EP0805234B1 - Procédé de fabrication du papier - Google Patents

Procédé de fabrication du papier Download PDF

Info

Publication number
EP0805234B1
EP0805234B1 EP19970107188 EP97107188A EP0805234B1 EP 0805234 B1 EP0805234 B1 EP 0805234B1 EP 19970107188 EP19970107188 EP 19970107188 EP 97107188 A EP97107188 A EP 97107188A EP 0805234 B1 EP0805234 B1 EP 0805234B1
Authority
EP
European Patent Office
Prior art keywords
slurry
polymer
weight
pulp
papermaking
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.)
Revoked
Application number
EP19970107188
Other languages
German (de)
English (en)
Other versions
EP0805234A3 (fr
EP0805234A2 (fr
Inventor
Ramasubramanyam Nagarajan
Jane B. Wong Shing
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.)
ChampionX LLC
Original Assignee
Nalco Chemical Co
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
Family has litigation
First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=24573387&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=EP0805234(B1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Nalco Chemical Co filed Critical Nalco Chemical Co
Publication of EP0805234A2 publication Critical patent/EP0805234A2/fr
Publication of EP0805234A3 publication Critical patent/EP0805234A3/fr
Application granted granted Critical
Publication of EP0805234B1 publication Critical patent/EP0805234B1/fr
Anticipated expiration legal-status Critical
Revoked legal-status Critical Current

Links

Images

Classifications

    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H23/00Processes or apparatus for adding material to the pulp or to the paper
    • D21H23/02Processes or apparatus for adding material to the pulp or to the paper characterised by the manner in which substances are added
    • D21H23/04Addition to the pulp; After-treatment of added substances in the pulp
    • D21H23/06Controlling the addition
    • D21H23/14Controlling the addition by selecting point of addition or time of contact between components
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20Macromolecular organic compounds
    • D21H17/33Synthetic macromolecular compounds
    • D21H17/34Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H17/37Polymers of unsaturated acids or derivatives thereof, e.g. polyacrylates
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20Macromolecular organic compounds
    • D21H17/33Synthetic macromolecular compounds
    • D21H17/34Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H17/37Polymers of unsaturated acids or derivatives thereof, e.g. polyacrylates
    • D21H17/375Poly(meth)acrylamide
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20Macromolecular organic compounds
    • D21H17/33Synthetic macromolecular compounds
    • D21H17/34Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H17/41Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing ionic groups
    • D21H17/44Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing ionic groups cationic
    • D21H17/45Nitrogen-containing groups
    • D21H17/455Nitrogen-containing groups comprising tertiary amine or being at least partially quaternised
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/63Inorganic compounds
    • D21H17/67Water-insoluble compounds, e.g. fillers, pigments
    • D21H17/675Oxides, hydroxides or carbonates
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/63Inorganic compounds
    • D21H17/67Water-insoluble compounds, e.g. fillers, pigments
    • D21H17/68Water-insoluble compounds, e.g. fillers, pigments siliceous, e.g. clays

Definitions

  • the present invention is in the technical field of papermaking and more particularly in the technical field of wet-end additives to papermaking furnish.
  • aqueous cellulosic suspension or slurry is formed into a paper sheet.
  • the cellulosic slurry is generally diluted to a consistency (percent dry weight of solids in the slurry) of less than 1 percent and often below 0.5 percent ahead of the paper machine, while the finished sheet must have less then 6 weight percent water.
  • a consistency percent dry weight of solids in the slurry
  • the dewatering method of the least cost in the process is drainage, and thereafter more expensive methods are used, for instance vacuum, pressing, evaporation and the like, and in practice a combination of such methods are employed to dewater, or dry the sheet to the desired water content. Since drainage is both the first dewatering method employed and the least expensive, improvement in the efficiency of drainage will decrease the amount of water required to be removed by other methods and hence improve the overall efficiency of dewatering and reduce the cost thereof.
  • a papermaking furnish contains generally particles that range in size from about the 2 to 3 millimeter size of cellulosic fibers to fillers at a few microns, and to colloids. Within this range are cellulosic fines, mineral fillers (employed to increase opacity, brightness and other paper characteristics) and other small particles that generally, without the inclusion of one or more retention aids, would in significant portion pass through the spaces (pores) between the cellulosic fibers in the fiber mat being formed during papermaking.
  • a coagulant/flocculant system added ahead of the paper machine.
  • a coagulant for instance a low molecular weight cationic synthetic polymer or a cationic starch
  • coagulant generally reduces the negative surface charges present on the particles in the furnish, particularly cellulosic fines and mineral fillers, and thereby accomplishes a degree of agglomeration of such particles, followed by the addition of a flocculant.
  • Such flocculant generally is a high molecular weight anionic synthetic polymer which bridges the particles and/or agglomerates, from one surface to another, binding the particles into large agglomerates.
  • the presence of such large agglomerates in the furnish as the fiber mat of the paper sheet is being formed increases retention.
  • the agglomerates are filtered out of the water onto the fiber web, where unagglomerated particles would to a great extent pass through such paper web.
  • a flocculated agglomerate generally does not interfere with the drainage of the fiber mat to the extent that would occur if the furnish were gelled or contained an amount of gelatinous material, when such flocs are filtered by the fiber web the pores thereof are to a degree reduced, reducing the drainage efficiency therefrom. Hence the retention is being increased with some degree of deleterious effect on the drainage.
  • Another system uses the combination of cationic starch followed by colloidal silica to increase the amount of material retained on the web by the method of charge neutralization and adsorption of smaller agglomerates.
  • This system is described in United States Patent No. 4,388,150, inventors Sunden et al., issued June 14, 1983.
  • Dewatering generally, and particularly dewatering by drainage, is believed improved when the pores of the paper web are less plugged, and it is believed that retention by adsorption in comparison to retention by filtration reduces such pore plugging.
  • Formation is determined by the variance in light transmission within a paper sheet, and a high variance is indicative of poor formation.
  • retention increases to a high level, for instance a retention level of 80 to 90 percent, the formation parameter generally abruptly declines from good formation to poor formation. It is at least theoretically believed that as the retention mechanisms of a given papermaking process shift from filtration to adsorption, the deleterious effect on formation, as high retention levels are achieved, will diminish, and a good combination of high retention with good formation is attributed to the use of bentonite in U. S. Patent No. 4,913,775.
  • additives that can be delivered to the paper machine without undue problems.
  • An additive that is difficult to dissolve, slurry or otherwise disperse in the aqueous medium may require expensive equipment to feed it to the paper machine..
  • the additive is often maintained in aqueous slurry form by virtue of high energy input equipment.
  • additives that are easily dissolved or dispersed in water require less energy and expense and their uniformity of feed is more reliable.
  • the claimed invention comprises a papermaking process comprising forming an aqueous cellulosic papermaking slurry, subjecting the slurry to one or more shear stages, adding to the slurry a mineral filler prior to at least one of the shear stages, adding to the slurry after the addition of the mineral filler and prior to at least one of the shear stages from 0.5 to 100 ppm by weight of dry pulp contained in the slurry of a cationic dispersion polymer obtainable by dispersion polymerization of a monomer mixture soluble in an aqueous solution of a polyvalent anionic salt said polymer being selected from the group consisting of copolymers of acrylamide and dimethylaminoethylacrylate methyl chloride quaternary salt (DMAEA.MCQ), dimethylaminoethylmethacrylate methyl chloride quaternary salt (DMAEM.MCQ), dimethylaminoethylacrylate benzyl chloride quaternary salt (DM
  • a water soluble polymer is added to a cellulosic slurry before the formation of a paper product.
  • the water soluble polymer should become substantially dispersed within the slurry before formation of the paper product in any case.
  • the microparticle of the invention is added after shearing of the slurry.
  • the addition of the polymer in an aqueous medium for instance as a water solution or dispersing, facilitates the dispersion of the polymer of the slurry.
  • the polymer is added to the cellulosic slurry before the processing steps of draining and forming the paper sheet.
  • the present process is believed applicable to all grades and types of paper products, and further applicable for use on all types of pulps including, without limitation, chemical pulps, including sulfate and sulfite pulps from both hard and soft woods and acid pulps, thermo-mechanical pulps, mechanical pulps, recycle pulps and ground wood pulps, although it is believed that the advantages of the process of the present invention are best achieved when the pulp employed is of the chemical pulp type, particularly alkaline chemical pulp.
  • the filler used in the cellulosic slurry is anionic, or at least partially anionic.
  • Other mineral, or inorganic, fillers may, however, be used, such as calcium carbonate, clay, titanium dioxide, or talc or a combination may be present.
  • the amount of alkaline inorganic filler, such as one of the alkaline carbonates, generally employed in a papermaking stock is from 10 to 30 parts by weight of the filler, as CaCO 3 , per hundred parts by weight of dry pulp in the slurry, but the amount of such filler may at times be as low as 5, or even 2, parts by weight, and as high as 40 or 50 parts by weight, same basis.
  • the dispersion polymerization process used to manufacture the polymers of the invention offer numerous advantages which have previously been unavailable. Since the polymers of the invention are synthesized entirely in water, no oil solvent is required. This is significant since:
  • Another major advantage is that the bulk viscosity of the polymer is low, unlike some oil dispersion latex polymers. This physical property enables any standard chemical pump to deliver the material at the injunction site.
  • a new class of water-soluble dispersion polymers have been discovered to be more effective in increasing drainage and retention than currently available chemical treatments.
  • the polymer dispersion is prepared in an aqueous solution of a polyvalent anionic salt.
  • the polymer dispersion achieves fine particle sizes and aqueous solubilities not available with other polymers used for this application.
  • there does not appear to be a problem with overfeeding the polymer dispersion which is a drawback with latex polymers.
  • the dispersion polymer of the invention is added to a cellulosic papermaking slurry.
  • the polymer is added in an effective amount of from 0.5 to 100 ppm. More preferably, the amount of the polymer added is from 2 to 40 ppm; and most preferably from 4 to 25 ppm. It is believed, that there does not appear to be a maximum dosage at which the polymers adversely affect the system. At some higher doses the beneficial effect may plateau, and on a cost basis such higher doses, probably above about 100 ppm, are not cost effective.
  • the polymers of the invention are preferably added to the system in neat form. However, in some applications, the polymers can be added as an aqueous solution.
  • the preferred polymers of the invention are manufactured by Hymo Corporation, Japan. Methods for manufacturing the polymer dispersion used in the invention is described in detail in U. S. Patent No. 5,006,590 and U. S. Patent No. 4,929,655, assigned to Kyoritsu Yuki Co., Ltd., Tokyo, Japan.
  • an organic or inorganic microparticle is added to the slurry after the introduction of shear.
  • the organic microparticle is a medium molecular weight anionic polymer such as the copolymers of acrylic acid described in U.S. Patent No. 5,098,520 or medium molecular weight anionic sulfonated polymers such as those described in U.S. Patent No. 5,185,062.
  • the inorganic microparticle may be preferably chosen from among bentonite and silica sol.
  • the dispersion polymer used to treat the cellulosic papermaking slurry may further be prepared from a water-soluble monomer mixture containing at least 5 mole % of a cationic monomer represented by the general formula (I): wherein R 1 is H or CH 3 ; R 2 and R 3 are each an alkyl group having 1 to 2 carbon atoms; R 4 is benzyl or CH 3 ; A 1 is an oxygen atom or NH; B 1 is an alkyl group having 2 to 4 carbon atoms or a hydroxypropyl group and X 1 is a counter anion.
  • a cationic monomer represented by the general formula (I): wherein R 1 is H or CH 3 ; R 2 and R 3 are each an alkyl group having 1 to 2 carbon atoms; R 4 is benzyl or CH 3 ; A 1 is an oxygen atom or NH; B 1 is an alkyl group having 2 to 4 carbon atoms or a hydroxypropyl group and X 1 is
  • the above water-soluble monomer mixture is soluble in the aqueous solution of the polyvalent anionic salt.
  • the polymer generated from the monomer mixture is, however, insoluble in the aqueous polyvalent anionic salt solution.
  • the polymer of the monomer mixture can also be used as the seed polymer. The seed polymer is described in detail below.
  • the above cationic monomer represented by the general formula (I) preferably is a quaternary ammonium salt obtained by the reaction of methyl chloride or benzyl chloride and dimethylaminoethyl acrylate, diethylaminoethyl acrylate, dimethylaminohydroxypropyl acrylate, dimethylaminopropyl acrylamide, dimethylaminoethyl methacrylate, dimethylaminoethyl methacrylate, diethylaminoethyl methacrylate and dimethylaminopropyl methacrylamide.
  • the concentration of the above-mentioned monomers in the polymerization reaction mixture is suitably in the range of 1.0 to 30% by weight for the methyl chloride quaternary ammonium salt. Preferably, the concentration is from 10 to 20% by weight.
  • the concentration in the polymerization reaction mixture is suitably in the range of from 1.0 to 35% by weight. Preferably, the concentration is from 10 to 20% by weight.
  • Monomers preferably copolymerized with the cationic monomer as represented by the general formula (I) include acrylamide, methacrylamide and the cationic monomers represented by the general formula (II): wherein R 5 is H or CH 3 ; R 6 and R 7 are each an alkyl group having 1 to 2 carbon atoms; R 8 is H or an alkyl group having 1 to 2 carbon atoms; A 2 is an oxygen atom or NH; B 2 is an alkyl group having 2 to 4 carbon atoms or a hydroxypropyl group and X 2 is a counter anion.
  • Preferable monomers represented by the formula (II) include the ammonium salts of dimethylaminoethyl acrylate, diethylaminoethyl acrylate, dimethylaminopropyl acrylamide, diethylaminopropyl acrylamide and dimethylhydroxypropyl acrylate, dimethylaminoethyl methacrylate, diethylaminoethyl methacrylate, dimethylaminopropyl methacrylamide, diethylaminopropyl methacrylamide and dimethylhydroxypropyl methacrylate as well as the methylated and ethylated quaternary salts.
  • the more preferable cationic monomers represented by the general formula (II) are the salts and methylated quaternary salts of dialkylaminoethyl acrylate and dialkylaminoethyl methacrylate.
  • the polyvalent anionic salt to be incorporated in the aqueous solution is suitably a sulfate, a phosphate or a mixture thereof.
  • Preferable salts include ammonium sulfate, sodium sulfate, magnesium sulfate, aluminum sulfate, ammonium hydrogen phosphate, sodium hydrogenphosphate and potassium hydrogenphosphate.
  • these salts may be each used as an aqueous solution thereof having a concentration of 15% or above.
  • a dispersant is present in the aqueous anionic salt solution in which the polymerization of the above monomers occurs.
  • the dispersant is a water-soluble high molecular weight cationic polymer.
  • the dispersant is soluble in the above-mentioned aqueous salt solution.
  • the dispersant is preferably used in an amount of from 1 to 10% by weight based on the total weight of the monomers.
  • the dispersant is composed of 20 mole % or more of cationic monomer units represented by the formula (II).
  • the residual mole % is acrylamide or methacrylamide.
  • the performance of the dispersant is not greatly affected by molecular weight.
  • the molecular weight of the dispersant is preferably in the range of 10,000 to 10,000,000 g/mol (daltons).
  • a multifunctional alcohol such as glycerin or polyethylene glycol can be coexistent in the polymerization system. The deposition of the fine particles is smoothly carried out in the presence of these alcohols.
  • water-soluble radical-forming agent for the polymerizations a usual water-soluble radical-forming agent can be employed, but preferably water-soluble azo compounds such as 2,2'-azobis(2-amidinopropane) hydrochloride and 2,2'-azobis(N,N'-dimethyleneisobutylamine) hydrochloride are used.
  • water-soluble azo compounds such as 2,2'-azobis(2-amidinopropane) hydrochloride and 2,2'-azobis(N,N'-dimethyleneisobutylamine) hydrochloride are used.
  • a seed polymer can be added before the beginning of the polymerization of the above monomers for the purpose of obtaining a fine dispersion.
  • the seed polymer is a water-soluble cationic polymer insoluble in the aqueous solution of the polyvalent anionic salt.
  • the seed polymer is preferably a polymer prepared from the above monomer mixture by the process described herein. Nevertheless, the monomer composition of the seed polymer need not always be equal to that of the water-soluble cationic polymer formed during polymerization. However, like the water-soluble polymer formed during polymerization, the seed polymer should contain at least 5 mole percent of cationic monomer units represented by the general formula (I).
  • the seed polymer used in one polymerization reaction can be the water-soluble polymer prepared in a previous reaction which used the same monomer mixture.
  • Microparticle A (colloidal silica)
  • Dispersed silica in water with a particle size of 4 nm Dispersed silica in water with a particle size of 4 nm.
  • Microparticle C (bentonite)
  • Dispersion Polymers Polymer A 10 mole% DMAEA.BCQ RSV 19.6 dl/g Polymer B 10 Mole % DMAEA.MCQ RSV 21.4 dl/g Polymer C 20 mole % DMAEA.MCQ RSV 27.6 dl/g Latex Polymer Polymer D 10 mole% DMAEA.MCQ RSV 19.7 dl/g
  • the Reduced Specific Viscosity (RSV) was measured at a concentration of 0.045% polymer in a solution of 0.125M NaNO 3 solution.
  • the Britt Jar Test employed in Examples 1 to 3 used a Britt CF Dynamic Drainage Jar developed by K. W. Britt of New York State University, which generally consists of an upper chamber of about 1 liter capacity and a bottom drainage chamber, the chamber being separated by a support screen and a drainage screen. Below the drainage chamber is a downward extending flexible tube equipped with a clamp for closure.
  • the upper chamber is provided with a variable speed, high torque motor equipped with a 51-mm (2-inch) 3-bladed propeller to create controlled shear conditions in the upper chamber.
  • the test was conducted by placing the cellulosic stock in the upper chamber and then subjecting the stock to the following sequence: Time Action 0 seconds Commence shear stirring at 750 rpm, (add starch, if needed). 10 seconds Add the cationic polymer, increase speed to 2000 rpm. 40 seconds Reduce shear stirring to 750 rpm. 50 seconds Add the microparticle. 60 seconds Open the tube clamp to commence drainage, and continue drainage for 30 seconds.
  • the material so drained from the Britt jar (the "filtrate") is collected and diluted with water to one-fourth of its initial volume.
  • the turbidity of such diluted filtrate measured in Formazin Turbidity Units or FTU's, is then determined.
  • the turbidity of such a filtrate is inversely proportional to the papermaking retention performance; the lower the turbidity value, the higher is the retention of filler and/or fines.
  • the turbidity values were determined using a Hach Spectrophotometer, model DR2000.
  • Percent Improvement 100 X (Turbidity u - Turbidity t ) / Turbidity u where Turbidity u is the turbidity reading result for the blank for which no polymer or microparticle, and wherein Turbidity t is the turbidity reading result of the test using polymer, or polymer and microparticle.
  • the filtration tests used in Examples 1 to 8 measured the drainage (water removal) rate of the test stock subjected to the various chemical treatments.
  • a filtration cell mounted upright on a stand, was used. The capacity of this cell is about 220 milliliters.
  • a 200 mesh drainage screen (76 ⁇ m screen with 8% opening) served as the filter medium.
  • the stock was filtered by gravity. The filtrate was collected in a cup placed on a weighing balance below the cell. This balance was interfaced with a computer so that the displayed weight was recorded continuously over time. The computer automatically recorded the change of weight over time.
  • the cellulosic stock was treated in the aforementioned Britt jar.
  • the treated stock was transferred to the cell and filtered until completion.
  • the rate of filtrate collection is an indication of the drainage performance; the higher the filtrate collection rate, the higher is the improvement in drainage.
  • the cellulosic stock or slurry used in Examples 1 to 3 and 8 was comprised of 70 weight percent fiber and 30 weight percent filler, diluted to an overall consistency of 0.5 percent with formulation water.
  • the fiber was a 60/40 blend by weight of bleached hardwood Kraft and bleached softwood Kraft, separately beaten to a Canadian Freeness value range of from 320 to 360 C.F.S.
  • the filler was a commercial calcium carbonate , provided in dry form.
  • the formulation water contained 60 ppm calcium hardness (added as CaCl 2 ), 18 ppm magnesium hardness (added as MgSO 4 ) and 134 ppm bicarbonate alkalinity ( added as NaHCO 3 ).
  • the pH of the final thin stock was pH 7.2.
  • the cellulosic stock or slurry used in Examples 4 to 5 was comprised of 93 weight percent fiber and 7 weight percent filler, diluted to an overall consistency of 0.54 percent with formulation water.
  • the fiber was a 50/50 blend by weight of bleached hardwood Kraft and bleached softwood Kraft, separately beaten to a Canadian Freeness value range of from 320 to 360 C.F.S.
  • the fillers were clay as predispersed kaolin and titanium dioxide, commercially provided in dry form.
  • the pH was adjusted to pH 4.00 using dilute sulfuric acid, following which alum (0.005% of final slurry) and sizing agent rosin (0.0025 wt% of final slurry) were added.
  • the formulation water contained 60 ppm calcium hardness (added as CaCl 2 ), 18 ppm magnesium hardness (added as MgSO 4 ) and 134 ppm bicarbonate alkalinity ( added as NaHCO 3 ).
  • the stock used in Examples 6 and 7 was obtained as thick stock (consistency of 4.11 %) from a paper mill. It was a mixture of OCC, newsprint, and boxboard. It was diluted to an overall consistency of 0.8% with formulation water containing 60 ppm calcium hardness (added as CaCl 2 ), 18 ppm magnesium hardness (added as MgSO 4 ) and 134 ppm bicarbonate alkalinity ( added as NaHCO 3 ). The final pH of the thin stock was pH 6.5. The percent ash of the thin stock was 7.3 wt%.
  • the filtration test also described above was employed to determine the drainage performances of dispersion Polymer A in comparison to the inverse emulsion Polymer D, with microparticle C as the microparticle.
  • cationic potato starch was charged to the test stock in the amount of 4.5 kg/1000 kg (10 lb/ton) of dry weight of slurry solids. The results are shown for each of the programs tested in Figure 7 as graphs of collected filtrate weight versus time.

Landscapes

  • Paper (AREA)

Claims (7)

  1. Procédé de fabrication du papier comprenant les étapes qui consistent à former une suspension épaisse cellulosique aqueuse à papier, à soumettre la suspension épaisse à une ou plusieurs étapes de cisaillement, à ajouter à la suspension épaisse une charge minérale avant au moins une des étapes de cisaillement, à ajouter à la suspension épaisse, après l'addition de la charge minérale et avant au moins une des étapes de cisaillement, de 0,5 à 100 ppm, en poids de pâte sèche contenue dans la suspension épaisse, d'un polymère cationique en dispersion pouvant être obtenu par la polymérisation en dispersion d'un mélange de monomères soluble dans une solution aqueuse de sel anionique polyvalent, ledit polymère étant choisi dans l'ensemble comprenant les copolymères d'acrylamide et de sel quaternaire de chlorure de méthyle et d'acrylate de diméthylaminoéthyle, sel quaternaire de chlorure de méthyle et de méthacrylate de diméthylaminoéthyle, sel quaternaire de chlorure de benzyle et d'acrylate de diméthylaminoéthyle et sel quaternaire de chlorure de benzyle et de méthacrylate de diméthylaminoéthyle, ledit polymère étant insoluble dans la solution aqueuse ;
       à cisailler la suspension épaisse ;
       à ajouter une certaine quantité de microparticules, choisies dans l'ensemble comprenant un copolymère d'acide acrylique, la bentonite et un sol siliceux, à la suspension épaisse ;
       à égoutter la suspension épaisse pour former une feuille ; et
       à sécher cette feuille pour former une feuille de papier.
  2. Procédé selon la revendication 1, dans lequel la suspension épaisse est égouttée sur un tamis de fabrication de papier et pompée en direction du site du tamis de fabrication de papier avant l'égouttage.
  3. Procédé selon la revendication 1, dans lequel la suspension épaisse est choisie dans l'ensemble comprenant une suspension pâteuse acide, une suspension pâteuse chimique alcaline, une suspension pâteuse thermomécanique, une suspension pâteuse mécanique, une suspension pâteuse de récupération et une suspension pâteuse mécanique de défibreur.
  4. Procédé selon la revendication 1, dans lequel la charge minérale est choisie dans l'ensemble comprenant le blanc de titane, l'argile, le talc et le carbonate alcalin de calcium.
  5. Procédé selon la revendication 1, dans lequel la charge minérale est ajoutée à la suspension épaisse en une quantité de 2 à 50 parties pour cent parties en poids de pâte sèche contenue dans la suspension épaisse.
  6. Procédé selon la revendication 1, dans lequel le polymère en dispersion est ajouté à la suspension épaisse en une quantité de 2 à 40 ppm en poids de pâte sèche contenue dans la suspension épaisse.
  7. Procédé selon la revendication 6, dans lequel le polymère en dispersion est ajouté à la suspension épaisse en une quantité de 4 à 25 ppm en poids de pâte sèche contenue dans la suspension épaisse.
EP19970107188 1996-05-01 1997-04-30 Procédé de fabrication du papier Revoked EP0805234B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US64167196A 1996-05-01 1996-05-01
US641671 2000-08-18

Publications (3)

Publication Number Publication Date
EP0805234A2 EP0805234A2 (fr) 1997-11-05
EP0805234A3 EP0805234A3 (fr) 1999-07-21
EP0805234B1 true EP0805234B1 (fr) 2002-07-03

Family

ID=24573387

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19970107188 Revoked EP0805234B1 (fr) 1996-05-01 1997-04-30 Procédé de fabrication du papier

Country Status (9)

Country Link
EP (1) EP0805234B1 (fr)
AU (1) AU729008B2 (fr)
BR (1) BR9701967A (fr)
CA (1) CA2204050C (fr)
DE (1) DE69713677T2 (fr)
ES (1) ES2176553T3 (fr)
ID (1) ID16844A (fr)
MY (1) MY123120A (fr)
NO (1) NO326449B1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9487916B2 (en) 2007-09-12 2016-11-08 Nalco Company Method of improving dewatering efficiency, increasing sheet wet web strength, increasing sheet wet strength and enhancing filler retention in papermaking

Families Citing this family (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6238521B1 (en) 1996-05-01 2001-05-29 Nalco Chemical Company Use of diallyldimethylammonium chloride acrylamide dispersion copolymer in a papermaking process
US6310124B1 (en) 1996-10-03 2001-10-30 Cytec Technology, Corp. Aqueous dispersions
US6235205B1 (en) 1996-10-03 2001-05-22 Cytec Technology Corp. Aqueous dispersions
US6262168B1 (en) 1998-03-11 2001-07-17 Cytec Technology Corp. Aqueous dispersions
KR100403840B1 (ko) * 1998-04-27 2003-11-01 악조 노벨 엔.브이. 제지 방법
EP0953680A1 (fr) * 1998-04-27 1999-11-03 Akzo Nobel N.V. Procédé pour la fabrication du papier
US7306700B1 (en) 1998-04-27 2007-12-11 Akzo Nobel Nv Process for the production of paper
KR100278510B1 (ko) * 1998-08-24 2001-03-02 한성욱 콜로이달 실리카를 포함하는 미립자보류용 수용성 고분자 분산액 및 그 제조방법
US6331229B1 (en) * 1999-09-08 2001-12-18 Nalco Chemical Company Method of increasing retention and drainage in papermaking using high molecular weight water-soluble anionic or monionic dispersion polymers
US6818100B2 (en) 2000-08-07 2004-11-16 Akzo Nobel N.V. Process for sizing paper
AU2002222352A1 (en) * 2001-12-12 2003-06-23 Green Technology Inc. Use of hydrophillic polymer dispersion containing a colloidal silica or an inorganic flocculant as retention and drainage aids in paper making process
AU2002310569A1 (en) * 2002-05-27 2003-12-12 Green Technology Inc. Process for preparing a dispersion polymer
KR100681327B1 (ko) * 2002-10-31 2007-02-15 주식회사 오병 콜로이달 실리카를 함유하는 고농축 벤토나이트 액상슬러리 및 그 제조방법
DE10307201A1 (de) * 2003-02-20 2004-05-19 Voith Paper Patent Gmbh Verfahren zur Herstellung einer Faserstoffsuspension für die Erzeugung füllstoffhaltiger Papiere
CN1323211C (zh) * 2004-06-21 2007-06-27 徐清明 造纸矿物复合助留剂及其制备方法与应用
US9752283B2 (en) 2007-09-12 2017-09-05 Ecolab Usa Inc. Anionic preflocculation of fillers used in papermaking
US8172983B2 (en) * 2007-09-12 2012-05-08 Nalco Company Controllable filler prefloculation using a dual polymer system
US8778140B2 (en) * 2007-09-12 2014-07-15 Nalco Company Preflocculation of fillers used in papermaking
US8747617B2 (en) 2007-09-12 2014-06-10 Nalco Company Controllable filler prefloculation using a dual polymer system
PT106170A (pt) * 2012-02-20 2013-08-20 Fapajal Fabrica De Papel Do Tojal S A Processo de fixação de cargas de carbonato de cálcio em papéis leves crepados (tissu) sem impacto negativo nas características do papel
WO2018211173A1 (fr) 2017-05-16 2018-11-22 Kemira Oyj Procédé de production de solutions polymères

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4913775A (en) * 1986-01-29 1990-04-03 Allied Colloids Ltd. Production of paper and paper board
GB8602121D0 (en) * 1986-01-29 1986-03-05 Allied Colloids Ltd Paper & paper board
US5178730A (en) * 1990-06-12 1993-01-12 Delta Chemicals Paper making
SE9504081D0 (sv) * 1995-11-15 1995-11-15 Eka Nobel Ab A process for the production of paper

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9487916B2 (en) 2007-09-12 2016-11-08 Nalco Company Method of improving dewatering efficiency, increasing sheet wet web strength, increasing sheet wet strength and enhancing filler retention in papermaking

Also Published As

Publication number Publication date
EP0805234A3 (fr) 1999-07-21
DE69713677T2 (de) 2002-10-31
CA2204050C (fr) 2006-06-20
EP0805234A2 (fr) 1997-11-05
CA2204050A1 (fr) 1997-11-01
MX9703180A (es) 1998-05-31
BR9701967A (pt) 1998-09-15
DE69713677D1 (de) 2002-08-08
NO972022D0 (no) 1997-04-30
NO326449B1 (no) 2008-12-08
ID16844A (id) 1997-11-13
ES2176553T3 (es) 2002-12-01
NO972022L (no) 1997-11-03
AU1915897A (en) 1997-11-06
MY123120A (en) 2006-05-31
AU729008B2 (en) 2001-01-25

Similar Documents

Publication Publication Date Title
EP0805234B1 (fr) Procédé de fabrication du papier
US5098520A (en) Papermaking process with improved retention and drainage
EP0534656B1 (fr) Procédé de fabrication de papier
US5185062A (en) Papermaking process with improved retention and drainage
EP1167392B1 (fr) Materiaux convenant à l'utilisation dans la fabrication du papier
EP0017353B1 (fr) Production de papier et de carton
US5266164A (en) Papermaking process with improved drainage and retention
AU696483B2 (en) Production of paper
US5595629A (en) Papermaking process
EP1216260B1 (fr) Procede mettant en oeuvre des polymeres dispersion anioniques ou non ioniques, de poids moleculaire eleve, solubles dans l'eau, pour augmenter la retention et le drainage dans la pate a papier
US6059930A (en) Papermaking process utilizing hydrophilic dispersion polymers of dimethylaminoethyl acrylate methyl chloride quaternary and acrylamide as retention and drainage aids
US6007679A (en) Papermaking process
EP0790351A2 (fr) Procédé de fabrication de papier à l'aide d'un agent de rétention et d'égouttage multipolymère
NO324301B1 (no) Hydrofile dispersjons-polymerer for papiranvendelser
MXPA97003180A (en) Process for pa manufacturing
CA2235637A1 (fr) Processus ameliore de fabrication du papier
MXPA98003266A (en) Improved process for pa manufacturing
WO2003050354A1 (fr) Utilisation d'une dispersion polymere hydrophile contenant une silice colloidale ou un floculant inorganique en tant qu'aides de retention et de drainage dans un processus de fabrication de papier
JPH11302994A (ja) 製紙方法
MXPA99006145A (en) Processes of making paper and materials for use in this

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

AK Designated contracting states

Kind code of ref document: A2

Designated state(s): DE ES FI FR GB IT SE

PUAL Search report despatched

Free format text: ORIGINAL CODE: 0009013

AK Designated contracting states

Kind code of ref document: A3

Designated state(s): DE ES FI FR GB IT SE

17P Request for examination filed

Effective date: 19990812

17Q First examination report despatched

Effective date: 20010117

RTI1 Title (correction)

Free format text: PAPERMAKING PROCESS

GRAG Despatch of communication of intention to grant

Free format text: ORIGINAL CODE: EPIDOS AGRA

GRAG Despatch of communication of intention to grant

Free format text: ORIGINAL CODE: EPIDOS AGRA

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): DE ES FI FR GB IT SE

REF Corresponds to:

Ref document number: 69713677

Country of ref document: DE

Date of ref document: 20020808

REG Reference to a national code

Ref country code: ES

Ref legal event code: FG2A

Ref document number: 2176553

Country of ref document: ES

Kind code of ref document: T3

ET Fr: translation filed
PLBI Opposition filed

Free format text: ORIGINAL CODE: 0009260

PLBQ Unpublished change to opponent data

Free format text: ORIGINAL CODE: EPIDOS OPPO

PLBQ Unpublished change to opponent data

Free format text: ORIGINAL CODE: EPIDOS OPPO

PLBI Opposition filed

Free format text: ORIGINAL CODE: 0009260

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 20030418

Year of fee payment: 7

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: SE

Payment date: 20030422

Year of fee payment: 7

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 20030423

Year of fee payment: 7

Ref country code: FI

Payment date: 20030423

Year of fee payment: 7

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 20030430

Year of fee payment: 7

PLBF Reply of patent proprietor to notice(s) of opposition

Free format text: ORIGINAL CODE: EPIDOS OBSO

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: ES

Payment date: 20030508

Year of fee payment: 7

26 Opposition filed

Opponent name: EKA CHEMICALS AB

Effective date: 20030401

26 Opposition filed

Opponent name: BASF AKTIENGESELLSCHAFTPATENTE, MARKEN UND LIZENZE

Effective date: 20030401

Opponent name: EKA CHEMICALS AB

Effective date: 20030401

PLAX Notice of opposition and request to file observation + time limit sent

Free format text: ORIGINAL CODE: EPIDOSNOBS2

PLAX Notice of opposition and request to file observation + time limit sent

Free format text: ORIGINAL CODE: EPIDOSNOBS2

PLBB Reply of patent proprietor to notice(s) of opposition received

Free format text: ORIGINAL CODE: EPIDOSNOBS3

RDAF Communication despatched that patent is revoked

Free format text: ORIGINAL CODE: EPIDOSNREV1

RDAG Patent revoked

Free format text: ORIGINAL CODE: 0009271

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: PATENT REVOKED

27W Patent revoked

Effective date: 20040208

GBPR Gb: patent revoked under art. 102 of the ep convention designating the uk as contracting state

Free format text: 20040208

REG Reference to a national code

Ref country code: SE

Ref legal event code: ECNC

PLAB Opposition data, opponent's data or that of the opponent's representative modified

Free format text: ORIGINAL CODE: 0009299OPPO