EP0187666B1 - Verfahren zur internen Leimung bei des Herstellung von Papier, Karton, Pappen und anderen cellulosehaltigen Materialien - Google Patents

Verfahren zur internen Leimung bei des Herstellung von Papier, Karton, Pappen und anderen cellulosehaltigen Materialien Download PDF

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Publication number
EP0187666B1
EP0187666B1 EP86100189A EP86100189A EP0187666B1 EP 0187666 B1 EP0187666 B1 EP 0187666B1 EP 86100189 A EP86100189 A EP 86100189A EP 86100189 A EP86100189 A EP 86100189A EP 0187666 B1 EP0187666 B1 EP 0187666B1
Authority
EP
European Patent Office
Prior art keywords
dicyandiamide
resin
cationic
sizing
paper
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
Application number
EP86100189A
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German (de)
English (en)
French (fr)
Other versions
EP0187666A1 (de
Inventor
Rudolf Dr. Eichinger
Horst Dr. Michaud
Josef Dr. Seeholzer
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.)
Evonik Operations GmbH
Original Assignee
SKW Trostberg AG
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
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Application filed by SKW Trostberg AG filed Critical SKW Trostberg AG
Priority to AT86100189T priority Critical patent/ATE47733T1/de
Publication of EP0187666A1 publication Critical patent/EP0187666A1/de
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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
    • D21H17/46—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H17/47—Condensation polymers of aldehydes or ketones
    • D21H17/49—Condensation polymers of aldehydes or ketones with compounds containing hydrogen bound to nitrogen
    • D21H17/50—Acyclic compounds

Definitions

  • the invention relates to a method for internal sizing in the production of paper, cardboard, cardboard and other cellulose-containing materials with and without fillers and / or coating pigments under neutral to weakly basic pH conditions without the use of aluminum salts.
  • Paper production requires a mediator or a fixing agent to bind the resin glue to the fiber surface, since both the resin glue and the cellulose fibers are electronegatively charged and repel each other.
  • Alum aluminum sulfate hydrate
  • Alum is used almost exclusively for this purpose in the production of the paper in an acidic medium, with the best sizing being achieved at a pH value of 4.5 to 5.5.
  • papers produced in this way are not resistant to aging as a result of progressive hydrolysis.
  • aluminum sulfate reacts with calcium carbonate, which is often used as a pigment and filler under neutral conditions, with the elimination of carbon dioxide, which leads to foaming and hole formation on the paper web. Failing calcium sulfate leads to deposits on the machine, so that trouble-free paper production is not possible. Since no substitute has yet been found for the aluminum sulfate, it is not possible to use the usual resin glue in paper production under neutral conditions, but had to fall back on synthetic glue, which made paper production considerably more expensive.
  • a modified pseudo-neutral paper making method is described in Japanese Patent Laid-Open No. 83-174696.
  • a dicyandiamide-formaldehyde condensation product is added to the aluminum sulfate as an additional agent.
  • this method still has the disadvantage that an expensive diketene resin has to be used.
  • European patent application 112 525 proposes an agent for the neutral sizing of cellulose-containing materials, which consists of water, an alcohol which is soluble in water to an unlimited extent, alkali metal or aluminum hydroxide and a saturated or unsaturated fatty acid with 12 to 24 carbon atoms.
  • the aim of the neutral paper production process is to largely reduce or eliminate the use of aluminum sulfate and to replace kaolin as filler or pigment with calcium carbonate.
  • the latter is less expensive than kaolin and its whiteness exceeds that of kaolin. Due to the more favorable flow behavior of calcium carbonate, higher degrees of filling can also be achieved in the paper. In addition, the corrosion on the machine equipment is reduced and the quality of the paper, in particular its resistance to aging, is significantly improved.
  • ketene resins are used together with cationic resins as wet strength agents, whereby a certain sizing effect is achieved.
  • Co-condensation products of dicyandiamide, urea and formaldehyde are used as cationic resins.
  • EP-A 82 373 discloses a process for sizing paper, in which a very special cationic resin is used.
  • the resin to be used according to this process is obtained in a three-step process from dicyandiamide formaldehyde, a polyaminopolyamide, an ammonium salt and from epihalohydrin, acrylamide or urea.
  • This condensation resin is used as a reaction accelerator (promoter) for diketene glues.
  • the present invention is based on the object of developing a paper production process which operates in neutral to weakly basic pH ranges and avoids the disadvantages of the previously known processes under these conditions.
  • This object is achieved by a process for internal sizing in the production of paper, cardboard, cardboard and other cellulose-containing materials with and without fillers and / or pigments by natural or synthetic sizing agents under neutral to weakly basic pH conditions without the use of aluminum salts, which characterized in that the sizing is carried out with the addition of a cationic dicyandiamide resin based on a condensation product of dicyandiamide, with formaldehyde and at least one inorganic or organic acid and / or at least one ammonium or amine salt thereof.
  • the cationic dicyandiamide resins are able to flocculate and fix natural sizing agents under neutral to weakly basic pH conditions. Even without the addition of aluminum sulfate, full sizing can therefore be achieved with the aid of such dicyandiamide resins.
  • Cationic dicyandiamide resins which have a high positive charge and which are therefore able to precipitate anionic, high molecular weight substances quickly and practically quantitatively have proven to be particularly suitable. These resins are expediently not made too acidic, so that after mixing with the stock suspension the pH does not drop significantly below 7.
  • the cationic dicyandiamide resins used according to the invention can be prepared, for example, by reacting 1 mol of dicyandiamide with 1.0 to 4.0 mol of formaldehyde in the presence of 0.1 to 2.0 mol of at least one inorganic or organic acid and / or at least one ammonium or amine salt thereof and optionally up to 0.5 mol of a di- or polyvalent amine.
  • Condensation products prepared in this way have pH values of about 3 to about 5, are miscible with water in any ratio and can be used well as an approximately 50% aqueous solution.
  • acids such as B. strong inorganic acids such as hydrochloric acid, sulfuric acid or nitric acid.
  • weakly acidic organic acids such as. B. formic acid, acetic acid or oxalic acid is used.
  • ammonium salt can be used in resin production such.
  • B. ammonium salts of strong inorganic acids such as ammonium chloride or ammonium sulfate or ammonium salts of organic acids such as ammonium formate or acetate can be used.
  • amine salts salts of organic amines with inorganic or organic acids such as.
  • B. ethylenediamine formate or triethylenetetramine hydrochloride can be used.
  • the salts mentioned can also be used in a mixture with inorganic or organic acids.
  • Divalent or polyvalent aliphatic amines can be used as the amine component to be added. Ethylene diamine, propylene diamine, diethylene triamine and triethylene tetramine are preferably used. Their derivatives substituted on the nitrogen by hydroxyl groups can also be used, such as, for. B. mono- or diethanolamine. If amines are added, their amount is preferably at least 0.05 mol per mol of dicyandiamide.
  • Formaldehyde can be used in any form, preferably in the form of its 30 to 40% by weight aqueous solutions.
  • Neutral to weakly basic pH values are understood to mean those between pH 6.5 and 8.5, preferably between 7.0 and 8.0.
  • the condensation products obtained by the process described are clear, colorless, water-miscible products.
  • cationic dicyandiamide resins produced by other processes can also be used within the scope of the invention.
  • the amount of cationic dicyandiamide resin to be used is based on the amount of material (cellulose) and is generally 0.1 to 10% by weight; 0.2 to 5% by weight of dicyandiamide resin is preferably used, advantageously in the form of an approximately 50% strength aqueous solution.
  • Suitable products are e.g. B. rosin, animal glue, casein, starch, waxes, fatty acids and tall resins.
  • synthetic glues products based on ketene dimers, polyvinyl alcohols or polyvinyl acetates are particularly suitable. Products used as ketene dimers are those which have been produced on the basis of alkyl-substituted, dimeric ketene with an oxetanone structure, starting from long-chain fatty acids, and which are sold under the brand name Aquapel.
  • modified resin glues such as z. B. by implementing z. B.
  • rosin can be obtained with dienophilic acids and are commercially available under the brand name Purtin 3 N / S.
  • extremely finely divided dispersions of specially modified, reinforced resins e.g. Furtin BVR 510) can be used with advantage.
  • the method according to the invention now surprisingly allows combinations of cationic dicyandiamide resin with the chemically very different glue components mentioned above, to flocculate them and fix them on the fiber.
  • full or partial sizing of the paper can be achieved with natural, synthetic or modified resin glues without the aid of further aids.
  • All fillers and pigments customary in paper production can also be used in the process according to the invention, such as, for. B. kaolin, aluminum silicates, calcium silicates, oxyhydrates of aluminum, talc, satin white, gypsum, barium sulfate, barium carbonate, magnesite, zinc oxide, titanium dioxide.
  • calcium carbonate is preferably used. This can consist of natural calcium carbonate in finely ground form or it can also be precipitated calcium carbonate. Calcium carbonate is preferred because its whiteness z. B. exceeds that of kaolin and its favorable flow behavior allows particularly high filling levels in the paper to be achieved. This also has a positive influence on the paper properties: opacity is increased, whiteness is improved, aging resistance is increased and mechanical properties are increased.
  • a cationic dicyandiamide-formaldehyde resin 84 parts by weight of dicyandiamide are placed in a stirred vessel equipped with a reflux condenser with 220 parts by weight of 30% strength aqueous formaldehyde and 43 parts by weight of ammonium chloride. At room temperature, 7.7 parts by weight of ethylenediamine (78%) are then added with stirring. The reaction starts immediately and the temperature of the reaction mixture rises to 90 to 95 ° C. The reaction is complete after about 10 minutes. Then water is added to adjust the concentration of 50% by weight of solid in the resin.
  • ammonium chloride instead of ammonium chloride, an inorganic or organic acid such as. B. hydrochloric acid or formic acid can be used.
  • Leaves are formed on a Rapid-Köthen sheet former using bleached pine pulp with a freeness of 24 ° SR, resin glue (free resin glue Furtin 3N) and 50% aqueous cationic dicyandiamide resin (made from dicyandiamide, formaldehyde, ammonium chloride and ethylenediamine) and thermally formed on cylinders for 3 minutes treated at 120 ° C for a long time. After the air conditioning, the sizing was determined by the water absorption using the Cobb test (60 sec.) In accordance with DIN 531 32. The use of the cationic dicyandiamide resin was compared to alum as a sizing agent, the pH adjusting itself.
  • resin glue free resin glue Furtin 3N
  • aqueous cationic dicyandiamide resin made from dicyandiamide, formaldehyde, ammonium chloride and ethylenediamine
  • Sheet formation using calcium carbonate as a filler Sheet formation using calcium carbonate as a filler.
  • test conditions were the same as in Example 1, but weakly anionic calcium carbonate was added as a filler.
  • the weight ratio of pulp to filler was 1 2.
  • the filler was processed for 5 minutes in an Ultra Turrax (dispersing device), then mixed with the pulp for 3 minutes and then the glue and the cationic dicyandiamide resin were added.
  • Example 2 The same cationic dicyandiamide resin and the same calcium carbonate quality were used as in Example 2.
  • a synthetic product based on diketene (Aquapel 2) was used for sizing. The quality of the sizing was determined using the Cobb test.
  • Example 4 The same dicyandiamide resin and the same resin size were used as in Example 4. Weakly anionic calcium carbonate was used as the filler. The sheets were produced in a manner analogous to that given in Example 1.
  • Example 6 Using the cationic dicyandiamide resin mentioned in Example 6, the same specially modified resin size and weakly anionic calcium carbonate as filler, sheets were produced in accordance with Example 1, the Cobb values of which are shown in the following table.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Paper (AREA)
  • Cartons (AREA)
  • Wrappers (AREA)
  • Steroid Compounds (AREA)
EP86100189A 1985-01-08 1986-01-08 Verfahren zur internen Leimung bei des Herstellung von Papier, Karton, Pappen und anderen cellulosehaltigen Materialien Expired EP0187666B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT86100189T ATE47733T1 (de) 1985-01-08 1986-01-08 Verfahren zur internen leimung bei des herstellung von papier, karton, pappen und anderen cellulosehaltigen materialien.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3500408 1985-01-08
DE19853500408 DE3500408A1 (de) 1985-01-08 1985-01-08 Verfahren zur herstellung von papier, karton, pappen und anderen cellulosehaltigen materialien unter neutralen bis schwach basischen ph-bedingungen

Publications (2)

Publication Number Publication Date
EP0187666A1 EP0187666A1 (de) 1986-07-16
EP0187666B1 true EP0187666B1 (de) 1989-11-02

Family

ID=6259431

Family Applications (1)

Application Number Title Priority Date Filing Date
EP86100189A Expired EP0187666B1 (de) 1985-01-08 1986-01-08 Verfahren zur internen Leimung bei des Herstellung von Papier, Karton, Pappen und anderen cellulosehaltigen Materialien

Country Status (8)

Country Link
US (1) US5026457A (da)
EP (1) EP0187666B1 (da)
AT (1) ATE47733T1 (da)
CA (1) CA1274059A (da)
DE (2) DE3500408A1 (da)
DK (1) DK2986A (da)
FI (1) FI81861C (da)
NO (1) NO165810C (da)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8157961B2 (en) 2005-11-01 2012-04-17 International Paper Company Paper substrate having enhanced print density
US8460511B2 (en) 2008-10-01 2013-06-11 International Paper Company Paper substrate containing a wetting agent and having improved printability
US8465622B2 (en) 2007-12-26 2013-06-18 International Paper Company Paper substrate containing a wetting agent and having improved print mottle

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3742764A1 (de) * 1987-12-17 1989-06-29 Sueddeutsche Kalkstickstoff Flockungs- und/oder fixiermittel fuer die papierleimung
US5755930A (en) * 1994-02-04 1998-05-26 Allied Colloids Limited Production of filled paper and compositions for use in this
US5685815A (en) * 1994-02-07 1997-11-11 Hercules Incorporated Process of using paper containing alkaline sizing agents with improved conversion capability
US5846663A (en) 1994-02-07 1998-12-08 Hercules Incorporated Method of surface sizing paper comprising surface sizing paper with 2-oxetanone ketene multimer sizing agent
US5725731A (en) * 1995-05-08 1998-03-10 Hercules Incorporated 2-oxetanone sizing agents comprising saturated and unsaturated tails, paper made with the 2-oxetanone sizing agents, and use of the paper in high speed converting and reprographic operations
US5827398A (en) * 1996-02-13 1998-10-27 Allied Colloids Limited Production of filled paper
WO1997041302A1 (en) * 1996-04-29 1997-11-06 Minerals Technologies Inc. Rosin-sized paper composition and method of making
US20060288906A1 (en) * 2005-04-27 2006-12-28 Martin Wulf Process of preparation of specific color effect pigments
JP4995831B2 (ja) * 2005-11-01 2012-08-08 インターナショナル・ペーパー・カンパニー 高印刷濃度を有する紙基材
WO2009012292A1 (en) * 2007-07-16 2009-01-22 Luzenac America, Inc. Wax coatings, methods of making coated articles and coated articles therefrom

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0082373A1 (en) * 1981-12-08 1983-06-29 Hercules Incorporated Dicyandiamide-formaldehyde condensates and process for preparing the same

Family Cites Families (21)

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Publication number Priority date Publication date Assignee Title
DE1070916B (da) * 1959-12-10
CA618976A (en) * 1961-04-25 Badische Anilin- And Soda-Fabrik Aktiengesellschaft Process of sizing paper
CH233160A (de) * 1942-06-23 1944-07-15 Ag J R Geigy Verfahren zur Darstellung von Textilhilfsmitteln.
DE1034858B (de) * 1952-03-18 1958-07-24 Jacques Wolf & Co Verfahren zur Herstellung eines in waessriger Loesung stabilen und nicht gelierendenHarzes aus Dicyandiamid und Formaldehyd
DE1012282B (de) * 1952-06-16 1957-07-18 Sueddeutsche Kalkstickstoff Mittel zur Veredelung von Textilien, Papier, Leder od. dgl.
DE1029561B (de) * 1955-07-25 1958-05-08 Boehme Fettchemie Gmbh Verfahren zur Herstellung von wasserloeslichen, haertbaren, kationischen Kondensationsprodukten aus Dicyandiamid und Formaldehyd
US3016325A (en) * 1955-11-01 1962-01-09 Electro Chem Fiber Seal Corp Process of combining water-insoluble additament with organic fibrous material
DE1078768B (de) * 1957-02-13 1960-03-31 Basf Ag Verfahren zur Herstellung kationischer Kondensationsprodukte
FR1127272A (fr) * 1957-03-28 1956-12-12 Sueddeutsche Kalkstickstoff Produit pour l'affinage de textiles, papiers, cuirs ou autres
FR1218904A (fr) * 1958-03-26 1960-05-13 Basf Ag Procédé pour le collage du papier
US3410649A (en) * 1967-03-01 1968-11-12 Diamond Shamrock Corp Cationic resins which are the reaction product of formaldehyde and the reaction product of amino bases with a methylolated amine salt
US3582461A (en) * 1968-02-14 1971-06-01 Diamond Shamrock Corp Pitch control in pulp and papermaking processes
GB1373788A (en) * 1971-10-20 1974-11-13 Hercules Powder Co Ltd Sizing method and composition for use therein
US3957574A (en) * 1971-10-20 1976-05-18 Hercules Powder Company Limited Sizing method and composition for use therein
US3840486A (en) * 1972-07-03 1974-10-08 Hercules Inc Water-soluble,thermosettable resinous compositions prepared from dicyandiamide,hcho,ammonium salt and a salt of an aminopolyamide and method for preparing the same
DE2514908C3 (de) * 1975-04-05 1980-08-21 Cassella Ag, 6000 Frankfurt Hilfsmittel für die Herstellung von Papier und Pappe und seine Verwendung
CA1144691A (en) * 1977-08-19 1983-04-12 David H. Dumas Sizing accelerator
CH632546A5 (de) * 1977-08-26 1982-10-15 Ciba Geigy Ag Verfahren zur herstellung von geleimtem papier oder karton unter verwendung von polyelektrolyten und salzen von epoxyd-amin-polyaminoamid-umsetzungsprodukten.
JPS6028959B2 (ja) * 1977-11-22 1985-07-08 ライオン・アクゾ株式会社 紙の表面サイジング方法
US4240935A (en) * 1978-12-22 1980-12-23 Hercules Incorporated Ketene dimer paper sizing compositions
JPS58174696A (ja) 1982-04-06 1983-10-13 三菱製紙株式会社 中性紙

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0082373A1 (en) * 1981-12-08 1983-06-29 Hercules Incorporated Dicyandiamide-formaldehyde condensates and process for preparing the same

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8157961B2 (en) 2005-11-01 2012-04-17 International Paper Company Paper substrate having enhanced print density
US8465622B2 (en) 2007-12-26 2013-06-18 International Paper Company Paper substrate containing a wetting agent and having improved print mottle
US8460511B2 (en) 2008-10-01 2013-06-11 International Paper Company Paper substrate containing a wetting agent and having improved printability

Also Published As

Publication number Publication date
FI855199A0 (fi) 1985-12-31
FI81861C (fi) 1990-12-10
FI855199L (fi) 1986-07-09
DK2986D0 (da) 1986-01-03
DE3500408A1 (de) 1986-07-10
NO165810C (no) 1991-04-10
NO165810B (no) 1991-01-02
NO855124L (no) 1986-07-09
DK2986A (da) 1986-07-09
EP0187666A1 (de) 1986-07-16
FI81861B (fi) 1990-08-31
US5026457A (en) 1991-06-25
ATE47733T1 (de) 1989-11-15
DE3666709D1 (en) 1989-12-07
CA1274059A (en) 1990-09-18

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