EP1733093B1 - Papiere mit hohem durchdringungswiderstand gegen fette und öle und verfahren zu deren herstellung - Google Patents

Papiere mit hohem durchdringungswiderstand gegen fette und öle und verfahren zu deren herstellung Download PDF

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Publication number
EP1733093B1
EP1733093B1 EP20050739014 EP05739014A EP1733093B1 EP 1733093 B1 EP1733093 B1 EP 1733093B1 EP 20050739014 EP20050739014 EP 20050739014 EP 05739014 A EP05739014 A EP 05739014A EP 1733093 B1 EP1733093 B1 EP 1733093B1
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EP
European Patent Office
Prior art keywords
paper
water
polyvinyl alcohols
acetalised
polyvinyl
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
EP20050739014
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German (de)
English (en)
French (fr)
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EP1733093A1 (de
Inventor
Bernd Ullmann
Thomas Claussen
Robert Fuss
Richard Weilbacher
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Kuraray Europe GmbH
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Kuraray Europe GmbH
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Filing date
Publication date
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Publication of EP1733093A1 publication Critical patent/EP1733093A1/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
    • 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
    • D21H17/03—Non-macromolecular organic compounds
    • D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
    • D21H17/14—Carboxylic acids; Derivatives thereof
    • D21H17/15—Polycarboxylic acids, e.g. maleic acid
    • D21H17/16—Addition products thereof with hydrocarbons
    • 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
    • D21H17/03—Non-macromolecular organic compounds
    • D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
    • D21H17/17—Ketenes, e.g. ketene dimers
    • 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
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/249921—Web or sheet containing structurally defined element or component
    • Y10T428/249994—Composite having a component wherein a constituent is liquid or is contained within preformed walls [e.g., impregnant-filled, previously void containing component, etc.]

Definitions

  • the invention relates to a process for producing impregnated papers inside or outside the paper machine, according to which the papers are given a high penetration resistance to fats and oils.
  • a method is known, according to which a paper web consisting of pulp fibers is passed through a hot, aqueous zinc chloride solution or through a sulfuric acid bath, thereby achieving a high density of fat by partial hydrolysis of the pulps.
  • a paper equipped with a high penetration resistance to greases and oils according to this method is no longer recyclable.
  • this packaged item is a food or an animal feed
  • these organic fluorine compounds enter the food chain.
  • they since they are neither degraded by human or animal metabolism, they remain in the body. They are suspected of harming human and animal biological genetic material.
  • these papers are regularly wet-proofed because of their use for packaging of dry or moist, greasy foods and for this epichlorohydrin resins are used which contain the harmful substances monochloropropanediol (MCPD) and dichloropropanol (DCP).
  • MCPD monochloropropanediol
  • DCP dichloropropanol
  • a paper produced by such a method has only a low fat density, tested according to generally accepted and standardized test methods.
  • Methods are furthermore known according to which high melt penetration resistance to fats and oils is imparted to papers by melting polymers and / or waxes and / or hotmelts and / or paraffins on the path of the extrusion coating.
  • EP 0 697 622 A1 and EP 0 545 043 A1 disclose the coating of papers with a hydrophobizing sizing agent such as polyolefins and polyvinyl alcohols as the water-soluble resin. These papers are suitable as photographic supports; Information about their penetration resistance to oils or greases can not be found in these publications. As the water-soluble component of the sizing agent, only polyvinyl alcohol is disclosed.
  • the invention has set itself the goal to give a paper by way of a novel design of chemical technology high penetration resistance to fats and oils, it remains recyclable, printable and no harmful substances such as heavy metals, fluorocarbon compounds, monochloropropane, dichloropropanol or Contains formaldehyde due to the formulation.
  • the invention has for its object to provide a paper which has a high penetration resistance to fats and oils, which can be recycled well printable and free of the above-mentioned harmful substances, and to provide a method for producing such a paper.
  • the object is achieved by a paper according to claim 1 and a method according to claim 11.
  • the freeness is determined as Schopper-Riegler number (° SR) according to ISO 5267-1. According to the invention a value of 65-90 ° SR, in particular of 78-82 ° SR is preferred. It is also possible to use low-grade papers (cardboard) with a freeness of 15-65 ° SR, in particular 30-65 ° SR.
  • ASA alkenyl succinic anhydride
  • ALD alkyl ketene dimers
  • tree resin resin sizing agents
  • the alkenylsuccinic anhydride (ASA) used for sizing is, for example, a reaction product of maleic anhydride and alpha-olefins having 16 to 20 carbon atoms. According to the invention, it is preferably used in an amount of 0.05 to 0.3% by mass, preferably 0.1% by mass, based on the dry paper. For this purpose it is emulsified with the aid of a protective colloid, for example cationic starch. A representation of this so-called.
  • ASA sizing with other citations are, for example T. Gliese, alkenylsuccinic anhydride (ASA) as sizing agent, The paper 2003, T141-T145 ,
  • the treatment with the aqueous impregnating liquor may have taken place both in the paper machine and outside it.
  • the fleet may contain other auxiliaries such as crosslinkers, complexing agents, etc.
  • the binder system consists of water-soluble binders and possibly water-insoluble polymers.
  • Water-insoluble polymers are preferably polyacrylonitriles, polyacrylates, polyvinyl acetates and polystyrene-polyacrylate copolymers. Their proportion should not be so great that the paper is no longer recyclable and is according to the invention at most 20% by mass.
  • Water-soluble binders according to the invention are preferably carboxyl-containing polyvinyl alcohols (vinyl alcohol-carboxylic acid copolymers), ethylene-vinyl alcohol copolymers, acetalated ethylene-vinyl alcohol copolymers, acetalated polyvinyl alcohols, polyvinyl butyrals, silanol-containing, cationically modified polyvinyl alcohols, acetalated silanol groups, acetalated cationic modified polyvinyl alcohols, acetalized carboxyl-containing polyvinyl alcohols, gelatin, galactomannans, alginates, carboxymethylcellulose and mixtures of several selected from these classes of binders.
  • carboxyl-containing polyvinyl alcohols (vinyl alcohol-carboxylic acid copolymers), ethylene-vinyl alcohol copolymers, acetalated ethylene-vinyl alcohol copolymers, acetalated polyvinyl alcohols, polyvinyl butyral
  • acetalization of the optionally silanol-containing, carboxyl-containing polyvinyl alcohols or cationically modified polyvinyl alcohols and the ethylene-vinyl alcohol copolymers C1-C10-alkanals or substituted or unsubstituted aromatic aldehydes each individually or as a mixture can be used.
  • Particularly suitable are formaldehyde, acetaldehyde, propionaldehyde, benzaldehyde and / or benzaldehydesulfonic acid as alkali metal salt (sodium salt).
  • the binder system comprises polyvinyl alcohol and gelatin.
  • polyvinyl alcohol content of Binder system realized by a mixture of at least two different polyvinyl alcohols, of which at least one has a viscosity of less, the other and the other one of more than 35 mPa.s.
  • Viscosity of polyvinyl alcohol in this application is understood to mean the viscosity measured according to DIN 53015 on an aqueous solution with 4% by mass at 20 ° C.
  • the impregnating liquor for producing the paper sheet according to the invention preferably contains a crosslinking agent, more preferably glyoxal in a concentration of 2 to 15% by mass, based on the total amount of binder and crosslinker.
  • the concentration of the impregnating liquor is advantageously between 2 and 15, preferably between 5 and 7.5% by mass of dry substance.
  • the application weight of the impregnating liquor, calculated as dry matter, is advantageously between 0.3 and 1.5 g / m 2 per side.
  • the process for the production of the paper sheet according to the invention comprises the production of a base paper from pulp, mechanical pulp or recycled waste paper with the aforementioned grindings, the sizing of this paper in the mass, in particular with alkenylsuccinic anhydride (ASA), and the impregnation of the glued base paper with an impregnating liquor a binder system of 80 to 100 parts by weight of water-soluble binders and 20 to 0 parts by weight of water-insoluble polymers in dispersion.
  • ASA alkenylsuccinic anhydride
  • the impregnation can take place both in the paper machine and outside it. Usual devices, eg. B. size presses, film presses, etc. can be used for this purpose.
  • the base paper is dried before impregnation to a solids content of 95 to 99%. After impregnation, a drying process also follows the desired final moisture content.
  • Carboxyl-containing polyvinyl alcohol also by viscosity and degree of hydrolysis as above.
  • Suitable products are types KL-318 and KL-506 from Kuraray Specialties Europe.
  • PVA-K Cationically modified polyvinyl alcohol
  • CM-318, C-118 and C-506 from Kuraray Specialties Europe.
  • Silanol group-containing polyvinyl alcohol also by viscosity and degree of hydrolysis as above.
  • Suitable products are e.g. the type R-1130 from Kuraray Specialties Europe.
  • PEVA Ethylene-vinyl alcohol copolymer
  • Suitable products are marketed under the trademark Exceval by Kuraray Specialties Europe, for example type HR-3010.
  • PEVA can be prepared by copolymerization of vinyl acetate and ethylene and subsequent Hydrolysis of vinyl acetate to vinyl alcohol units are prepared.
  • Acetalized polyvinyl alcohols such as polyvinyl butyral (PVB) also characterized by viscosity, degree of hydrolysis and degree of acetalization. To maintain the solubility in water, the degree of acetalization is at most 30 mol%.
  • PVB polyvinyl butyral
  • the acetalated polyvinyl alcohols which can be used according to the invention are obtained by acetalization of a polyvinyl acetate prepared by hydrolysis.
  • polyvinyl acetate homopolymers of vinyl acetate as well as copolymers of olefins such as ethylene, Proplyen or other ⁇ -olefins can be used with vinyl acetate.
  • the polymers obtained after hydrolysis contain 0 to 15 mol% of olefin units, 50 to 99.9 mol%, preferably 75 to 99.9 mol%, particularly preferably 85 to 99.9 mol% vinyl alcohol units and 0.1 to 50 mol%, preferably 0.1 to 25 mol%, particularly preferably 0.1 to 15 mol% Vinylacetatein whatsoever.
  • the acetalization with the mentioned aldehydes is carried out to a degree of acetalization of 1 to 30 mol%, preferably 1 to 20 mol%.
  • the described silanol-containing, carboxyl-containing and cationically modified polyvinyl alcohols can be acetalated.
  • Suitable products are the types GELITA Imagel MA (39 mN / m) and GELITA Imagel BP (56 mN / m, brands of Stoess AG).
  • Carboxymethyl cellulose is useful in commercial form.
  • Alginate may be used as sodium alginate, for example, available from Kimica Corp., Japan.
  • the formulations listed in Table 1 comprise mass fractions of the dry matter of the impregnating liquor, which also contains essentially only water.
  • the dry content of the liquor may be between 2 and 15% by mass, preferably between 5 and 7.5% by mass. In addition to the appropriate ranges, preferred values are given for each ingredient.
  • the Imticiangnierflotten invention can be prepared by dissolving the ingredients in water at 90 to 95 ° C, possibly after swelling of each of the dry ingredients in cold water.
  • the impregnating liquors prepared in this way are applied to a base paper made of pulp having a freeness of 65 to 90 ° SR, preferably 78-82 ° SR, which has been mass-pasted with alkylene succinic acid, inside or outside the paper machine, on one or both sides.
  • a preferred range of application weight is between 0.3 and 1.5 g / m 2 per side, calculated as dry matter in the liquor.
  • the impregnation of the paper web is carried out using one of the well-known application methods inside or outside the paper machine and subsequent drying of the web on drying cylinders or non-contact, e.g. in suspended dryers.
  • the invention can be carried out in a wide range of basis weights of the base paper. Preference is given to papers or with 28-350 g / m 2 .
  • a paper web produced in the manner according to the invention has a high penetration resistance to fats and oils, measured according to generally recognized and standardized test methods as in Examples 1 to 3, although the individual components are polyvinyl alcohol or gelatin or CMC or ethylene-vinyl alcohol. Copolymer or alginates or galactomannans or starch derivatives only low penetration resistance to oils and fats develop.
  • the papers produced in the manner according to the invention have a wet strength of 5 to 20%, determined in accordance with DIN ISO 3781, without having to use wet strength agents.
  • Examples 1 and 2 describe the prior art and Example 3 describes the inventive method.
  • Examples 4 to 14 relate to polymers which can be used according to the invention, examples 15 to 30 to the papers impregnated with these polymers.
  • Example 2 The relevant test results determined on the finished paper are shown in Table 2.
  • the impregnating media described in the examples were applied to unsized base paper by a size press (Examples 1 and 2 prior art), while in Example 3 the impregnating liquor was applied to alkenylsuccinic anhydride gel with a size press (Inventive).
  • All raw papers mentioned in Examples 1, 2 and 3 are made from pulps which have been given a freeness of 78 ° SR to 82 ° SR.
  • the impregnation takes place at a speed of the paper web of about 600 m / min. The job is done on both sides of the paper web. Drying after impregnation is initially carried out without contact in an infrared dryer and then with drying cylinders.
  • red-dyed palm kernel fat is applied to the test specimen on a surface of 50 cm 2 using a template.
  • the step V indicates the breakdowns after 10 minutes, which are counted on an underlaid white paper sheet.
  • Stage IV is also determined after a test period of 10 minutes, but the palm kernel fat was loaded with a pressure of 20 N / cm 2 .
  • the same load is applied to stages III, II, and I, but the test duration is 60 minutes (stage III); 24 hours (level II) and 36 hours (level I).
  • a time of 1800 s corresponds to a high penetration resistance to fats and oils.
  • the paper Due to the use of epichlorohydrin resins for wet consolidation, the paper contains the critical substances monochloropropanediol and dichloropropanol in the legally permissible amount. It also contains organically bound fluorine, which is suspected of being mutagenic.
  • the predried paper web is then impregnated with a dry content of 95 to 99% in a size press with an impregnating liquor consisting of 12 parts by weight of polyvinyl alcohol with a viscosity of 28 mPa.s, determined as above, and a degree of hydrolysis of 99%, 7 parts by mass CMC with a medium viscosity, 7 parts by weight of a galactomannan, 70 parts by weight of a potato starch ester having film-forming properties and 10 parts by weight of a 40% glyoxal solution, and water consists.
  • an impregnating liquor consisting of 12 parts by weight of polyvinyl alcohol with a viscosity of 28 mPa.s, determined as above, and a degree of hydrolysis of 99%, 7 parts by mass CMC with a medium viscosity, 7 parts by weight of a galactomannan, 70 parts by weight of a potato starch ester having film-forming properties and 10 parts by weight of a 40% gly
  • the impregnation liquor contains no fluorocarbon compounds. It has a pH of 6.2 - 6.8, a viscosity of 24 to 27 s flow time from the Ford cup, nozzle 4 mm, and a concentration of dry matter of 6.1 to 6.3%.
  • the coating weight on the raw paper is 0.6 g / m 2 per side, ie 1.2 g / m 2 in total.
  • the paper web is dried again after impregnation to a final dry content of 93%.
  • the paper Due to the use of epichlorohydrin resins for wet consolidation, the paper contains monochloropropanediol and dichloropropanol in the legally permitted amount. However, it has only low penetration resistance to fats and oils.
  • a paper web is produced from fibrous materials as described in Example 1.
  • the pulp suspension is not added to epichlorohydrin resin, but the pulp suspension is 0.1% alkenylsuccinic anhydride (Baysize 18-Bayer) and 0.9% cationic potato starch (HI-CAT 145). Roquette Fromme), based on paper added.
  • the predried paper web is now impregnated at a dry content of 96 to 99% in the size press with an impregnating liquor composed of 7 parts by weight of a polyvinyl alcohol having a viscosity of 15 mPa.s, determined as above, and a degree of hydrolysis of 79%, 25 Parts by weight of a polyvinyl alcohol having a viscosity of 28 mPa.s and a degree of hydrolysis of 99%, 12 parts by weight of a polyvinyl alcohol having a viscosity of 40 mPa.s and a degree of hydrolysis of 88%, 15 parts by weight of a polyvinyl alcohol having a viscosity of 56 mPa.s and a degree of hydrolysis of 88%, 15 parts by weight of a carboxyl group-containing polyvinyl alcohol having a viscosity of 18 mPa.s and a degree of hydrolysis of 84%, 17 parts by weight of a gelatin having a surface tension of 38
  • the impregnating liquor has a pH of 6.4 to 6.9, a viscosity of 30 to 32 s flow time from the Ford cup, nozzle 4 mm, and a concentration of 7.2 to 7.4%.
  • the dry application was 1.2 g / m 2 per side.
  • GD means large-area punctures, with numerous punctures, the number of punctures greater than 1 mm 2 is indicated behind the slash.
  • Example 3 of the invention achieves the same high penetration resistances as in the prior art Example 1 without using fluorocarbon compounds.
  • the paper prepared according to Inventive Example 3 has a high penetration resistance to fats and oils, is free of organically bound halogen including epichlorohydrin resin and fluorocarbon compounds, is free of heavy metals, is recyclable, is printable with both water and solvent based inks and is within created the paper machine in the context of the manufacturing process.
  • Table 3 lists examples of formulations with the polymers according to Examples 4 to 14 for coating papers.
  • Table 4 shows the penetration resistance of these papers.
  • Table 3 example 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 PVA 56 mPa.s, 98% 0-95 0-95 0-95 0-95 Prefers 22 22 22 22 glyoxal 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 0-15 Prefers 8th 8th 8th 8th 8th 8th 8th 8th 8th 8th 8th 8th 8th 8th 8th Polyvinyl butyral according to Ex. 4 to 9 5-90 5-90 5-90 5-90 Prefers 70 70 70 70 70 Polyvinyl butyral according to Ex.

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EP20050739014 2004-03-31 2005-03-31 Papiere mit hohem durchdringungswiderstand gegen fette und öle und verfahren zu deren herstellung Expired - Lifetime EP1733093B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE102004016590 2004-03-31
DE200410019734 DE102004019734A1 (de) 2004-03-31 2004-04-20 Papiere mit hohem Durchdringungswiderstand gegen Fette und Öle und Verfahren zu deren Herstellung
PCT/DE2005/000577 WO2005095710A1 (de) 2004-03-31 2005-03-31 Papiere mit hohem durchdringungswiderstand gegen fette und öle und verfahren zu deren herstellung

Publications (2)

Publication Number Publication Date
EP1733093A1 EP1733093A1 (de) 2006-12-20
EP1733093B1 true EP1733093B1 (de) 2014-01-22

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Country Link
US (1) US8110071B2 (https=)
EP (1) EP1733093B1 (https=)
JP (1) JP4886674B2 (https=)
CA (1) CA2559954C (https=)
DE (2) DE102004019734A1 (https=)
NO (1) NO20064952L (https=)
TW (1) TWI387671B (https=)
WO (1) WO2005095710A1 (https=)

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JP4886674B2 (ja) 2012-02-29
DE102004019734A1 (de) 2005-11-03
US20080233385A1 (en) 2008-09-25
DE112005001291A5 (de) 2007-06-14
WO2005095710A1 (de) 2005-10-13
EP1733093A1 (de) 2006-12-20
JP2007530808A (ja) 2007-11-01
CA2559954C (en) 2013-06-25
NO20064952L (no) 2006-12-14
TW200613612A (en) 2006-05-01
TWI387671B (zh) 2013-03-01
CA2559954A1 (en) 2005-10-13
US8110071B2 (en) 2012-02-07

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