EP0608744A1 - Filaments d'acétate de cellulose, solution de filage optiquement isotrope à cet effet et son utilisation pour la fabrication des filaments - Google Patents

Filaments d'acétate de cellulose, solution de filage optiquement isotrope à cet effet et son utilisation pour la fabrication des filaments Download PDF

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Publication number
EP0608744A1
EP0608744A1 EP94100584A EP94100584A EP0608744A1 EP 0608744 A1 EP0608744 A1 EP 0608744A1 EP 94100584 A EP94100584 A EP 94100584A EP 94100584 A EP94100584 A EP 94100584A EP 0608744 A1 EP0608744 A1 EP 0608744A1
Authority
EP
European Patent Office
Prior art keywords
spinning solution
filaments
cellulose acetate
approximately
degree
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.)
Granted
Application number
EP94100584A
Other languages
German (de)
English (en)
Other versions
EP0608744B1 (fr
Inventor
Ties Dipl.-Chem. Dr. Karstens
Wolfgang Dipl.-Ing. Koppe
Joachim Dipl.-Chem. Dr. Schätzle
Günter Dipl.-Ing. Maurer
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Cerdia Produktions GmbH
Original Assignee
Rhone Poulenc Rhodia AG
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Rhone Poulenc Rhodia AG filed Critical Rhone Poulenc Rhodia AG
Publication of EP0608744A1 publication Critical patent/EP0608744A1/fr
Application granted granted Critical
Publication of EP0608744B1 publication Critical patent/EP0608744B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D01F2/24—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives
    • D01F2/28—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives from organic cellulose esters or ethers, e.g. cellulose acetate
    • D01F2/30—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives from organic cellulose esters or ethers, e.g. cellulose acetate by the dry spinning process
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D01F2/24—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives
    • D01F2/28—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives from organic cellulose esters or ethers, e.g. cellulose acetate
    • 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
    • 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
    • Y10T428/2933—Coated or with bond, impregnation or core
    • Y10T428/2964—Artificial fiber or filament
    • Y10T428/2965—Cellulosic

Definitions

  • the invention relates to filaments based on a cellulose acetate soluble in acetone, an optically isotropic spinning solution for the production of filaments, which contains a cellulose acetate dissolved in acetone and optionally further additives, and the use of this spinning solution for producing the designated filaments.
  • DE-OS 27 05 382 describes an extensive group of cellulose derivatives, including also cellulose acetates. These are to be transferred to an anisotropic spinning solution in order to produce filaments using conventional spinning processes. According to Table I, the degree of substitution (DS) of the cellulose acetate should be between 1.89 and 2.45. Halogenated and phenolic compounds are predominantly specified as suitable solvents for this. In connection with the other cellulose derivatives specified in DE-OS 27 05 382, acetone is also listed in a large number of solvents. The cellulose derivatives should be present in the spinning solution in an amount of at least 15% by volume in order to meet the requirement for optical anisotropy.
  • a cellulose acetate with a degree of substitution (DS) of 1.89 is not soluble in acetone.
  • DS degree of substitution
  • DE-OS 27 05 382 Cellulose derivatives with an average degree of polymerization (DP) of at least 100 anhydroglucose units have a sufficiently high molecular weight to be suitable for the production of filaments. Precise statements on the degree of polymerization of the cellulose acetate and the degree of substitution between 1.89 to 2.45 are not found in DE-OS 27 05 382.
  • the invention is therefore based on the object of proposing filaments based on a cellulose acetate soluble in acetone and a spinning solution which is particularly suitable for their production and which remedy the disadvantages of the prior art described above, in particular the poor economy, without the properties of the filaments being eliminated , in particular the tensile strength and the elongation, are impaired in comparison to known products.
  • filaments based on a cellulose acetate soluble in acetone which is characterized in that the degree of polymerization (DP) of the cellulose acetate is between about 110 and 210.
  • the range of the degree of polymerization between about 150 and 180 and in particular between about 160 and 180 is particularly preferred.
  • the degree of substitution (DS) is preferably set between about 2.2 and 2.7. It is particularly preferred if the degree of substitution (DS) is between approximately 2.4 and 2.6 and very particularly preferably between approximately 2.4 and 2.5.
  • cellulose-2.5-acetate If the term "cellulose-2.5-acetate” is used below, then this term should be understood in an abstract manner. This means that the degree of substitution of 2.5 can be more or less greatly exceeded or undershot, with the only requirement being that a cellulose-2,5-acetate of this type is soluble in acetone at room temperature (about 20 ° C.) is. In any case, the number "2.5" in the chemical name "cellulose-2,5-acetate” should include the cellulose acetates previously designated with the preferred degree of substitution.
  • the titer of the filaments according to the invention is not critical. It is preferably between about 1 and 14 dtex, in particular between about 1.5 and 9 dtex. It is the fineness designation for filaments, i.e. a weight per length, the unit of which is the dtex.
  • the parameters of the filaments according to the invention are preferably set such that their tensile strength is between approximately 0.9 and 1.2 cN / dtex, in particular between approximately 1.0 and 1.2 cN / dtex, and the elongation is between approximately 10 and 30%. in particular between about 15 and 25%. They therefore meet the requirements placed on the known filaments of this type in order to make them suitable for the fields of application described below.
  • this optically isotropic spinning solution is characterized in that the concentration of the cellulose-2,5-acetate in the spinning solution is about 35 to 47% by mass and the degree of polymerization (DP) of the cellulose-2,5-acetate between about 110 and 210 lies. It is preferred here that the cellulose-2,5-acetate has the degrees of polymerization and substitution already mentioned above in connection with the description of the filaments.
  • the concentration (c) in the spinning solution is at most 8% by mass and in particular at most 6% by mass below the critical Concentration (c *), measured at room temperature (about 20 ° C), is. If this critical concentration of cellulose-2,5-acetate is exceeded to higher concentrations of the spinning solution without the action of external forces, such as shear forces (c> c *), the spinning solution is converted from the isotropic to the anisotropic state.
  • optically isotropic spinning solution In order to further improve the optically isotropic spinning solution according to the invention, various additives such as pigments and water can be incorporated into it.
  • the optically isotropic spinning solution according to the invention preferably contains up to about 6% by mass and in particular about 2 to 4% by mass of water.
  • the incorporation of water has the advantage that the viscosity of the spinning solution is reduced with the result of improved spinnability.
  • the spinning solution preferably contains a finely divided pigment, in particular a white pigment, such as preferably titanium dioxide.
  • the particle size is expediently in the range from about 0.3 ⁇ m to 0.5 ⁇ m.
  • the amount of finely divided pigment in the spinning solution is preferably about 0.4 to 0.8% by mass, based on the proportion of cellulose-2,5-acetate in the spinning solution.
  • the mass percentage range from about 0.4 to 0.6 is very particularly preferred.
  • an optically isotropic acetone spinning solution with a substantially higher content of cellulose-2,5-acetate can be produced and spun, in particular after the usual dry spinning.
  • e.g. (Cigarettes) filtertow because of the high concentration of spinning solution, much less acetone has to be recovered per unit weight of filtertow than under the previous conditions. In this way, e.g. same filter tow production, which significantly reduces the costs associated with the recovery of acetone.
  • a spinning solution can be produced and processed at a much higher concentration than before using the inventive spinning solution with the same viscosity.
  • the advantages mentioned above are therefore achieved with an optically isotropic acetone spinning solution with a high concentration of cellulose-2,5-acetate.
  • the anisotropy or isotropy can be determined by visual inspection. An anisotropic phase looks cloudy and / or "mother-of-pearl", while the isotropic phase is always clear.
  • the respective isotropic or anisotropic state of a spinning solution can also be determined microscopically with crossed Nicols. If, for example, a sample of an anisotropic spinning solution is observed between the slide and the cover glass of a microscope after the cover glass has been pressed down between crossed Nicols, at least part of the solution is translucent.
  • the temperature also plays a role here; if the temperature of an anisotropic cellulose acetate solution is raised from room temperature initially, then the anisotropic phase may gradually transition to the isotropic phase. If the temperature is increased further, the entire spinning solution is converted into an isotropic system.
  • the temperature ranges at which these transitions take place vary depending on the type of cellulose derivative, its concentration in the spinning solution and its degree of substitution.
  • filaments obtained according to the invention are not restricted in comparison with the known filaments of this type. They can be used for the production of filter tow (bundles of filaments combined into a band), for tobacco smoke filters, in particular cigarette filters, but also for example for the production of - textile - yarns for linings or of mixed fabrics with cotton.
  • the present invention could be explained as follows: the starting point is an isotropic acetone solution of cellulose-2,5-acetate of the type described, the concentration of which can be raised to close to the critical concentration value (c *), from which an anisotropic phase arises. If such an isotropic solution is introduced into the spinneret channels (capillaries), then the shear forces in the spinneret channel caused by the flow forces cause predominantly orientation and thus anisotropy. In the area of the capillary and after exiting the capillary, the isotropic phase does not differ from a real anisotropic phase. For this reason, almost identical fiber strengths are obtained in both cases.
  • the relaxation time of the oriented polymer chains is longer than the time within which the critical concentration (c *) is reached by the evaporation of the acetone.
  • the rate of evaporation is higher than the rate of relaxation.
  • the anisotropic state occurs, for example, at a concentration of cellulose-2,5-acetas of approximately 47 to 48% by mass in the acetone solution, if its DP value is approximately 150 and its DS value is approximately 2.45. This information is only an example.
  • the acetone spinning solution of the cellulose-2,5-acetate should be transferred into a concentration range in which the system shows anisotropy by means of rapid evaporation.
  • a sotropic spinning solution can be used in accordance with the invention and that filaments can be obtained in a highly economical manner, which previously could only be produced with anisotropic spinning solutions.
  • a spinning solution with the following composition was used: Dimensions-% Cellulose acetate (DP: 150; DS: 2.45) 43.2 water 3rd acetone 53.8
  • the spinning solution was spun in a conventional dry spinning system which had a nozzle plate with 125 nozzle channels.
  • the nozzle channels were triangular in cross section. The triangle had an edge length of 45 ⁇ m.
  • the nozzle temperature was 47 ° C and the nozzle pressure was 88 bar.
  • the spinning speed was 340 m / min with a draw factor of 1.6.
  • a temperature of 70 ° C prevailed in the spinning shaft with a total length of 4 m located under the spinneret. 10 m3 of acetone-air mixture were suctioned off per hour.
  • the filaments obtained had the following physical properties: Titer: 3.1 dtex Tensile strenght: 1.0 cN / dtex Strain: 19.4%
  • the 125 filaments obtained by the process according to this example were combined into a filament bundle. 80 such filament bundles were combined into a cigarette filter tow.
  • a spinning solution with the following composition was used: Dimensions-% Cellulose acetate (DP: 170; DS: 2.47) 42.1 water 3rd acetone 54.9
  • the spinning solution was spun on the same dry spinning system as in Example 1, but the nozzle plate had 240 nozzle channels.
  • the nozzle channels would be triangular in cross section.
  • the triangle had an edge length of 45 ⁇ m.
  • the nozzle temperature was adjusted to 52 ° C and the nozzle pressure was 80 bar.
  • the spinning speed was 310 m / min with a stretching factor of 1.3.
  • the temperature in the spinning shaft located under the spinneret with a total length of 4 m was 70 ° C. 10 m3 of acetone-air mixture were suctioned off per hour.
  • the filaments obtained had the following physical properties: Titer: 3.6 dtex Tensile strenght: 1.1 cN / dtex Strain: 20.5%
EP94100584A 1993-01-26 1994-01-17 Filaments d'acétate de cellulose, solution de filage optiquement isotrope à cet effet et son utilisation pour la fabrication des filaments Expired - Lifetime EP0608744B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4302055 1993-01-26
DE4302055A DE4302055C1 (de) 1993-01-26 1993-01-26 Celluloseacetat-Filamente sowie ein Verfahren zu deren Herstellung

Publications (2)

Publication Number Publication Date
EP0608744A1 true EP0608744A1 (fr) 1994-08-03
EP0608744B1 EP0608744B1 (fr) 1999-03-31

Family

ID=6478940

Family Applications (1)

Application Number Title Priority Date Filing Date
EP94100584A Expired - Lifetime EP0608744B1 (fr) 1993-01-26 1994-01-17 Filaments d'acétate de cellulose, solution de filage optiquement isotrope à cet effet et son utilisation pour la fabrication des filaments

Country Status (11)

Country Link
US (1) US5449555A (fr)
EP (1) EP0608744B1 (fr)
JP (1) JP2950490B2 (fr)
KR (1) KR960011600B1 (fr)
CN (1) CN1100478A (fr)
AT (1) ATE178368T1 (fr)
BR (1) BR9400301A (fr)
CA (1) CA2113142A1 (fr)
DE (2) DE4302055C1 (fr)
ES (1) ES2131594T3 (fr)
RU (1) RU2085629C1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999004071A1 (fr) * 1997-07-16 1999-01-28 Rhodia Acetow Gmbh Filaments d'acetate de cellulose a section trilobee

Families Citing this family (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3342763B2 (ja) * 1994-02-04 2002-11-11 ダイセル化学工業株式会社 シガレットフィルター素材
AU680730B2 (en) * 1994-03-01 1997-08-07 Kuraray Co., Ltd. Regenerated cellulose fiber dyeable with disperse dye and textile product containing the same
CN1102357C (zh) * 1994-09-22 2003-03-05 大世吕化学工业株式会社 烟草过滤材料、烟草过滤嘴和生产烟草过滤材料的方法
US5491024A (en) * 1995-03-14 1996-02-13 Hoechst Celanese Corporation Photodegradable cellulose ester tow
EP0763544B1 (fr) * 1995-03-31 2003-09-24 Daicel Chemical Industries, Ltd. Acetate de cellulose a bonne aptitude au moulage et procede de preparation associe
JP3942669B2 (ja) * 1995-03-31 2007-07-11 ダイセル化学工業株式会社 物理強度に優れたセルロースアセテート、及びその製造法
DE69626254T2 (de) * 1995-03-31 2003-07-24 Daicel Chem Celluloseacetat mit ausgezeichneter festigkeit und verfahren zur herstellung
US8461234B2 (en) 2003-03-14 2013-06-11 Eastman Chemical Company Refinish coating compositions comprising low molecular weight cellulose mixed esters
US7893138B2 (en) * 2003-03-14 2011-02-22 Eastman Chemical Company Low molecular weight carboxyalkylcellulose esters and their use as low viscosity binders and modifiers in coating compositions
US8124676B2 (en) 2003-03-14 2012-02-28 Eastman Chemical Company Basecoat coating compositions comprising low molecular weight cellulose mixed esters
US8039531B2 (en) 2003-03-14 2011-10-18 Eastman Chemical Company Low molecular weight cellulose mixed esters and their use as low viscosity binders and modifiers in coating compositions
GB2504495A (en) * 2012-07-30 2014-02-05 British American Tobacco Co Fleece for smokeless tobacco pouch
RU2515313C2 (ru) * 2012-08-27 2014-05-10 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Тюменский государственный нефтегазовый университет" (ТюмГНГУ) Способ модификации диацетатцеллюлозных волокон

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US1620636A (en) * 1923-03-07 1927-03-15 Dreyfus Henry Manufacture of artificial threads and filaments
US1688531A (en) * 1922-08-11 1928-10-23 Dreyfus Henry Manufacture of artificial silk, artificial horsehair, and the like
US2829027A (en) * 1953-12-28 1958-04-01 Eastman Kodak Co Dry spinning process for making y-shaped filaments
US5269996A (en) * 1992-09-14 1993-12-14 Eastman Kodak Company Process for the production of fine denier cellulose acetate fibers

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US2065518A (en) * 1928-11-10 1936-12-29 Celanese Corp Method of making yarns, filaments, and the like and product thereof
GB652844A (en) * 1948-11-24 1951-05-02 Courtaulds Ltd Improvements in and relating to the production of artificial threads, fibres, filaments, staple fibres and the like
US2806474A (en) * 1953-06-29 1957-09-17 Yarsley Victor Emmanuel Production of filter elements
US3670069A (en) * 1969-09-15 1972-06-13 Itt Process for forming hydroxyethyl cellulose fibers having high water absorption and high water retention properties
US3961007A (en) * 1973-10-23 1976-06-01 E & J Gallo Winery Continuous process for making fibrous cellulose acetate filter material
US3839527A (en) * 1973-10-12 1974-10-01 Itt Water and organic solvent resistant cellulose acetate-methylolated guanamine polymer fiber
US4040856A (en) * 1975-06-17 1977-08-09 Crown Zellerbach Corporation Production of discrete cellulose acetate fibers by emulsion flashing
JPS5214335A (en) * 1975-07-22 1977-02-03 Matsushita Electric Ind Co Ltd Direct current control circuit
JPS5296230A (en) * 1976-02-09 1977-08-12 Du Pont Manufacture of optically isomerized dope and cellulose fiber
JPS5739210A (en) * 1980-08-20 1982-03-04 Mitsubishi Rayon Co Ltd Production of cellulose acetate fiber
JPS6017441B2 (ja) * 1981-07-10 1985-05-02 ダイセル化学工業株式会社 新規なセルロ−スアセテ−トの製造方法
DE3246417A1 (de) * 1982-12-15 1984-06-20 Akzo Gmbh, 5600 Wuppertal Wasserunloesliche fasern aus celluloseacetat, cellulosepropionat und cellulosebutyrat mit einem extrem hohen absorptionsvermoegen fuer wasser und physiologische fluessigkeiten
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Publication number Priority date Publication date Assignee Title
US1688531A (en) * 1922-08-11 1928-10-23 Dreyfus Henry Manufacture of artificial silk, artificial horsehair, and the like
US1620636A (en) * 1923-03-07 1927-03-15 Dreyfus Henry Manufacture of artificial threads and filaments
US2829027A (en) * 1953-12-28 1958-04-01 Eastman Kodak Co Dry spinning process for making y-shaped filaments
US5269996A (en) * 1992-09-14 1993-12-14 Eastman Kodak Company Process for the production of fine denier cellulose acetate fibers

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999004071A1 (fr) * 1997-07-16 1999-01-28 Rhodia Acetow Gmbh Filaments d'acetate de cellulose a section trilobee
US6177194B1 (en) 1997-07-16 2001-01-23 Rhodia Acetow Gmbh Cellulose acetate filaments with a trilobal cross section

Also Published As

Publication number Publication date
BR9400301A (pt) 1994-08-16
EP0608744B1 (fr) 1999-03-31
KR940018496A (ko) 1994-08-18
ES2131594T3 (es) 1999-08-01
JPH06280107A (ja) 1994-10-04
CN1100478A (zh) 1995-03-22
DE4302055C1 (de) 1994-03-24
JP2950490B2 (ja) 1999-09-20
US5449555A (en) 1995-09-12
RU2085629C1 (ru) 1997-07-27
DE59408019D1 (de) 1999-05-06
CA2113142A1 (fr) 1994-07-27
ATE178368T1 (de) 1999-04-15
KR960011600B1 (ko) 1996-08-24

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