EP0574335B1 - Verfahren zur Herstellung von Papier oder Pappe mit verbesserter Retention - Google Patents

Verfahren zur Herstellung von Papier oder Pappe mit verbesserter Retention Download PDF

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Publication number
EP0574335B1
EP0574335B1 EP93420231A EP93420231A EP0574335B1 EP 0574335 B1 EP0574335 B1 EP 0574335B1 EP 93420231 A EP93420231 A EP 93420231A EP 93420231 A EP93420231 A EP 93420231A EP 0574335 B1 EP0574335 B1 EP 0574335B1
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EP
European Patent Office
Prior art keywords
polyacrylamide
branched
bentonite
fact
retention
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.)
Expired - Lifetime
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EP93420231A
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English (en)
French (fr)
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EP0574335A1 (de
Inventor
René Hund
Eric Philibert
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SNF SA
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SNF SA
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Classifications

    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP 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
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20—Macromolecular organic compounds
    • D21H17/33—Synthetic macromolecular compounds
    • D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H17/41—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing ionic groups
    • D21H17/44—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing ionic groups cationic
    • D21H17/45—Nitrogen-containing groups
    • D21H17/455—Nitrogen-containing groups comprising tertiary amine or being at least partially quaternised
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP 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
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20—Macromolecular organic compounds
    • D21H17/33—Synthetic macromolecular compounds
    • D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H17/37—Polymers of unsaturated acids or derivatives thereof, e.g. polyacrylates
    • D21H17/375—Poly(meth)acrylamide
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP 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
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/63—Inorganic compounds
    • D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
    • D21H17/68—Water-insoluble compounds, e.g. fillers, pigments siliceous, e.g. clays
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP 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
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/06—Paper forming aids
    • D21H21/10—Retention agents or drainage improvers

Definitions

  • the invention relates to a method for manufacturing paper or cardboard with improved retention.
  • bentonite to the pulp, which can optionally be added to other mineral products, such as aluminum sulphates, or even synthetic polymers, in particular polyethyleneimine (see for example documents DE-A-2 262 906 and US-A-2 368 635).
  • the invention overcomes these drawbacks.
  • This improvement is characterized in that the polyacrylamide is branched and is easily soluble in water, and is introduced into the suspension in the form of powder dissolved, at the rate of 0.03 to one per thousand (0.03 to 1% o) by weight, of the dry weight of the fibrous suspension.
  • the invention consists, among all the polyacrylamides, in using the branched polyacrylamides in the form of powder dissolved.
  • this selection allows, in the paper application for the retention of fillers and fines, to reach a level of performance unmatched before.
  • the use of branched polymers also makes it possible to better retain the bentonite on the sheet, and therefore to limit its negative effects on the subsequent water treatment.
  • the choice of this branched polyacrylamide increases the fixing power of the bentonite on the sheet, thereby bringing about a synergy, therefore a re-coagulation which reduces the content of the bentonite in the white waters.
  • the branched polyacrylamide is a cationic copolymer of acrylamide and of an unsaturated cationic ethylenic monomer, chosen from the group comprising dimethylaminoethyl acrylate (ADAME), dimethylaminoethyl methacrylate (MADAME), quaternized or salified , dimethyldiallylammonium chloride (DADMAC), chloride acrylamide propyltrimethylammonium (APTAC), and methacrylamidopropyltrimethylammonium chloride (MAPTAC).
  • ADAME dimethylaminoethyl acrylate
  • MADAME dimethylaminoethyl methacrylate
  • DADMAC dimethyldiallylammonium chloride
  • APITAC chloride acrylamide propyltrimethylammonium
  • MATAC methacrylamidopropyltrimethylammonium chloride
  • this copolymer is branched by a branching agent consisting of a polyfunctional compound having at least two reactive groups chosen from the group comprising double bonds, aldehyde bonds or epoxy bonds.
  • branching agent consisting of a polyfunctional compound having at least two reactive groups chosen from the group comprising double bonds, aldehyde bonds or epoxy bonds.
  • branched polymer As is known, a branched polymer, designated in the American language by the expression "branched”, is a polymer which has all along the chain of branches, groups or branches arranged globally in a plane and no longer in the three directions , as is a crosslinked polymer; such branched polymers, of high molecular weight, easily soluble in water, are well known as flocculating agents.
  • These branched polyacrylamides are distinguished from crosslinked polyacrylamides (frequently designated by the American expression “crosslinked”), in that in the latter, the groups are arranged three-dimensionally to lead to products which are practically insoluble and of infinite molecular weight;
  • the branching agent is methylene bis acrylamide (MBA), introduced in an amount of five to two hundred (5 to 200) moles per million moles of monomers.
  • MBA methylene bis acrylamide
  • the amount of branched polyacrylamide introduced is between thirty and a thousand grams / ton (30 and 1000 g / t) of dry paste; it has been observed that if the amount is less than 0.03% o, no significant retention is obtained; similarly, if this quantity exceeds 0.1% o, no proportional improvement is observed; however, unlike linear cationic polyacrylamides, as described in the documents EP-A-0 017 353 and 235 893 referred to in the preamble, no reverse effect of dispersion by recirculation in the closed circuits of the excess of polymer not retained on the sheet is observed.
  • the amount of branched polyacrylamide introduced is between 0.05 and 0.5 per thousand (% o) of the amount of the dry paste.
  • the branched polymer is used in the form of a diluted powder; indeed, if a branched emulsion polymer is used, the essential presence in these emulsions of surfactants, promotes the formation of foams during the manufacture of paper and the appearance of disparities in the physical properties of the finished paper (change in absorbance where part of the oil phase of the emulsion is retained on the sheet).
  • Bentonite also known as "swecting smectic clay", from the montmorillonite family, is well known and does not need to be described here in detail; these compounds, formed of microcrystallites, have sites on the surface with a high cation exchange capacity capable of retaining water (see for example document US-A-4 305 781, which corresponds to document EP-A-0 017 353 , mentioned above, and FR-A-2 283 102).
  • a semi-sodium bentonite is preferably used, which is introduced just upstream from the headbox, at a rate of 0.1 to 0.5 percent (0.1 to 0.5%) of the dry weight of the fibrous suspension.
  • the powdered branched polyacrylamide is first dissolved in water, then this solution is introduced into the paste castle of the fibrous suspension circuit, at a rate of 0.05 to 0, 5 per thousand (0.05 to 0.5% o) by dry weight of the dry weight of this fibrous suspension, then the mixture is stirred and sheared, and finally we always add, with stirring, upstream of the headbox, bentonite at 0.1 to 0.5 percent (0.1 to 0.5%) by weight dry fiber suspension.
  • the branched polymer dissolved beforehand is introduced at a concentration of between 0.1 and 3 g / liter in front of the pulp feed pump in the pulp circuit, preferably in the pulp castle, and the bentonite is introduced just upstream of the headbox.
  • a solution is obtained whose pH is 3.6 to which is added, still with stirring, one thousand (1000) ppm of catalyst: isobutyronitrile (AZDN) (or 15 kilograms).
  • AZDN isobutyronitrile
  • the solution is cooled to 0 ° C and degassed by bubbling nitrogen.
  • a transfer agent (mercaptoethanol) is then added at a rate of ten (10) ppm relative to the feed, (ie 0.15 kg) as a reaction limiter.
  • a gel is then obtained which is left to age for two hours, then which is ground, dried with hot air and re-embossed again, until a particle size of less than one millimeter is obtained.
  • a perfectly soluble white powder is then obtained up to forty grams per liter (40 g / l) at room temperature, having an insoluble content of less than 0.02 percent (0.02%).
  • This branched polyacrylamide powder has a Brookfield viscosity close to 2.6 cps (UL, 0.1% in a 1 M Nacl solution at 25 ° C at sixty revolutions per minute (60 rpm)).
  • This polymer has a cationicity of ten (10) mole percent and a cationicity, measured by the colloidal method, lower than the theoretical cationicity. However, after shearing, this cationicity increases, which attests to the branched and non-linear nature of this polymer. Finally, this polymer has an increase in cationicity after shearing of the order of 20%.
  • a paper pulp is prepared comprising 80% of pulp proper at the rate of thirty five percent (35%) of bleached hardwood, ten percent (10%) of broken-coated and thirty five percent (35%) of bleached kraft, and twenty percent (20%) calcium carbonate.
  • the fibrous suspension is diluted in water at the rate of 2.5 grams / liter.
  • the pH of this suspension is 7.5.
  • Example 1 is repeated, replacing the branched polyacrylamide with a linear cationic polyacrylamide of the type described in document FR-B-2 390 983, marketed by the Applicant under the name FO 4190 PG, of viscosity UL 2.9 and commonly used for stationery retention.
  • FO 4190 PG linear cationic polyacrylamide of the type described in document FR-B-2 390 983, marketed by the Applicant under the name FO 4190 PG, of viscosity UL 2.9 and commonly used for stationery retention.
  • the following results are obtained. % o FO 4190 PG % retention 0.2 70 0.5 78 0.75 75
  • a cross-linked emulsion is prepared containing ten mole percent of chloromethylated ADAME with 10 ppm of MBA but without limiter, having a UL viscosity of 2.75.
  • This polyacrylamide is completely crosslinked, therefore sparingly soluble.
  • this emulsion is used as in Example 2 in the amount of 0.2 per thousand.
  • Example 3 The same emulsion is used as in Example 3. It is put in water, then it is sheared by an ULTRATURRAX mixer, sold by the company IKA (Germany), rotating at ten thousand revolutions per minute. After thirty minutes, a maximum increase in cationicity of 35% is then obtained.
  • a solution is obtained whose pH is 3.6 to which is added, still with stirring, one thousand (1000) ppm of catalyst: isobutyronitrile (AZDN) (or 15 kilograms).
  • AZDN isobutyronitrile
  • the solution is cooled to 0 ° C and degassed by bubbling nitrogen.
  • a transfer agent (mercaptoethanol) is then added at a rate of fifty (50) ppm relative to the feed (ie 0.75 kg) as a reaction limiter.
  • a gel is then obtained which is left to age for two hours, then which is ground, dried with hot air and re-embossed again, until a particle size of less than one millimeter is obtained.
  • a perfectly soluble white powder is then obtained up to forty five grams per liter (45 g / l) at room temperature, having an insolubility rate of less than 0.02 percent (0.02%).
  • This branched polyacrylamide powder has a Brookfield viscosity of 1.8 (UL, 0.1% in a 1M NaCl solution at 25 ° C at sixty revolutions per minute (60 rpm)).
  • This polymer has a cationicity of forty five (45) mole percent and a cationicity, measured by the colloidal method, lower than the theoretical cationicity. However, after shearing, this cationicity increases, which attests to the branched and non-linear nature of this polymer. Finally, this polymer has an increase in cationicity after shearing of the order of 23%.
  • a paper pulp is prepared comprising thirty percent (30%) of recovered paper, thirty percent (30%) of bleached kraft, twenty percent (20%) of calcium carbonate, ten percent (10%) of broken -bed and ten percent (10%) of bleached hardwood.
  • This fibrous suspension is diluted in water at the rate of 2.5 grams / liter.
  • the pH of this suspension is 7.6.
  • Kaolin retention was studied in a slightly acidic medium.
  • the fibrous composition is 40% refined bleached kraft and 60% bleached hardwood. 20% load is introduced relative to the fibers. Bonding is carried out with reinforced rosin at a rate of 1.3 percent dry; the pH is adjusted to 5 with alumina sulfate.
  • Example 4 On this suspension, comparison tests were carried out with the branched powder polyacrylamide used in Example 1 in accordance with the invention, the linear powder polymer of the prior art used in Example 2 (FO 4190 PG); the sheared emulsion polymer also from the prior art used in Example 4.
  • the method according to the invention which consists, among the polyacrylamides, of having chosen the branched polyacrylamides in powder form in association with bentonite, not only makes it possible to improve the retention rate unexpectedly compared to the other polyacrylamides, therefore the effectiveness of the treatment, but also makes it possible to improve the clarity of the waters under canvas and this, without opposite effect. In addition, it makes it possible to successfully process loaded pasta.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Paper (AREA)

Claims (5)

  1. Verfahren zur Herstellung von Papier oder Pappe mit verbesserter Retention, bei dem ein Polyacrylamid und Bentonit zur Fasersuspension hinzugegeben werden,
    dadurch gekennzeichnet, daß das Polyacrylamid verzweigt und in Wasser leicht löslich ist und in Form eines Pulvers zugefügt wird, das in einer Menge im Bereich von 0,03 bis 1,0 Gewichtspromille (0,03 bis 1,0 %o), bezogen auf das Trockengewicht der Fasersuspension, aufgelöst wird.
  2. Verfahren nach Anspruch 1,
    dadurch gekennzeichnet, daß das verzweigte Polyacrylamid ein kationisches Copolymer des Acrylamids und eines kationischen ethylenisch-ungesättigten Monomeren ist, das ausgewählt ist aus der Gruppe Dimethylaminoethylacrylat (DMAEA), Dimethylaminoethylmetharylat (DMAEMA), die quaternisiert sind oder in Salzform vorliegen, Dimethyldiallylammoniumchlorid (DADMAC), Acrylamidopropyltrimethylammoniumchlorid (APTAC) und Methacrylamidopropyltrimethylammoniumchlorid (MAPTAC), und daß das Polyacrylamid mit einem Verzweigungsmittel verzweigt wird, das aus einer polyfunktionellen Verbindung mit mindestens zwei reaktiven Gruppierungen besteht, die aus der Gruppe Doppelbindungen, Aldehydbindungen und Epoxidbindungen gewählt sind.
  3. Verfahren nach Anspruch 2,
    dadurch gekennzeichnet, daß das Verzweigungsmittel Methylenbisacrylamid (MBA) ist und in einer Menge im Bereich von fünf bis zweihundert (5 bis 200) Mol pro Mol-million Monomere hinzugegeben wird.
  4. Verfahren nach einem der Ansprüche 1 bis 3,
    dadurch gekennzeichnet, daß das Bentonit ein zur Hälfte Natrium enthaltendes Bentonit ist.
  5. Verfahren nach einem der Ansprüche 1 bis 4,
    dadurch gekennzeichnet, daß das pulverförmige verzweigte polyacrylamid zunächst in Wasser gelöst wird, die entstandene Lösung dann in den Papierbreibehälter eines Papierbreikreislaufs in einer Menge im Bereich von 0,05 bis 0,5 %o Trockengewicht, bezogen auf das Trockengewicht der Fasersuspension eingegeben wird, die Mischung anschließend gerührt und geschert wird und anschließend unter ständigem Rühren das Bentonit in einer Menge im Bereich von 0,1 bis 0,5 Prozent (0,1 bis 0,5%), bezogen auf das Trockengewicht der Fasersuspension, oberhalb des Stoffauflaufkastens, hinzugegeben wird.
EP93420231A 1992-06-11 1993-06-08 Verfahren zur Herstellung von Papier oder Pappe mit verbesserter Retention Expired - Lifetime EP0574335B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9207308A FR2692292B1 (fr) 1992-06-11 1992-06-11 Procédé de fabrication d'un papier ou d'un carton à rétention améliorée.
FR9207308 1992-06-11

Publications (2)

Publication Number Publication Date
EP0574335A1 EP0574335A1 (de) 1993-12-15
EP0574335B1 true EP0574335B1 (de) 1996-04-17

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ID=9430812

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EP93420231A Expired - Lifetime EP0574335B1 (de) 1992-06-11 1993-06-08 Verfahren zur Herstellung von Papier oder Pappe mit verbesserter Retention

Country Status (5)

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US (1) US5393381A (de)
EP (1) EP0574335B1 (de)
CA (1) CA2097127C (de)
DE (1) DE69302221T2 (de)
FR (1) FR2692292B1 (de)

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GB9410920D0 (en) * 1994-06-01 1994-07-20 Allied Colloids Ltd Manufacture of paper
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US5989392A (en) * 1997-09-10 1999-11-23 Nalco Chemical Company Method of using polyammonium quaternary for controlling anionic trash and pitch deposition in pulp containing broke
US20030150575A1 (en) * 1998-06-04 2003-08-14 Snf Sa Paper and paperboard production process and corresponding novel retention and drainage aids, and papers and paperboards thus obtained
FR2779452B1 (fr) * 1998-06-04 2000-08-11 Snf Sa Procede de fabrication de papier et carton et nouveaux agents de retention et d'egouttage correspondants, et papiers et cartons ainsi obtenus
FR2779752B1 (fr) * 1998-06-12 2000-08-11 Snf Sa Procede de fabrication de papier et carton et nouveaux agents de retention correspondants, et papiers et cartons ainsi obtenus
US6835282B2 (en) * 1998-10-16 2004-12-28 Grain Processing Corporation Paper web with pre-flocculated filler incorporated therein
US6103065A (en) * 1999-03-30 2000-08-15 Basf Corporation Method for reducing the polymer and bentonite requirement in papermaking
US6294622B1 (en) * 1999-09-27 2001-09-25 Ecole Polytechnique Federale De Lausanne (Epfl) Polymer flocculants with improved dewatering characteristics
TW550325B (en) * 1999-11-08 2003-09-01 Ciba Spec Chem Water Treat Ltd Manufacture of paper and paperboard
TW524910B (en) 1999-11-08 2003-03-21 Ciba Spec Chem Water Treat Ltd Manufacture of paper and paperboard
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US6605674B1 (en) 2000-06-29 2003-08-12 Ondeo Nalco Company Structurally-modified polymer flocculants
MY140287A (en) 2000-10-16 2009-12-31 Ciba Spec Chem Water Treat Ltd Manufacture of paper and paperboard
DE20220979U1 (de) * 2002-08-07 2004-10-14 Basf Ag Papierprodukt
DE10237378A1 (de) * 2002-08-12 2004-03-11 Basf Ag Vernetzte kationische Copolymere mit Reglern und ihre Verwendung in haarkosmetischen Zubereitungen
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DE102004044379B4 (de) * 2004-09-10 2008-01-10 Basf Ag Verfahren zur Herstellung von Papier, Pappe und Karton und Verwendung einer Retentionsmittelkombination
DE102004063005A1 (de) * 2004-12-22 2006-07-13 Basf Ag Verfahren zur Herstellung von Papier, Pappe und Karton
GB0518059D0 (en) * 2005-09-06 2005-10-12 Dow Corning Delivery system for releasing active ingredients
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US20100000693A1 (en) * 2006-10-31 2010-01-07 Basf Se Method for producing a multi layer fiber web from cellulose fibers
DE102008000811A1 (de) 2007-03-29 2008-10-09 Basf Se Verfahren zur Herstellung von Papier
ES2691384T3 (es) * 2008-09-02 2018-11-27 Basf Se Procedimiento para la fabricación de papel, cartón y cartulina usando endo-beta-1,4-glucanasas como agente de drenaje
EP2477707B8 (de) 2009-09-15 2017-07-26 Suncor Energy Inc. Verfahren zur trocknung von bruchfeinmaterial
CN102596351B (zh) 2009-09-15 2015-07-29 顺科能源公司 对油砂熟化细尾矿进行絮凝和脱水的方法
US9068776B2 (en) 2009-10-30 2015-06-30 Suncor Energy Inc. Depositing and farming methods for drying oil sand mature fine tailings
FR2987375A1 (fr) * 2012-02-27 2013-08-30 Snf Sas Nouveau procede de fabrication de papier mettant en oeuvre un copolymere base ayant reagi avec un aldehyde comme agent de resistance a sec, de retention, d'egouttage et de machinabilite
US10370626B2 (en) 2016-05-23 2019-08-06 Ecolab Usa Inc. Reduced misting acidic cleaning, sanitizing, and disinfecting compositions via the use of high molecular weight water-in-oil emulsion polymers
CA3025288C (en) 2016-05-23 2021-05-18 Ecolab Usa Inc. Reduced misting alkaline and neutral cleaning, sanitizing, and disinfecting compositions via the use of high molecular weight water-in-oil emulsion polymers
CN109661493B (zh) 2016-09-07 2021-11-16 凯米罗总公司 用于制造纸、纸板或类似物的方法和组合物的用途
WO2018160818A1 (en) 2017-03-01 2018-09-07 Ecolab Usa Inc. Reduced inhalation hazard sanitizers and disinfectants via high molecular weight polymers
CN110462132B (zh) * 2017-03-29 2022-08-05 凯米拉公司 生产纸，纸板或类似物的方法
MX2022000454A (es) 2019-07-12 2022-04-18 Ecolab Usa Inc Limpiador alcalino de niebla reducida mediante el uso de polímeros en emulsión solubles en álcali.
WO2022061104A1 (en) 2020-09-18 2022-03-24 Ecolab Usa Inc. Reduced misting peracid based cleaning, sanitizing, and disinfecting compositions via the use of high molecular weight polymers

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Also Published As

Publication number Publication date
CA2097127C (fr) 2003-01-28
DE69302221T2 (de) 1996-10-10
FR2692292B1 (fr) 1994-12-02
EP0574335A1 (de) 1993-12-15
CA2097127A1 (fr) 1993-12-12
FR2692292A1 (fr) 1993-12-17
US5393381A (en) 1995-02-28
DE69302221D1 (de) 1996-05-23

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