EP1013823A1 - Tissue paper product and lotion for its manufacture - Google Patents
Tissue paper product and lotion for its manufacture Download PDFInfo
- Publication number
- EP1013823A1 EP1013823A1 EP99123068A EP99123068A EP1013823A1 EP 1013823 A1 EP1013823 A1 EP 1013823A1 EP 99123068 A EP99123068 A EP 99123068A EP 99123068 A EP99123068 A EP 99123068A EP 1013823 A1 EP1013823 A1 EP 1013823A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- tissue paper
- weight
- paper product
- percent
- lotion
- 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.)
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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
- D21H21/22—Agents rendering paper porous, absorbent or bulky
-
- 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
- D21H17/04—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
- D21H17/06—Alcohols; Phenols; Ethers; Aldehydes; Ketones; Acetals; Ketals
-
- 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
- D21H17/07—Nitrogen-containing compounds
-
- 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
-
- 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
-
- 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
- D21H17/53—Polyethers; Polyesters
-
- 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
- D21H17/59—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 silicon
Definitions
- the invention relates to a very particularly soft Tissue paper product made by treating a Celullose fiber material with a special lotion.
- the Dry crepe process is the crepe on a drying cylinder carried out, of which the tissue paper product with a crepe scraper is replaced as soon as it reaches the intended Final dry matter content of 93 to 97%.
- the wet crepe process is also used, which is similar to the Dry crepe process, but at lower dry contents below 80%, usually around 55 to 65% dryness expires, which is followed by drying on subsequent Drying cylinders of a dryer section up to the final dry content connects.
- the creped, end-dry raw tissue paper is then wound up on tubes to mother rolls and stands in this form for further processing into finished products to disposal.
- tissue paper product is smoothed, Edge embossing, sometimes combined with a flat one and / or selective gluing to generate layer adhesion the individual layers to be brought together as well as Longitudinal section, folding, cross section, storage and merging several individual wipes and their packaging in so-called wipe bags or special boxes as well as their merging larger packaging or containers.
- This lotion can also contain a polyhydroxy compound contained in an amount of up to 20 percent by weight.
- the Polyhydroxy compound should have a molecular weight between 10 and 4,000, preferably between 100 and 1,000 and preferably from glycerin, a polyethylene glycol, a Polypropylene glycol or preferably from dipropylene glycol or their mixtures exist.
- the lotion according to the invention is liquid at room temperature and can add other ingredients besides those mentioned known additives such as perfumes, disinfectants, Deodorants and stabilizers included.
- An essential component of the lotion according to the invention is in the mineral oil, alkyl ethoxylate or fatty acid ester to see. These substances act as plasticizers.
- mineral oil can be a liquid hydrocarbon with 16 to 32 carbon atoms be used.
- Preferred examples of the fatty acid esters suitable for this are methyl palmitate, methyl stearate, isopropyl laurate, isopropyl myristate, Isopropyl palmitate and ethylhexyl palmitate.
- Alkyl ethoxylates are also used as softening additives suitable the lotion of the invention.
- Typical examples of such Alkyl ethoxylates include 3 to 10 lauryl ethoxylates Oxyethylene units, lauryl ethoxylates with 23 to 25 oxyethylene units, Cetyl ethoxylates with 10 oxyethylene units, Stearyl ethoxylates with 10 to 12 oxyethylene units.
- This Alkyl ethoxylates can be used alone in the lotion according to the invention or in combination with mineral oils and / or fatty acid esters be used.
- P refers Polydimethylsiloxanes that are substituted or carry unsubstituted alkyl, aryl or alkenyl groups and generally have no more than 10 carbon atoms.
- the viscosity of the polydimethylsiloxanes can vary widely Vary the range as long as the polysiloxane remains liquid or can be dissolved or dispersed in the lotion.
- the mechanical strength of the tissue paper product reduce in a dry or moist state.
- the fatty plasticizer and the polysiloxane due to their liquid consistency tend to To completely penetrate tissue paper product while doing the Binding properties of the cellulose fibers to one another weaknesses. That can last until the complete loss of Binding properties of the fibers result in the mechanical Strength would be completely lost.
- This Migration tendency now has the addition of the cationic quaternary ammonium salt. Because of its bipolar Structure is deposited on the surface of the tissue paper product and goes with its long hydrophobic alkyl groups Addition compounds with the hydrophobic groups of mineral oils, alkyl ethoxylates and fatty acid esters as well with the polysiloxanes.
- quaternary ammonium salts which are well suited in the context of the present invention are dialkyldimethylammonium salts such as the ditallow dimethylammonium chloride, the ditallow dimethylammonium methyl sulfate, which can be partially or completely hydrogenated.
- Biodegradable mono- and diester derivatives of the quaternary ammonium compounds of the formula II are also very suitable and Formula III in which R 1 is a C 14 to C 22 alkyl group, R 2 is a C 1 to C 6 alkyl or hydroxyalkyl group and R 3 is a C 1 to C 20 alkyl group and X is a physiologically acceptable anion.
- Another group of ammonium salts which are very suitable for the tissue paper products according to the invention are quaternary imidazolinium salts of the formula IV where R 4 is an alkyl group having 1 to 6 carbon atoms and R 5 is a or one Is a group in which R 6 is an alkyl group having 10 to 18 carbon atoms and X - is a physiologically acceptable anion.
- tissue paper product of the invention is both by Treatment with an aqueous or an anhydrous one Lotion can be made using the Anhydrous lotions are preferred because these only cover the surface of the tissue paper and therefore its strength cannot interfere.
- the tactile and surface properties of tissue paper are replaced by an anhydrous one Lotion influenced particularly favorably.
- the raw tissue paper product to which the lotion is to be applied can be single-layer or multi-layer, but preferably two to four layers and have an embossed or unembossed surface.
- the individual paper webs can be mechanically connected to one another by edge embossing or knurling, glued flat or at certain points, or else connected to one another in some other way.
- a basis weight range of 10 to 40 g / m 2 preferably a basis weight range between 15 and 25 g / m 2, has also proven to be particularly favorable.
- the lotion which is preferably in the form of an emulsion can be used with any roller and spray application process or in an impregnation process on the Raw tissue paper product can be applied.
- any roller and spray application process or in an impregnation process on the Raw tissue paper product can be applied.
- it is recommended to use high Shear forces, for example due to high-speed stirrers, frequent pumping or by ultrasonic mixing for to ensure a thorough mixing of the lotion.
- the lotion according to the invention is composed such that the tissue product soaked with it during the usual application period and the normally prevailing atmospheric humidity due to its hydroscopic properties not too dehydration. Also a water vapor proof, resealable packaging is not required.
- the lotion can be used in the wet part of a tissue paper machine, at the end of the wire section, in front of or within the press section or also in the dryer section arranged after the press section be added to the raw tissue paper product.
- Prefers is the addition of the lotion in the tissue making machine by spray application, during the reeling process apply a thin film of the lotion to the tissue paper product becomes.
- the already creped tissue web as a result of the previous drying process still a residual temperature between 20 and about 70 ° C, what for the distribution of the lotion and their penetration into the tissue material is favorable.
- a spray application via a nozzle bar can also Use of centrifugal rotors or brushing plants as well as the indirect transfer of a lotion film via roller applicators come into question.
- the order can also be placed directly on the Tissue paper web done.
- the addition is preferred the lotion inside the processing machine on the The outer layer of the multi-layer web before or during smoothing.
- the present invention therefore also relates to a method for the manufacture of a tissue paper product in which the Cellulose fiber material with 0.005 to 5 percent by weight, based on the dry fiber weight of the raw tissue paper product, of the lotion described above becomes.
- tissue paper product is used according to the invention understood regardless of the fiber raw material to be used.
- the method according to the invention can also be used for tissue paper products apply that only partially from native pulps exist and for example also reprocessed Fibers or suitable for paper production Contain plastic fibers. It is particularly preferred as Tissue web to use a multilayer web and at least one of the outer layers of the multi-layer lotion apply.
- the process variant is particularly preferred, in which a smoothing by at least one Passage of the tissue web through a nip of a pair of rollers takes place in which a roller with a steel surface Counter roll with a steel, plastic, paper or Rubber surface, but preferably a plastic surface, assigned.
- These rollers are hydraulic or pneumatic compressed or for calibration on gap hazards. That is, one of the two rollers is firmly positioned, while the second roller is pressed against a stop, so that the two rollers cannot touch, but rather at a certain, measurable and reproducible distance to stand by each other.
- the tissue webs passed through this gap are compressed to the gap width and smoothed in the process.
- the structure of the surface is standardized, i.e. a uniform thickness is brought about.
- the tissue paper product so made is as toilet paper, as a facial tissue, as a tissue or as Excellent paper towel.
- a Rohtissuepapierbahn having a basis weight of about 18 g / m 2 and a fiber dry content of about 95%, an aqueous lotion consisting perliquidum from 10 percent by weight of paraffin, 4 weight percent of the ditallow-dimethylammonium chloride and 15 weight percent of the polysiloxane Tegopren® 3021, a polyether siloxane with the Cloud point of 38 ° C, with good swirling in an amount of 4%, based on the weight of the raw tissue paper product, sprayed and subjected to post-smoothing.
- the application was carried out symmetrically on the outer surfaces of the finished sheet.
- Example 2 The application procedure according to Example 1 was repeated, although the lotion also contains 7.5 percent by weight Glycerin were added. It became a smooth tissue paper product with a silky-feeling surface won that such a high mechanical dry and wet strength exhibited that it was used both as a tissue and as a also excellent as toilet paper could.
Abstract
Description
Gegenstand der Erfindung ist ein ganz besonders weiches Tissuepapierprodukt, das durch die Behandlung eines Celullosefasermaterials mit einer speziellen Lotion gewonnen wird.The invention relates to a very particularly soft Tissue paper product made by treating a Celullose fiber material with a special lotion.
Es ist bekannt, dass Hygienepapiere als Taschentücher, Gesichtstücher, Papierhandtücher und Toilettenpapiere ausgedehnte Anwendung finden. Je nach dem vorgesehenen Verwendungszweck werden unterschiedliche Eigenschaften von Tissuepapieren verlangt. So sind bei Küchentüchern und noch in noch höherem Maße bei Handtüchern Festigkeit, insbesondere Festigkeit im nassen Zustand und hohe Saugleistung erforderlich, um den Ansprüchen des Verbrauchers zu genügen. Bei anderen Produkten wie Taschentüchern oder Gesichtstüchern sind Weichheit der Oberfläche und eine sehr gute Anschmiegsamkeit die hervorstechendsten Eigenschaften, die den Gebrauchswert dieser Produkte bestimmen. Bei Toilettenpapieren wird eine Kombination von hoher Nass- und Trockenfestigkeit sowie besonderer Weichheit vom Verbraucher verlangt.It is known that sanitary paper as handkerchiefs, Facial tissues, paper towels and toilet paper find extensive application. Depending on the intended Different uses of Tissue papers are required. So are kitchen towels and still to an even greater extent with towels strength, in particular Strength when wet and high suction power required, to meet the needs of the consumer. At other products such as handkerchiefs or facial tissues Softness of the surface and very good conformability the most salient features, the utility value determine these products. With toilet paper one Combination of high wet and dry strength as well demands particular softness from the consumer.
Die zur Erzeugung der Weichheit eines Tissuepapieres üblichen Maßnahmen lassen sich in drei Hauptkategorien einteilen:
- 1.
- Auswahl geeigneter Rohstoffe, insbesondere der Zellstoffe;
- 2.
- maschinentechnische Maßnahmen wie die Mahlung, Blattbildung, Trocknung, Kreppung und Glättung; und
- 3.
- chemische Zusatz- und Hilfsstoffe.
- 1.
- Selection of suitable raw materials, especially pulp;
- 2nd
- mechanical measures such as grinding, sheet formation, drying, creping and smoothing; and
- 3rd
- chemical additives.
Der Herstellungsprozess von Tissueprodukten umfaßt unabhängig von seinen verschiedenen Varianten die folgenden verfahrenstechnischen Schritte:The manufacturing process of tissue products involves independent of its different variants the following procedural Steps:
Suspendieren der Faserstoffe in Wasser, eventuelle Zugabe von chemischen Hilfsmittel zur gezielten Beeinflussung von Produkteigenschaften und Verfahrensablauf, Aktivierung der Faseroberflächen zur Erschließung des Festigkeitspotentials der Faserrohstoffe durch mechanische Behandlung wie Mahlung in einem Refiner, Blattbildung durch Ablegung der Fasern, orientiert oder in wirrer Lage auf einem oder zwischen zwei endlos umlaufenden Sieben der Papiermaschine unter gleichzeitiger Entfernung der Hauptmenge an Verdünnungswasser bis auf Trockengehalte zwischen 12 und 35%, Trocknung des gebildeten primären Faservlieses in einem oder mehreren Schritten auf mechanischem oder thermischem Wege bis zu einem Endtrockengehalt von rund 93 bis 97%. Zu den für die Tissueerzeugung relevantesten Schritten gehört weiterhin der Kreppvorgang, der beim konventionellen Prozess dominierend die Eigenschaften des fertigen Tissueprodukts beeinflußt. Beim Trockenkreppverfahren wird die Kreppung auf einem Trockenzylinder durchgeführt, von dem das Tissuepapierprodukt mit einem Kreppschaber abgelöst wird, sobald es den angestrebten Endtrockengehalt von 93 bis 97% erreicht hat. Bei älteren Verfahren mit geringeren Anforderungen an die Tissuequalität wird auch das Nasskreppverfahren angewendet, das ähnlich dem Trockenkreppverfahren, jedoch bei niedrigeren Trockengehalten unter 80%, üblicherweise bei etwa 55 bis 65% Trockengehalt abläuft, an das sich eine Nachtrocknung auf anschließenden Trockenzylindern einer Trockenpartie bis zum Endtrockengehalt anschließt. Das gekreppte, endtrockene Rohtissuepapier wird dann auf Hülsen zu Mutterrollen aufgewickelt und steht in dieser Form für die weitere Verarbeitung zu Fertigprodukten zur Verfügung.Suspend the fibrous material in water, possibly adding chemical auxiliaries for the targeted influencing of Product properties and process flow, activation of Fiber surfaces for tapping the strength potential of the fiber raw materials by mechanical treatment such as grinding in a refiner, sheet formation by laying down the fibers, oriented or in a confused position on one or between two endless rotating sieves of the paper machine under simultaneous Removal of the bulk of the dilution water up to to dry contents between 12 and 35%, drying of the formed primary nonwoven fabric in one or more Mechanical or thermal steps up to one Final dry content of around 93 to 97%. Among those for tissue production The most relevant steps continue to be the Crepe process that dominates the conventional process Properties of the finished tissue product affected. At the Dry crepe process is the crepe on a drying cylinder carried out, of which the tissue paper product with a crepe scraper is replaced as soon as it reaches the intended Final dry matter content of 93 to 97%. For older people Processes with lower demands on tissue quality the wet crepe process is also used, which is similar to the Dry crepe process, but at lower dry contents below 80%, usually around 55 to 65% dryness expires, which is followed by drying on subsequent Drying cylinders of a dryer section up to the final dry content connects. The creped, end-dry raw tissue paper is then wound up on tubes to mother rolls and stands in this form for further processing into finished products to disposal.
Zur Erzeugung mehrlagiger Tissuepapiere wie Taschentüchern, Toilettenpapieren, Handtüchern oder Küchentüchern wird in einem Zwischenschritt häufig noch die Zahl der Papierlagen erhöht, indem mehrere einlagige Mutterrollen zu einer mehrlagigen Mutterrolle aufgewickelt werden.For the production of multi-layer tissue papers such as handkerchiefs, Toilet paper, towels or kitchen towels are in an intermediate step is often the number of paper layers increased by adding multiple single ply parent rolls to one multilayer mother roll can be wound up.
Weitere Verarbeitungsprozesse beispielsweise zu Faltprodukten wie Taschentüchern oder Kosmetiktüchern erfolgen in nachgeschalteten, separaten Arbeitsgängen, wobei spezielle, für die Aufgabe konstruierte Verarbeitungsmaschinen eingesetzt werden. Dabei erfolgt ein Glätten des Tissuepapierproduktes, Randprägungen, teilweise kombiniert mit einer flächigen und/oder punktuellen Verleimung zur Erzeugung von Lagenhaftung der miteinander in Verbund zu bringenden Einzellagen sowie Längsschnitt, Faltung, Querschnitt, Ablage und Zusammenführung mehrerer Einzeltücher und deren Verpackung in sog. Tüchertaschen oder speziellen Kartons sowie deren Zusammenführung zu größeren Umverpackungen oder Gebinden.Further processing processes, for example into folded products like handkerchiefs or facial tissues take place in downstream, separate operations, being special, for the task constructed processing machines used become. The tissue paper product is smoothed, Edge embossing, sometimes combined with a flat one and / or selective gluing to generate layer adhesion the individual layers to be brought together as well as Longitudinal section, folding, cross section, storage and merging several individual wipes and their packaging in so-called wipe bags or special boxes as well as their merging larger packaging or containers.
Es ist nun auch schon bekannt, dass sich die Gebrauchseigenschaften des Tissuepapierproduktes durch den Einsatz von Chemikalien bei seiner Herstellung beeinflussen lassen. Besonders bewährt hat sich die Zuführung der Chemikalien in Form einer Lotion, die auf das rohe Tissuepapierprodukt während seiner Erzeugung, während der Ausbildung der Mehrlagigkeit oder während der nachfolgenden Verarbeitung aufgebracht werden kann. Unter Lotionen werden dabei sowohl wasserhaltige als auch wasserfreie Zubereitungen verstanden, die im allgemeinen Polyhydroxyverbindungen wie Glycol oder Polyethylenglycol oder auch Polysiloxane enthalten. Trotz zahlreicher Rezepturvorschläge für derartige Lotionen ist bisher allerdings nicht bekannt geworden, dass sich eine ganz unerwartete Weichheitssteigerung bei Tissuepapierprodukten erreichen läßt, wenn ein Mineralöl oder Fettsäureester zusammen mit einer quaternären Ammoniumverbindung und einem Polysiloxan zur Behandlung eines rohen Tissuepapierproduktes eingesetzt werden, ohne dass dabei dessen mechanische Eigenschaften nachteilig beeinflußt werden.It is now also known that the usage properties of the tissue paper product through the use of Allow chemicals to influence its manufacture. The supply of the chemicals in Form a lotion on the raw tissue paper product during its creation, during the formation of the multilayer or during subsequent processing can be applied. Lotions are both understood water-containing as well as water-free preparations, the generally polyhydroxy compounds such as glycol or Contain polyethylene glycol or polysiloxanes. Despite numerous recipe suggestions for such lotions So far, however, it has not become known that a whole unexpected increase in softness in tissue paper products if a mineral oil or fatty acid ester together with a quaternary ammonium compound and a Polysiloxane for the treatment of a raw tissue paper product be used without the mechanical Properties are adversely affected.
Gegenstand der Erfindung ist deshalb ein Tissuepapierprodukt,
das mit einer wasserhaltigen oder wasserfreien Lotion
behandelt worden ist, enthaltend
Zusätzlich kann diese Lotion noch eine Polyhydroxyverbindung in einer Menge von bis zu 20 Gewichtsprozent enthalten. Die Polyhydroxyverbindung sollte ein Molekulargewicht zwischen 10 und 4.000, vorzugsweise zwischen 100 und 1.000 aufweisen und vorzugsweise aus Glycerin, einem Polyethylenglycol, einem Polypropylenglycol oder bevorzugt aus Dipropylenglycol oder deren Mischungen bestehen.This lotion can also contain a polyhydroxy compound contained in an amount of up to 20 percent by weight. The Polyhydroxy compound should have a molecular weight between 10 and 4,000, preferably between 100 and 1,000 and preferably from glycerin, a polyethylene glycol, a Polypropylene glycol or preferably from dipropylene glycol or their mixtures exist.
Die erfindungsgemäße Lotion ist bei Zimmertemperatur flüssig und kann außer den genannten Bestandteilen noch weitere an sich bekannte Zusatzstoffe wie Parfüme, Desinfektionsmittel, Deodorantien und Stabilisatoren enthalten.The lotion according to the invention is liquid at room temperature and can add other ingredients besides those mentioned known additives such as perfumes, disinfectants, Deodorants and stabilizers included.
Ein essentieller Bestandteil der erfindungsgemäßen Lotion ist in dem Mineralöl, dem Alkylethoxylat oder dem Fettsäureester zu sehen. Diese Stoffe wirken als Weichmacher. Als Mineralöl kann ein flüssiger Kohlenwasserstoff mit 16 bis 32 Kohlenstoffatomen eingesetzt werden. Geeignete Fettsäureester leiten sich von einer gesättigten oder ungesättigten Fettsäure mit 12 bis 28 Kohlenstoffatomen, vorzugsweise 16 bis 22 Kohlenstoffatomen ab. Diese Fettsäuren sind mit einem 1 bis 8 Kohlenstoffatome umfassenden aliphatischen Alkohol verestert. Bevorzugte Beispiele der hierfür geeigneten Fettsäureester sind Methylpalmitat, Methylstearat, Isopropyllaurat, Isopropylmyristat, Isopropylpalmitat und Ethylhexylpalmitat.An essential component of the lotion according to the invention is in the mineral oil, alkyl ethoxylate or fatty acid ester to see. These substances act as plasticizers. As mineral oil can be a liquid hydrocarbon with 16 to 32 carbon atoms be used. Conduct suitable fatty acid esters with a saturated or unsaturated fatty acid 12 to 28 carbon atoms, preferably 16 to 22 carbon atoms from. These fatty acids are with a 1 to 8 Aliphatic alcohol comprising carbon atoms esterified. Preferred examples of the fatty acid esters suitable for this are methyl palmitate, methyl stearate, isopropyl laurate, isopropyl myristate, Isopropyl palmitate and ethylhexyl palmitate.
Auch Alkylethoxylate sind als weichmachende Zusatzstoffe zu der erfindungsgemäßen Lotion geeignet. Hierzu gehören Ethoxylate, die sich von Fettalkoholen mit 12 bis 18 Kohlenstoffatomen ableiten und im allgemeinen zwischen 3 bis 30 Oxyethyleneinheiten tragen. Typische Beispiele für solche Alkylethoxylate umfassen Laurylethoxylate mit 3 bis 10 Oxyethyleneinheiten, Laurylethoxylate mit 23 bis 25 Oxyethyleneinheiten, Cetylethoxylate mit 10 Oxyethyleneinheiten, Stearylethoxylate mit 10 bis 12 Oxyethyleneinheiten. Diese Alkylethoxylate können in der erfindungsgemäßen Lotion allein oder in Kombination mit Mineralölen und/oder Fettsäureestern eingesetzt werden. Besteht dieser fetthaltige Weichmacher aus mehreren unterschiedlichen Komponenten, dann werden diese in der Regel in etwa gleichen Teilen eingesetzt. Mindestens sollte jede der genannten Komponenten jedoch etwa 10 Gewichtsprozent der Fettbestandteile der Weichmachermischung ausmachen, wenn überhaupt eine Mischung dieser Verbindungen zum Einsatz kommt.Alkyl ethoxylates are also used as softening additives suitable the lotion of the invention. This includes Ethoxylates, which are derived from fatty alcohols with 12 to 18 carbon atoms and generally between 3 to 30 Wear oxyethylene units. Typical examples of such Alkyl ethoxylates include 3 to 10 lauryl ethoxylates Oxyethylene units, lauryl ethoxylates with 23 to 25 oxyethylene units, Cetyl ethoxylates with 10 oxyethylene units, Stearyl ethoxylates with 10 to 12 oxyethylene units. This Alkyl ethoxylates can be used alone in the lotion according to the invention or in combination with mineral oils and / or fatty acid esters be used. Is this fat-containing plasticizer? several different components, then these are in generally used in roughly equal parts. At least however, each of the components mentioned should be about 10 percent by weight make up the fat components of the plasticizer mixture, if any, a mixture of these compounds to Commitment comes.
Die weichheitsverbessernden Eigenschaften der erfindungsgemäßen Lotion beruhen nun aber ganz entscheidend auch auf der gleichzeitigen Anwesenheit eines Polysiloxans. Bevorzugt werden hierfür Polydimethylsiloxane, die substituierte oder unsubstituierte Alkyl-, Aryl- oder Alkenylgruppen tragen und im allgemeinen nicht mehr als 10 Kohlenstoffatome aufweisen. Die Viskosität der Polydimethylsiloxane kann über einen weiten Bereich variieren, solange das Polysiloxan flüssig bleibt oder in der Lotion gelöst oder dispergiert werden kann. Hochviskose Polysiloxane, die selbst nicht mehr fließfähig sind, können so als Bestandteil der Lotion auf das Tissuepapierprodukt aufgebracht werden, indem man beispielsweise das Polysiloxan zum Beispiel in Polyethylenglykol oder Glyzerin oder deren Mischungen löst und ggf. auch noch mit einem Tensid emulgiert. Auch Polyethersiloxane, die unter dem Handelsnamen Tegopren® vertrieben werden, sind als Bestandteil der erfindungsgemäßen Lotion zur Herstellung eines weichen Tissuepapierproduktes sehr geeignet.The softness-improving properties of the invention Lotion are now also based on the simultaneous presence of a polysiloxane. Prefers Polydimethylsiloxanes that are substituted or carry unsubstituted alkyl, aryl or alkenyl groups and generally have no more than 10 carbon atoms. The viscosity of the polydimethylsiloxanes can vary widely Vary the range as long as the polysiloxane remains liquid or can be dissolved or dispersed in the lotion. Highly viscous Polysiloxanes that can no longer flow themselves so as part of the lotion on the tissue paper product be applied by, for example, the polysiloxane for example in polyethylene glycol or glycerin or their Dissolves mixtures and, if necessary, also emulsifies with a surfactant. Also polyether siloxanes, which are sold under the trade name Tegopren® are sold as part of the invention Lotion for making a soft tissue paper product very suitable.
Die gewünschten weichmachenden Eigenschaften der Lotion könnten allerdings die mechanischen Festigkeiten des Tissuepapierproduktes im trockenen oder feuchten Zustand herabsetzen. Der fetthaltige Weichmacher und das Polysiloxan haben aufgrund ihrer flüssigen Konsistenz die Tendenz, das Tissuepapierprodukt völlig zu durchdringen und dabei die Bindungseigenschaften der Cellulosefasern aneinander zu schwächen. Das kann bis zum vollständigen Verlust der Bindungseigenschaften der Fasern führen, wodurch die mechanische Festigkeit vollkommen verlorengehen würde. Dieser Wanderungstendenz wirkt nun der Zusatz des kationischen quaternären Ammoniumsalzes entgegen. Aufgrund seiner bipolaren Struktur lagert es sich auf der Oberfläche des Tissuepapierproduktes an und geht mit seinen langen hydrophoben Alkylgruppen Anlagerungsverbindungen mit den hydrophoben Gruppen der Mineralöle, Alkylethoxylate und der Fettsäureester sowie mit den Polysiloxanen ein. Diese Verbindungen werden deshalb durch die quaternären Ammoniumverbindungen an der Oberfläche des Tissuepapierproduktes fixiert und dringen nicht in das Fasergewebe ein. Damit ist auch die Gefahr einer Lockerung der Bindungsstellen der Fasern aneinander beseitigt. Gleichzeitig wird dadurch sichergestellt, dass die die weichmachende Wirkung verursachenden Substanzen an der Oberfläche des Tissuepapierproduktes gehalten werden und dadurch ihre volle Wirkung zur Erzeugung einer seidigen, samtenen, weichen Tissuepapier-Oberfläche entfalten können.The desired softening properties of the lotion However, the mechanical strength of the tissue paper product reduce in a dry or moist state. The fatty plasticizer and the polysiloxane due to their liquid consistency tend to To completely penetrate tissue paper product while doing the Binding properties of the cellulose fibers to one another weaknesses. That can last until the complete loss of Binding properties of the fibers result in the mechanical Strength would be completely lost. This Migration tendency now has the addition of the cationic quaternary ammonium salt. Because of its bipolar Structure is deposited on the surface of the tissue paper product and goes with its long hydrophobic alkyl groups Addition compounds with the hydrophobic groups of mineral oils, alkyl ethoxylates and fatty acid esters as well with the polysiloxanes. These connections are therefore through the quaternary ammonium compounds on the surface of the tissue paper product fixed and do not penetrate into it Fiber fabric. So there is also a risk of loosening Binding points of the fibers to each other eliminated. At the same time This ensures that the softening Effect causing substances on the surface of the Tissue paper product are kept and thereby their full Effect to create a silky, velvety, soft Tissue paper surface can unfold.
Beispiele für quaternäre Ammoniumsalze, die im Rahmen der vorliegenden Erfindung gut geeignet sind, sind Dialkyldimethylammoniumsalze wie das Ditallow-dimethylammoniumchlorid, das Ditallow-dimethylammoniummethylsulfat, die teilweise oder vollständig hydriert sein können. Sehr gut geeignet sind auch bioabbaubare Mono- und Diesterderivate der quaternäre Ammoniumverbindungen der Formel II und der Formel III in denen R1 eine C14 bis C22 Alkylgruppe, R2 eine C1 bis C6 Alkyl- oder Hydroxyalkylgruppe und R3 eine C1 bis C20 Alkylgruppe und X ein physiologisch verträgliches Anion ist.Examples of quaternary ammonium salts which are well suited in the context of the present invention are dialkyldimethylammonium salts such as the ditallow dimethylammonium chloride, the ditallow dimethylammonium methyl sulfate, which can be partially or completely hydrogenated. Biodegradable mono- and diester derivatives of the quaternary ammonium compounds of the formula II are also very suitable and Formula III in which R 1 is a C 14 to C 22 alkyl group, R 2 is a C 1 to C 6 alkyl or hydroxyalkyl group and R 3 is a C 1 to C 20 alkyl group and X is a physiologically acceptable anion.
Eine weitere Gruppe von Amoniumsalzen, die für die erfindungsgemäßen Tissuepapierprodukte sehr geeignet sind, sind quaternäre Imidazoliniumsalze der Formel IV wobei R4 eine Alkylgruppe mit 1 bis 6 Kohlenstoffatomen und R5 eine oder eine Gruppe ist, in der R6 eine Alkylgruppe mit 10 bis 18 Kohlenstoffatomen bedeutet und X- ein physiologisch verträgliches Anion ist.Another group of ammonium salts which are very suitable for the tissue paper products according to the invention are quaternary imidazolinium salts of the formula IV where R 4 is an alkyl group having 1 to 6 carbon atoms and R 5 is a or one Is a group in which R 6 is an alkyl group having 10 to 18 carbon atoms and X - is a physiologically acceptable anion.
Obwohl das erfindungsgemäße Tissuepapierprodukt sowohl durch Behandlung mit einer wasserhaltigen oder mit einer wasserfreien Lotion hergestellt werden kann, wird der Einsatz von wasserfreien Lotionen bevorzugt, weil diese nur die Oberfläche des Tissuepapieres benetzen und deshalb dessen Festigkeit nicht beeinträchtigen können. Die taktilen und Oberflächeneigenschaften des Tissuepapieres werden durch eine wasserfreie Lotion besonders günstig beeinflußt.Although the tissue paper product of the invention is both by Treatment with an aqueous or an anhydrous one Lotion can be made using the Anhydrous lotions are preferred because these only cover the surface of the tissue paper and therefore its strength cannot interfere. The tactile and surface properties of tissue paper are replaced by an anhydrous one Lotion influenced particularly favorably.
Das Rohtissuepapierprodukt, auf das die Lotion aufgetragen werden soll, kann einlagig oder mehrlagig, vorzugsweise allerdings zwei- bis vierlagig sein und eine geprägte oder ungeprägte Oberfläche aufweisen. Die einzelnen Papierbahnen können miteinander durch Randprägung oder Rändelung mechanisch verbunden, flächig oder punktuell verklebt oder auch in sonstiger weise miteinander verbunden sein. Für die einzelnen Bahnen hat sich weiterhin ein Flächengewichtsbereich von 10 bis 40 g/m2, vorzugsweise ein Flächengewichtsbereich zwischen 15 und 25 g/m2 als besonders günstig erwiesen.The raw tissue paper product to which the lotion is to be applied can be single-layer or multi-layer, but preferably two to four layers and have an embossed or unembossed surface. The individual paper webs can be mechanically connected to one another by edge embossing or knurling, glued flat or at certain points, or else connected to one another in some other way. For the individual webs, a basis weight range of 10 to 40 g / m 2 , preferably a basis weight range between 15 and 25 g / m 2, has also proven to be particularly favorable.
Die Lotion, welche vorzugsweise in Form einer Emulsion vorliegt, kann mit jedem beliebigen Walzen- und Sprühauftragungsverfahren oder in einem Imprägnierverfahren auf das Rohtissuepapierprodukt aufgebracht werden. Hierbei ist darauf zu achten, dass es nicht zu einer Entmischung der Emulsion kommt. Deshalb ist zu empfehlen, durch Anwendung hoher Scherkräfte, zum Beispiel durch schnellaufende Rührer, häufiges Umpumpen oder durch eine Ultraschalldurchmischung für eine innige Durchmischung der Lotion zu sorgen.The lotion, which is preferably in the form of an emulsion can be used with any roller and spray application process or in an impregnation process on the Raw tissue paper product can be applied. Here is on it to ensure that there is no segregation of the emulsion is coming. Therefore, it is recommended to use high Shear forces, for example due to high-speed stirrers, frequent pumping or by ultrasonic mixing for to ensure a thorough mixing of the lotion.
Die erfindungsgemäße Lotion ist so zusammengesetzt, dass das damit getränkte Tissueprodukt während des üblichen Anwendungszeitraumes und bei den normalerweise herrschenden Luftfeutigkeiten aufgrund seiner hydroskopischen Eigenschaften nicht zu einer Austrocknung kommen kann. Auch eine wasserdampfdichte, wieder verschließbare Verpackung ist nicht erforderlich.The lotion according to the invention is composed such that the tissue product soaked with it during the usual application period and the normally prevailing atmospheric humidity due to its hydroscopic properties not too dehydration. Also a water vapor proof, resealable packaging is not required.
Die Lotion kann sowohl im Nassteil einer Tissuepapiermaschine, am Ende der Siebpartie, vor oder innerhalb der Pressenpartie oder auch in der nach der Pressenpartie angeordneten Trockenpartie dem Rohtissuepapierprodukt zugegeben werden. Bevorzugt ist die Zugabe der Lotion in der Tissueherstellungsmaschine durch Sprühauftrag, wobei während des Aufrollvorganges ein dünner Film der Lotion auf das Tissuepapierprodukt aufgetragen wird. Dabei hat die bereits gekreppte Tissuebahn als Folge des vorausgegangenen Trocknungsvorganges noch eine Resttemperatur zwischen 20 und etwa 70°C, was für die Verteilung der Lotion und deren Eindringen in das Tissuematerial günstig ist. Neben einem Sprühauftrag über einen Düsenbalken kann auch der Einsatz von Schleuderrotoren oder Bürstwerken sowie die indirekte Übertragung eines Lotionfilmes über Walzenauftragswerke in Frage kommen. Der Auftrag kann auch direkt auf der Tissuepapierbahn erfolgen. Bevorzugt ist allerdings die Zugabe der Lotion innerhalb der Verarbeitungsmaschine auf die Außenlage der mehrlagigen Bahn vor oder während der Glättung.The lotion can be used in the wet part of a tissue paper machine, at the end of the wire section, in front of or within the press section or also in the dryer section arranged after the press section be added to the raw tissue paper product. Prefers is the addition of the lotion in the tissue making machine by spray application, during the reeling process apply a thin film of the lotion to the tissue paper product becomes. The already creped tissue web as a result of the previous drying process still a residual temperature between 20 and about 70 ° C, what for the distribution of the lotion and their penetration into the tissue material is favorable. Next a spray application via a nozzle bar can also Use of centrifugal rotors or brushing plants as well as the indirect transfer of a lotion film via roller applicators come into question. The order can also be placed directly on the Tissue paper web done. However, the addition is preferred the lotion inside the processing machine on the The outer layer of the multi-layer web before or during smoothing.
Die vorliegende Erfindung betrifft deshalb auch ein Verfahren zur Herstellung eines Tissuepapier-Produktes, bei dem das Cellulosefasermaterial mit 0,005 bis 5 Gewichtsprozent, bezogen auf das Trockenfasergewicht des Rohtissuepapierproduktes, der vorstehend beschriebenen Lotion imprägniert wird. Der Begriff Tissuepapierprodukt wird erfindungsgemäß unabhängig von dem zu verwendenden Faserrohstoff verstanden. Das erfindungsgemäße Verfahren läßt sich auch für Tissuepapierprodukte anwenden, die nur teilweise aus nativen Zellstoffen bestehen und beispielsweise auch noch wiederaufbereitete Fasern oder zur Papierherstellung geeignete Kunststoffasern enthalten. Besonders bevorzugt ist es, als Tissuebahn eine mehrlagige Bahn einzusetzen und auf wenigstens eine der Außenlagen der mehrlagigen Bahn der Lotion zu applizieren. Besonders bevorzugt ist dabei die Verfahrensvariante, bei der eine Nachglättung durch wenigstens einen Durchgang der Tissuebahn durch einen Spalt eines Walzenpaares erfolgt, bei dem eine Walze mit einer Stahloberfläche einer Gegenwalze mit einer Stahl-, Kunststoff-, Papier- oder Gummioberfläche, vorzugsweise aber einer Kunststoffoberfläche, zugeordnet ist. Diese Walzen werden hydraulisch oder pneumatisch zusammengedrückt oder aber zum Kalibrieren auf Spalt gefahren. D.h., eine der beiden Walzen ist fest positioniert, während die zweite Walze gegen einen Anschlag gedrückt wird, so dass sich die beiden Walzen nicht berühren können, sondern in einem bestimmten, messbaren und reproduzierbaren Abstand zueinander stehen. Die durch diesen Spalt geführten Tissuebahnen werden auf Spaltbreite komprimiert und dabei geglättet. Hierbei wird die Gefügestruktur der Oberfläche vereinheitlicht, d.h. es wird eine gleichmäßige Dicke herbeigeführt.The present invention therefore also relates to a method for the manufacture of a tissue paper product in which the Cellulose fiber material with 0.005 to 5 percent by weight, based on the dry fiber weight of the raw tissue paper product, of the lotion described above becomes. The term tissue paper product is used according to the invention understood regardless of the fiber raw material to be used. The method according to the invention can also be used for tissue paper products apply that only partially from native pulps exist and for example also reprocessed Fibers or suitable for paper production Contain plastic fibers. It is particularly preferred as Tissue web to use a multilayer web and at least one of the outer layers of the multi-layer lotion apply. The process variant is particularly preferred, in which a smoothing by at least one Passage of the tissue web through a nip of a pair of rollers takes place in which a roller with a steel surface Counter roll with a steel, plastic, paper or Rubber surface, but preferably a plastic surface, assigned. These rollers are hydraulic or pneumatic compressed or for calibration on gap hazards. That is, one of the two rollers is firmly positioned, while the second roller is pressed against a stop, so that the two rollers cannot touch, but rather at a certain, measurable and reproducible distance to stand by each other. The tissue webs passed through this gap are compressed to the gap width and smoothed in the process. The structure of the surface is standardized, i.e. a uniform thickness is brought about.
Das so hergestellt Tissuepapierprodukt ist als Toilettenpapier, als Gesichtstuch, als Papiertaschentuch oder als Papierhandtuch hervorragend geeignet.The tissue paper product so made is as toilet paper, as a facial tissue, as a tissue or as Excellent paper towel.
Die vorliegende Erfindung wird durch die folgenden Ausführungsbeispiele näher erläutert: The present invention is illustrated by the following exemplary embodiments explained in more detail:
Auf eine Rohtissuepapierbahn mit einem Flächengewicht von etwa 18 g/m2 und einem Fasertrockengehalt von etwa 95% wurde eine wässrige Lotion bestehend aus 10 Gewichtsprozent Paraffinum perliquidum, 4 Gewichtsprozent des Ditallow-dimethylammoniumchlorids und 15 Gewichtsprozent des Polysiloxans Tegopren® 3021, eines Polyethersiloxans mit dem Trübungspunkt von 38°C, unter guter Verwirbelung in einer Menge von 4%, bezogen auf das Gewicht des Rohtissuepapierproduktes gesprüht und einer Nachglättung unterzogen. Der Auftrag erfolgte symmetrisch auf die Außenflächen des Fertigtuches.A Rohtissuepapierbahn having a basis weight of about 18 g / m 2 and a fiber dry content of about 95%, an aqueous lotion consisting perliquidum from 10 percent by weight of paraffin, 4 weight percent of the ditallow-dimethylammonium chloride and 15 weight percent of the polysiloxane Tegopren® 3021, a polyether siloxane with the Cloud point of 38 ° C, with good swirling in an amount of 4%, based on the weight of the raw tissue paper product, sprayed and subjected to post-smoothing. The application was carried out symmetrically on the outer surfaces of the finished sheet.
Das Auftragungsverfahren nach Beispiel 1 wurde wiederholt, wobei allerdings der Lotion auch noch 7,5 Gewichtsprozent Glycerin zugesetzt waren. Es wurde ein geschmeidiges Tissuepapierprodukt mit einer sich seidig anfühlenden Oberfläche gewonnen, das eine so hohe mechanische Trocken- und Nassfestigkeit aufwies, dass es sowohl als Papiertaschentuch als auch als Toilettenpapier ausgezeichnet Verwendung finden konnte.The application procedure according to Example 1 was repeated, although the lotion also contains 7.5 percent by weight Glycerin were added. It became a smooth tissue paper product with a silky-feeling surface won that such a high mechanical dry and wet strength exhibited that it was used both as a tissue and as a also excellent as toilet paper could.
Es wurde eine wasserfreie Lotion durch Vermischen von 85% Paratfinum perliquidum, 10,8% Plurafac® A ( ein linearer, 18 Kohlenstoffatome umfassender Alkohol, der mit 27 Mol Etylenoxid umgesetzt wurde), 3% eines Polydimethylpolysiloxans (Dow Q2-7224) und 1,2% eines dihydrierten Tallow-dimethylammoniumchlorids (DTDMAC) hergestellt. Diese Lotion wurde in einer Menge von 2%, bezogen auf das Gewicht des Rohtissuepapierproduktes, auf die Außenseiten der Tissuepapierbahn aufgesprüht. Es entstand ein Tissuepapierprodukt, welches sich samtweich anfühlte, und eine hohe mechanische Festigkeit aufwies.It became an anhydrous lotion by mixing 85% Paratfinum perliquidum, 10.8% Plurafac® A (a linear, 18th Alcohol containing carbon atoms, containing 27 moles of ethylene oxide was implemented), 3% of a polydimethylpolysiloxane (Dow Q2-7224) and 1.2% of a dihydrogenated Tallow dimethylammonium chloride (DTDMAC). This lotion was made in one Quantity of 2%, based on the weight of the raw tissue paper product, sprayed onto the outside of the tissue paper web. The result was a tissue paper product, which itself felt velvety soft, and high mechanical strength exhibited.
Claims (11)
Applications Claiming Priority (2)
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DE1998158616 DE19858616B4 (en) | 1998-12-18 | 1998-12-18 | Tissue paper product and its use, and lotion for the treatment of the tissue product |
DE19858616 | 1998-12-18 |
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EP1013823A1 true EP1013823A1 (en) | 2000-06-28 |
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EP99123068A Withdrawn EP1013823A1 (en) | 1998-12-18 | 1999-11-20 | Tissue paper product and lotion for its manufacture |
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US20080230196A1 (en) * | 2007-03-22 | 2008-09-25 | Kou-Chang Liu | Softening compositions for treating tissues which retain high rate of absorbency |
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DE19858616A1 (en) | 2000-06-21 |
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