WO2021259636A1 - Mélange adhésif aqueux pour coller des matériaux en papier et procédé pour sa production - Google Patents

Mélange adhésif aqueux pour coller des matériaux en papier et procédé pour sa production Download PDF

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Publication number
WO2021259636A1
WO2021259636A1 PCT/EP2021/065405 EP2021065405W WO2021259636A1 WO 2021259636 A1 WO2021259636 A1 WO 2021259636A1 EP 2021065405 W EP2021065405 W EP 2021065405W WO 2021259636 A1 WO2021259636 A1 WO 2021259636A1
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WIPO (PCT)
Prior art keywords
adhesive mixture
aqueous adhesive
weight
mixture according
starch
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PCT/EP2021/065405
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German (de)
English (en)
Inventor
Peter Bitomsky
Monika Sebald
Malte Kleemeier
Andreas Hartwig
Anatoli DAVYDOV
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PAPIERTECHNISCHE STIFTUNG (PTS)
Fraunhofer Gesellschaft zur Foerderung der Angewandten Forschung eV
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PAPIERTECHNISCHE STIFTUNG (PTS)
Fraunhofer Gesellschaft zur Foerderung der Angewandten Forschung eV
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Priority to EP21732004.3A priority Critical patent/EP4172285A1/fr
Publication of WO2021259636A1 publication Critical patent/WO2021259636A1/fr
Anticipated expiration legal-status Critical
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J103/00—Adhesives based on starch, amylose or amylopectin or on their derivatives or degradation products
    • C09J103/02—Starch; Degradation products thereof, e.g. dextrin
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica

Definitions

  • the present invention relates to an aqueous adhesive mixture for bonding paper materials comprising starch and silica sol. It also relates to a bonded paper product, bonded with the aqueous adhesive mixture according to the invention, and the use of an aqueous adhesive mixture according to the invention for adhering paper surfaces. It also relates to a method for producing a corresponding aqueous adhesive mixture.
  • Corrugated cardboard is made up of one or more layers of corrugated paper that is glued to one layer or between several layers of another paper or cardboard. Depending on the number of layers of the corrugated paper and the thus glued cover and intermediate layers, there is a subdivision into one-sided, single-wall, two- and three-wall corrugated cardboard. Corrugated cardboard is manufactured in a corrugated cardboard plant (WPA).
  • WPA corrugated cardboard plant
  • the wave and ceiling are pressed together.
  • the paper is heated and moistened in the preheater. This gives the necessary elasticity so that the paper can be deformed.
  • this is passed between two corrugated rollers that mesh like a gear.
  • the wave is shaped ("corrugated").
  • vacuum or overpressure systems hold the corrugated paper web on the corrugating roller until it is fixed by gluing it to the top sheet.
  • Glue based on starch is then applied to the tips of the corrugated peaks of the corrugated paper, whereby the corrugation is glued to a smooth cover sheet to form the one-sided corrugated cardboard.
  • the corrugated cardboard sheets are pulled over heating plates (up to 180 ° C).
  • the heat required for gluing is supplied to the glue points and the paper.
  • excess moisture is also removed.
  • Starch adhesives based on corn, potatoes, wheat and, in small quantities, also based on peas are used almost exclusively for gluing corrugated cardboard.
  • Starch is a vegetable polysaccharide that consists of aD-glucose units. Depending on the fruit and provenance, it consists of different carbohydrate proportions of poorly soluble amylose and more easily soluble amylopectin.
  • the key process in the manufacture of corrugated cardboard is the firm adhesive bond between the corrugated paper web and the liner within a few milliseconds, if possible.
  • the starch adhesives most frequently used for this purpose are preferably manufactured using the so-called Stein-Hall process.
  • To produce a Stein-Hall glue in the first step approx. 11% by weight to 14% by weight of the total starch content is completely gelatinized in the presence of water and sodium hydroxide solution with the introduction of heat.
  • the starch portion contained in the so-called “primary batch” is also referred to as primary or carrier starch and is used to adjust the viscosity and the water retention capacity.
  • the starch dissolved in the paste also serves as an anti-settling agent for the remaining starch content, which is added in its native granular form in the subsequent step and is referred to as secondary starch.
  • borax sodium tetraborate
  • Further additives are plasticizers, defoamers and rheological auxiliaries as required.
  • Fig. 1 shows schematically a flow chart for the production of a Stein-Hall glue with boron.
  • the mixture contains 11-14% by weight carrier starch and 86-89% by weight secondary starch.
  • the total solids content is about 25-27%.
  • Sodium hydroxide is added to the primary batch in order to reduce the gelatinization point to approx. 53-55 ° C.
  • Table 1 Exemplary Stein-Hall recipe
  • Borax as a rheological additive in corrugated cardboard adhesives
  • borax sodium tetraborate Na 2 ß 4 07 10 H2O
  • H3BO3 boric acid
  • the reaction between caustic soda and sodium tetraborate when the primary and secondary batches are mixed together produces sodium metaborate, which at high pH values (10-13) forms so-called borax bridges between neighboring starch molecules through a condensation reaction and hydrogen bonds.
  • the three-dimensional cross-linking of the starch molecules by borax results in highly branched polymer chains, which increase the molecular weight of the starch.
  • the significantly increased immobilization of the starch molecules leads to higher viscosity and improved adhesive and fluid properties. shafts of the adhesive.
  • borax has a positive influence on the water retention capacity of the adhesive. Its high viscosity counteracts the loss of water and primary strength in the adhesive zone (penetration into the fiber interior). In this way, enough starch remains for optimal gelatinization.
  • borax also acts as a preservative.
  • Borax as a hazardous substance Boron compounds are extremely harmful to health. The acute effects include irritation to the mucous membranes, gastrointestinal disorders, effects on the central nervous system and skin damage after massive intoxication. Since borax is mainly absorbed through the respiratory tract, breathing and body protection measures are mandatory in glue kitchens. For these reasons, borax is undesirable in packaging that comes into direct contact with food. Borax is classified as a water-polluting substance (WGK 1: slightly water-polluting) and must not be discharged into the wastewater. Since experience shows that boron substances only degrade after 8 to 10 years, they also represent an indirect burden on the environment due to the long retention time in waste paper recycling. Alternative borax-free starch adhesives would make a decisive contribution to environmental relief. Their use could relieve the waste paper cycle and thus contribute to its self-cleaning.
  • borax-free formulations are described as a function of the shear rate, which are relevant for processing from the adhesive supply to the application. Together with the gel points, the rheological data obtained are compared with a classic Stein-Hall recipe based on borax, and processing advantages are highlighted. However, the temperature-dependent increase in viscosity, which is essential for heat sealing, is not shown. The quality of the bonded joints with regard to dry and wet strengths is also not discussed in detail. Since the further use of borax is kept open as an option within the scope of the claims, the concept as a full replacement is questioned.
  • document DE 10249838 A1 proposes further water-soluble polymer compounds with thickening properties such as carboxymethyl cellulose, methyl cellulose, hydroxyethyl cellulose, carrageenan, guar gum, pectin, sodium alginate, carboxylated starch or polyvinyl alcohol.
  • the same concept is followed here as in the idea described above.
  • the basic viscosity of the adhesive is increased, whereby the rheology of pseudoplastic liquids is present, which dilute with the application of shear during the delivery of the adhesive and build up viscosity after application without shear.
  • the resulting final viscosity does not come close to the viscosity when using borax, so that special application rollers are described in the context of the process in order to enable the concept to be implemented successfully.
  • water glasses sodium and potassium silicates
  • WO 2013087530 A1 As a substitute for borax, water glasses (sodium and potassium silicates) are proposed in document DE 2629103 A1, which are added in place of borax or in combination with borax and are intended to meet the rheological requirement profile. Due to their inorganic structure, these adhesives are characterized by their pronounced brittleness, so that use in corrugated cardboard bonding is out of the question. Water glasses were already in use as adhesives decades ago, but they did not hold up and were replaced by starch-based systems. Another approach is the substitution of borax by sodium aluminate or aluminum sodium dioxide described in WO 2013087530 A1 when gluing cardboard boxes.
  • EP 0972812 A1 and DE 102006045384 A1 each describe adhesive formulations which include, inter alia, starch and silica sol, although the use of boron-containing substances in the adhesive formulations described is not limited or even completely excluded.
  • the problem becomes the necessary reduction of boron contents in adhesive mixtures for bonding paper materials is not recognized or addressed in any of the documents EP 0972812 A1 and DE 102006045384 A1.
  • an adhesive mixture which is suitable for gluing paper materials and comprises a component which at least partially also provides the advantages of boron-containing compounds necessary for the production of corrugated cardboard gluing, so that the amount of boron can be reduced in the adhesive mixture while maintaining the adhesive and processing properties. It was preferred that boron-containing compounds can be completely dispensed with.
  • the existing machine configurations should preferably be able to remain in place when the adhesive mixture sought is used. It should therefore preferably be possible to adapt the adhesive mixtures to the requirements of current corrugated cardboard production plants so that the industrial use of the adhesive mixtures sought is ensured.
  • one or more of the following or, with particular preference, all points should be possible:
  • the corrugated cardboard can be recycled without restriction, manufactured with a new adhesive system
  • an aqueous adhesive mixture for bonding paper materials comprising starch and silica sol and comprising ⁇ 0.5% by weight boron, based on the total weight of the anhydrous adhesive mixture after curing.
  • Paper materials in the context of the present invention are preferably corrugated cardboard base papers based on cellulose, which can be divided into liner papers and corrugated papers. Depending on the mechanical strength, liner papers can be divided into Kraftliner, Testliner and Schrenz. The latter in particular have a more or less high proportion of waste paper. Corrugated papers are mainly processed for the corrugation and are characterized by their high rigidity. For processing corrugated paper, corrugated pulp and semi-cellulose are available. The basis weights vary based on the type of paper between 50 and 450 g / m 2 .
  • Starch in the sense of the present invention corresponds to the definition of starch described above.
  • Preferred starch to be used according to the invention comes from wheat, corn, potatoes, rice, peas and mixtures thereof. Particularly preferred starch comes from wheat, corn, potatoes and their mixtures.
  • silica sols are colloidal dispersions of polysilicic acid particles with 10-60% by weight, preferably 10-30% by weight, of the particles in water.
  • the primary particles present in this state as non-agglomerated are preferably anionically stabilized against agglomeration in the pH range from 1-14, in particular in the pH range> 8. They have mean particle sizes in the range from 1 to 200 nm, preferably 1 to 50 nm, more preferably 1 to 15 nm.
  • the particle sizes can preferably be distributed monomodally or bimodally, more preferably monomodally.
  • the mean particle size is determined by means of electromicroscopy, the largest diameter appearing in the electron microscope being the diameter to be evaluated and the numerical mean being determined from at least 100 particles.
  • the particle size can be determined in solution by means of dynamic light scattering (DLS).
  • the median (D50 value) of the particle size distribution is given as the particle size.
  • the particle size can be determined by transmission electron microscopy. For this purpose, at least 100 particles are measured and a particle size distribution is formed.
  • all manufacturing steps in the manufacture of silica sols preferably take place in the liquid phase.
  • the particle growth takes place after dealkalization by ion exchange to the required particle size with subsequent particle stabilization (preferred).
  • the polysilicic acid / silicon dioxide particles are preferably predominantly approximately spherical (ie the ratio of the largest to the smallest diameter of a sphere is a maximum of 2, preferably a maximum of 1.5).
  • silicon sol comprises electrostatically stabilized polysilicic acid / silicon dioxide particles, it being preferred that all corresponding particles are electrostatically stabilized.
  • “silica sol” in the sense of the present invention to include surface-modified polysilicic acid / silicon dioxide particles, it also being possible for all of the polysilicic acid / silicon dioxide particles to be modified accordingly.
  • An optional surface modification with aluminum is preferred, which can be done, for example, by adding aluminum salts.
  • the surface can preferably be organically modified by reaction with silanes. By modifying silanes, it is possible to sterically stabilize the particles in addition to the preferably electrostatic stabilization.
  • metering into silica sol in the context of the present invention represents the provision of a substance which imparts properties similar to or in some cases even more favorable properties in terms of paper bonding than boron-containing compounds to the aqueous adhesive mixture.
  • boron is not necessarily excluded as a component of the aqueous adhesive mixture for the purposes of the present invention, it is possible to reduce the boron content considerably or even to do without it, which is of course desirable in the context of the concerns described above about the boron-containing compounds.
  • an aqueous adhesive mixture according to the invention comprising boron in the range from> 0% by weight to ⁇ 0.05% by weight, or 0% by weight, based in each case on the total weight of the anhydrous adhesive mixture after curing.
  • An aqueous adhesive mixture according to the invention is particularly preferred, comprising boron in the range from> 0% by weight to ⁇ 0.005% by weight or 0% by weight, based in each case on the total weight of the anhydrous adhesive mixture after curing.
  • An aqueous adhesive mixture according to the invention, comprising no boron is very particularly preferred.
  • borax is based on the cross-linking of free hydroxyl groups of the starch with the formation of boric acid starch esters and / or hydrogen bonds, which result in the required jump in viscosity and the formation of the “green bond”.
  • crosslinking reactions based on silica sols are conceivable, which are present as colloids in an aqueous medium and are stabilized against agglomeration and gelation by electrostatic charging of their particle surfaces. Stabilization is usually carried out by adding alkali, which generates a negative electrical charge in the same direction for all the silica sol particles. If the stabilization is lost, the irreversible agglomeration takes place through the transition from the uncrosslinked sol to the spatially crosslinked gel state.
  • an aqueous adhesive mixture comprising (i) no cations in addition to those of the silica sol and sodium hydroxide solution or (ii) divalent and / or polyvalent cations.
  • various silica sol qualities are of interest. It is therefore possible to achieve the desired properties by selecting suitable silica sols. It is basically the case that the larger the specific surface area of the silica sol particles or the smaller the particles, the greater their reactivity.
  • an aqueous adhesive mixture according to the invention is preferred, the silica sol having an average particle size of 1 nm-200 nm, preferably 1 nm-50 nm, more preferably 1 nm -15 nm and / or the specific surface area of the particles in the silica sol being 25 m 2 / g-1500 m 2 / g, preferably 100 m 2 / g-1500 m 2 / g, more preferably 200 m 2 / g -1000 m 2 / g.
  • the desired properties can also be influenced by the fact that a suitable amount of silica sol is present; accordingly, it is preferred according to the invention that the proportion of silicon dioxide-containing particles from the silica sol in the adhesive mixture according to the invention based on the total weight of the anhydrous adhesive mixture after curing is 1 wt. -% to 15% by weight, preferably 1% by weight to 5% by weight.
  • the specific surface area of the particles in the silica sol is determined using the BET method in case of doubt.
  • the rate of gelation and the strength of the resulting gel depend on the type, concentration, electrolyte concentration and type of electrolyte.
  • the increase in viscosity occurs very quickly after an incubation period (processing time), which speaks in favor of the surprisingly adequate replacement of borax.
  • the alkaline or acidic, anionic or the acidic, cationic types of silica sol, in contrast to borax, do not require labeling according to the Hazardous Substances Ordinance and the corresponding EC guidelines and are toxicologically harmless.
  • Silica sols belong to the class of silicic acids. Other representatives of this class are water glasses, silica gels and precipitated and pyrogenic silicas.
  • aqueous adhesive mixture according to the invention is preferred, the starch in both granular and colloidally dispersed form.
  • an aqueous adhesive mixture according to the invention is preferred, the adhesive mixture being a Stein-Hall glue.
  • a Stein-Hall glue is produced as described above.
  • boron is not an essential component of a Stein-Hall glue.
  • Stein-Hall glues have been used successfully in paper bonding for a long time, especially in the manufacture of corrugated cardboard.
  • Part of the invention is also a bonded paper product, bonded with an adhesive mixture according to the invention.
  • a paper product according to the invention which comprises a corrugated cardboard is particularly preferred, the corrugated cardboard having been glued with the adhesive mixture according to the invention.
  • corrugated cardboard is to be understood in the sense of the description given above.
  • Part of the invention is also the use of an aqueous adhesive mixture according to the invention for gluing paper surfaces together, in particular for producing corrugated cardboard.
  • part of the invention is a method for producing an aqueous adhesive mixture according to the invention, comprising the steps a) providing starch, b) providing silica sol, c) optionally providing further constituents and d) dispersing the provided constituents, although this is of course preferred is that the components mentioned are provided in a preferred variant described above.
  • Part of the invention is also a method for producing a bonded paper product according to the invention, comprising the steps of a) providing an aqueous adhesive mixture according to the invention, b) providing the paper parts to be glued together and c) gluing the paper parts to be glued together with the aqueous adhesive mixture.
  • the goal of an alternative to borax in corrugated cardboard glue was achieved, among other things, by combining colloidal silica sols in the presence of polyvalent ions in the form of aqueous salt solutions.
  • aqueous salt solutions as a co-additive is a sufficient but not necessary condition in all cases. This means that when using colloidal silica sols according to the invention, the aim can also be achieved without the addition of polyvalent ions in the form of aqueous salt solutions.
  • the successful testing of this system was demonstrated using the example of a silica sol and an aqueous calcium hydroxide solution in the context of pilot plant and operational tests and was proof of its practical suitability.
  • the adhesive mixtures according to the invention are preferably based on the conventional composition and the usual production process for Stein-Hall glues. Essentially, the addition of borax has been replaced by the addition of silica sol and salt solution. The processing and the running properties of the adhesive mixtures according to the invention were inconspicuous in industrial corrugated cardboard plants. The borax-free bonding had no negative impact on the strength and wet strength properties of the corrugated cardboard produced. In addition, the achieved bond strength shaft / ceiling was at least equivalent to the borax-containing reference. The unrestricted recyclability of the packaging material could also be confirmed with the complete replacement of borax. Measured against the performance spectrum of borax-containing glue systems, the expectations of the new additive system are more than fulfilled.
  • the adhesive mixtures according to the invention have the following advantages:
  • the adhesive mixtures according to the invention allow high processing speeds.
  • silica sols differ in their particle size distribution and in their specific surface area. With Levasil 200A / 30, there is also a surface-modified variant in which surface-bound silicon has been partially replaced by aluminum.
  • Examples 1 to 7 Brabender viscograph measurements of aqueous wheat starch suspensions
  • the individual mixtures are heated from 30 ° C. to 85 ° C. at a constant heating rate of 1.5 K min- 1.
  • the temperature is held at 85 ° C. for 5 minutes and then cooled to a final temperature of 45 ° C. at a cooling rate of 1.5 K min -1.
  • the rotational speed is 75 rev min -1.
  • the compositions of the mixtures are shown in Table 3.
  • Table 3 Composition of aqueous wheat starch suspensions
  • the influence of the different additives can be compared on the basis of the Brabender curves obtained.
  • Fig. 2 shows the Brabender viscograph measurements with silica sols in comparison with the established borax system and Gilunal A.
  • the curve for the mixture from Example 2 shows the measurement profile of a typical starch glue with the addition of borax.
  • the falling curve from a measuring time of 60 minutes is due to the already complete gelation of the glue, so that the measuring device is no longer able to measure further rheological effects.
  • the measurements show that both types of silica sol in different proportions (Examples 4 to 7), in contrast to Gilunal A (Example 3), have a pronounced crosslinking effect which, due to a significant increase in viscosity, decreases as a result of the onset of gelation during the cooling phase a measuring time of 50 minutes. This behavior is comparable to the effect of borax (example 2).
  • Examples 8 to 10 Production of corrugated cardboard under operating conditions In the production of single-wall corrugated cardboard, two borax-containing Stein-Hall glues (Examples 8 and 9) were produced and compared with a borax-free alternative (Example 10) under operating conditions.
  • Table 3 Compositions of Stein-Hall glues of Examples 8 to 10
  • the glue preparation proceeds according to the following scheme.
  • the primary starch is added to the primary water heated to 30 ° C and mixed.
  • the agitator is set to approx. 1000 rpm.
  • the sodium hydroxide solution is then stirred in, the speed of the stirrer being increased to 1500 rpm and shearing for 15 minutes.
  • the secondary water, the secondary starch and borax are added one after the other.
  • the preparation of example 10 takes place in that instead of borax, first the silica sol (Levasil CT24PL) and finally calcium hydroxide are added in the form of an aqueous dispersion.
  • the salt is dissolved or dispersed in water beforehand by removing 14 times the amount of secondary water based on the weight of the salt itself.
  • the stirrer speed is increased to 1500 rpm - max. 2000 rpm - and the Stein-Hall approach is sheared for a further 15 minutes to complete.
  • the examples are in the “target range”.
  • Example 8 containing borax
  • Example 9 containing borax
  • Experiment B Connection of shaft and inner ceiling with example 8 (containing borax) and connection of the outer ceiling with example 10 (borax-free)
  • the pressure effect at which the wave no longer regresses is represented by the value FCT FmaxLokai.
  • the BCT test compression test
  • DIN 55440-1 A closed, unfilled packaging is used for testing
  • FCTFmaxLocal PAT Bonding Single Facer (inner ceiling)
  • Table 4 Strength data of corrugated cardboard made with linen from examples 8 to 10
  • the ECT, FCT, PAT and BCT tests on the finished corrugated cardboard show only marginal differences in relation to the different production speeds.
  • the borax-free example 10 with silica sol additive can be used in all machine groups of the corrugator without any loss of strength.
  • the different corrugated cardboard samples were examined for their recyclability. The tests included the defibering behavior, the potential for sticky formation (fault-free sheet formation) and the properties of the recovered fiber material with regard to optical inhomogeneities. Based on the tests carried out and in accordance with the criteria of the PTS method PTS-RH: 021/97, the samples are rated as "recyclable". Consequently, the addition of silica sol (Example 10) did not have any adverse effects on the recyclability of corrugated cardboard.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

La présente invention concerne un mélange adhésif aqueux pour le collage de matériaux en papier, lequel mélange comprend de l'amidon et un sol de silice. L'invention concerne également un produit de papier collé, collé à l'aide du mélange adhésif aqueux selon l'invention, et l'utilisation d'un mélange adhésif aqueux selon l'invention pour coller des surfaces de papier ensemble. L'invention concerne en outre un procédé de production d'un mélange adhésif aqueux correspondant.
PCT/EP2021/065405 2020-06-26 2021-06-09 Mélange adhésif aqueux pour coller des matériaux en papier et procédé pour sa production Ceased WO2021259636A1 (fr)

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EP21732004.3A EP4172285A1 (fr) 2020-06-26 2021-06-09 Mélange adhésif aqueux pour coller des matériaux en papier et procédé pour sa production

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DE102020116925.6 2020-06-26
DE102020116925.6A DE102020116925A1 (de) 2020-06-26 2020-06-26 Wässrige Klebstoffmischung zum Verkleben von Papiermaterialien sowie ein Verfahren zum Herstellen derselben

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CN118185509A (zh) * 2024-04-03 2024-06-14 东莞市锐峰纸品有限公司 一种低温胶粘剂及其制备方法和含低温胶粘剂的瓦楞纸生产工艺

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DE2124917A1 (en) * 1971-05-19 1972-12-07 Degussa Stabilisation of natural starch solns - at room temp by addn of powdered synthetic silica
DE2629103A1 (de) 1975-06-30 1977-01-13 Philadelphia Quartz Co Staerke-silicat-klebstoffzusammensetzungen und verfahren zu ihrer herstellung
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