EP1530657B1 - Formulation of a highly viscous mineral oil for the production of filters for tobacco - Google Patents

Formulation of a highly viscous mineral oil for the production of filters for tobacco Download PDF

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Publication number
EP1530657B1
EP1530657B1 EP03732455A EP03732455A EP1530657B1 EP 1530657 B1 EP1530657 B1 EP 1530657B1 EP 03732455 A EP03732455 A EP 03732455A EP 03732455 A EP03732455 A EP 03732455A EP 1530657 B1 EP1530657 B1 EP 1530657B1
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EP
European Patent Office
Prior art keywords
sorbitan
formulation
weight
ethylene oxide
oxide units
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EP03732455A
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German (de)
French (fr)
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EP1530657A1 (en
Inventor
Hubert Dobbelstein
Shefqet Emini
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EMINI, SHEFQET
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Shefqet Emini
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Classifications

    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
    • D06M13/2243—Mono-, di-, or triglycerides
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/06—Use of materials for tobacco smoke filters
    • A24D3/08—Use of materials for tobacco smoke filters of organic materials as carrier or major constituent
    • A24D3/10—Use of materials for tobacco smoke filters of organic materials as carrier or major constituent of cellulose or cellulose derivatives
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/06—Use of materials for tobacco smoke filters
    • A24D3/14—Use of materials for tobacco smoke filters of organic materials as additive
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/02—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M7/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made of other substances with subsequent freeing of the treated goods from the treating medium, e.g. swelling, e.g. polyolefins
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic
    • D06M2101/08—Esters or ethers of cellulose
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/40—Reduced friction resistance, lubricant properties; Sizing compositions

Definitions

  • the present invention relates to a formulation for use as a lubricant in the manufacture of filaments.
  • the threads are first prepared by a spinning process, which is preferably the solvent spinning process, and then further processed by applying the formulation of the invention on the surface of the threads as a lubricant.
  • the threads produced are preferably cellulose acetate threads and these threads are used to make filters for tobacco products, especially cigarette filters.
  • the patent GB 896,599 describes tobacco filters that can be used in cigarettes, pipes, cigarette holders or cigar tips.
  • the filter elements described consist of bundles of continuous synthetic filaments, wherein water-insoluble calcium or magnesium salts are finely distributed on the surface of the filaments. These finely divided particles are fixed by oils on the fibers. In addition to mineral oils, these oils may also be high-boiling liquid esters of natural origin, liquid esters of natural fats or liquid high molecular weight fatty alcohols.
  • the patent GB 765,962 describes a tobacco filter element consisting of cellulose acetate fibers.
  • the cellulose acetate filter material is subjected to various processing steps, such as stretching and crimping of the fibers.
  • electrostatic charging of the fibers must be prevented, and on the other hand, the surface of the fiber must be provided with a lubricant so that the fiber can be subjected to these processing steps.
  • This lubricant contains a mineral oil with a purity that would make it suitable for the manufacture of pharmaceutical products.
  • a rigid tobacco smoke filter consisting of a bundle of optionally crimped continuous filaments and a paper wrapper is described.
  • the filaments consist of a mixture of a polyalphaolefin and a plasticizer-soluble polymer of an organic plasticizer.
  • Liquid organic plasticizers which can be used in addition to light, medium and heavy mineral oils, liquid high-boiling organic esters or water-insoluble propylene glycols or polybutylene glycols.
  • a cleaning composition containing white mineral oil is described.
  • the emulsion is used for the treatment and cleaning of metal surfaces.
  • the emulsion of the invention contains 20-50 wt.% Of a mineral oil having a viscosity of 50-380 Saybolt seconds, measured at 100 ° F and 0.5 to 10 wt.% Of an emulsifier.
  • nonionic emulsifiers has been found to be advantageous.
  • sorbitan esters and polyglycerides of fatty acids are also mentioned.
  • emulsifier should be present in the emulsion as is just necessary to form a stable emulsion. In this case, 0.5 to 10% by weight of the emulsifier are present in the emulsion, with 1 to 5% by weight of emulsifier being preferred. If more emulsifier is present in the emulsion, milky stains or streaks may remain on the cleaned surface after cleaning.
  • a thread which normally contains cellulose acetate
  • a spinning process which is preferably the solvent spinning process.
  • an acetone solution of cellulose acetate and matting agent TiO 2 is pressed through shower-like nozzles (spinnerets).
  • the holes usually have cross sections in the form of an equilateral triangle.
  • a heated spin shaft Below the spinnerets is a heated spin shaft. The air sucked through the spinning shaft heats up and absorbs the solvent which diffuses out of the formed filament, acetone, which almost is completely recovered.
  • the solution solidifies under considerable volume shrinkage to a filament.
  • the filaments When using triangular holes, the filaments have a Y-section.
  • the filaments in the thread When a thread composed of several filaments leaves the spinning shaft, the filaments in the thread are densely packed without, however, sticking to each other.
  • the thread At the exit of the spinning shaft, the thread typically contains a residual fraction of about 1 to 6% by weight of acetone.
  • the thread is provided with a preparation (avivage), which serves mainly as a lubricant for the subsequent processing steps. This preparation is carried out by an oiler or by means of an applicator roll.
  • the content of acetone in the threads is first further reduced, a plurality of threads are combined to form the so-called rope and the rope is subjected to a crimping process by means of a crimping machine, which preferably works according to the stuffer box principle.
  • this rope is passed through a conical machine part and thus compressed to its final thickness, ie the thickness of the filter to be produced.
  • a glycerol triacetate-containing composition is applied to the filter tow. This further preparation, after leaving the compression part by curing, fixes the filter in the desired shape and thickness.
  • the formulation applied after the threads have dried acts as a lubricant. It ensures, inter alia, that the friction which occurs during the subsequent processing steps does not exceed a value which leads to the breakage or undesired heating of the threads or the rope. Both would cause unwanted rejects.
  • the lubricant enables higher machine speeds. The formulation must withstand the high shear forces associated with this process without loss of effect.
  • This lubricant usually consists of an emulsion which is prepared from a mixture of low-viscosity mineral oil and emulsifier. Other components may be included in the emulsion.
  • the mineral oils remain on the threads after the manufacture of the filters and the corresponding tobacco products containing these filters. For example, when smoking a cigarette containing such a filter, some of the mineral oil that is on the filter may be absorbed by the smoker.
  • MK Baldwin et al. MK Baldwin et al .; "Feeding studies in council with mineral hydrocarbon grade grade white mineral oils", Toxicol. Pathol. 20, 426 (1992 )
  • Smith et al. JH Smith et al .; "Ninety-day feeding study in Fischer's 344-rats highly refined petroleum-derived food-grade white oils and waxes", Toxicol. Pathol.
  • the object of the present invention is to provide a stable and storable emulsion containing high viscosity mineral oils having a viscosity of at least 8.5 mm 2 / s at 100 ° C. For this it is necessary to find emulsifiers for the preparation of a processible formulation. The formulation is then used in exchange for the formulations containing low viscosity mineral oils.
  • the object of the present invention is achieved by a formulation for use as a preparation in the production of threads containing a) 30-80 wt .-% of a mineral oil having a viscosity of at least 8.5 mm 2 / s at 100 ° C and b) 11 60% by weight of an emulsifier selected from sorbitan monoesters, derivatives of sorbitan monoesters, sorbitan diesters, derivatives of sorbitan diesters, sorbitan triesters, derivatives of sorbitan triesters, polyglycerol esters, derivatives of polyglycerol esters, polyricinoleate, derivatives of polyricinoleate and mixtures thereof, the formulation comprising a water in oil or an oil-in-water emulsion.
  • an emulsifier selected from sorbitan monoesters, derivatives of sorbitan monoesters, sorbitan diesters, derivatives of sorbitan diesters, sorbitan
  • the stability of a formulation which may be in the form of an emulsion can be determined by the turbidity of the formulation. It basically applies that a higher turbidity indicates a lower stability.
  • the processing stability of the formulation can be checked by checking the turbidity of the formulation during processing. No or little increase in turbidity is particularly advantageous, while a greater increase in turbidity indicates inadequate formulation stability.
  • the storage stability of a formulation can be checked by checking the turbidity after, for example, five days storage at 23 ° C.
  • the viscosity at 100 ° C. is at least 8.5 mm 2 / s.
  • the mineral oil used preferably has a viscosity of from 8.5 to 1000, particularly preferably from 8.5 to 20 and very particularly preferably from 8.5 to 11 mm 2 / s.
  • the proportion of hydrocarbons in the high-viscosity mineral oil having less than 25 carbon atoms is not more than 5% by weight.
  • the average molecular weight of the high-viscosity mineral oil should not be less than 480 g / mol.
  • the emulsifiers used according to the invention are selected from sorbitan monoesters, derivatives of sorbitan monoesters, sorbitan diesters, derivatives of sorbitan diesters, sorbitan triesters, derivatives of sorbitan triesters, polyglycerol esters, derivatives of polyglycerol esters and mixtures thereof.
  • the esters may preferably be esters with fatty acids.
  • the fatty acid all fatty acids can be used, such as e.g. Stearic acid, oleic acid, lauric acid and ricinoleic acid ([R (Z)] - 12-hydroxy-9-octadecenoic acid).
  • the fatty acids used may alternatively be derived from corn, cottonseed oil, palm oil, peanut oil, sesame oil, soybean oil, safflower oil, castor oil or other oils of native origin.
  • the fatty acids can be hydrogenated or non-hydrogenated, and condensed or non-condensed.
  • the sorbitan triester be selected from the group consisting of sorbitan triesters with fatty acids containing 10-25 carbon atoms, ethoxylated sorbitan triesters with fatty acids containing 10-25 carbons and containing 5-30 moles of ethylene oxide units per mole of sorbitan triester, and mixtures thereof.
  • the sorbitan triester may be selected from the group consisting of sorbitan tristearate, ethoxylated sorbitan tristearate with 5-30 moles of ethylene oxide units per mole of sorbitan tristearate, sorbitan trioleate, ethoxylated sorbitan trioleate with 5-30 mole ethylene oxide units per mole sorbitan trioleate, sorbitan trilaurate, ethoxylated sorbitan trilaurate with 5-30 mole ethylene oxide units per mole Sorbitan trilaurate and mixtures thereof.
  • the Polyglycerinesteranteil may be composed of at least 75% di-, tri- and Tetraglycerinestern.
  • the polyglycerol ester is formed from the group of polyglycerol esters with fatty acids containing 10-25 carbon atoms, derivatives of polyglyceric acids with fatty acids containing 10-25 carbon atoms, polyglycerol polyricinoleate, derivatives of polyglycerol polyricinoleate and mixtures thereof ,
  • the formulation contains as emulsifier a) sorbitan tristearate or ethoxylated sorbitan tristearate with 5-30 mol ethylene oxide units per mole sorbitan tristearate, b) polyglycerol polyricinoleate and c) sorbitan monolaurate and d) ethoxylated sorbitan monolaurate with 5-30 mol ethylene oxide units per mole sorbitan monolaurate and e ) Sorbitan monooleate.
  • emulsifier a) sorbitan tristearate or ethoxylated sorbitan tristearate with 5-30 mol ethylene oxide units per mole sorbitan tristearate, b) polyglycerol polyricinoleate and c) sorbitan monolaurate and d) ethoxylated sorbitan monolaurate with 5-30 mol ethylene oxide units per mole sorbitan monolaurate and e ) Sorbit
  • the emulsifier is present as a mixture of at least two emulsifiers, based on the weight of the formulation, 1 to 15% by weight of ethoxylated sorbitan tristearate with 5 to 30 mol of ethylene oxide units per mole of sorbitan tristearate in the mixture of emulsifiers and / or from 1 to 15% by weight of polyglycerol polyricinoleate and / or polyricinoleate in the mixture of emulsifiers.
  • the emulsifier is present as a mixture of at least two emulsifiers, based on the weight of the formulation 1 to 15 wt .-% ethoxylated sorbitan monolaurate with 5 to 30 moles of ethylene oxide per mole of sorbitan monolaurate in the mixture of emulsifiers and / or based on the weight of the formulation contains from 1 to 15% by weight of sorbitan monooleate with from 5 to 30 mol of ethylene oxide units per mole of sorbitan monooleate in the mixture of emulsifiers.
  • the formulation of the invention contains 30-80 wt.% Of the mineral oil, preferably 40-80 wt .-%, particularly preferably 45-75 wt .-% and most preferably 55-72 wt.% Of the mineral oil.
  • the formulation preferably contains 15-60% by weight of the emulsifier, more preferably 20-60% by weight, particularly preferably 25-55% by weight of the emulsifier.
  • the formulation according to the invention is a water-in-oil or an oil-in-water emulsion.
  • the formulation according to the invention is applied after the spinning process in emulsion form on the surface of the threads, which are processed into filters for tobacco products.
  • the mineral oil remains on the surface of the threads or the dew.
  • the filaments used contain cellulose acetate containing on average 1.5 to 3 acetate groups per unit cellulose.
  • filaments also means fibers which can be produced by the process described here.
  • filters for tobacco products can be produced filters for tobacco products. It is preferred that the filters are cigarette filters. In all operations, the applied emulsion remains on the threads and thus on the rope. Thus, to a certain extent, the emulsion is still present in the filters for tobacco products and the tobacco itself.
  • the emulsion according to the invention is illustrated by the following examples, but without being limited to these examples.
  • Formulation 1 [% by weight] Formulation 2 [% by weight]
  • Mineral oil Primol ® 352 1 64,50 60,00 Sorbitan monolaurate + 20 EO 2 12,80 11,60 sorbitan 8.20 13,00 Sorbitan tristearate + 20 EO 2 - 4.40 Polyglycerol polyricinoleate 3.10 3.00 sorbitan 5.77 - water rest rest 1
  • Primol ® 352 is a high viscosity mineral oil of ESSO AG viscosity according to ASTM D 445: 71 mm 2 / s at 40 ° C, 9.0 mm 2 / s at 100 ° C 2 + 20 EO means 20 moles of ethylene oxide units per mole of ester
  • Formulations 1 and 2 from Table 1 both contain the combination according to the invention of a mineral oil having a viscosity of at least 8.5 mm 2 / s at 100 ° C. and the emulsifier according to the invention.
  • the emulsions can be prepared by standard methods.
  • Primol 352 is initially charged at room temperature and, while stirring continuously, the raw materials are added in the order of sorbitan monolaurate, sorbitan monolaurate + 20 EO, sorbitan monooleate, polyglycerol polyricinoleate and water.
  • Formulation 1 is stirred for a further 30 minutes.
  • primer 352 heated to 50 ° C. is initially charged in a stirrer.
  • the further raw materials are added in the order of sorbitan monolaurate, sorbitan monolaurate + 20 EO, sorbitan tristearate + 20 EO, polyglycerol polyricinoleate and water. After stirring for 30 minutes at 50 ° C, the formulation is allowed to cool to room temperature and stirred at this temperature for a further 30 minutes.
  • Both formulations are used to produce cellulose acetate filaments by the solvent spinning method. In this case, no negative influence of the formulations according to the invention was shown in the production of the threads.
  • Formulation 1 and Formulation 2 show storage stability at 23 ° C and five days, comparable to the formulations commonly used, and no increase in clouding of the emulsion due to shear forces occurred during processing of the filaments into filters. Both formulations behaved similarly to the commonly used formulations.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Edible Oils And Fats (AREA)
  • Colloid Chemistry (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Manufacture Of Tobacco Products (AREA)
  • Fats And Perfumes (AREA)

Abstract

Fiber lubricant comprises 30-90 wt.% of a mineral oil with a viscosity of at least 8.5 mm2/second at 100 degrees C and 11-60 wt.% of an emulsifier selected from sorbitan mono-, di- and triesters, polyglycerol esters, polyricinolates and their derivatives. Independent claims are also included for: (1) fibers coated with the lubricant after spinning; (2) cigarette filter comprising the fibers.

Description

Die vorliegende Erfindung bezieht sich auf eine Formulierung zur Verwendung als Schmiermittel bei der Herstellung von Fäden. Die Fäden werden zunächst nach einem Spinnverfahren, das bevorzugt das Lösungsmittelspinnverfahren ist, hergestellt und anschließend unter Aufbringung der erfindungsgemäßen Formulierung auf die Oberfläche der Fäden als Schmiermittel weiterverarbeitet. Die hergestellten Fäden sind bevorzugt Celluloseacetatfäden und diese Fäden werden zur Herstellung von Filtern für Tabakwaren, speziell Zigarettenfiltern, verwendet.The present invention relates to a formulation for use as a lubricant in the manufacture of filaments. The threads are first prepared by a spinning process, which is preferably the solvent spinning process, and then further processed by applying the formulation of the invention on the surface of the threads as a lubricant. The threads produced are preferably cellulose acetate threads and these threads are used to make filters for tobacco products, especially cigarette filters.

Die Patentschrift GB 896,599 beschreibt Tabakfilter, die in Zigaretten, Pfeifen, Zigarettenspitzen oder Zigarrenspitzen eingesetzt werden können. Die beschriebenen Filterelemente bestehen aus Bündeln kontinuierlicher synthetischer Filamente, wobei wasserunlösliche Calcium- oder Magnesiumsalze fein verteilt auf der Oberfläche der Filamente vorhanden sind. Diese fein verteilten Partikel werden durch Öle auf den Fasern fixiert. Diese Öle können neben Mineralölen auch hochsiedende flüssige Ester nativer Herkunft, flüssige Ester von natürlichen Fetten oder flüssige hochmolekulare Fettalkohole sein.The patent GB 896,599 describes tobacco filters that can be used in cigarettes, pipes, cigarette holders or cigar tips. The filter elements described consist of bundles of continuous synthetic filaments, wherein water-insoluble calcium or magnesium salts are finely distributed on the surface of the filaments. These finely divided particles are fixed by oils on the fibers. In addition to mineral oils, these oils may also be high-boiling liquid esters of natural origin, liquid esters of natural fats or liquid high molecular weight fatty alcohols.

Die Patentschrift GB 765,962 beschreibt ein Tabakfilterelement, das aus Celluloseacetatfasern besteht. Bei der Herstellung von Zigarettenfiltern wird das Celluloseacetatfiltermaterial vielfältigen Verarbeitungsschritten unterworfen, wie z.B. dem Recken und dem Kräuseln der Fasern. Bei diesen Verarbeitungsschritten muss einerseits eine elektrostatische Aufladung der Fasern verhindert werden und andererseits muss die Oberfläche der Faser mit einem Schmiermittel versehen werden, so dass die Faser diesen Verarbeitungsschritten unterworfen werden kann. Hierbei zeigte sich, dass die Präparierung mit einem Schmiermittel, das zu keiner Elektrizitätsentladung führt, am geeignetsten ist. Dieses Schmiermittel enthält ein Mineralöl mit einer Reinheit, mit der es sich auch zur Herstellung pharmazeutischer Produkte eignen würde.The patent GB 765,962 describes a tobacco filter element consisting of cellulose acetate fibers. In the production of cigarette filters, the cellulose acetate filter material is subjected to various processing steps, such as stretching and crimping of the fibers. In these processing steps, on the one hand, electrostatic charging of the fibers must be prevented, and on the other hand, the surface of the fiber must be provided with a lubricant so that the fiber can be subjected to these processing steps. This showed that the preparation with a lubricant that does not lead to an electric discharge is most suitable. This lubricant contains a mineral oil with a purity that would make it suitable for the manufacture of pharmaceutical products.

In der DE 12 12 459 wird ein steifes Tabakrauchfilter, das aus einem Bündel gegebenenfalls gekräuselter fortlaufender Fäden und einer Papierumhüllung besteht, beschrieben. Die Fäden bestehen aus einer Mischung eines Polyalphaolefins und eines weichmacherlöslichen Polymeren eines organischen Weichmachers. Als flüssiger organischer Weichmacher können neben leichten, mittleren und schweren Mineralölen auch flüssige hochsiedende organische Ester oder wasserunlösliche Propylenglycole oder Polybutylenglycole verwendet werden.In the DE 12 12 459 A rigid tobacco smoke filter consisting of a bundle of optionally crimped continuous filaments and a paper wrapper is described. The filaments consist of a mixture of a polyalphaolefin and a plasticizer-soluble polymer of an organic plasticizer. Liquid organic plasticizers which can be used in addition to light, medium and heavy mineral oils, liquid high-boiling organic esters or water-insoluble propylene glycols or polybutylene glycols.

In dem US-Patent 4,330,422 wird eine Reinigungszusammensetzung, die weißes Mineralöl enthält, beschrieben. Die Emulsion wird zur Behandlung und Reinigung von Metalloberflächen verwendet. Die erfindungsgemäße Emulsion enthält 20-50 Gew.% eines Mineralöls mit einer Viskosität von 50-380 Saybolt-Sekunden, gemessen bei 100° F und 0,5 bis 10 Gew.% eines Emulgators. Um eine solche Emulsion herzustellen hat sich die Verwendung von nichtionischen Emulgatoren als vorteilhaft herausgestellt. Neben einer Vielzahl von Emulgatoren werden u.a. Sorbitanester und Polyglyceride von Fettsäuren angegeben. Zur Erzielung eines sehr guten Reinigungseffektes sollte nur so viel Emulgator in der Emulsion vorhanden sein, wie gerade eben notwendig ist, um eine stabile Emulsion zu bilden. Hierbei sind 0,5 bis 10 Gew-% des Emulgators in der Emulsion vorhanden, wobei 1 bis 5 Gew-% an Emulgator bevorzugt sind. Ist mehr Emulgator in der Emulsion vorhanden, so können nach Reinigung milchige Flecken oder Streifen auf der gereinigten Oberfläche zurückbleiben.By doing U.S. Patent 4,330,422 For example, a cleaning composition containing white mineral oil is described. The emulsion is used for the treatment and cleaning of metal surfaces. The emulsion of the invention contains 20-50 wt.% Of a mineral oil having a viscosity of 50-380 Saybolt seconds, measured at 100 ° F and 0.5 to 10 wt.% Of an emulsifier. To prepare such an emulsion, the use of nonionic emulsifiers has been found to be advantageous. In addition to a large number of emulsifiers, sorbitan esters and polyglycerides of fatty acids are also mentioned. To achieve a very good cleaning effect, only as much emulsifier should be present in the emulsion as is just necessary to form a stable emulsion. In this case, 0.5 to 10% by weight of the emulsifier are present in the emulsion, with 1 to 5% by weight of emulsifier being preferred. If more emulsifier is present in the emulsion, milky stains or streaks may remain on the cleaned surface after cleaning.

Die Herstellung von Filtern für Tabakwaren findet in der Regel nach einem Prozess statt, bei dem zunächst ein Faden, der normalerweise Celluloseacetat enthält, mit Hilfe eines Spinnverfahrens, das bevorzugt das Lösungsmittelspinnverfahren ist, hergestellt wird.
Beim acetonischen Verfahren wird eine acetonische Lösung von Celluloseacetat und Mattierungsmittel TiO2 durch brauseähnliche Düsen (Spinndüsen) gepresst. Die Bohrungen haben üblicherweise Querschnitte in Form eines gleichseitigen Dreieckes. Unterhalb der Spinndüsen befindet sich ein beheizter Spinnschacht. Die durch den Spinnschacht gesaugte Luft erwärmt sich und nimmt das aus dem gebildeten Filament ausdiffundierende Lösungsmittel Aceton auf, welches fast vollständig zurückgewonnen wird. Hierbei verfestigt sich die Lösung unter erheblichem Volumenschwund zu einem Filament. Bei der Verwendung von dreieckigen Bohrungen haben die Filamente einen Y-Querschnitt. Wenn ein Faden, der aus mehreren Filamenten zusammengesetzt wird den Spinnschacht verlässt, so sind die Filamente im Faden dicht gepackt, ohne jedoch aneinander zu kleben.
Am Ausgang des Spinnschachts enthält der Faden typischerweise einen Restanteil von ca. 1 bis 6 Gew-% Aceton. Hier wird der Faden mit einer Präparation (Avivage), die hauptsächlich als Schmiermittel für die nachfolgenden Verarbeitungsschritte dient, versehen. Diese Präparation erfolgt durch einen Öler oder mit Hilfe einer Auftragswalze. In den nachfolgen Schritten wird zunächst der Gehalt an Aceton in den Fäden weiter reduziert, mehrere Fäden zu dem sogenannten Tau zusammengeführt und das Tau einem Kräuselungsprozess mittels einer Kräuselmaschine, die vorzugsweise nach dem Stauchkammerprinzip arbeitet, unterworfen. Zur Herstellung von Filtern für Tabakwaren wird dieses Tau durch ein konisches Maschinenteil geführt und so auf seine endgültige Dicke, also der Dicke des herzustellenden Filters komprimiert. Vor Einlauf in dieses konische Maschinenteil wird eine Glycerintriacetat enthaltende Zusammensetzung auf das Filtertau aufgebracht. Diese weitere Präparierung sorgt nach dem Verlassen des Komprimierteils durch Aushärten zu einer Fixierung des Filters in der gewünschten Form und Dicke.The manufacture of filters for tobacco products usually takes place after a process in which first a thread, which normally contains cellulose acetate, is produced by means of a spinning process, which is preferably the solvent spinning process.
In the acetone process, an acetone solution of cellulose acetate and matting agent TiO 2 is pressed through shower-like nozzles (spinnerets). The holes usually have cross sections in the form of an equilateral triangle. Below the spinnerets is a heated spin shaft. The air sucked through the spinning shaft heats up and absorbs the solvent which diffuses out of the formed filament, acetone, which almost is completely recovered. Here, the solution solidifies under considerable volume shrinkage to a filament. When using triangular holes, the filaments have a Y-section. When a thread composed of several filaments leaves the spinning shaft, the filaments in the thread are densely packed without, however, sticking to each other.
At the exit of the spinning shaft, the thread typically contains a residual fraction of about 1 to 6% by weight of acetone. Here, the thread is provided with a preparation (avivage), which serves mainly as a lubricant for the subsequent processing steps. This preparation is carried out by an oiler or by means of an applicator roll. In the subsequent steps, the content of acetone in the threads is first further reduced, a plurality of threads are combined to form the so-called rope and the rope is subjected to a crimping process by means of a crimping machine, which preferably works according to the stuffer box principle. To produce filters for tobacco products, this rope is passed through a conical machine part and thus compressed to its final thickness, ie the thickness of the filter to be produced. Before entering this conical machine part, a glycerol triacetate-containing composition is applied to the filter tow. This further preparation, after leaving the compression part by curing, fixes the filter in the desired shape and thickness.

Bei der Zusammenführung der Fäden zum Tau und der Komprimierung des Taus auf die endgültige Dicke dient die nach dem Trocknen der Fäden aufgebrachte Formulierung als Schmiermittel. Sie stellt u.a. sicher, dass die Reibung, die während der nachfolgenden Verarbeitungsschritte auftritt, einen Wert nicht überschreitet, der zum Abriß oder zu einer unerwünschten Erwärmung der Fäden bzw. des Taus führt. Beides würde unerwünschten Ausschuß bedingen. Zusätzlich werden durch das Schmiermittel höhere Maschinengeschwindigkeiten ermöglicht. Die Formulierung muss die bei diesem Prozess auftretenden hohen Scherkräfte ohne Wirkungsverlust überstehen.When merging the threads into the rope and compressing the rope to the final thickness, the formulation applied after the threads have dried acts as a lubricant. It ensures, inter alia, that the friction which occurs during the subsequent processing steps does not exceed a value which leads to the breakage or undesired heating of the threads or the rope. Both would cause unwanted rejects. In addition, the lubricant enables higher machine speeds. The formulation must withstand the high shear forces associated with this process without loss of effect.

Dieses Schmiermittel besteht üblicherweise aus einer Emulsion, die aus einer Mischung aus niedrigviskosem Mineralöl und Emulgator hergestellt wird. Weitere Komponenten können in der Emulsion enthalten sein.This lubricant usually consists of an emulsion which is prepared from a mixture of low-viscosity mineral oil and emulsifier. Other components may be included in the emulsion.

Die Mineralöle verbleiben nach der Herstellung der Filter und der entsprechenden Tabakwaren, die diese Filter enthalten, auf den Fäden.
Beim Rauchen z.B. einer Zigarette, die ein solches Filter enthält, kann ein Teil des Mineralöls, das sich auf dem Filter befindet, vom Raucher aufgenommen werden. Mitte der 90'er Jahre haben Baldwin et al. ( M.K. Baldwin et al.; "Feeding studies in rats with mineral hydrocarbon food grade white mineral oils", Toxicol. Pathol. 20, 426 (1992 )) sowie Smith et al. ( J.H. Smith et al.; "Ninety-day feeding study in Fischer 344-rats of highly refined petroleum-derived food-grade white oils and waxes", Toxicol. Pathol. 24, 214 (1996 )) 90-Tage-Verfütterungsstudien mit Fischer 344-Ratten durchgeführt und folgende pathologischen Merkmale gefunden: Zunahme des Gewichts und der Mineralölmenge in der Leber, Zunahme der Leberenzyme im Serum sowie Gewichtszunahme der Lymphknoten. Diese Effekte sind mit niedrigviskosen Mineralölen signifikant ausgeprägter als mit mittel- und hochviskosen Mineralölen. Hochviskose Mineralöle sind nach dem "Scientific Committee for Food" der europäischen Kommission dadurch gekennzeichnet, dass ihre Viskosität größer 8,5 mm2/s bei 100°C bzw. größer 70 mm2/s bei 40°C ist. In der EU (Directive 1999/91/EC of 23.11.1999 amending Directive 90/128/EEC "relating to plastic materials and articles intended to come into contact with foodstuff, OJ 310/41 (4.12.1999)) wird die Verwendung von niedrigviskosen Mineralölen für Produkte mit indirektem Lebensmittelkontakt nach 2002 nicht mehr erlaubt sein. Versuche, hochviskose Mineralöle in eine Formulierung einzuarbeiten, die den technischen Anforderungen des Herstellens von Filtermaterialien entsprechen, sind bislang gescheitert. Die Emulgatoren, die zur Emulgierung von niedrigviskosen Mineralölen eingesetzt werden, führen zu keiner stabilen und verarbeitbaren Formulierung, wenn hochviskose Mineralöle eingesetzt werden. Erschwerend kommt hinzu, dass an die Emulgatoren hohe Anforderungen in bezug auf die Lebensmittelunbedenklichkeit und eine eventuelle Veränderung des Geschmacks der Filterzigaretten gestellt werden.The mineral oils remain on the threads after the manufacture of the filters and the corresponding tobacco products containing these filters.
For example, when smoking a cigarette containing such a filter, some of the mineral oil that is on the filter may be absorbed by the smoker. In the mid 90's Baldwin et al. ( MK Baldwin et al .; "Feeding studies in council with mineral hydrocarbon grade grade white mineral oils", Toxicol. Pathol. 20, 426 (1992 )) as well as Smith et al. ( JH Smith et al .; "Ninety-day feeding study in Fischer's 344-rats highly refined petroleum-derived food-grade white oils and waxes", Toxicol. Pathol. 24, 214 (1996 )) 90-day feeding studies with Fischer 344 rats and found the following pathological features: increase in weight and amount of mineral oil in the liver, increase in liver enzymes in the serum and weight gain of the lymph nodes. These effects are significantly more pronounced with low-viscosity mineral oils than with medium- and high-viscosity mineral oils. According to the "Scientific Committee for Food" of the European Commission, high-viscosity mineral oils are characterized in that their viscosity is greater than 8.5 mm 2 / s at 100 ° C. or greater than 70 mm 2 / s at 40 ° C. In the EU (Directive 1999/91 / EC of 23.11.1999 amending Directive 90/128 / EEC "relating to plastic materials and articles intended to come into contact with food stuff, OJ 310/41 (4.12.1999)) the use of low-viscosity mineral oils are no longer permitted for products with indirect food contact after 2002. Attempts to incorporate highly viscous mineral oils in a formulation that meet the technical requirements of producing filter materials have so far failed: The emulsifiers used for emulsifying low-viscosity mineral oils This is compounded by the fact that high demands are placed on the emulsifiers in terms of food safety and a possible change in the taste of the filter cigarettes.

Die Aufgabe der vorliegenden Erfindung ist es, eine stabile und lagerfähige Emulsion bereit zu stellen, die hochviskose Mineralöle mit einer Viskosität von mindestens 8,5 mm2/s bei 100°C enthält. Hierzu ist es notwendig, Emulgatoren zur Herstellung einer verarbeitbaren Formulierung zu finden. Die Formulierung wird dann im Austausch gegen die verwendeten Formulierungen, die niedrigviskose Mineralöle enthalten, eingesetzt.The object of the present invention is to provide a stable and storable emulsion containing high viscosity mineral oils having a viscosity of at least 8.5 mm 2 / s at 100 ° C. For this it is necessary to find emulsifiers for the preparation of a processible formulation. The formulation is then used in exchange for the formulations containing low viscosity mineral oils.

Die Aufgabe der vorliegenden Erfindung wird durch eine Formulierung zur Verwendung als Präparation bei der Herstellung von Fäden enthaltend a) 30-80 Gew.-% eines Mineralöls mit einer Viskosität von mindestens 8,5 mm2/s bei 100°C und b) 11-60 Gew.-% eines Emulgators ausgewählt aus Sorbitanmonoester, Derivate von Sorbitanmonoestern, Sorbitandiestern, Derivate von Sorbitandiestern, Sorbitantriestern, Derivate von Sorbitantriestern, Polyglycerinestern, Derivate von Polyglycerinestern, Polyricinoleat, Derivate von Polyricinoleat und Mischungen derselben erreicht, wobei die Formulierung eine Wasser-in-Öl oder eine Öl-in-Wasser Emulsion ist.The object of the present invention is achieved by a formulation for use as a preparation in the production of threads containing a) 30-80 wt .-% of a mineral oil having a viscosity of at least 8.5 mm 2 / s at 100 ° C and b) 11 60% by weight of an emulsifier selected from sorbitan monoesters, derivatives of sorbitan monoesters, sorbitan diesters, derivatives of sorbitan diesters, sorbitan triesters, derivatives of sorbitan triesters, polyglycerol esters, derivatives of polyglycerol esters, polyricinoleate, derivatives of polyricinoleate and mixtures thereof, the formulation comprising a water in oil or an oil-in-water emulsion.

Unerwarteterweise zeigte sich, dass solche Formulierungen eine vergleichbare und teilweise sogar bessere Lager- und Verarbeitungsstabilität haben. Die Stabilität einer Formulierung, die als Emulsion vorliegen kann, lässt sich durch die Trübung der Formulierung bestimmen. Dabei gilt grundsätzlich, dass eine höhere Trübung eine geringere Stabilität anzeigt. Die Verarbeitungsstabilität der Formulierung lässt sich dadurch prüfen, indem die Trübung der Formulierung während der Verarbeitung überprüft wird. Dabei ist keine oder eine geringe Zunahme der Trübung besonders vorteilhaft, während eine stärkere Zunahme der Trübung auf eine nicht ausreichende Formulierungssstabilität schließen lässt. Die Lagerstabilität einer Formulierung lässt sich durch Überprüfung der Trübung nach z.B. fünf Tagen Lagerung bei 23°C überprüfen. Ist eine Zunahme der Trübung nach einer solchen Lagerzeit nicht feststellbar oder sehr gering, so ist die Lagerstabilität der Formulierung als sehr gut zu beurteilen, während eine Zunahme der Trübung bzw. ein eventuelles Entmischen der Phasen als schlechte Lagerstabilität zu charakterisieren ist.Unexpectedly, it has been found that such formulations have comparable and sometimes even better storage and processing stability. The stability of a formulation which may be in the form of an emulsion can be determined by the turbidity of the formulation. It basically applies that a higher turbidity indicates a lower stability. The processing stability of the formulation can be checked by checking the turbidity of the formulation during processing. No or little increase in turbidity is particularly advantageous, while a greater increase in turbidity indicates inadequate formulation stability. The storage stability of a formulation can be checked by checking the turbidity after, for example, five days storage at 23 ° C. If an increase in turbidity after such a storage time is not detectable or very low, then the storage stability of the formulation is to be assessed as very good, while an increase in turbidity or a possible segregation of the phases is to be characterized as poor storage stability.

Bei dem erfindungsgemäßen hochviskosen Mineralöl ist die Viskosität bei 100°C gemessen nach ASTM D 445 mindestens 8,5 mm2/s. Das eingesetzte Mineralöl hat bevorzugt eine Viskosität von 8,5 bis 1000, besonders bevorzugt von 8,5 bis 20 und ganz besonders bevorzugt von 8,5 bis 11 mm2/s.In the case of the high-viscosity mineral oil according to the invention, the viscosity at 100 ° C., measured according to ASTM D 445, is at least 8.5 mm 2 / s. The mineral oil used preferably has a viscosity of from 8.5 to 1000, particularly preferably from 8.5 to 20 and very particularly preferably from 8.5 to 11 mm 2 / s.

Es ist bevorzugt, dass der Anteil an Kohlenwasserstoffen in dem hochviskosen Mineralöl mit weniger als 25 Kohlenstoffatomen nicht mehr als 5 Gew.-% beträgt. Das mittlere Molekulargewicht des hochviskosen Mineralöls sollte nicht weniger als 480 g/mol betragen.It is preferable that the proportion of hydrocarbons in the high-viscosity mineral oil having less than 25 carbon atoms is not more than 5% by weight. The average molecular weight of the high-viscosity mineral oil should not be less than 480 g / mol.

Die erfindungsgemäß eingesetzten Emulgatoren sind ausgewählt aus Sorbitanmonoester, Derivate von Sorbitanmonoestern, Sorbitandiester, Derivate von Sorbitandiestern, Sorbitantriester, Derivate von Sorbitantriestern, Polyglycerinester, Derivate von Polyglycerinestern und Mischungen derselben. Die Ester können bevorzugt Ester mit Fettsäuren sein. Als Fettsäure können alle Fettsäuren verwendet werden, wie z.B. Stearinsäure, Ölsäure, Laurinsäure und Ricinolsäure ([R-(Z)]-12-Hydroxy-9-Octadecensäure). Die eingesetzten Fettsäuren können alternativ aus Mais, Baumwollöl, Palmöl, Erdnussöl, Sesamöl, Sojabohnenöl, Safloröl, Ricinusöl oder anderen Ölen nativer Herkunft gewonnen werden. Hierbei können die Fettsäuren hydriert oder nicht hydriert, sowie kondensiert oder nicht kondensiert vorliegen.The emulsifiers used according to the invention are selected from sorbitan monoesters, derivatives of sorbitan monoesters, sorbitan diesters, derivatives of sorbitan diesters, sorbitan triesters, derivatives of sorbitan triesters, polyglycerol esters, derivatives of polyglycerol esters and mixtures thereof. The esters may preferably be esters with fatty acids. As the fatty acid, all fatty acids can be used, such as e.g. Stearic acid, oleic acid, lauric acid and ricinoleic acid ([R (Z)] - 12-hydroxy-9-octadecenoic acid). The fatty acids used may alternatively be derived from corn, cottonseed oil, palm oil, peanut oil, sesame oil, soybean oil, safflower oil, castor oil or other oils of native origin. Here, the fatty acids can be hydrogenated or non-hydrogenated, and condensed or non-condensed.

Es ist bevorzugt, dass der Sorbitantriester ausgewählt wird aus der Gruppe Sorbitantriester mit Fettsäuren, die 10-25 Kohlenstoffatome enthalten, ethoxylierte Sorbitantriester mit Fettsäuren, die 10-25 Kohlenstoffe enthalten und 5-30 mol Ethylenoxideinheiten pro mol Sorbitantriester enthalten und Mischungen derselben. Besonders bevorzugt kann der Sorbitantriester ausgewählt werden aus der Gruppe Sorbitantristearat, ethoxyliertes Sorbitantristearat mit 5-30 mol Ethylenoxideinheiten pro Mol Sorbitantristearat, Sorbitantrioleat, ethoxyliertes Sorbitantrioleat mit 5-30 mol Ethylenoxideinheiten pro mol Sorbitantrioleat, Sorbitantrilaurat, ethoxyliertes Sorbitantrilaurat mit 5 bis 30 mol Ethylenoxideinheiten pro mol Sorbitantrilaurat und Mischungen derselben.It is preferred that the sorbitan triester be selected from the group consisting of sorbitan triesters with fatty acids containing 10-25 carbon atoms, ethoxylated sorbitan triesters with fatty acids containing 10-25 carbons and containing 5-30 moles of ethylene oxide units per mole of sorbitan triester, and mixtures thereof. More preferably, the sorbitan triester may be selected from the group consisting of sorbitan tristearate, ethoxylated sorbitan tristearate with 5-30 moles of ethylene oxide units per mole of sorbitan tristearate, sorbitan trioleate, ethoxylated sorbitan trioleate with 5-30 mole ethylene oxide units per mole sorbitan trioleate, sorbitan trilaurate, ethoxylated sorbitan trilaurate with 5-30 mole ethylene oxide units per mole Sorbitan trilaurate and mixtures thereof.

Wenn als Emulgator ein Polygylcerinester eingesetzt wird, dann kann der Polyglycerinesteranteil zusammengesetzt aus mindestens 75% Di-, Tri- und Tetraglycerinestern bestehen. Hierbei ist es bevorzugt, dass der Polyglycerinester ausgebildet wird aus der Gruppe Polyglycerinester mit Fettsäuren, die 10-25 Kohlenstoff atome enthalten, Derivate von Polyglycerinsäuren mit Fettsäuren, die 10-25 Kohlenstoffatome enthalten, Polyglycerin-Polyrizinoleat, Derivate von Polyglycerin-Polyrizinoleat und Mischungen derselben.If a polyglycerol ester is used as the emulsifier, then the Polyglycerinesteranteil may be composed of at least 75% di-, tri- and Tetraglycerinestern. Hereby it is preferred that the polyglycerol ester is formed from the group of polyglycerol esters with fatty acids containing 10-25 carbon atoms, derivatives of polyglyceric acids with fatty acids containing 10-25 carbon atoms, polyglycerol polyricinoleate, derivatives of polyglycerol polyricinoleate and mixtures thereof ,

In einer bevorzugten Ausführungsform enthält die Formulierung als Emulgator a) Sorbitantristearat oder ethoxyliertes Sorbitantristearat mit 5-30 mol Ethylenoxideinheiten pro mol Sorbitantristearat, b) Polyglycerin-Polyrizinoleat und c) Sorbitanmonolaurat und d) ethoxyliertes Sorbitanmonolaurat mit 5-30 mol Ethylenoxideinheiten pro mol Sorbitanmonolaurat und e) Sorbitanmonooleat.In a preferred embodiment, the formulation contains as emulsifier a) sorbitan tristearate or ethoxylated sorbitan tristearate with 5-30 mol ethylene oxide units per mole sorbitan tristearate, b) polyglycerol polyricinoleate and c) sorbitan monolaurate and d) ethoxylated sorbitan monolaurate with 5-30 mol ethylene oxide units per mole sorbitan monolaurate and e ) Sorbitan monooleate.

In einer weiteren Ausführungsform ist, falls der Emulgator als Mischung von mindestens zwei Emulgatoren vorliegt, bezogen auf das Gewicht der Formulierung 1 bis 15 Gew.-% ethoxyliertes Sorbitantristearat mit 5 bis 30 mol Ethylenoxideinheiten pro mol Sorbitantristearat in der Mischung der Emulgatoren und/oder bezogen auf das Gewicht der Formulierung 1 bis 15 Gew.-% Polyglyzerin-Polyricinoleat und/oder Polyricinoleat in der Mischung der Emulgatoren enthalten.In a further embodiment, if the emulsifier is present as a mixture of at least two emulsifiers, based on the weight of the formulation, 1 to 15% by weight of ethoxylated sorbitan tristearate with 5 to 30 mol of ethylene oxide units per mole of sorbitan tristearate in the mixture of emulsifiers and / or from 1 to 15% by weight of polyglycerol polyricinoleate and / or polyricinoleate in the mixture of emulsifiers.

Weiterhin ist bevorzugt, dass falls der Emulgator als Mischung von mindestens zwei Emulgatoren vorliegt, bezogen auf das Gewicht der Formulierung 1 bis 15 Gew.-% ethoxyliertes Sorbitanmonolaurat mit 5 bis 30 mol Ethylenoxideinheiten pro mol Sorbitanmonolaurat in der Mischung der Emulgatoren und/oder bezogen auf das Gewicht der Formulierung 1 bis 15 Gew.-% Sorbitanmonooleat mit 5 bis 30 mol Ethylenoxideinheiten pro mol Sorbitanmonooleat in der Mischung der Emulgatoren enthalten ist.It is further preferred if the emulsifier is present as a mixture of at least two emulsifiers, based on the weight of the formulation 1 to 15 wt .-% ethoxylated sorbitan monolaurate with 5 to 30 moles of ethylene oxide per mole of sorbitan monolaurate in the mixture of emulsifiers and / or based on the weight of the formulation contains from 1 to 15% by weight of sorbitan monooleate with from 5 to 30 mol of ethylene oxide units per mole of sorbitan monooleate in the mixture of emulsifiers.

Die erfindungsgemäße Formulierung enthält 30-80 Gew.% des Mineralöls, bevorzugt 40-80 Gew.-%, besonders bevorzugt 45-75 Gew.-% und ganz besonders bevorzugt 55-72 Gew.% des Mineralöls.The formulation of the invention contains 30-80 wt.% Of the mineral oil, preferably 40-80 wt .-%, particularly preferably 45-75 wt .-% and most preferably 55-72 wt.% Of the mineral oil.

In der Formulierung sind bevorzugt 15-60 Gew.-% des Emulgators, weiter bevorzugt 20-60 Gew.-%, besonders bevorzugt 25-55 Gew.-% des Emulgators, vorhanden.The formulation preferably contains 15-60% by weight of the emulsifier, more preferably 20-60% by weight, particularly preferably 25-55% by weight of the emulsifier.

Die erfindungsgemäße Formulierung ist eine Wasser-in-Öl oder eine Öl-in-Wasser-Emulsion. Die erfindungsgemäße Formulierung wird nach dem Spinnvorgang in Emulsionsform auf die Oberfläche der Fäden, die zu Filtern für Tabakwaren verarbeitet werden, aufgebracht. Bei dieser Verarbeitung verbleibt das Mineralöl auf der Oberfläche der Fäden bzw. des Taus. Es ist bevorzugt, dass die verwendeten Fäden Celluloseacetat enthalten, das im Mittel 1,5 bis 3 Acetatgruppen pro Celluloseeinheit enthält.The formulation according to the invention is a water-in-oil or an oil-in-water emulsion. The formulation according to the invention is applied after the spinning process in emulsion form on the surface of the threads, which are processed into filters for tobacco products. In this processing, the mineral oil remains on the surface of the threads or the dew. It is preferred that the filaments used contain cellulose acetate containing on average 1.5 to 3 acetate groups per unit cellulose.

Unter der Bezeichnung Fäden sind im Sinne dieser Erfindung auch Fasern zu verstehen, die nach dem hier beschriebenen Verfahren hergestellt werden können.For the purposes of this invention, the term filaments also means fibers which can be produced by the process described here.

Aus diesen Fäden lassen sich Filter für Tabakwaren herstellen. Hierbei ist es bevorzugt, dass die Filter Zigarettenfilter sind. Bei allen Arbeitsschritten verbleibt die aufgebrachte Emulsion auf den Fäden und somit auf dem Tau. Somit ist die Emulsion zu einem gewissen Anteil auch noch in den Filtern für Tabakwaren und den Tabakwaren selbst vorhanden.From these threads can be produced filters for tobacco products. It is preferred that the filters are cigarette filters. In all operations, the applied emulsion remains on the threads and thus on the rope. Thus, to a certain extent, the emulsion is still present in the filters for tobacco products and the tobacco itself.

Die erfindungsgemäße Emulsion wird an folgenden Beispielen erläutert, ohne jedoch auf diese Beispiele beschränkt zu sein.The emulsion according to the invention is illustrated by the following examples, but without being limited to these examples.

BeispieleExamples

Tabelle 1Table 1 Komponentencomponents Formulierung 1 [Gew.-%]Formulation 1 [% by weight] Formulierung 2 [Gew.-%]Formulation 2 [% by weight] Mineralöl Primol® 3521 Mineral oil Primol ® 352 1 64,5064,50 60,0060,00 Sorbitanmonolaurat + 20 EO2 Sorbitan monolaurate + 20 EO 2 12,8012,80 11,6011,60 Sorbitanmonolauratsorbitan 8,208.20 13,0013,00 Sorbitantristearat + 20 EO2 Sorbitan tristearate + 20 EO 2 --- 4,404.40 Polyglycerin-PolyrizinoleatPolyglycerol polyricinoleate 3,103.10 3,003.00 Sorbitanmonooleatsorbitan 5,775.77 --- Wasserwater Restrest Restrest 1Primol® 352 ist ein hochviskoses Mineralöl der ESSO AG Viskosität nach ASTM D 445: 71 mm2/s bei 40°C, 9,0 mm2/s bei 100°C
2 + 20 EO bedeutet 20 mol Ethylenoxideinheiten pro mol Ester 1 Primol ® 352 is a high viscosity mineral oil of ESSO AG viscosity according to ASTM D 445: 71 mm 2 / s at 40 ° C, 9.0 mm 2 / s at 100 ° C
2 + 20 EO means 20 moles of ethylene oxide units per mole of ester

Die Formulierungen 1 und 2 aus Tabelle 1 enthalten beide die erfindungsgemäße Kombination aus einem Mineralöl mit einer Viskosität von wenigstens 8,5 mm2/s bei 100°C und dem erfindungsgemäßen Emulgator. Die Emulsionen lassen sich nach Standardmethoden herstellen.
Zur Herstellung der Formulierung 1 wird Primol 352 bei Raumtemperatur vorgelegt und unter ständigem Rühren werden die Rohstoffe in der Reihenfolge Sorbitanmonolaurat, Sorbitanmonolaurat + 20 EO, Sorbitanmonooleat, Polyglyzerin-Polyricinoleat und Wasser zugegeben. Formulierung 1 wird für weitere 30 Minuten gerührt.
Zur Herstellung der Formulierung 2 wird auf 50°C erwärmtes Primol 352 in einem Rührer vorgelegt. Unter ständigem Rühren und bei 50°C werden die weiteren Rohstoffe in der Reihenfolge Sorbitanmonolaurat, Sorbitanmonolaurat + 20 EO, Sorbitantristearat + 20 EO, Polyglycerin-Polyrizinoleat und Wasser zugegeben. Nach 30 Minuten rühren bei 50 °C lässt man die Formulierung auf Raumtemperatur abkühlen und rührt sie bei dieser Temperatur für weitere 30 Minuten.Formulations 1 and 2 from Table 1 both contain the combination according to the invention of a mineral oil having a viscosity of at least 8.5 mm 2 / s at 100 ° C. and the emulsifier according to the invention. The emulsions can be prepared by standard methods.
To prepare Formulation 1, Primol 352 is initially charged at room temperature and, while stirring continuously, the raw materials are added in the order of sorbitan monolaurate, sorbitan monolaurate + 20 EO, sorbitan monooleate, polyglycerol polyricinoleate and water. Formulation 1 is stirred for a further 30 minutes.
To prepare formulation 2, primer 352 heated to 50 ° C. is initially charged in a stirrer. With continuous stirring and at 50 ° C, the further raw materials are added in the order of sorbitan monolaurate, sorbitan monolaurate + 20 EO, sorbitan tristearate + 20 EO, polyglycerol polyricinoleate and water. After stirring for 30 minutes at 50 ° C, the formulation is allowed to cool to room temperature and stirred at this temperature for a further 30 minutes.

Beide Formulierungen werden zur Herstellung von Celluloseacetatfäden nach dem Lösungsmittelspinnverfahren eingesetzt. Hierbei zeigte sich bei der Herstellung der Fäden kein negativer Einfluss der erfindungsgemäß eingesetzten Formulierungen. Formulierung 1 und Formulierung 2 zeigen eine Lagerstabilität bei 23°C und fünf Tagen, die mit den üblicherweise eingesetzten Formulierungen vergleichbar ist und während der Verarbeitung der Fäden zu Filtern trat keine Zunahme der Trübung der Emulsion bedingt durch auftretende Scherkräfte ein. Beide Formulierungen verhielten sich vergleichbar mit den üblicherweise eingesetzten Formulierungen. Both formulations are used to produce cellulose acetate filaments by the solvent spinning method. In this case, no negative influence of the formulations according to the invention was shown in the production of the threads. Formulation 1 and Formulation 2 show storage stability at 23 ° C and five days, comparable to the formulations commonly used, and no increase in clouding of the emulsion due to shear forces occurred during processing of the filaments into filters. Both formulations behaved similarly to the commonly used formulations.

Claims (14)

  1. Formulation for use as a lubricant in the manufacture of yarns, containing:
    a) 30 to 80 % by weight of a mineral oil having a viscosity of at least 8.5 mm2/s at 100 °C, and
    b) 11 to 60 % by weight of an emulsifier selected from sorbitan monoesters, derivatives of sorbitan monoesters, sorbitan diesters, derivatives of sorbitan diesters, sorbitan triesters, derivatives of sorbitan triesters, polyglycerol esters, derivatives of polyglycerol esters, polyricinoleate, derivatives of polyricinoleate and mixtures thereof; and further characterised in that
    the formulation is a water-in-oil or an oil-in-water emulsion.
  2. Formulation according to claim 1, characterised in that the sorbitan triester is selected from the group containing sorbitan triesters having fatty acids which comprise 10 to 25 carbon atoms, ethoxylated sorbitan triesters having fatty acids which comprise 10 to 25 carbon atoms and comprise 5 to 30 mol ethylene oxide units per mol sorbitan triester, and mixtures thereof.
  3. Formulation according to claim 2, characterised in that the sorbitan triester is selected from the group containing sorbitan tristearate, ethoxylated sorbitan tristearate comprising 5 to 30 mol ethylene oxide units per mol sorbitan tristearate, sorbitan trioleate, ethoxylated sorbitan trioleate comprising 5 to 30 mol ethylene oxide units per mol sorbitan trioleate, sorbitan trilaurate, ethoxylated sorbitan trilaurate comprising 5 to 30 mol ethylene oxide units per mol sorbitan trilaurate, and mixtures thereof.
  4. Formulation according to claim 1, characterised in that the polyglycerol ester is selected from the group containing polyglycerol ester having fatty acids which comprise 10 to 25 carbon atoms, derivatives of polyglycerol ester having fatty acids which comprise 10 to 25 carbon atoms, polyglycerol polyricinoleate, derivatives of polyglycerol polyricinoleate, and mixtures thereof.
  5. Formulation according to one or more of claims 1 to 4, characterised in that the emulsion comprises 15 to 60 % by weight of emulsifier.
  6. Formulation according to one or more of claims 1 to 5, characterised in that said formulation comprises as emulsifiers:
    a) sorbitan tristearate or ethoxylated sorbitan tristearate comprising 5 to 30 mol ethylene oxide units per mol sorbitan tristearate,
    b) polyglycerol polyricinoleate
    c) sorbitan monolaurate
    d) ethoxylated sorbitan monolaurate comprising 5 to 30 mol ethylene oxide units per mol sorbitan monolaurate, and
    e) sorbitan monooleate.
  7. Formulation according to one or more of claims 1 to 6, characterised in that if the emulsifier is in the form of a mixture of at least two emulsifiers, then 1 to 15 % by weight, based on the weight of the formulation, of ethoxylated sorbitan tristearate having 5 to 30 mol ethylene oxide units per mol sorbitan tristearate is included in the mixture of emulsifiers and/or 1 to 15 % by weight, based on the weight of the formulation, of polyglycerol polyricinoleate and/or polyricinoleate is included in the mixture of emulsifiers.
  8. Formulation according to one or more of claims 1 to 7, characterised in that if the emulsifier is in the form of a mixture of at least two emulsifiers, then 1 to 15 % by weight, based on the weight of the formulation, of ethoxylated sorbitan monolaurate having 5 to 30 mol ethylene oxide units per mol sorbitan monooleate is included in the mixture of emulsifiers and/or 1 to 15 % by weight, based on the weight of the formulation, of sorbitan monooleate having 5 to 30 mol ethylene oxide units per mol sorbitan monolaurate is included in the mixture of emulsifiers.
  9. Formulation according to claim 1, characterised in that the mineral oil has a viscosity of 8.5 to 1000 mm2/s at 100 °C.
  10. Yarns obtained by a spinning method, wherein the yarns are prepared, subsequent to spinning, with the formulation according to one or more of claims 1 to 9 as a lubricant which is applied to the surface of the yarn.
  11. Yarns according to claim 10, characterised in that the yarns comprise cellulose acetate with an average of 1.5 to 3 acetate groups per cellulose unit.
  12. Cigarette filter, comprising yarns according to either claim 10 or claim 11.
  13. Use of the formulation according to one or more of claims 1 to 9 as a lubricant in the manufacture of yarns for filters for tobacco products.
  14. Use of the formulation according to claim 13, characterised in that the yarns are used for manufacturing cigarette filters.
EP03732455A 2002-07-11 2003-05-24 Formulation of a highly viscous mineral oil for the production of filters for tobacco Expired - Lifetime EP1530657B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP03732455A EP1530657B1 (en) 2002-07-11 2003-05-24 Formulation of a highly viscous mineral oil for the production of filters for tobacco

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
EP02015405 2002-07-11
EP02015405A EP1380684A1 (en) 2002-07-11 2002-07-11 Formulation of a high viscosity mineral oil for the production of filters for tobacco articles
EP03732455A EP1530657B1 (en) 2002-07-11 2003-05-24 Formulation of a highly viscous mineral oil for the production of filters for tobacco
PCT/EP2003/005440 WO2004007831A1 (en) 2002-07-11 2003-05-24 Formulation of a highly viscous mineral oil for the production of filters for tobacco

Publications (2)

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EP1530657A1 EP1530657A1 (en) 2005-05-18
EP1530657B1 true EP1530657B1 (en) 2010-04-28

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EP02015405A Withdrawn EP1380684A1 (en) 2002-07-11 2002-07-11 Formulation of a high viscosity mineral oil for the production of filters for tobacco articles
EP03732455A Expired - Lifetime EP1530657B1 (en) 2002-07-11 2003-05-24 Formulation of a highly viscous mineral oil for the production of filters for tobacco

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EP02015405A Withdrawn EP1380684A1 (en) 2002-07-11 2002-07-11 Formulation of a high viscosity mineral oil for the production of filters for tobacco articles

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US (1) US7153447B2 (en)
EP (2) EP1380684A1 (en)
AT (1) ATE466130T1 (en)
AU (1) AU2003238389A1 (en)
DE (1) DE50312667D1 (en)
WO (1) WO2004007831A1 (en)

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EP3409829B1 (en) * 2017-05-30 2020-08-12 Rhodia Acetow GmbH Composition comprising hydrocarbons, emulsifiers and water, its use and products comprising such composition

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Also Published As

Publication number Publication date
WO2004007831A1 (en) 2004-01-22
ATE466130T1 (en) 2010-05-15
EP1530657A1 (en) 2005-05-18
DE50312667D1 (en) 2010-06-10
US7153447B2 (en) 2006-12-26
US20040007687A1 (en) 2004-01-15
EP1380684A1 (en) 2004-01-14
AU2003238389A1 (en) 2004-02-02

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