EP1399623B1 - Apprets pour papier conferant une resistance a l'humidite - Google Patents

Apprets pour papier conferant une resistance a l'humidite Download PDF

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Publication number
EP1399623B1
EP1399623B1 EP02778852.0A EP02778852A EP1399623B1 EP 1399623 B1 EP1399623 B1 EP 1399623B1 EP 02778852 A EP02778852 A EP 02778852A EP 1399623 B1 EP1399623 B1 EP 1399623B1
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EP
European Patent Office
Prior art keywords
paper
wet strength
weight
acid
epihalohydrin
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
Application number
EP02778852.0A
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German (de)
English (en)
Other versions
EP1399623A1 (fr
Inventor
Ellen KRÜGER
Martin Wendker
Stefan Frenzel
Claus BÖTTCHER
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BASF SE
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BASF SE
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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
    • D21H21/18—Reinforcing agents
    • D21H21/20—Wet strength 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
    • D21H17/46—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H17/54—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen
    • 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
    • D21H17/46—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H17/54—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen
    • D21H17/56—Polyamines; Polyimines; Polyester-imides
    • 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
    • D21H17/71—Mixtures of material ; Pulp or paper comprising several different materials not incorporated by special processes
    • D21H17/72—Mixtures of material ; Pulp or paper comprising several different materials not incorporated by special processes of organic material

Definitions

  • the invention relates to wet strength equipment for paper and to a process for producing wet strength finished paper.
  • a polymer combination which is prepared by crosslinking a polymer blend of a polyamidoamine and a vinylamine polymer with an epihalohydrin.
  • Such reaction products are added to the stock in the manufacture of paper to increase the dry and wet strength of paper.
  • Vinylamine units containing copolymers are known which are prepared by hydrolysis of copolymers of N-vinyl formamide and other ethylenically unsaturated monomers.
  • the copolymers containing vinylamine units are added to the pulp in papermaking to increase the dry and wet strength of paper.
  • reaction products formed in the reaction of epihalohydrins with compounds containing amino groups have the disadvantage that they have larger amounts of chlorine-containing by-products.
  • the invention further relates to the use of the wet strength agents described above in the production of paper as an additive to the paper stock before sheet formation in amounts of 0.1 to 4 wt .-%, based on dry fiber.
  • Water-soluble polyamidoamines crosslinked with an epihalohydrin are suitable as component (a) of the paper wet strength agent according to the invention.
  • Be polyamidoamines For example, prepared by condensation of dicarboxylic acids with polyalkylenepolyamines, cf. US-A-2,926,154 and WO-A-98/32798 , For example, from 0.8 to 1.4 moles of a polyalkylenepolyamine are used per mole of dicarboxylic acid.
  • aliphatic dicarboxylic acids having 2 to 10 carbon atoms, e.g. Oxalic acid, malonic acid, succinic acid, maleic acid, glutaric acid, adipic acid, azelaic acid and lauric acid.
  • Preferred dicarboxylic acids are adipic acid and glutaric acid.
  • polyalkylenepolyamines examples include diethylenetriamine, tripropylenetetramine, tetraethylenepentamine, methyl-bis- (3-aminopropyl) amine, diaminopropylethylenediamine, bis-aminopropylethylenediamine and aminopropylethylenediamine.
  • the condensation of the dicarboxylic acids with the polyalkylenepolyamines takes place at higher temperatures, eg. B. at 110 to 220 ° C.
  • the water formed during the condensation is distilled off from the reaction mixture.
  • the condensation can also be carried out in the presence of lactones or lactams of carboxylic acids having 4 to 8 C atoms.
  • the reaction with epihalohydrins, preferably epichlorohydrin is carried out in aqueous solution at temperatures of e.g. 20 to 100 ° C, preferably 30 to 80 ° C.
  • the reaction of the polyamidoamines with Epihalohydrinen is only so far out that the resulting reaction products remain dissolved in water.
  • reaction solution Once the viscosity of the reaction solution has reached the desired level, further reaction is carried out by adding an acid, e.g. Acetic or formic acid, stopped.
  • the cationic polymers may be e.g. derived from synthetic and natural cationic polymers.
  • Suitable natural polymers include, for example, cationic polysaccharides, cationic starch, cationic amylose and derivatives thereof, cationic amylopectin and its derivatives, and cationic guar derivatives.
  • the synthetic cationic polymers include, for example, polyethyleneimines. They are z. B. prepared by polymerization of ethyleneimine in aqueous solution in the presence of acid-releasing compounds, acids or Lewis acids. Polyethyleneimines are commercially available, they have, for example Molar masses of 200 to 2,000,000, preferably from 200 to 1,000,000. Polyethyleneimines having molecular weights of 500 to 800,000 are particularly preferably used in the process according to the invention.
  • Another class of synthetic cationic compounds are polymers containing vinylamine units.
  • it is for example of open-chain N-vinylcarboxamides of the formula in which R 1 and R 2 may be identical or different and are hydrogen and C 1 - to C 6 -alkyl.
  • the monomers mentioned can be polymerized either alone, in mixture with one another or together with other monoethylenically unsaturated monomers. Preferably starting from homopolymers or copolymers of N-vinylformamide.
  • Suitable monoethylenically unsaturated monomers which are copolymerized with the N-vinylcarboxamides are all compounds which can be copolymerized therewith.
  • Examples include vinyl esters of saturated carboxylic acids of 1 to 6 carbon atoms such as vinyl formate, vinyl acetate, vinyl propionate and vinyl butyrate.
  • Suitable comonomers are ethylenically unsaturated C 3 - to C 6 -carboxylic acids, for example acrylic acid, methacrylic acid, maleic acid, crotonic acid, itaconic acid and vinyl ester acid and their alkali metal and alkaline earth metal salts, esters, amides and nitriles of said carboxylic acids, for example methyl acrylate, methyl methacrylate, ethyl acrylate and ethyl methacrylate.
  • C 3 - to C 6 -carboxylic acids for example acrylic acid, methacrylic acid, maleic acid, crotonic acid, itaconic acid and vinyl ester acid and their alkali metal and alkaline earth metal salts, esters, amides and nitriles of said carboxylic acids, for example methyl acrylate, methyl methacrylate, ethyl acrylate and ethyl methacrylate.
  • carboxylic acid esters are derived from glycols or polyalkylene glycols, in each case only one OH group esterified, for example hydroxyethyl acrylate, hydroxyethyl methacrylate, hydroxypropyl acrylate, hydroxybutyl acrylate, hydroxypropyl methacrylate, hydroxybutyl methacrylate and acrylic acid monoesters of polyalkylene glycols having a molecular weight of 500 to 10,000.
  • Esters of ethylenically unsaturated carboxylic acids with aminoalcohols such as, for example, dimethylaminoethyl acrylate, dimethylaminoethyl methacrylate, Diethylaminoethyl acrylate, diethylaminoethyl methacrylate, dimethylaminopropyl acrylate, dimethylaminopropyl methacrylate, diethylaminopropyl acrylate, dimethylaminobutyl acrylate and diethylaminobutyl acrylate.
  • aminoalcohols such as, for example, dimethylaminoethyl acrylate, dimethylaminoethyl methacrylate, Diethylaminoethyl acrylate, diethylaminoethyl methacrylate, dimethylaminopropyl acrylate, dimethylaminopropyl methacrylate, diethylaminopropyl acrylate
  • the basic acrylates can be used in the form of the free bases, the salts with mineral acids such as hydrochloric acid, sulfuric acid or nitric acid, the salts with organic acids such as formic acid, acetic acid, propionic acid or sulfonic acids or in quaternized form.
  • Suitable quaternizing agents are, for example, dimethyl sulfate, diethyl sulfate, methyl chloride, ethyl chloride or benzyl chloride.
  • Suitable comonomers for the monomers of formula I are amides of ethylenically unsaturated carboxylic acids such as acrylamide, methacrylamide and N-alkyl mono- and diamides of monoethylenically unsaturated carboxylic acids having alkyl radicals of 1 to 6 carbon atoms, e.g. N-methylacrylamide, N, N-dimethylacrylamide, N-methylmethacrylamide, N-ethylacrylamide, N-propylacrylamide and tert. Butylacrylamide and basic (meth) acrylamides, such.
  • N-vinylpyrrolidone N-vinylcaprolactam
  • acrylonitrile methacrylonitrile
  • N-vinylimidazole substituted N-vinylimidazoles
  • N-vinyl-2-methylimidazole N-vinyl-4-methylimidazole
  • N-vinyl-5-methylimidazole N-vinyl-2-ethylimidazole
  • N-vinylimidazolines such as N-vinylimidazoline, N-vinyl-2-methylimidazoline and N- vinyl-2-ethylimidazoline.
  • N-vinylimidazoles and N-vinylimidazolines are used, except in the form of the free bases, also in neutralized or quaternized form with mineral acids or organic acids, the quaternization preferably being carried out with dimethyl sulfate, diethyl sulfate, methyl chloride or benzyl chloride. Also suitable are diallyldialkylammonium halides, e.g. Diallyldimethylammonium.
  • Suitable comonomers for N-vinylcarboxamides are monomers containing sulfo groups, such as, for example, vinylsulfonic acid, allylsulfonic acid, methallylsulfonic acid, styrenesulfonic acid, the alkali metal or ammonium salts of these acids or 3-sulfopropyl acrylate.
  • the homopolymers of the N-vinylcarboxamides of the formula I and their copolymers can be hydrolyzed to 1 to 100, advantageously 5 to 100, preferably 10 to 100 mol%. In most cases, the degree of hydrolysis of the homopolymers and copolymers is 20 to 95 mol%. The degree of hydrolysis of the homopolymers is synonymous with the content of the polymers of vinylamine units.
  • copolymers e.g. In addition to the hydrolysis of the N-vinylformamide units, hydrolysis of the ester groups to form vinyl alcohol units may occur. This is especially the case when carrying out the hydrolysis of the copolymers in the presence of sodium hydroxide solution. Polymerized acrylonitrile is also chemically altered upon hydrolysis. This produces, for example, amide groups or carboxyl groups.
  • the polymers containing vinylamine units may optionally contain up to 20 mol% of amidine units, e.g. B. by intramolecular reaction of an amino group with an adjacent amide z. B. of copolymerized N-vinylformamide formed.
  • the polymers containing vinylamine units also include hydrolyzed graft polymers of N-vinylformamide on polysaccharides, polyalkylene glycols and polyvinyl acetate.
  • the grafted onto the polymers N-vinylformamide units are converted by hydrolysis with elimination of formyl groups in the corresponding vinylamine units containing polymers.
  • Vinylamine units containing graft polymers are, for example, in US-A-5,334,287 . US-A-6,048,945 and US-A-6,060,566 described.
  • the cationic polymers in the form of salt-free aqueous solutions or in low-salt aqueous solutions containing at most up to 5 wt .-%, preferably at most up to 2 wt .-% of an inorganic salt used.
  • salt-free or low-salt solutions can be prepared, for example, by ultrafiltration or by precipitation of the neutral salts with organic solvents, such as acetone, methyl ethyl ketone or alcohols.
  • the molecular weight M w of the cationic polymers is at least 15,000 and is preferably in the range of 50,000 to 10 million.
  • the molecular weight M w of the cationic polymers is determined by light scattering.
  • the cationic polymers have, for example, a charge density of at least 1.5, preferably 4 to 15 meq / g (measured at pH 7).
  • Wood pulp includes, for example, groundwood, thermomechanical pulp (TMP), chemothermomechanical pulp (CTMP), pressure groundwood, semi-pulp, high yield pulp, and refiner mechanical pulp (RMP).
  • Suitable pulps are, for example, sulphate, sulphite and soda pulps.
  • the unbleached pulps also referred to as unbleached kraft pulp, are used.
  • Suitable annual plants for the production of pulps are, for example, rice, wheat, sugar cane and kenaf.
  • Waste paper is also used alone or in admixture with other fibers to make the pulps.
  • Waste paper also belongs to waste paper, which gives rise to the white pitch due to the content of binders for coating and printing inks.
  • the reason for the formation of so-called stickies is given by adhesives derived from self-adhesive labels and envelopes, as well as glues from the backsliding of books and so-called hotmelts.
  • the fibers mentioned can be used alone or mixed with one another.
  • the wet strength agents of components (a) and (b) according to the present invention contain, for example, from 0.1 to 20, preferably from 0.2 to 5,% by weight of a cationic natural and / or synthetic polymer.
  • the wet strength agents are in the production of paper to the pulp in amounts of 0.1 to 5 wt .-%, preferably 0.5 to 4 wt .-%, each based on dry pulp dosed.
  • the components (a) and (b) may also be added to the paper stock separately from each other in the paper-making ratio described above. It is thus possible, for example, first to add component (a) to the paper stock and then to meter component (b), for example, just before the headbox.
  • the order of the components can also be reversed, as well as both components can be added simultaneously through a two-fluid nozzle or through two separately arranged metering in the pulp.
  • wet strength of paper is increased by increasing the amount of a conventional wet strength agent, e.g. a crosslinked with epichlorohydrin polyamidoamine according to component (a), can not be increased above a certain value, obtained with the wet strength according to the invention a further increase in the wet strength of the paper.
  • a conventional wet strength agent e.g. a crosslinked with epichlorohydrin polyamidoamine according to component (a)
  • the percentages in the examples are by weight.
  • the wet tear length was determined according to DIN ISO 3781 after a water storage of 15 minutes.

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  • Paper (AREA)

Claims (5)

  1. Apprêts pour papier conférant une résistance à l'humidité, caractérisés en ce qu'ils contiennent des mélanges de
    (a) 1 à 99,9 % en poids d'une polyamidoamine réticulée avec une épihalohydrine et
    (b) 0,1 à 20 % en poids d'au moins un autre polymère cationique du groupe des
    - polymères contenant des unités vinylamine et/ou
    - condensés de dicyandiamide-formaldéhyde.
  2. Apprêts conférant une résistance à l'humidité selon la revendication 1, caractérisés en ce qu'ils contiennent en tant que
    (a) une polyamidoamine réticulée avec de l'épichlorhydrine et
    (b) un polyvinylformamide hydrolysé à hauteur de 1 à 100 % en moles.
  3. Procédé de fabrication de papier par déshydratation d'une pâte à papier en présence d'un apprêt conférant une résistance à l'humidité, caractérisé en ce que des mélanges de
    (a) 1 à 99,9 % en poids d'une polyamidoamine réticulée avec une épihalohydrine et
    (b) 0,1 à 20 % en poids d'au moins un autre polymère cationique du groupe des
    - polymères contenant des unités vinylamine et/ou
    - condensés de dicyandiamide-formaldéhyde sont utilisés en tant qu'apprêt conférant une résistance à l'humidité.
  4. Procédé de fabrication de papier selon la revendication 3, caractérisé en ce que tout d'abord (a) une polyamidoamine réticulée avec une épihalohydrine, puis (b) au moins un autre polymère cationique sont ajoutés à la pâte à papier, l'ordre d'ajout des composants à la pâte à papier est inversé ou les composants (a) et (b) sont ajoutés simultanément, les composants (a):(b) étant à chaque fois utilisés en un rapport en poids de 1 à 99,9 sur 0,1 à 20.
  5. Utilisation des apprêts conférant une résistance à l'humidité selon les revendications 1 à 2 lors de la fabrication de papier en tant qu'additif pour la pâte à papier avant la formation de feuilles en quantités de 0,1 à 4 % en poids, par rapport à la matière fibreuse sèche.
EP02778852.0A 2001-06-11 2002-05-29 Apprets pour papier conferant une resistance a l'humidite Expired - Lifetime EP1399623B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10127829 2001-06-11
DE10127829 2001-06-11
PCT/EP2002/005900 WO2002101144A1 (fr) 2001-06-11 2002-05-29 Apprets pour papier conferant une resistance a l'humidite

Publications (2)

Publication Number Publication Date
EP1399623A1 EP1399623A1 (fr) 2004-03-24
EP1399623B1 true EP1399623B1 (fr) 2015-01-07

Family

ID=7687616

Family Applications (1)

Application Number Title Priority Date Filing Date
EP02778852.0A Expired - Lifetime EP1399623B1 (fr) 2001-06-11 2002-05-29 Apprets pour papier conferant une resistance a l'humidite

Country Status (6)

Country Link
US (2) US20040149411A1 (fr)
EP (1) EP1399623B1 (fr)
JP (1) JP2004529279A (fr)
CN (1) CN100436707C (fr)
CA (1) CA2447136A1 (fr)
WO (1) WO2002101144A1 (fr)

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CN104017207A (zh) * 2014-06-12 2014-09-03 上海东升新材料有限公司 抄纸断纸控制剂及其制备方法
CN104074098A (zh) * 2014-06-25 2014-10-01 金东纸业（江苏）股份有限公司 一种造纸浆料的配制方法以及造纸浆料
KR102063409B1 (ko) * 2015-12-25 2020-01-07 세이코 피엠씨 가부시키가이샤 폴리아크릴아미드계 제지용 첨가제 및 그의 제조 방법, 및 종이의 제조 방법
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Also Published As

Publication number Publication date
CN1531613A (zh) 2004-09-22
JP2004529279A (ja) 2004-09-24
US20040149411A1 (en) 2004-08-05
EP1399623A1 (fr) 2004-03-24
WO2002101144A1 (fr) 2002-12-19
CN100436707C (zh) 2008-11-26
CA2447136A1 (fr) 2002-12-19
US20090008051A1 (en) 2009-01-08
US8025767B2 (en) 2011-09-27

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