EP0885321B1 - Non-tisse de fusion-soufflage, son procede de production et ses utilisations - Google Patents

Non-tisse de fusion-soufflage, son procede de production et ses utilisations Download PDF

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Publication number
EP0885321B1
EP0885321B1 EP96944588A EP96944588A EP0885321B1 EP 0885321 B1 EP0885321 B1 EP 0885321B1 EP 96944588 A EP96944588 A EP 96944588A EP 96944588 A EP96944588 A EP 96944588A EP 0885321 B1 EP0885321 B1 EP 0885321B1
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EP
European Patent Office
Prior art keywords
melt
plasticizer
blown
blown web
web
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
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EP96944588A
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German (de)
English (en)
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EP0885321A1 (fr
Inventor
Günter Maurer
Paul Rustemeyer
Eberhard Teufel
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Cerdia Produktions GmbH
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Rhodia Acetow GmbH
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Classifications

    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/013—Regenerated cellulose series
    • 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
    • A24D3/067—Use of materials for tobacco smoke filters characterised by functional properties
    • A24D3/068—Biodegradable or disintegrable
    • 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
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/425—Cellulose series
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/02—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments
    • D04H3/07—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments otherwise than in a plane, e.g. in a tubular way
    • D04H3/077—Stick, rod or solid cylinder shaped
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
    • D04H3/16—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between thermoplastic filaments produced in association with filament formation, e.g. immediately following extrusion
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913—Rod, strand, filament or fiber
    • Y10T428/298—Physical dimension
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
    • Y10T442/60—Nonwoven fabric [i.e., nonwoven strand or fiber material]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
    • Y10T442/60—Nonwoven fabric [i.e., nonwoven strand or fiber material]
    • Y10T442/603—Including strand or fiber material precoated with other than free metal or alloy
    • Y10T442/607—Strand or fiber material is synthetic polymer
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
    • Y10T442/60—Nonwoven fabric [i.e., nonwoven strand or fiber material]
    • Y10T442/659—Including an additional nonwoven fabric
    • Y10T442/668—Separate nonwoven fabric layers comprise chemically different strand or fiber material
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
    • Y10T442/60—Nonwoven fabric [i.e., nonwoven strand or fiber material]
    • Y10T442/68—Melt-blown nonwoven fabric

Definitions

  • the invention relates to a melt-blown fleece based on cellulose esters, especially of cellulose acetate. with fibers with an average fiber diameter of less than about 10 ⁇ m, a method particularly suitable for its production, and advantageous uses of the melt-blown nonwoven.
  • a material is referred to as a nonwoven fabric if a) the fiber content is more than 50% by weight (except chemically digested vegetable fibers) and the fibers have a slenderness ratio of greater than 300 or b) the following conditions are met: 1) the fiber content is more than 30 % By weight (except chemically digested plant fibers) and the fibers have a slenderness ratio greater than 300 and 2) the density is less than 0.40 g / cm 3 .
  • melt-blown process can, without wishing to see any limitation here, represent as follows; i.e., the melt blown filaments, fibers and nonwovens generally generated as follows:
  • the respective plastic is placed in an extruder in which it is melted becomes.
  • the melt reaches the spinning head, which is the melt-blown nozzle includes, which is a central part of the process.
  • the melt is on the brought required processing temperature.
  • the nozzle itself contains a number of Capillary holes. There are openings for on both sides of the nozzle bores the pressurized primary process air.
  • There is a deposit device underneath the nozzle arranged in the form of a driven sieve belt or a sieve drum which the fibers are sucked in and deposited into a fleece.
  • US Pat. No. 4,869,275 also addresses the melt-blown process for producing a nonwoven from various starting materials.
  • Suitable starting materials are polyolefins (polypropylene, polyethylene and ethylene / propylene copolymers), polystyrene, polyester (polyethylene terephthalate), nylon (6, 66 and 610), polymethylene methacrylates and generally also cellulose acetate.
  • This patent does not contain any statements as to what degree of substitution this cellulose acetate has when it is used in the process described. Even the unusual indication that even cellulose acetate is suitable ("even cellulose acetate" / see column 5, paragraph 1) indicates that this is only of limited suitability.
  • cellulose acetate is not taken into account in the description of the particularly practical embodiments. Due to the decomposition of cellulose acetate, which can be expected by the known method, the quality of the melt-blown nonwoven obtained would also deteriorate insofar as a satisfactory degree of whiteness does not develop. With regard to the decomposition of cellulose acetates at higher temperatures, it should be noted that a noticeable chemical decomposition occurs from 180 ° C., which can be recognized by the formation of furfural, among other things.
  • the invention The task is to develop a melt-blown fleece of the type described at the outset in such a way that it is not thermoplastic up to a temperature of about 180 ° C, one has a desirably high reflection factor or whiteness and, if desired, advantageous filter materials, in particular filter materials of cigarettes and can be used for the filtration of gases or liquids, in particular blood.
  • the invention proposes a particularly advantageous method for Production of such a melt-blown nonwoven.
  • this object is achieved in that it is about 0 to 10% by mass contains an extractable plasticizer, a reflection factor (R ⁇ ), determined by DIN 53 145 Part 1 (1992), of more than about 60% and the cellulose ester one Degree of substitution DS has from about 1.5 to 3.0.
  • R ⁇ reflection factor
  • the invention thus provides access to melt-blown nonwovens made from cellulose esters that have little or even contain no plasticizer, which was not previously thought possible could.
  • the melt-blown fleece according to the invention contains fibers from cellulose esters. It can it is, for example, cellulose acetate, acetobutyrate, acetopropionate and propionate and the like. Cellulose acetate is preferred.
  • the degree of substitution DS of the cellulose esters used according to the invention is between about 1.5 to 3.0, especially between about 1.7 to 2.7, the range being about 2.2 to 2.6 is very particularly preferred. If the value falls below 1.5, then damage to the polymer structure through dehydration is to be feared. Though The desired success can also be achieved with a degree of substitution of approximately 3.0 achieve, however, at this value an undesirable crystallization and Phase separation occur. These undesirable disadvantages can be overcome with a encountered higher extractable plasticizer content of up to about 10% by mass become. However, if a lower plasticizer content is aimed for, then it is advantageous, at the same time the degree of substitution DS to at least about 2.7, in particular lower at least about 2.6.
  • melt-blown fleece according to the invention only up to about 10% by mass, in particular about 2 to 8% by mass of an extractable plasticizer, especially in the form of a water extractable plasticizer.
  • the invention thus carries the relevant Intended uses where the amount of plasticizer is not too high may, since the product otherwise dominates undesirably through the plasticizer becomes. Rather, the product properties are said to be largely based on the cellulose ester go back.
  • the exact setting of the plasticizer content within the specified range of about 0 to 10% by mass depends on the respective Purpose of the fleece. Accordingly, it is left to the skilled person here in individual cases quantitatively increase the amount of plasticizer within the scope of the invention optimize.
  • plasticizer content of about 5 to 10 % By mass, especially if triacetin is used as plasticizer becomes. So it is known that triacetin affects the taste of tobacco smoke and the specific retentions of cellulose acetate positively influenced. Over 10% by mass any plasticizer content would adversely affect the usage properties limit that the melting point is too low and plasticizer migration sweating and exhalation and also undesirable Bonding can occur. Furthermore, in the case of use in filter rods A high plasticizer content has a negative impact on the filter rod hardness. At Applications that are subject to food law regulations will Plasticizer content kept as low as possible within the scope of the invention, especially set to near 0. The same applies to medical applications such as e.g. in blood filters.
  • the plasticizer used in the invention must not only have a plasticizing effect unfold. Rather, the plasticizer made from the melt-blown fleece, that after the completion of the manufacturing process a content above 10% by mass contains plasticizers, so far can be extracted with a suitable solvent, that the frame according to the invention is set from about 0 to 10% by mass.
  • the cellulose ester fibers in their chemical and physical structure remain largely unchanged.
  • Plasticizers have proven to be suitable Triacetin, ethylene and propylene carbonate, citric acid triethyl ester, triethylene glycol diacetate, Carbowax® (polyethylene glycols with a MW from 200 to 14000, manufactured by from UCC, USA) and / or sulfolane (tetrahydrothiophene-1,1-dioxide).
  • Triacetin is particularly useful because it is quick and effective with Water can be extracted.
  • the degree of polymerization DP of the cellulose esters mentioned, in particular the Cellulose acetate is not critical and can be in a relatively wide range. It However, particularly advantageous results are achieved if it is between about 150 to 400, in particular between about 180 to 350. When falling below one Degree of polymerization of about 150 would result in too high a proportion of oligomers are present, so that when extracting the plasticizer a large part of the Cellulose ester would be extracted. If the upper limit of about 400 is exceeded, then the melt index in the melt blown process explained below becomes high, which would adversely affect this. This problem could arise reducing in individual cases by increasing the plasticizer content, this would but mean additional effort in realizing the invention, especially in connection with the removal or recovery of the Plasticizer.
  • a minimum reflection factor, also called whiteness, of Fleece is determined according to DIN 53 145 Part 1 (1992) measured according to ISO 2469 (1977).
  • an Elrepho device from Zeiss used. A fleece sample placed in 8 layers is combined with one Ullbrichtkugel diffusely exposed and perpendicular to the sample plane (measuring geometry d / 0) 457 nm measured (using a spectral band filter).
  • a minimum reflection factor also called whiteness
  • the reflection factor or whiteness is included in the scope of the invention more than 60%, especially more than 70% or even about 90%.
  • the whiteness is in particular a measure of the purity of the product according to the invention. Any this is brownish or yellowish, which means that in the production undesirable and uncontrollable decomposition products have arisen.
  • the Customers would therefore use such a product if used in the Reject cigarette industry.
  • the disadvantage of one unsatisfactory degrees of whiteness not even by incorporating white pigments, such as titanium dioxide, are eliminated during the manufacturing process. It is consequently a particularly clear statement about the chemical purity of the cellulose ester fibers. This aspect plays an outstanding role in different areas, so for example when using the fleece in the bio-medical field, in particular in blood filtration.
  • the cellulose acetate in the form of a Polymer blends especially with aliphatic polyesters and / or acetylated starches, is present.
  • This can not only optimize the desired properties, such as for example the biodegradability associated with aliphatic Polyesters (cf. DE-C-39 14 022), but there is also the Possibility of saving costs. This arises in another area of application from EP-A-0 622 407, to which reference is made.
  • the fiber diameter as is generally obtained by the melt-blown process, below about 10 microns lie, in particular between about 2 to 8 microns.
  • the standard diameter one by one Filament obtained by the dry spinning process is generally between about 15 and 40 ⁇ m. Fibers of a smaller diameter have the advantage that they a larger specific surface and thus also a greater activity in the desired fields of application, especially in the field of filtration.
  • As part of the Invention can be easily fibers of an average fiber diameter of set less than about 8 ⁇ m.
  • the particularly advantageous practical area lies between about 5 and 8 ⁇ m.
  • the fiber diameter is the middle one Diameter. Here, a number of fibers are measured by scanning electron microscopy and then averaged.
  • melt obtained, if desired, active substances added such as Agro actives, pharmaceutical actives, selective and others Filtration aids, e.g. for selective retention, flavorings, additives for biological Degradability, etc. They are preferably compatible with the melt.
  • the melt-blown fleece according to the invention can advantageously be produced by that a cellulose ester, especially cellulose acetate, a degree of substitution DS of about 1.5 to 3.0, especially about 1.7 to 2.7, with a plasticizer in one Mass ratio of about 2: 1 to 1: 4 mixed with heating and melted is transferred, the mixture of plasticizer and cellulose ester Melt index MFI (210 / 2.16) according to DIN 53 735 from about 400 to 5 g / 10 min, in particular 300 to 50 g / 10 min, the melt in a melt-blown spinning device processed into a melt-blown fleece and then the Plasticizers up to a proportion of about 0 to 10% by mass with a solvent for the plasticizer is extracted.
  • a cellulose ester especially cellulose acetate, a degree of substitution DS of about 1.5 to 3.0, especially about 1.7 to 2.7
  • a plasticizer in one Mass ratio of about 2: 1 to 1: 4 mixed with heating and melted is transferred
  • these are preferably at a temperature of more than about 100 ° C. warmed up.
  • the particularly suitable melting temperature depends on the individual case and leaves determine yourself by a specialist purely by hand. However, a temperature of 240 ° C must not be exceeded, otherwise undesirable signs of decomposition occur.
  • the melt-blown nonwoven obtained according to the invention has a low, as shown Share of extractable plasticizer from about 0 to 10% by mass.
  • Share of extractable plasticizer from about 0 to 10% by mass.
  • Through the Process control according to the invention is a decomposition of the cellulose ester used largely excluded. It is not necessary to avoid undesirable oxidative processes to work in a protective gas atmosphere.
  • the melt uses the melt-blown process immediately after its production is subjected, since otherwise undesirable degradation reactions occur can.
  • a particular advantage of the method according to the invention is that it can be done continuously. This is how mixing and spinning takes place advantageously in a single operation, by mixing the extruder is immediately fed to the melt-blown nozzle.
  • the method according to the invention provides thus represents a significant simplification in terms of procedural management.
  • the mass ratio of plasticizer to cellulose ester is about 3: 2 to 2: 3, consequently, in the practical embodiment, preferably set to about 1: 1 becomes, which also corresponds to the requirement of US Pat. No. 3,509,009.
  • a suitable solvent for the Provides plasticizers Accordingly, according to the invention, a solvent is used for Extraction of the plasticizer used, however, the chemical and physical Structure of the cellulose ester fibers is not affected.
  • the method according to the invention is then in the melt-blown spinning device controlled particularly advantageously when the on the spinneret and the spinning head Spinning device a temperature of about 180 to 240 ° C, in particular of about 200 up to 230 ° C. If the value falls below about 180 ° C, then can that lead to an insufficient fineness of the process product. At If the upper limit of 240 ° C is exceeded, undesired degradation begins.
  • plasticizers which can be used in the context of the invention have already been mentioned above discussed, in particular on the advantageous use of water-extractable Plasticizer in the form of triacetin.
  • a water extractable The melt-blown fleece obtained is used to extract the plasticizer Plasticizer simply passed into a water bath.
  • the method according to the invention can run here with the particular advantage that a normal water bath (about Room temperature), i.e. can be used for extraction without heating.
  • a hot extract bath even from Disadvantage, since the melt-blown fleece then has such a melting range that whose structure is impaired or even destroyed.
  • the fleece leaving the melt-blown spinning device on a storage device in particular in the form of a sieve or sieve belt or a sieve drum, transferred, pressed to set the desired strength and then the plasticizer is extracted.
  • a storage device in particular in the form of a sieve or sieve belt or a sieve drum
  • the melt-blown fleece can be ordered from Presses can also be structured. The structuring is done in order for the later To obtain use advantageous structure, for example in the case of use Longitudinal corrugation in cigarette filters combined with an increase in surface area.
  • melt-blown fleece filaments in particular cellulose acetate filaments
  • melt-blown fleece leaving the spinning device to form a composite structure on a carrier, in particular in Form of a fleece from a cellulose acetate filter tow, a flat one Filtertow or made of paper.
  • a carrier fleece the person skilled in the art, depending on the end use, the suitable fleece determine easily.
  • the Melt-blown fleece according to the invention in filter cigarettes preferably by one Go out cellulose acetate fleece. Any closed ones are also possible Carriers, such as the paper already mentioned.
  • the respectively received Composite structures can advantageously be pressed and / or to regulate their strength be structured.
  • a particular advantage of the method according to the invention is that the Desired melt-blown nonwoven can be made without it being special Additives, such as any processing aids, are required.
  • the melt-blown nonwoven according to the invention is suitable particularly advantageous as a filter material.
  • the fleece is e.g. in Tobacco smoke filters, especially in cigarette filters, and especially in double filters for ultralight cigarettes, for the filtration of gases and liquids, such as Sterile filtration of beverages and particularly advantageous for the filtration of blood used.
  • melt-blown fleece according to the invention is used in cigarette filters, then these can be easily disintegrated. Furthermore, a low degree of substitution DS leads Cellulose esters, especially cellulose acetate, at a particularly favorable price biodegradability.
  • the filter materials according to the invention not only show a better filtering effect than the previously known materials, but they also fully meet the taste requirements. This is especially true for cellulose acetate in Connection with a residual content of triacetin plasticizer.
  • Cellulose acetate with a DP of 220 and a DS of 2.5 was added by means of a gravimetric metering device into the filling opening of the 1st zone of a co-rotating 2-screw laboratory extruder with a screw diameter of 25 mm, a length of 48 D and 15 zones.
  • triacetin was supplied as a plasticizer in a ratio of 2: 3 (1: 1.5) using a reciprocating pump.
  • the temperatures of zones 5-11 were 150 and zones 12-15 175 ° C.
  • a homogeneous melt was obtained at a screw speed of 150 rpm.
  • the melt obtained in this way was continuously transferred into a strand via a round die, and the strand was cooled below the melting temperature and comminuted into cylindrical granules of 2 mm in diameter and 3 mm in length with the aid of a strand granulator.
  • the granules thus obtained were fed to a melt-blown laboratory spinning device consisting of extruder, intermediate block, melting tube, spinneret nozzle, hot air device, tray and winder.
  • the temperatures in the extruder of the melt-blown laboratory spinning device were increased from 100 ° C at the inlet to 170 ° C at the extruder outlet.
  • the intermediate block and the melting tube were set to 200 ° C.
  • the temperature in the spinning head was 230 ° C.
  • the air temperature was 265 ° C.
  • the air volume was set to 70 m 3 / h. These process parameters resulted in a melt pressure of 125 bar.
  • the mass throughput was 7.7 kg / h.
  • the fibers produced with the spinning device were placed on a storage belt and continuously drawn off under the spinning device in such a way that a weight per unit area of 132 g / m 2 was obtained.
  • the fleece was wound up into a roll by means of a winding device.
  • the fleece roll was then fed to a washing device filled with water consisting of two troughs connected in series and the plasticizer contained in the fleece was washed out to a residual content of 0.3%.
  • the fleece was then dried with a drying device at 160 ° C. to a residual moisture content of 4.8%.
  • the average fiber diameter of the fleece thus obtained was 8.4 ⁇ m.
  • the reflection factor (R ⁇ ) based on the barium sulfate white standard, was 65%.
  • Cellulose acetate with a DP of 220 and a DS of 2.5 was added by means of a gravimetric metering device into the filling opening of the 1st zone of a co-rotating 2-screw laboratory extruder with a screw diameter of 25 mm, a length of 48 D and 15 zones.
  • triacetin was supplied as a plasticizer in a ratio of 3: 2 (1.5: 1.0) using a reciprocating pump.
  • the temperatures in the 1st and 2nd zone were 50 in the 3rd 100 and in the 4th zone 120 ° C.
  • the temperatures of zones 5-10 were 140 and zones 11-15 150 ° C.
  • the mass throughput was 3.2 kg / h.
  • a homogeneous melt was obtained at a screw speed of 190 rpm.
  • the melt obtained in this way was fed directly to a laboratory melt-blown spinning device described in Example 1, which, in contrast to Example 1, no longer required an extruder since the material to be processed was already in the form of a melt.
  • the melt-blown spinning unit was connected directly after the co-rotating twin-screw laboratory extruder.
  • the intermediate block and the melting tube were set to 170 ° C.
  • the temperature in the spinneret nozzle was 210 ° C, air temperature 255 ° C.
  • the air volume was set to 60 m 3 / h. With these process parameters, a melt pressure of only 73 bar was established.
  • the fibers produced with the spinning device were placed on a storage belt and continuously drawn off under the spinning device in such a way that a weight per unit area of 176 g / m 2 resulted.
  • the fleece obtained in this way was fed directly into a washing device as described in Example 1 and the plasticizer contained in the fleece was washed out to a residual content of 5.5%.
  • the fleece was then dried with a drying device at 150 ° C. to a residual moisture content of 6.3%.
  • the average fiber diameter of the fleece thus obtained was 5.7 ⁇ m.
  • the reflection factor (R ⁇ ) was 74% based on the barium sulfate white standard.

Claims (27)

  1. Voile melt-blown à base d'esters de cellulose, notamment d'acétate de cellulose, comportant des fibres ayant un diamètre moyen de moins d'environ 10 µm, caractérisé en ce qu'il contient environ 0 à 10 % en masse d'un plastifiant extractible, il présente un facteur de réflexion (R∞), déterminé d'après la norme DIN 53 145, Partie 1 (1992), de plus de 60 % environ et l'ester de cellulose présente un degré de substitution DS d'environ 1,5 à 3,0.
  2. Voile melt-blown suivant la revendication 1, caractérisé en ce que le plastifiant est extractible par l'eau.
  3. Voile melt-blown suivant la revendication 1 ou 2, caractérisé en ce que le plastifiant se présente sous forme de triacétine, de carbonate d'éthylène, de carbonate de propylène, d'ester triéthylique d'acide citrique, de diacétate de triéthylène-glycol, de polyéthylène-glycol de bas poids moléculaire et/ou de sulfolane.
  4. Voile melt-blown suivant au moins l'une des revendications précédentes, caractérisé en ce que le degré de substitution DS est d'environ 1,7 à 2,7, notamment d'environ 2,2 à 2,6.
  5. Voile melt-blown suivant au moins l'une des revendications précédentes, caractérisé en ce que l'ester de cellulose a un degré de polymérisation DP d'environ 150 à 400, notamment d'environ 180 à 350.
  6. Voile melt-blown suivant au moins l'une des revendications 1 à 5, caractérisé en ce que la teneur en plastifiant s'élève à environ 2 à 8 % en masse.
  7. Voile melt-blown suivant au moins l'une des revendications 1 à 6, caractérisé en ce que le facteur de réflexion (R∞) s'élève à plus d'environ 70 %.
  8. Voile melt-blown suivant au moins l'une des revendications 1 à 7, caractérisé en ce que l'acétate de cellulose se présente sous forme d'un blend polymère, notamment avec des polyesters aliphatiques et/ou des amidons acétylés.
  9. Procédé de production d'un voile melt-blown suivant au moins l'une des revendications précédentes, caractérisé en ce qu'un ester de cellulose, notamment l'acétate de cellulose, de degré de substitution DS d'environ 1,5 à 3,0, notamment d'environ 1,7 à 2,7, est mélangé à chaud avec un plastifiant dans un rapport en masse d'environ 2:1 à 1:4 et le mélange est transformé en une masse fondue, le mélange de plastifiant et d'ester de cellulose présentant un indice de fusion MFI (210/2.16) selon la norme DIN 53 735 d'environ 400 à 5 g/10 min, notamment de 300 à 50 g/10 min, la masse fondue est transformée en un voile melt-blown dans un dispositif de filage par soufflage à l'état fondu, puis le plastifiant est extrait avec un solvant approprié jusqu'à une fraction d'environ 0 à 10 % en masse.
  10. Procédé suivant la revendication 9, caractérisé en ce que le rapport en masse du plastifiant à l'ester de cellulose est ajusté à une valeur d'environ 3:2 à 2:3.
  11. Procédé suivant la revendication 9 ou 10, caractérisé en ce que la température, lors du mélange du plastifiant avec l'ester de cellulose, est ajustée à une valeur d'environ 140 à 180°C.
  12. Procédé suivant l'une des revendications 9 à 11, caractérisé en ce que la température au niveau de la tête de filage et de la buse du dispositif de filage melt-blown est ajustée à une valeur d'environ 180 à 240°C, notamment d'environ 200 à 230°C.
  13. Procédé suivant au moins l'une des revendications 9 à 12, caractérisé en ce que le mélange de la cellulose et du plastifiant est effectué dans une extrudeuse à deux vis synchrones.
  14. Procédé suivant au moins l'une des revendications 9 à 13, caractérisé en ce qu'un plastifiant extractible par l'eau est utilisé.
  15. Procédé suivant la revendication 14, caractérisé en ce que le voile melt-blown obtenu est amené à passer dans un bain d'eau en vue de l'extraction du plastifiant.
  16. Procédé suivant au moins l'une des revendications 9 à 15, caractérisé en ce que le voile sortant du dispositif de filage melt-blown est transféré à un dispositif de réception, pressé pour le réglage de l'épaisseur désirée, puis extrait.
  17. Procédé suivant la revendication 16, caractérisé en ce que le voile melt-blown est structuré par pressage.
  18. Procédé suivant la revendication 16 ou 17, caractérisé en ce que le voile melt-blown est déposé sur un tamis ou tamis à bande ou sur un tambour perforé.
  19. Procédé suivant au moins l'une des revendications 9 à 18, caractérisé en ce que des filaments, notamment des filaments d'acétate de cellulose, sont introduits en même temps au cours de la formation du voile melt-blown.
  20. Procédé suivant au moins l'une des revendications précédentes, caractérisé en ce que le voile melt-blown sortant du dispositif de filage est déposé sur un support en vue de la formation d'un corps composite.
  21. Composé suivant la revendication 20, caractérisé en ce que le support est une nappe formée d'une étoupe de filtre en acétate de cellulose, d'une étoupe de filtre apprêtée en surface ou de papier.
  22. Procédé suivant la revendication 20 ou 21, caractérisé en ce que le corps composite est pressé et/ou structuré pour la régulation de son épaisseur.
  23. Utilisation d'un voile melt-blown suivant au moins l'une des revendications 1 à 8 comme matière filtrante.
  24. Utilisation d'un voile melt-blown suivant la revendication 23 dans des filtres pour la fumée de tabac, notamment dans des filtres de cigarettes.
  25. Utilisation d'un voile melt-blown suivant la revendication 24 dans des filtres doubles pour cigaretttes ultra-légères.
  26. Utilisation d'un voile melt-blown suivant la revendication 23 pour la filtration de gaz ou de liquides.
  27. Utilisation d'un voile melt-blown suivant la revendication 26 pour la filtration de sang.
EP96944588A 1996-03-08 1996-12-18 Non-tisse de fusion-soufflage, son procede de production et ses utilisations Expired - Lifetime EP0885321B1 (fr)

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Application Number Priority Date Filing Date Title
DE19609143A DE19609143C1 (de) 1996-03-08 1996-03-08 Melt-blown-Vlies, Verfahren zu dessen Herstellung und dessen Verwendungen
DE19609143 1996-03-08
PCT/EP1996/005686 WO1997033026A1 (fr) 1996-03-08 1996-12-18 Non-tisse de fusion-soufflage, son procede de production et ses utilisations

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WO (1) WO1997033026A1 (fr)

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DE19609143C1 (de) 1997-11-13
AU1302297A (en) 1997-09-22
JP3251018B2 (ja) 2002-01-28
WO1997033026A1 (fr) 1997-09-12
US6207601B1 (en) 2001-03-27
EP0885321A1 (fr) 1998-12-23
DE59605210D1 (de) 2000-06-15
JPH11506175A (ja) 1999-06-02
ATE192789T1 (de) 2000-05-15

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