Buckman Laboratories, Memphis TN) to evaluate its performance in reducing the amount of suspend and colloidal material in the Krofta accepts, and specifically focusing on microstickies that were monitored and counted as part of the evaluation. The evaluation was run over a time period of four weeks, in which the BULAB® 5453 Bentonite was substituted in production runs for an existing inorganic program used in the paper production facility, which was considered the "baseline” for purposes of these studies. The baseline material had been used and monitored in a prior four week production period. Microstickies were detected and enumerated in the manner described below.
  • the microstickies test procedure uses a 1 L sample that is treated with a specific dye; a smaller sample of the treated 1 L sample is then analyzed under the microscope to determine the microstickies count. When reporting the data, testers are extrapolating the microstickies count back to a 1 L sample size, which will provide a quantitative value that can be easily related back to the process.
  • the microstickies data is displayed as the number of microstickies per 1 L of sample.
  • Macrostickies did increase during the bentonite evaluation, but it is believed the slight increase is attributed to the high deink production rates during the same time frame.

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  • Analytical Chemistry (AREA)
  • Food Science & Technology (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Medicinal Chemistry (AREA)
  • Pathology (AREA)
  • Wood Science & Technology (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
  • Paper (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)

Abstract

L'invention concerne un procédé pour détecter des contaminants organiques dans de la pâte et des fibres, lequel procédé utilise des colorants hydrophobes, tels que des colorants fluorescents.
PCT/US2008/063693 2007-05-16 2008-05-15 Procédés pour détecter des contaminants organiques dans de la pâte et des fibres WO2008144383A1 (fr)

Priority Applications (7)

Application Number Priority Date Filing Date Title
JP2010508570A JP2010529421A (ja) 2007-05-16 2008-05-15 パルプ及び繊維中の有機夾雑物を検出する方法
CN200880016268A CN101680173A (zh) 2007-05-16 2008-05-15 检测纸浆和纤维中有机污染物的方法
EP20080755527 EP2145046A1 (fr) 2007-05-16 2008-05-15 Procédés pour détecter des contaminants organiques dans de la pâte et des fibres
CA 2685307 CA2685307A1 (fr) 2007-05-16 2008-05-15 Methodes de detection de contaminants organiques dans la pulpe et dans la fibre
AU2008255038A AU2008255038A1 (en) 2007-05-16 2008-05-15 Methods to detect organic contaminants in pulp and fiber
MX2009011956A MX2009011956A (es) 2007-05-16 2008-05-15 Metodos para detectar contaminantes organicos en la pulpa y fibra.
BRPI0810276A BRPI0810276A2 (pt) 2007-05-16 2008-05-15 "método para detectar contaminantes orgánicos em polpa e fibra e amostra de polpa e fibra"

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US93041407P 2007-05-16 2007-05-16
US60/930,414 2007-05-16

Publications (1)

Publication Number Publication Date
WO2008144383A1 true WO2008144383A1 (fr) 2008-11-27

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PCT/US2008/063693 WO2008144383A1 (fr) 2007-05-16 2008-05-15 Procédés pour détecter des contaminants organiques dans de la pâte et des fibres

Country Status (10)

Country Link
US (1) US20090084510A1 (fr)
EP (1) EP2145046A1 (fr)
JP (1) JP2010529421A (fr)
CN (1) CN101680173A (fr)
AU (1) AU2008255038A1 (fr)
BR (1) BRPI0810276A2 (fr)
CA (1) CA2685307A1 (fr)
MX (1) MX2009011956A (fr)
WO (1) WO2008144383A1 (fr)
ZA (1) ZA200907481B (fr)

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JP2012521009A (ja) * 2009-03-17 2012-09-10 ナルコ カンパニー 製紙プロセスにおいて疎水性夾雑物をモニターするための疎水性染料の使用
WO2013030462A1 (fr) * 2011-09-02 2013-03-07 Kemira Oyj Dispositif et procédé pour caractériser un matériau solide présent dans des liquides
KR101911848B1 (ko) * 2011-04-05 2018-10-25 날코 컴퍼니 재생 공정 및 재생 펄프를 포함하는 페이퍼 또는 티슈 제조 공정에서 거대 점착물을 모니터링하는 방법
WO2020254729A1 (fr) * 2019-06-20 2020-12-24 Kemira Oyj Estimation d'un niveau de risque dans un traitement aqueux

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US20100236732A1 (en) * 2009-03-17 2010-09-23 Alessandra Gerli Use of fluorescence to monitor hydrophobic contaminants in a papermaking process
EP2490006A4 (fr) * 2009-10-14 2018-05-02 Nippon Paper Industries Co., Ltd. Procédé pour mesurer un degré de déposition de contaminants
CA2780056C (fr) 2009-12-18 2013-10-29 Fpinnovations Analyseur de macropolluants en ligne et procede
EP2399962B1 (fr) * 2010-06-28 2013-02-13 Kemira Germany GmbH Colorants fluorescents comme colorants à papier
US20130220003A1 (en) * 2012-02-24 2013-08-29 Mark Laurint Method and apparatus for measuring deposition of particulate contaminants in pulp and paper slurries
CN102841177B (zh) * 2012-08-13 2014-10-29 大连工业大学 一种绿氧成分的分析方法
CN104515757A (zh) * 2013-09-29 2015-04-15 艺康美国股份有限公司 利用荧光染料控制疏水性污染物的方法
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JP6566348B2 (ja) 2014-04-08 2019-08-28 国立大学法人弘前大学 新規なグルコース誘導体、および該誘導体を用いた細胞イメージング方法およびイメージング剤
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JP6222173B2 (ja) * 2015-06-26 2017-11-01 栗田工業株式会社 ピッチ分析方法及びピッチ処理方法
WO2017070315A1 (fr) * 2015-10-23 2017-04-27 Geosyntec Consultants, Inc. Utilisation de composés détectables visiblement en tant que composés de référence dans des dispositifs d'échantillonnage passif
JP2018124249A (ja) * 2017-02-03 2018-08-09 トヨタ紡織株式会社 靭皮繊維の解繊状態判定方法
RU2020102716A (ru) 2017-06-30 2021-07-30 Кемира Ойй Контроль качества волокнистой массы
WO2019104031A1 (fr) * 2017-11-21 2019-05-31 Solenis Technologies, L.P. Procédé de mesure de contaminants hydrophobes dans une suspension concentrée de pâte à papier ou un système de fabrication de papier
CN109211894A (zh) * 2018-11-16 2019-01-15 芬欧汇川(中国)有限公司 用于测定造纸过程白水、废水或纸张中聚乙烯醇含量的方法和系统
CN112305154B (zh) * 2020-10-16 2022-09-23 中石化石油工程技术服务有限公司 一种膨润土吸蓝量的自动分析检测仪及其检测方法

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US5080759A (en) * 1990-09-04 1992-01-14 Quaker Chemical Corporation Method for controlling stickies in pulp and papermaking processes using recycled paper
EP0825293A1 (fr) * 1996-08-20 1998-02-25 Nalco Chemical Company Elimination des contaminants hydrophobes des systèmes de clarification d'eau
WO1999027177A1 (fr) * 1997-11-21 1999-06-03 Thermo Black Clawson Inc. Procede de desencrage et d'elimination des autres contaminants du vieux papier
WO2001098579A2 (fr) * 2000-06-16 2001-12-27 Buckman Laboratories International, Inc. Procedes de lutte contre des contaminants organiques presents dans des fibres
US20030164336A1 (en) * 2000-07-27 2003-09-04 Weir Josephine Michelle Processes of reducing contamination from cellulosic suspensions
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JP2012521009A (ja) * 2009-03-17 2012-09-10 ナルコ カンパニー 製紙プロセスにおいて疎水性夾雑物をモニターするための疎水性染料の使用
EP2409147B1 (fr) * 2009-03-17 2014-07-30 Nalco Company Utilisation de colorants hydrophobes pour surveiller des contaminants hydrophobes dans un processus de fabrication de papier
KR101911848B1 (ko) * 2011-04-05 2018-10-25 날코 컴퍼니 재생 공정 및 재생 펄프를 포함하는 페이퍼 또는 티슈 제조 공정에서 거대 점착물을 모니터링하는 방법
WO2013030462A1 (fr) * 2011-09-02 2013-03-07 Kemira Oyj Dispositif et procédé pour caractériser un matériau solide présent dans des liquides
RU2614645C2 (ru) * 2011-09-02 2017-03-28 Кемира Ойй Устройство и способ характеристики твердого вещества, присутствующего в жидкостях
US10451605B2 (en) 2011-09-02 2019-10-22 Kemira Oyj Device and method for characterizing solid matter present in liquids
WO2020254729A1 (fr) * 2019-06-20 2020-12-24 Kemira Oyj Estimation d'un niveau de risque dans un traitement aqueux
US12174612B2 (en) 2019-06-20 2024-12-24 Kemira Oyj Estimating risk level in an aqueous process

Also Published As

Publication number Publication date
EP2145046A1 (fr) 2010-01-20
JP2010529421A (ja) 2010-08-26
CA2685307A1 (fr) 2008-11-27
US20090084510A1 (en) 2009-04-02
ZA200907481B (en) 2010-07-28
BRPI0810276A2 (pt) 2019-09-24
AU2008255038A1 (en) 2008-11-27
CN101680173A (zh) 2010-03-24
MX2009011956A (es) 2009-11-13

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