WO2014118804A1 - Fibre colorée en noir et formulation de colorant noir pour préparer ladite fibre - Google Patents

Fibre colorée en noir et formulation de colorant noir pour préparer ladite fibre Download PDF

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Publication number
WO2014118804A1
WO2014118804A1 PCT/IN2014/000069 IN2014000069W WO2014118804A1 WO 2014118804 A1 WO2014118804 A1 WO 2014118804A1 IN 2014000069 W IN2014000069 W IN 2014000069W WO 2014118804 A1 WO2014118804 A1 WO 2014118804A1
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WO
WIPO (PCT)
Prior art keywords
formulation
grams
range
black
total weight
Prior art date
Application number
PCT/IN2014/000069
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English (en)
Inventor
Indrannel Chatterjee RASIKA
Lodha Preeti
Kedar VAIBHAV
Original Assignee
Aditya Birla Science & Technology Company Limited
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.)
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Publication of WO2014118804A1 publication Critical patent/WO2014118804A1/fr

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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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D17/00—Pigment pastes, e.g. for mixing in paints
    • 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
    • D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
    • D01F2/08—Composition of the spinning solution or the bath
    • D01F2/12—Addition of delustering agents to the spinning solution
    • D01F2/14—Addition of pigments

Definitions

  • the present invention is directed to a black coloredfiber. More particularly the present invention is directed to a black coloredfiber prepared by dope-dyeing using a black colorant formulation, wherein the black colorant formulationincludesa surface active agent, a steric stabilizer,an anti-coagulating agent, a defoamer, and an alkali.
  • the black colorant formulation includesa surface active agent, a steric stabilizer,an anti-coagulating agent, a defoamer, and an alkali.
  • the dye enters into the compact structure of the fiber, for example, cellulose fiber, which results in low bleeding of dye from the fiber.
  • the compact structure of the fiber for example, cellulose fiber
  • the resultant fiber/fabric has a smooth surface feel.
  • the depth of shade of the solid color obtained in dope dyed fabric is typically lower than that achieved using piece-dyeing.
  • Methodhods of increasing the depth of shade by increasing the dye-loading in the fibre results in deterioration in spinning performance and adversely affects fibre physical properties.
  • a black coloredfiber has a lightness value 'L' in a range of from about 13.0 to about 9.0 and a color strength 'K/S' in a range of from about 22to about 50.
  • a black colored fiber is prepared by dope-dyeing using a black colorant formulation.
  • the black colorant formulation includes carbon black, a surface active agent, a steric stabilizer, an anti- coagulating agent, a defoamer, and an alkali.
  • the black colored fiber has a lightness value 'L' in a range of from about 13.0 to about 9.0and a color strength 'K/S' in a range of from about 22to about 50.
  • a black colorant formulation is provided in yet anotherembodiment.
  • the colorant formulation includes carbon black, a surface active agent, an anti-coagulating agent, a steric stabilizer,and a defoamer.
  • the carbon black is present in an amount in a range of from about30 grams to about 42grams based on the total weight of the formulation.
  • the surface active agent is present in an amount in a range of from about 2grams toabout 22gramsbased on the total weight of the formulation.
  • the anti-coagulating agent is present in an amount in a range of from about 0.1 grams to about 1.5 gramsbased on the total weight of the formulation.
  • the steric stabilizer is present in an amount in a range of from about0.5grams to about 2gramsbased on the total weight of the formulation.
  • the defoaming agent is present in arange of from about 0.1 grams to about 13 gramsbased on the total weight of the formulation.
  • the pH of the formulation is in a range of from about 8 to about 13.
  • the aqueous media is present in an amount in a range of from about 40 grams to about 60 gramsbased on the total weight of the formulation.
  • a black colorant pigment in still yet another embodiment, is provided a black colorant pigment.
  • the black colorant formulation described herein is then milled to obtain a black colorant pigment having an average particle size in the range of from about 60 nanometers to about 500 nanometers.
  • a black colored fiber-precursor in still yet another embodiment, is provided a black colored fiber-precursor.
  • the black colored fiber-precursor includes the black colorant pigment described herein above and a polymer dope.
  • the black colored fiber-precursor is spun to provide a black colored fiber.
  • a black colored fiber having a black colored pigment entrapped in the fiber during processing.
  • a process for preparing a black colorant pigment comprises a first step of mixing carbon black with a surface active agent, an anti-coagulating agent, a steric stabilizer, a defoamer, and water to form a black colorant formulation.
  • the black colorant formulation is then milled to obtain a black colorantpigment having an average particle size in the range of from about60 nanometers to about 500nanometers.
  • an improved black coloredfiber may be made possible.
  • the above disclosed technique also aims to provide an improved, efficient, and cost effective black colorant formulation, black colorant pigment, and black colored fiber-precursor.
  • FIG. 1 illustrates a visual representation of the dispersed state of the black colorant pigment prepared in accordance with the embodiments of the present invention in comparison to a PRIOR ART pigment.
  • Embodiments of the invention as disclosed herein provide ablack coloredfiber.
  • the invention also includes ablack colorant formulation.
  • the black colorant formulation is then used to prepare a black colorant pigment.
  • a black colored fiber-precursor is prepared using the black colorant pigment and a polymer dope.
  • the black colored fiber-precursor is then employed to prepare the black coloredfiber.
  • the black colorant formulation includes a surface active agent,an anti-coagulating agent, a steric stabilizer, and a defoamer, in an aqueous media with an alkaline pH.
  • the black colorant precursordisclosed herein hasan improved dispersibility and is accordingly capable of providing a fiber with a deeper shade of black(i.e., having a W lower 'L' value and a higher 'K/S value) than what is commercially available.
  • aqueous media refers to water.
  • first, second, third, etc. describe various elements or steps and these elements or steps should not be limited by these terms. These terms may be only used to distinguish one element or step from another element or step. Terms such as “first”, “second”, and other numerical terms when used herein do not imply a sequence or order unless clearly indicated by the context. Thus, first step discussed below could be termed a second step without departing from the teachings of the exemplary embodiments.
  • a black colored fiber has a lightness value 'L' in a range of from about 13.0 to about 9.0 and a color strength 'K/S' in a range of from about 22 to about 50.
  • the Lightness value measurements are based on a method available in literature called CIELAB and do not have any units.
  • the black colored fiber is prepared by dope-dyeing using a black colorant formulation.
  • the black colorant formulation includes carbon black, a surface active agent, a steric stabilizer, an anti-coagulating agent, a defoamer, and an alkali as described hereinabove.
  • the amount of carbon black employed may be determined by a person skilled in the art based on the fiber being dyed and the fiber forming process being employed. In one embodiment, as described herein, the amount of carbon black employed in the black colorant formulation is in a range of from about 30 grams to about 42 grams based on the total weight of the formulation. In another embodiment the amount of carbon black employed in the black colorant formulation is in a range of from about 32 grams to about 40 gramsbased on the total weight of the formulation. In yet another embodiment the amount of carbon black employed in the black colorant formulation is in a range of from about 35 grams to about 38 gramsbased on the total weight of the formulation.
  • the surface active agents used herein act as wetting agentsenabling improved dispersion of the contents that comprise the colorant formulation.
  • the surface active agent may include but are not limited to anionic, cationic, zwitterionie surface active agents with sulphate, sulphonate, carbonate and its alkaline and alkaline earth metal salts as head group and hydrogen tail Cg-C i 8 carbon.
  • the surface active agent includes the surface active agent is at least one non-ionic or anionic surface active agent selected from a group of non-ionic or anionic surface active agents consisting of alkyl phenoxy ethoxylated non-ionic surface active agents and ethoxylated alkyl alcohol surface active agents, polyethylene-block-poly propylene glycol-block -polyethylene glycol, and ethylenediamine tetrakis(propylene oxide-block-ethylene oxide) tetrol.
  • a group of non-ionic or anionic surface active agents consisting of alkyl phenoxy ethoxylated non-ionic surface active agents and ethoxylated alkyl alcohol surface active agents, polyethylene-block-poly propylene glycol-block -polyethylene glycol, and ethylenediamine tetrakis(propylene oxide-block-ethylene oxide) tetrol.
  • Suitable examples of surface active agents include but are not limited to Disperlon 360, Usol K985, Tamol, BYK2012, BY 190, Disponill080, Disperlon AQ380, Lutensol XL, Aerosol OS, Aerosol C61, Auxi WET, AuxiDisp 100, Auxisil WHS, Aerosol GPG, SDBS, Galaxy LAO, Auxi Wet NP 100, Capstone FS 64, Wetting Agent FS 1010, Diosperlon AQ600, Disperlon AQ 800, Auxi Wet CRS, SM 8709, Dow Wetting Agent, and Bloomer.
  • the amount of surface active agent employed in the black colorant formulation is in a range of from about 2 grams to about 22 grams based on the total weight of the formulation. In another embodiment the amount of surface active agent employed in the black colorant formulation is in a range of from about 3 grams to about 20 gramsbased on the total weight of the formulation. In yet another embodiment the am ⁇ nt of surface active agent employed in the black colorant formulation is in a range of from about 5 grams to about 15 gramsbased on the total weight of the formulation.
  • the anti-coagulating agent usedherein may assist in reducing the cohesive force between dispersedcarbon black particles.
  • Suitable examples of anti-coagulating agent include but are not limited to polymers such as acrylates and phenolates more specifically polyacrylate co-polymers.
  • the amount of anticoagulation agent employed in the black colorant fonnulation is in a range of from about 0.1 grams to about 1.5 grams based on the total weight of the formulation.
  • the amount of anti-coagulation agent employed in the black colorant fonnulation is in a range of from about 0.2 grams to about 1.2 gramsbased on the total weight of the fonnulation.
  • the amount of anti-coagulation agent employed in the black colorant fonmilation is in a range of from about 0.5 grams to about 1 grambased on the total weight of the formulation.
  • the defoamer(defoaming agent) used herein provides the reduced foaming in the fonnulation during milling.
  • Suitable examples of defoamers include but are not limited W tosilicon based defoamers.
  • the amount of defoaming agent employed in the black colorant formulation is in a range of from about 0.1 grams to about 13 grams based on the total weight of the formulation. In another embodiment the amount of defoaming agent employed in the black colorant formulation is in a range of from about 0.2 grams to about 12 gramsbased on the total weight of the formulation. In yet another embodiment the amount of defoaming agent employed in the black colorant formulation is in a range of from about 0.5 grams to about 10 gramsbased on the total weight of the formulation.
  • Steric stabilization is the process by which adsorbednonionic surfactantsor polyiners produce strong repulsion between particles and droplets in a dispersion.
  • Suitable examples of steric stabilizers include but are not limited to diethylene glycol and polyethylene glycol.
  • the amount of steric stabilizers employed in the black colorant formulation is in a range of from about 0.5 grams to about 2 grams based on the total weight of the formulation.
  • the amount of steric stabilizers employed in the black colorant formulation is in a range of from about 0.6 grams to about 1.8 gramsbased on the total weight of the formulation.
  • the amount of steric stabilizers employed in the black colorant formulation is in a range of from about 0.7 grams to about 1.5 gramsbased on the total weight of the formulation.
  • Stabilizing black colorant pigment in alkaline pH range of 8 to 13 helps to maintain the satiability of dispersion in cellulose dope.
  • An alkali may be used to maintain the pH in a range of from about 8 to 13, for example, alkali and alkaline metal hydroxides.
  • the carbon black, the surface active agent, the anti- coagulating agent, the steric stabilizer, and the defoamer may be dispersed in an aqueous media.
  • the aqueous media is present in an amount in a range of from about 40 grams to about 60 gramsbased on the total weight of the formulation.
  • the aqueous media is present in an amount in a range of from about 42 grams to about 58 gramsbased on the total weight of the formulation.
  • the aqueous media is present in an amount in a range of from about 45 grams to about 55 gramsbased on the total weight of the formulation.
  • the black colorant pigment described herein has an average particle size in the range of from about 60 nanometers to about 500 nanometers. In another embodiment, the black colorant pigment described herein has an average particle size in the range of from about 70 nanometers to about 490 nanometers. In yet another embodiment, the black colorant pigment described herein has an average particle size in the range of from about 75nanometers to about 480 nanometers. Using a pigment having this particle size not only provides a smooth spinning without any pressure built-up in the fiber forming process but also provides uniform coloring in the resultant black colored fiber.
  • the black colored pigment may be obtained by processing the black colored formulation to obtain a particle size in the range of from about 60 nanometers to about 500 nanometers.
  • the black colored formulation may be subjected to a milling process to obtain the black colored pigment.
  • a black colored fiber-precursor includes the black colorant pigment described herein above and a polymer dope.
  • the black colored fiber-precursor is spun to provide a black colored fiber.
  • the polymer dope may includecellulosic material such as viscose, rayon, and the like.
  • a black colored fiber having a black colored pigment entrapped in the fiber during processing.
  • the entrapment of the fiber during processing is obtained by dope-dyeing as described herein.
  • the black colored pigment and process employed herein result in a black colored fiber with smooth fiber surface, less use of dye pigment in process, high wash durability, and improved color fastness.
  • a process for preparing a black colorant pigment comprises a first step of mixing carbon black with a surface active agent, an anti-coagulating agent, a steric stabilizer, a defoamer, and water to form a black colorant formulation.
  • the black colorant formulation is then milled to obtain a black colorant pigment having an average particle size in the range of from about 60 nanometers to about 500 nanometers.
  • the colorant composition was made using the following process.
  • a formulation was made by charging asurface active agentauxiwet, sokalan FB-15, DEG,alkali, and carbon black with distilled mineral water to a one liter reactor.
  • the resultant mixture was stirred for about lhour at a temperature of about 25 degrees Celsius using an overhead stirrerat a stirring speed of about 500revolutions per minute to form a black colorant formulation.
  • Example 4, 5, and 6 and Comparative Example 2 Preparation of black colorant Pigment
  • the black colorant formulation prepared in Example 1 , 2, and 3 were individually milled in a Retsch MM 200 mixer mill using steel balls beads for about four hours to reduce the maximum particle size to below 0.5 microns.
  • the particle size was measured using Mastersizer 2000 and Zetasizer nano zs.
  • the resultant black colorant pigment had a disperseability of about 60 nanometer to about 500nanometer(D90) in an aqueous media.
  • FIG. 1 illustrates a visual representation of the dispersed state of the black colorant pigment prepared in accordance with the embodiments of the present invention (Example 4) in comparison to a PRIOR ART pigment (Comparative Example 2). As shown in FIG.
  • Example 7, 8,and 9 and Comparative Example 3 Preparation of black colored fiber-precursor and black colored fiber.
  • Example 4 The black colorantpigment prepared in Example 4, 5, and 6 were independently mixed with the viscose dopeindicated in Table 2 at 1 OOOrevolutions per minute to form black colored fiber-precursor in Examples 7, 8, and 9 respectively.
  • the resultant black colored fiber-precursor was individually spun through a spinneret 65 micron 40 holes, at aspinning rate of about 2.5 millilitres per minute to get a blackcoloredcellulosefiber.
  • the black colored cellulose fiber was then first washed with hot water at 90 degrees Celsius for 5 minutes.
  • the water wash was followed by an acid wash at 90 degrees Celsius using 17grams per liter aqueous sulphuric acid for 5 minutes followed by an alkali wash using 0.2 grams per liter aqueous sodium hydroxide solution at 90 degrees Celsius for 5 minutes.
  • the color strength of the black coloredfiber was measuredusing X-rite colour spectrophotometer. The absolute color values obtained are described in Table 3 below.
  • Example 7 The black coloured fiber prepared in Example 7, 8, and 9 were also characterized using the scanning electron microscopy (SEM). As shown in Table 3, the K/S values for Examples 7 to 9 is greater than that for the comparative sample of black fiber.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Artificial Filaments (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

L'invention concerne une fibre colorée en noir. La fibre colorée en noir présente un indice de clarté "L" se situant dans une plage d'environ 13,0 à environ 9,0 et une intensité de couleur 'K/S se situant dans une plage d'environ 22 à environ 50. Une formulation de colorant noir et un pigment colorant noir sont également décrits. L'invention concerne également des procédés.
PCT/IN2014/000069 2013-01-29 2014-01-29 Fibre colorée en noir et formulation de colorant noir pour préparer ladite fibre WO2014118804A1 (fr)

Applications Claiming Priority (2)

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IN259/MUM/2013 2013-01-29
IN259MU2013 2013-01-29

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WO2014118804A1 true WO2014118804A1 (fr) 2014-08-07

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106283244A (zh) * 2016-08-26 2017-01-04 阜宁澳洋科技有限责任公司 一种免印染黑色粘胶短纤维的制备方法
CN106916491A (zh) * 2015-12-24 2017-07-04 苏州宝化炭黑有限公司 高固含量、高着色力的炭黑水性色浆制备方法
CN109385919A (zh) * 2017-08-04 2019-02-26 福建大联新型材料发展有限公司 一种超纤合成革的制备方法
EP3696317A1 (fr) 2019-02-15 2020-08-19 Lenzing Aktiengesellschaft Fibre teinte dans la masse et son procédé de fabrication
CN115821409A (zh) * 2022-10-26 2023-03-21 赛得利(江苏)纤维有限公司 一种提高原液着色粘胶纤维黑度的方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2233344A (en) * 1937-01-18 1941-02-25 Ind Rayon Corp Manufacture of pigment-colored extrusion products
EP0843030A1 (fr) * 1995-07-31 1998-05-20 Asahi Kasei Kogyo Kabushiki Kaisha Fibres de polyester et produit de coloration d'une etoffe constituee d'un melange fibreux renfermant ces fibres de polyester
EP2146797A1 (fr) * 2007-05-10 2010-01-27 Clariant Finance (BVI) Limited Préparations de pigments à base d'eau

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2233344A (en) * 1937-01-18 1941-02-25 Ind Rayon Corp Manufacture of pigment-colored extrusion products
EP0843030A1 (fr) * 1995-07-31 1998-05-20 Asahi Kasei Kogyo Kabushiki Kaisha Fibres de polyester et produit de coloration d'une etoffe constituee d'un melange fibreux renfermant ces fibres de polyester
EP2146797A1 (fr) * 2007-05-10 2010-01-27 Clariant Finance (BVI) Limited Préparations de pigments à base d'eau

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106916491A (zh) * 2015-12-24 2017-07-04 苏州宝化炭黑有限公司 高固含量、高着色力的炭黑水性色浆制备方法
CN106283244A (zh) * 2016-08-26 2017-01-04 阜宁澳洋科技有限责任公司 一种免印染黑色粘胶短纤维的制备方法
CN106283244B (zh) * 2016-08-26 2018-11-23 阜宁澳洋科技有限责任公司 一种免印染黑色粘胶短纤维的制备方法
CN109385919A (zh) * 2017-08-04 2019-02-26 福建大联新型材料发展有限公司 一种超纤合成革的制备方法
EP3696317A1 (fr) 2019-02-15 2020-08-19 Lenzing Aktiengesellschaft Fibre teinte dans la masse et son procédé de fabrication
WO2020165363A1 (fr) 2019-02-15 2020-08-20 Lenzing Aktiengesellschaft Fibre teinte dans la masse et procédé pour sa fabrication
CN115821409A (zh) * 2022-10-26 2023-03-21 赛得利(江苏)纤维有限公司 一种提高原液着色粘胶纤维黑度的方法

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