EP0813573A1 - Composition contenant de fines particules solides - Google Patents

Composition contenant de fines particules solides

Info

Publication number
EP0813573A1
EP0813573A1 EP96905800A EP96905800A EP0813573A1 EP 0813573 A1 EP0813573 A1 EP 0813573A1 EP 96905800 A EP96905800 A EP 96905800A EP 96905800 A EP96905800 A EP 96905800A EP 0813573 A1 EP0813573 A1 EP 0813573A1
Authority
EP
European Patent Office
Prior art keywords
solid particles
composition according
cellulose
particles
composition
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.)
Withdrawn
Application number
EP96905800A
Other languages
German (de)
English (en)
Inventor
Abdulmajid Hashemzadeh
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.)
Acordis AG
Original Assignee
Akzo Nobel NV
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 Akzo Nobel NV filed Critical Akzo Nobel NV
Publication of EP0813573A1 publication Critical patent/EP0813573A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/08—Ingredients agglomerated by treatment with a binding agent
    • 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
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/04—Pigments
    • 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

Definitions

  • the invention relates to a composition
  • a composition comprising fine, solid particles such as inorganic or organic pigments, synthetic polymers and the like. contains which are provided with a coating or are dispersed in a matrix, the coating or the matrix consisting of a homogeneous mixture of cellulose, tertiary amine oxide, water and possibly other constituents.
  • Dispersions of solid particles such as pigments are required for a wide variety of applications.
  • An important application is e.g. matting cellulosic threads.
  • NMMO process a process in which cellulose in a mixture of N-methylmorpholine-N-oxide, water and optionally dissolved further components and further processed into threads in a manner known per se. If one tries to stir the pigments directly into the spinning mass, agglomerations occur, whereby spinning disturbances are automatically programmed. Furthermore, the uniformity of the threads obtained suffers.
  • compositions which contain finely divided dispersed or dispersible solid particles which are stable, do not tend to separate, can be readily distributed in cellulosic compositions which are simple to produce, are versatile and which in the further processing of moldings, for example when washing cellulosic threads not as a result of washing out emulsifiers and the like. lead to problems when working up the washing water and the solvent, ie compositions which also meet the strict requirements of environmental protection in a satisfactory manner.
  • compositions which contains fine, solid particles which are provided with a coating or are dispersed in a matrix and which are inert to the coating or matrix, the coating or the matrix consisting of a homogeneous mixture of cellulose , tertiary amine oxide, water and optionally other constituents and the composition consists of 0.5 to 10 wt% cellulose, 5 to 76 wt% solid particles and the remainder 100% of a mixture of tertiary amine oxide, water and optionally further constituents puts.
  • the tertiary amine oxide is preferably N-methylmorpholine-N-oxide.
  • the composition is composed of 40 to 50% by weight of solid particles, 1 to 2% by weight of cellulose (based on solid particles), 59 to 48% by weight of a mixture of tertiary amine oxide and water and optionally further constituents .
  • the cellulose has advantageous a DP (average degree of polymerization) of 500 to 700.
  • the tertiary amine oxide and water in the composition preferably have a weight ratio of from 75 to 90 to 25 to 10.
  • the solid particles can be inorganic or organic in nature.
  • the organic solid particles consist of synthetic polymers.
  • the compositions preferably contain inorganic or organic pigments, in particular titanium dioxide or barium sulfate.
  • compositions are preferably solid at room temperature. In a further embodiment of the invention, the compositions can also be liquid.
  • the composition can also be in the form of solid discrete particles.
  • the discrete particles can in particular have a powdery, granular or spherical shape.
  • Another object of the invention is a process for the preparation of compositions which contain fine, solid particles which are inert to the coating or the matrix, which is characterized in that solid particles in a solution of cellulose, tertiary amine oxide , Water and optionally other constituents and the dispersion obtained, if appropriate, cooled and comminuted or excess solution is withdrawn from the dispersion obtained and optionally cooled and comminuted, 0.5 to 10% by weight of cellulose and 5 to 76% by weight of solid being used to prepare the composition Particles and remainder to 100 a mixture of tertiary amine oxide, water and optionally other ingredients used. It is advantageous to apply high shear forces when distributing the solid particles.
  • the distribution of the solid particles in a solution having a viscosity of 5.0 to 100 mPas is preferably carried out, the viscosity being measured at 90.degree.
  • the liquid, finely divided dispersion is advantageously poured into molds, cooled and comminuted.
  • the liquid dispersion is sprayed into solid particles.
  • compositions according to the invention are advantageously used in pigmentation, in matting cellulose threads, films and membranes and in the production of cellulose threads, films and membranes stable against ultraviolet radiation.
  • Inert to the coating or the matrix means that the solid particles which are used to build up the composition do not decompose the coating or the matrix under processing conditions.
  • Non-inert compounds include copper oxide, iron-2 and iron-3-oxide, which in particular lead to a strong decomposition of N-methylmorpholine-N-oxide when they are heated with the amine oxide.
  • Inert inorganic compounds in the context of the invention include titanium dioxide, barium sulfate, sodium carbonate, carbon black and the like.
  • Correspondingly inert organic compounds include polymer powders such as PVC, polystyrene, thermoplastic starch and others.
  • flame-retardant substances such as phosphorus or nitrogen compounds, silicates or porous particles, which subsequently with active substances such as fragrances, anti-insect agents and the like. can be loaded, can be incorporated as inert particles.
  • Further constituents which may optionally be present in the composition are, above all, stabilizers such as propyl gallic acid, gallic acid, pyrogallol, ascorbic acid or dispersing agents (such as, for example, emulsifiers).
  • the implementation of the method according to the invention can e.g. done in the following way.
  • the solution must contain enough cellulose that when the solid particles are dispersed, the particles have at least one monomolecular layer of cellulose on the entire surface. It is advantageous if a multi-molecular layer envelops the dispersed particles in each case. It is very advantageous if the amount of solution is dimensioned such that the dispersed particles are embedded as in a matrix, the distance between the individual solid particles in the matrix is relatively large, e.g. is at least one particle diameter.
  • the amounts of cellulose, based on the dispersed particles, can be varied within relatively wide limits, i.e. a considerable excess can also be used. If an excess is used, the solid particles are initially suspended in the solution; after the mixture has solidified, the finely dispersed particles are present as if embedded in a matrix.
  • a matrix at room temperature is understood to mean a solid mass which essentially has a uniform, coherent structure in which the solid particles are finely divided, such as pigments in plastics.
  • elevated temperatures e.g.> 90 ° C
  • the matrix melts into a concentrated paste, with no flocculation of the particles.
  • the minimum amount required can theoretically be determined from the specific surface of the solid particles e.g. of the pigments and the hydrodynamic volume of the cellulose in the solution. In practice, however, the procedure is first to start an experiment with an excess of cellulose solution and then to subject the liquid dispersion to ultrafiltration, in which only the solution passes, whereas the particles coated with a monomolecular layer remain.
  • the required minimum amount can be calculated from the difference between the predetermined amount and the amount drawn off by ultrafiltration.
  • the constituents intended for the matrix or the casing are heated until a solution or melt is formed, and then the previously comminuted solid particles are stirred in.
  • the viscosity of the solution in which the solid particles are dispersed can be varied within relatively wide limits, it is expediently 0.5 to 200 mPa s, measured at 90 ° C.
  • the viscosity depends to a large extent on the concentration and the DP of the cellulose used.
  • the molecular weight of the cellulose used also has an influence on the dispersibility. It has DP from 600 to 700 proved to be particularly advantageous. In general, it can be said that the lower the DP, the better the cellulose is adsorbed on the dispersed particles.
  • the amounts of the individual components of the composition and also the process conditions in the preparation of the composition such as temperature, viscosity and the like. can be varied within relatively wide limits and adapted to the respective application.
  • the advantageous composition can easily be determined on the basis of simple preliminary tests.
  • the composition contains the individual components in approximately the following amounts.
  • Cellulose 0.5 to 10% by weight, solid particles 5 to 60% by weight and a mixture of tertiary amine oxide, water and optionally other constituents, the remainder 100%.
  • the temperature at which the solid particles are distributed in the solution depends on the NMMO: water ratio.
  • the monohydrate of N-methylmorpholine-N-oxide has a melting point of about 72 ° C., so that a few degrees above it is sufficient to be able to produce a dispersion.
  • very high concentrations of solid particles can be dispersed.
  • the mass is generally solidified, for example by pouring it into a mold and cooling.
  • the shaping can be comminuted without difficulty, for example by grinding.
  • celluloses of the most varied of origins and with the most varied degrees of polymerization can be used to produce the casing or the matrix, such as cotton backs, cotton fibers, microcrystalline cellulose, cellulose obtained from wood, etc.
  • the degrees of polymerization can easily be between 150 to 7000. Higher or lower values are not excluded. Mixtures of different degrees of polymerization can also be used.
  • compositions obtained can be readily distributed in cellulosic spinning masses which contain tertiary amine oxides, water and possibly other additives.
  • the particles are distributed very evenly very quickly.
  • threads, films and membranes can be matted with titanium dioxide in a particularly advantageous manner.
  • the production of barium sulfate-containing threads is also very simple, threads that have a particular stability against UV radiation.
  • X-ray contrast fibers containing barium sulfate can also be produced particularly advantageously for medical purposes.
  • compositions according to the invention can also be used in appropriate amounts in the preparation of the spinning mass. So you can mix and melt the composition with an NMMO / ⁇ O mixture and then add the cellulose, if necessary, excess water is removed.
  • the distribution of synthetic polymers can also be carried out without any problems.
  • dope can also be doped excellently.
  • the liquid dispersion can also be deformed into discrete particles by spraying. Spraying can be done using conventional equipment. The size of the particles can be easily controlled by varying the spray speed, the length of the spray path and the conditions in the spray channel, such as temperature and pressure.
  • Viscosity also plays a role; it is possible to adjust the viscosity, e.g. to control the shape of the discrete particles by varying the concentration or DP of the cellulose used.
  • the shape of the particles obtained in the spraying process can also be influenced by other additives. In this way, discrete particles can be produced in powder form, with spherical, granular, rod-like shapes, etc.
  • the degree of polymerization (DP) of cellulose was calculated in copper (II) ethylenediamine (Merck) by viscometric measurements of the intrinsic viscosity (ETA) according to the Staudinger equation:

Abstract

Cette composition contient de fines particules solides pourvues d'un enrobage ou dispersées dans une matrice, les particules étant inertes par rapport à l'enrobage ou à la matrice. L'enrobage ou la matrice sont constitués d'un mélange homogène de cellulose, d'oxyde d'amine tertiaire, d'eau et le cas échéant d'autres éléments. Ces compositions peuvent être utilisées pour donner un aspect mat à des fils, films et membrane cellulosiques, ou pour les pigmenter.
EP96905800A 1995-03-04 1996-02-26 Composition contenant de fines particules solides Withdrawn EP0813573A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19507589 1995-03-04
DE19507589 1995-03-04
PCT/EP1996/000782 WO1996027638A1 (fr) 1995-03-04 1996-02-26 Composition contenant de fines particules solides

Publications (1)

Publication Number Publication Date
EP0813573A1 true EP0813573A1 (fr) 1997-12-29

Family

ID=7755632

Family Applications (1)

Application Number Title Priority Date Filing Date
EP96905800A Withdrawn EP0813573A1 (fr) 1995-03-04 1996-02-26 Composition contenant de fines particules solides

Country Status (11)

Country Link
US (1) US5895795A (fr)
EP (1) EP0813573A1 (fr)
JP (1) JPH11501071A (fr)
KR (1) KR19980701923A (fr)
CN (1) CN1177364A (fr)
AU (1) AU4941696A (fr)
CA (1) CA2214402A1 (fr)
PL (1) PL322109A1 (fr)
SK (1) SK115397A3 (fr)
TW (1) TW442525B (fr)
WO (1) WO1996027638A1 (fr)

Families Citing this family (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6235392B1 (en) 1996-08-23 2001-05-22 Weyerhaeuser Company Lyocell fibers and process for their preparation
AT404846B (de) * 1997-06-16 1999-03-25 Chemiefaser Lenzing Ag Zusammensetzung enthaltend feine feststoffteilchen
DE19839856A1 (de) * 1998-09-02 2000-04-20 Metallgesellschaft Ag Präparationsmittel
AT407997B (de) 1999-08-10 2001-07-25 Chemiefaser Lenzing Ag Gefärbte cellulosische formkörper
WO2001013119A1 (fr) * 1999-08-17 2001-02-22 Luminex Corporation Encapsulation de particules fluorescentes
PL201205B1 (pl) * 2003-03-10 2009-03-31 Inst Wlokien Naturalnych Sposób wytwarzania modyfikowanych włókien celulozowych
DE10331342B4 (de) * 2003-07-11 2009-03-12 Thüringisches Institut für Textil- und Kunststoff-Forschung e.V. Thermostabile Form- oder Spinnmasse
AT502743B1 (de) 2005-08-26 2008-06-15 Chemiefaser Lenzing Ag Cellulosischer formkörper, verfahren zu seiner herstellung und dessen verwendung
DE102006033591B4 (de) * 2006-07-18 2008-10-16 Thüringisches Institut für Textil- und Kunststoff-Forschung e.V. Verfahren zur Stabilisierung der Spinnlösung bei der Herstellung von cellulosischen Verbundformkörpern
NO20065147L (no) * 2006-11-08 2008-05-09 Ntnu Tech Transfer As Nanokompositter basert på cellulosewhiskers og celluloseplast
CN102704023B (zh) * 2012-05-24 2014-04-16 恒天海龙股份有限公司 一种防x射线辐射纤维素纤维及其制备方法
EP4127280A4 (fr) * 2020-03-31 2024-04-17 Aditya Birla Science And Tech Company Pvt Ltd Procédé de préparation de fibre lyocell teintée par dopage
EP4155438A1 (fr) * 2021-09-28 2023-03-29 Lenzing Aktiengesellschaft Fibre lyocell comprenant un agent matant et utilisation pour la production d'un tissu textile

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3659660A (en) * 1970-04-10 1972-05-02 Dresser Ind Large diameter bit for shallow angle holes
DE3034685C2 (de) * 1980-09-13 1984-07-05 Akzo Gmbh, 5600 Wuppertal Cellulose-Form- und Spinnmasse mit geringen Anteilen an niedermolekularen Abbauprodukten
AT393841B (de) * 1990-03-01 1991-12-27 Chemiefaser Lenzing Ag Stabile form- bzw. spinnmasse
AT396930B (de) * 1992-01-23 1993-12-27 Chemiefaser Lenzing Ag Aminoxide
AT399519B (de) * 1993-09-14 1995-05-26 Chemiefaser Lenzing Ag Form- bzw. spinnmasse enthaltend cellulose und verfahren zur herstellung cellulosischer formkörper
AT402410B (de) * 1995-04-19 1997-05-26 Chemiefaser Lenzing Ag Verfahren zur herstellung einer cellulosesuspension

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO9627638A1 *

Also Published As

Publication number Publication date
SK115397A3 (en) 1998-02-04
TW442525B (en) 2001-06-23
US5895795A (en) 1999-04-20
WO1996027638A1 (fr) 1996-09-12
CA2214402A1 (fr) 1996-09-12
PL322109A1 (en) 1998-01-05
JPH11501071A (ja) 1999-01-26
CN1177364A (zh) 1998-03-25
AU4941696A (en) 1996-09-23
KR19980701923A (ko) 1998-06-25

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