EP0777692B1 - Produits de collage de papier, contenant des dispersions aqueuses sans solvant de polymeres cationiques, et procede de fabrication de papier colle au moyen de ces produits - Google Patents

Produits de collage de papier, contenant des dispersions aqueuses sans solvant de polymeres cationiques, et procede de fabrication de papier colle au moyen de ces produits Download PDF

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Publication number
EP0777692B1
EP0777692B1 EP95929873A EP95929873A EP0777692B1 EP 0777692 B1 EP0777692 B1 EP 0777692B1 EP 95929873 A EP95929873 A EP 95929873A EP 95929873 A EP95929873 A EP 95929873A EP 0777692 B1 EP0777692 B1 EP 0777692B1
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EP
European Patent Office
Prior art keywords
paper
copolymerizate
mole
sizing agents
meth
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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EP95929873A
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German (de)
English (en)
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EP0777692A1 (fr
Inventor
Kurt Dahmen
Richard Mertens
Thomas Müller
Johann Schulte
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.)
Stockhausen GmbH and Co KG
Original Assignee
Stockhausen GmbH and Co KG
Chemische Fabrik Stockhausen GmbH
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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
    • 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
    • D21H21/14—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 characterised by function or properties in or on the paper
    • D21H21/16—Sizing or water-repelling agents
    • 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

Definitions

  • the invention relates to compositions for the mass and / or surface sizing of paper, which contain aqueous, solvent-free dispersions of cationic polymers and a method for sizing paper using these agents.
  • Sizing is used in the manufacture of ink-resistant papers and printing papers of the papers on the surface or in bulk in order to improve the wettability of the cellulose and the absorption of water or aqueous liquids through the capillary system of the Reduce paper sheet and the inclusion of printing inks, the white and to improve the opacity and the mechanical properties of the paper sheet.
  • sizing process and the means usually used here in Ullmann's Encyclopedia, Volume 17 (1979) on pages 585 - 587 and on p. 599 described.
  • cationic polymers in the sizing process, which is characterized by It is known to have a high substantivity towards the cellulose fibers.
  • the Japanese Patent JP-A-04 108 196 describes cationic sizing agents based on of rosin and cationic polymers.
  • Japanese publication JP-A-04 091 290, JP-A-63 270 893 and JP-A-59 159 198 describe sizing agents made from alkyl ketene dimers and cationic polymers are formed.
  • DE 37 37 615 C2 sizing agents which are modified with carboxylic acids, represent so-called reinforced resins, which are caused by portions of cationic copolymers be dispersed.
  • the cationic copolymers are Solution polymerization shown and the preparation of the dispersed sizing agent happens from the anionically modified resins and the cationic copolymers in a complex procedure with removal of the solvent by distillation the copolymer, melting of the modified resin and dispersion in Water with the partial use of surfactants.
  • the Resin parts not bound in the paper pulp must contain the process water and, if necessary be removed using other tools.
  • DE 38 26 825 C2 describes cationic sizing agents which are derived from Methyl (meth) acrylate, butyl (meth) acrylate, acrylic acid and 10-30% by weight of N, N dimethylaminoethyl (meth) acrylate are formed and isopropanol or other organic Contain solvents.
  • the sizing agents described are unstable when stored and not sufficiently effective when used.
  • EP 416 427 B1 describes sizing agents based on aqueous, cationic polymer dispersions described, the polymer content from 2-20% by weight of a salt-forming, water-soluble monomer with alkylammonium, alkylsulfonium or alkylphosphonium groups are formed, which, however, always with cationic Polymers such as retention aids and protective colloids (poly-DADMAC) are used, so that these polymers are used in total in a relatively large amount will.
  • the dispersions described also contain emulsifiers and especially non-ionic surfactants, which in addition to the water-soluble retention aids Paper can impair the sizing effect and can pollute the process water.
  • the object of the invention was therefore to include the known cationic sizing agents To avoid avoiding their disadvantages, in particular to provide sizing agents, which can be manufactured more economically and environmentally friendly, are stable in storage and can be used alone as sizing agents without the use of further components and also have an improved effect.
  • the monomers of group a) are in an amount of 30-70 mol% in the copolymer available. If these limits are undershot, unstable dispersions are usually obtained, while a proportion of more than 70 mol% significantly worsens the sizing effect. A proportion of 40-60 mol% of these monomers is preferably used in the copolymer.
  • the monomers of group b) are hydrophobic esters or amides of acrylic acid and / or methacrylic acid. They essentially ensure the sizing effect. Suitable monomers are, for example, 2-ethylhexyl (meth) acrylate, n-octyl (meth) acrylate, isononyl (meth) acrylate, decyl (meth) acrylate, lauryl (meth) acrylate, isotridecyl (meth) acrylate, myristyl (meth) acrylate , Stearyl (meth) acrylate, C 18-22 (meth) acrylate, 2-ethylhexyl (meth) acrylamide, n-octyl (meth) acrylamide, isononyl (meth) acrylamide, decyl (meth) acrylamide, lauryl (meth) acrylamide, Isotridecyl (meth) acrylamide
  • Some of the monomers of group b) can be replaced by long-chain monoolefins. Suitable for this purpose are, for example, octene-1, decene-1, dodecene-1, tetradecene-1, hexadecene-1, octadecen-1, eicosen-1 and C 20-24 or C 30+ alpha-olefin sections. These monomers are also commercially available. They can be used in an amount of 0.001 to 1: 1 in relation to the monomer group b). Octadecene-1 and C 20-24 -alpha-olefin mixtures are preferably used.
  • beta unsaturated monomers are present.
  • Styrenes are suitable, for example, Vinyl esters, vinyl ethers, (meth) acrylic acid and / or (meth) acrylamide.
  • the sizing agents preferably used according to the invention contain copolymers, those with the rejection of organic solvents by bulk polymerization in on be made in a known manner.
  • the polymerization is carried out at temperatures of 20 to 200 ° C., preferably 60 to 160 ° C. carried out. It is initiated thermally, photochemically or redox-catalytically, preferably with the help of peroxo and / or azo compounds.
  • oil-soluble initiators such as, for example 2,2'-azobis (isobutyronitrile) (AIBN), 2,2'-azobis (2-methylbutyronitrile), 4,4'-azo (4-cyanopentanoic acid), 2,2'-azobis (2,4-dimethylvaleronitrile), di-tert-butyl peroxide, Dibenzoyl peroxide or tert-butyl peroxy-2-ethylhexanoate is preferred.
  • AIBN 2,2'-azobis (isobutyronitrile)
  • 2,2'-azobis (2-methylbutyronitrile) 2,2'-azobis (2-methylbutyronitrile)
  • 4,4'-azo (4-cyanopentanoic acid 4,4'-azo (4-cyanopentanoic acid
  • 2,2'-azobis (2,4-dimethylvaleronitrile di-tert-butyl peroxide
  • the number average molecular weight of the copolymers is 1000 to 100,000 g / mol.
  • the molar mass is preferably regulated by using known regulators such as, for example Mercaptoethanol or dodecyl mercaptan.
  • part or all of the amount of Monomers submitted at a suitable temperature, the initiator in whole or in part added to the polymerization mixture and the further reaction under adiabatic Conditions made, the resulting heat of polymerization Reaction batch warmed.
  • the copolymer is neutralized directly with dilute acid and emulsified in water.
  • the amount of acid is chosen so that in End product sets a pH of 8 to 3.
  • Both are inorganic for neutralization Acids such as hydrochloric acid or sulfuric acid, as well as organic acids in particular Carboxylic acids such as formic acid or acetic acid are suitable.
  • the initiator can be added again after neutralization or emulsification to reduce the residual monomer content.
  • oil-soluble and water-soluble initiator systems are then suitable.
  • copolymers are used whose Amino groups partially or completely with a suitable quaternizing agent be implemented.
  • suitable quaternizing agents are methyl chloride, Benzyl chloride, dimethyl sulfate and / or epichlorohydrin.
  • the amount of quaternizing agent is chosen so that a degree of quaternization of 1-100 mol% is preferred 5 to 50 mol%.
  • the reaction takes place in a molar ratio of amino group to Quaternizing agent from 100: 1 to 1: 1, or in one Molar ratio of amino group to epichlorohydrin of 50: 1 to 1: 1.
  • the solids content of the polymer dispersions to be used according to the invention is 10-60% by weight, preferably 20-50% by weight, particularly preferably 30-40 % By weight.
  • copolymer dispersions to be used according to the invention are surprisingly distinguished despite their production without any additional aids, due to good dispersion stability so that even after several weeks of storage at 50 ° C none Separation or coagulation of the polymer can be observed.
  • hydrophobizing sizing of papers especially writing and Suitable for printing papers.
  • they can be used for both mass gluing and Surface sizing agents are used.
  • the invention further relates to a method for paper sizing using the inventive Medium, both for mass and surface sizing.
  • the polymer dispersions are added to the thick or thin material with 0.1 - 3.0% active substance (based on dry substance), while with surface sizing 0.1 - 5.0 g active substance per m 2 onto the paper after Drying section is applied.
  • the polymer dispersions can be used to achieve an immediate sizing, ie the desired hydrophobization of the paper is achieved immediately after the manufacturing process.
  • the disadvantageous process of aging the freshly sized papers which is often necessary when using the sizes currently used to achieve hydrophobic effects and the associated paper properties, can therefore largely be dispensed with.
  • the amount of cationic polymer dispersions used can be outstanding Way to set a graded degree of sizing of the papers, which both acidic as well as reproducible in neutral or alkaline paper production is. Further aids are advantageously not required for the sizing.
  • Solvents and optionally regulators are in the same reactor as in regulation A. submitted and gassed with nitrogen. The mixture is then heated to the intended polymerization temperature and then leaves the from different inlets at the same time Monomers and the initiator (optionally diluted with further solvent) run over the intended response time. After the feed has ended, 2 React for hours. The polymer is then as in Preparation A neutralized and emulsified with dilute acid. The solvent becomes the solvent largely distilled off.
  • paper sheets with a basis weight of approx. 100 g / m 2 were produced in a Rapid-Koethen sheet former.
  • Short fiber pulp (birch sulfate) or waste paper (newspaper printing) or wood pulp were used as raw materials.
  • the sizing agent to be tested was added to the substance / water mixture and 15 Seconds mixed.
  • the sheet was then formed in the sheet former and in a vacuum dryer of the Rapid-Köthen device dried at 92 ° C for 10 minutes.
  • Table 1 shows that very good instant sizing can be achieved with the copolymers to be used according to the invention.
  • the comparative example shows no immediate sizing and, even after 24 hours, gives significantly worse values than the examples according to the invention.
  • Table 2 shows that when the copolymers are used according to the invention, an advantage over known solvents can also be found at lower use concentrations.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Paper (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Claims (9)

  1. Dispersions cationiques, aqueuses, dépourvues de solvant, de polymères cationiques, qui contiennent un agent d'encollage du papier, qui se caractérisent par une teneur en polymères cationiques, que l'on a obtenus par la polymérisation radicalaire en solution en dispersion, de préférence, dans la masse, à partir de
    a) 30 à 70% molaires d'au moins un monomère de la formule générale H2C=CR1-CO-X-R2-N(R3)2 dans laquelle
    R1 = H, CH3
    R2 = un radical alkylène en C2 à C4
    R3 = H, un radical alkyle en C1 à C4 et
    N = O, NH,
    avec
    b) 70 à 30% molaires d'au moins un monomère de la formule H2C=CR1-CO-X-R4 dans laquelle R1 et X possèdent les significations qui leur ont été attribuées à propos de la définition du composé (I) et
    R4 représente un radical alkyle en C8 à C30,
    ainsi que, éventuellement,
    c) 0 à 20% molaires d'au moins une monooléfine en C8 à C30 et
    d) 0 à 10% molaires d'au moins un autre monomère copolymérisable avec
    a), b) et éventuellement c),
    neutralisation subséquente et éventuellement quaternisation des copolymères, ainsi que dispersion dans l'eau ou des liquides aqueux, où la somme des monomères a), b), c) et d) totalise 100% molaires.
  2. Agent d'encollage du papier suivant la revendication 1, caractérisé en ce que les dispersions aqueuses de copolymères contiennent, à titre de monomères du groupe a), du N,N-diméthylaminopropyl(méth)acrylamide et/ou du (méth)acrylate de N,N-diméthylaminoéthyle, de préférence, du N,N-diméthylaminopropylacrylamide et/ou de l'acrylate de N,N-diméthylaminoéthyle et, à titre de monomère du groupe b), du (méth)acrylate de stéaryle.
  3. Agent d'encollage du papier suivant l'une quelconque des revendications 1 et 2, caractérisé par une teneur en un copolymère qui est neutralisé après la polymérisation avec des acides inorganiques et/ou organiques, de préférence, des acides carboxyliques et qui est émulsionné avec de l'eau, où la valeur du pH dans le produit final varie de 3,0 à 8,0 et, éventuellement, on fait réagir les radicaux amino des monomères du groupe a) avec un agent de quaternisation dans le rapport molaire des radicaux amino aux agents de quaternisation de 100: 1 à 1:1.
  4. Agent d'encollage du papier suivant l'une quelconque des revendications 1 à 3, caractérisé par une teneur en un copolymère quaternisé avec de l'épichlorhydrine dans le rapport molaire des radicaux amino à l'épichlorhydrine de 50:1 à 1:1.
  5. Agent d'encollage suivant l'une quelconques des revendications 1 à 4, caractérisé par une teneur en solides de 10 à 60% en poids en polymère.
  6. Agent d'encollage suivant la revendication 5, caractérisé par une teneur en solides de 20 à 50% en poids en polymère.
  7. Agent d'encollage suivant la revendication 6, caractérisé par une teneur en solides de 30 à 40% en poids en polymère.
  8. Procédé de fabrication de papier encollé dans la masse en recourant à l'emploi d'une dispersion de copolymère cationique, caractérisé en ce que l'on utilise, à titre d'agent d'encollage dans la masse, une dispersion d'un copolymère aqueux suivant l'une quelconque des revendications 1 à 7, que l'on mélange à la pâte épaisse ou à la pâte liquide en une proportion de 0,1% à 3,0% de copolymère, par rapport à la pâte de siccité absolue, sous agitation intensive, éventuellement en même temps qu'avec des charges inertes, des pigments et d'autres colorants, comme aussi d'autres adjuvants et on isole le papier encollé et on le sèche.
  9. Procédé de fabrication de papier encollé en surface, en recourant à l'emploi d'une dispersion de copolymère cationique, caractérisé en ce que l'on utilise, à titre d'agent d'encollage en surface, une dispersion aqueuse de copolymère suivant l'une quelconque des revendications 1 à 7, où on applique de 0,1 à 5,0 g de copolymère par m2 de papier après la sécherie.
EP95929873A 1994-08-25 1995-08-16 Produits de collage de papier, contenant des dispersions aqueuses sans solvant de polymeres cationiques, et procede de fabrication de papier colle au moyen de ces produits Expired - Lifetime EP0777692B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE4430069A DE4430069A1 (de) 1994-08-25 1994-08-25 Wäßrige, lösungsmittelfreie Dispersionen von kationischen Polymerisaten enthaltende Papierleimungsmittel und Verfahren zur Herstellung von geleimtem Papier unter Verwendung dieser Mittel
DE4430069 1994-08-25
PCT/EP1995/003232 WO1996006119A1 (fr) 1994-08-25 1995-08-16 Produits de collage de papier, contenant des dispersions aqueuses sans solvant de polymeres cationiques, et procede de fabrication de papier colle au moyen de ces produits

Publications (2)

Publication Number Publication Date
EP0777692A1 EP0777692A1 (fr) 1997-06-11
EP0777692B1 true EP0777692B1 (fr) 1998-04-01

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Country Status (8)

Country Link
US (1) US5954921A (fr)
EP (1) EP0777692B1 (fr)
AT (1) ATE164599T1 (fr)
CA (1) CA2194602A1 (fr)
DE (2) DE4430069A1 (fr)
FI (1) FI970770A0 (fr)
NO (1) NO970833L (fr)
WO (1) WO1996006119A1 (fr)

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DE19851024A1 (de) 1998-11-05 2000-05-11 Basf Ag Wäßrige Dispersionen von wasserlöslichen Polymerisaten von N-Vinylcarbonsäureamiden, Verfahren zu ihrer Herstellung und ihre Verwendung
DE19909653A1 (de) * 1999-03-05 2000-09-07 Stockhausen Chem Fab Gmbh Pulverförmige, vernetzte, wässrige Flüssigkeiten sowie Blut absorbierende Polymere, Verfahren zu ihrer Herstellung und ihre Verwendung
US6572736B2 (en) 2000-10-10 2003-06-03 Atlas Roofing Corporation Non-woven web made with untreated clarifier sludge
US6488812B2 (en) * 2000-12-14 2002-12-03 Kimberly-Clark Worldwide, Inc. Soft tissue with improved lint and slough properties
US20030032352A1 (en) * 2001-03-22 2003-02-13 Yihua Chang Water-dispersible, cationic polymers, a method of making same and items using same
US6893537B2 (en) * 2001-08-30 2005-05-17 Kimberly-Clark Worldwide, Inc. Tissue products containing a flexible binder
US20030127204A1 (en) * 2001-09-06 2003-07-10 Varnell Daniel F. Amphoteric polymer resins that increase the rate of sizing development
US7772138B2 (en) 2002-05-21 2010-08-10 Kimberly-Clark Worldwide, Inc. Ion sensitive, water-dispersible polymers, a method of making same and items using same
FI119250B (fi) * 2002-05-29 2008-09-15 Upm Kymmene Corp Menetelmä irrokepaperin valmistamiseksi
US7101456B2 (en) * 2002-09-20 2006-09-05 Kimberly-Clark Worldwide, Inc. Ion triggerable, cationic polymers, a method of making same and items using same
US7157389B2 (en) 2002-09-20 2007-01-02 Kimberly-Clark Worldwide, Inc. Ion triggerable, cationic polymers, a method of making same and items using same
US6960371B2 (en) 2002-09-20 2005-11-01 Kimberly-Clark Worldwide, Inc. Water-dispersible, cationic polymers, a method of making same and items using same
US6994865B2 (en) 2002-09-20 2006-02-07 Kimberly-Clark Worldwide, Inc. Ion triggerable, cationic polymers, a method of making same and items using same
US7141519B2 (en) * 2002-09-20 2006-11-28 Kimberly-Clark Worldwide, Inc. Ion triggerable, cationic polymers, a method of making same and items using same
US20040084162A1 (en) 2002-11-06 2004-05-06 Shannon Thomas Gerard Low slough tissue products and method for making same
US7988826B2 (en) * 2006-03-30 2011-08-02 Harima Chemicals, Inc. Cationic surface sizing agent and paper coated with the same
DE102011001796A1 (de) 2011-04-05 2012-10-11 Wilhelm Layher Verwaltungs-Gmbh Gerüststiel
WO2012163340A1 (fr) 2011-06-01 2012-12-06 Wilhelm Layher Verwaltungs-Gmbh Ensemble comprenant une pièce d'échafaudage et un élément d'échafaudage vertical

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Also Published As

Publication number Publication date
NO970833D0 (no) 1997-02-24
DE4430069A1 (de) 1996-02-29
WO1996006119A1 (fr) 1996-02-29
DE59501788D1 (de) 1998-05-07
ATE164599T1 (de) 1998-04-15
FI970770A (fi) 1997-02-24
EP0777692A1 (fr) 1997-06-11
FI970770A0 (fi) 1997-02-24
US5954921A (en) 1999-09-21
CA2194602A1 (fr) 1996-02-29
NO970833L (no) 1997-02-24

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