WO2002075029A1 - Method for producing cellulose/cellulose triacetate fabrics - Google Patents

Method for producing cellulose/cellulose triacetate fabrics Download PDF

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Publication number
WO2002075029A1
WO2002075029A1 PCT/KR2001/002039 KR0102039W WO02075029A1 WO 2002075029 A1 WO2002075029 A1 WO 2002075029A1 KR 0102039 W KR0102039 W KR 0102039W WO 02075029 A1 WO02075029 A1 WO 02075029A1
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WIPO (PCT)
Prior art keywords
cellulose
fibers
alkali
fabrics
diacetate
Prior art date
Application number
PCT/KR2001/002039
Other languages
French (fr)
Inventor
Ik-Soo Kim
Byoung-Hak Kim
Jong-Soo Ahn
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Sk Chemicals Co., Ltd
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Publication of WO2002075029A1 publication Critical patent/WO2002075029A1/en

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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • 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
    • 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

Definitions

  • the present invention relates to a novel method for producing fabrics in which cellulose is conjugated with cellulose triacetate.
  • Cellulose acetate fibers such as cellulose diacetate fibers and cellulose triacetate fibers, are deacetylated or saponified with alkali to form cellulose fibers.
  • cellulose diacetate fibers can be more easily saponified, in comparison with cellulose triacetate fibers.
  • the present inventors in consideration of the above fact, have conducted extensive studies into the production of cellulose/cellulose triacetate conjugated fabrics, resulting in the finding that strong alkai alone or in combination with weak alkali 'can selectively saponify the cellulose diacetate in cellulose diacetate/cellulose triacetate conjugated fibers, and various color tones can be expressed on the resulting conjugated fabrics consisting of cellulose and celluose triacetate, which have different intrinsic dyeing characteristics from each other.
  • the above object could be accomplished by a provision of a method for producing a cellulose/cellulose triacetate fabric, wherein a conjugated fabric comprising cellulose diacetate fibers with a degree of substitution of 2.0 to 2.75 and cellulose triacetate fibers with a degree of substitution of 2.75 or higher is treated with alkali to convert the cellulose diacetate to cellulose.
  • Fig. 1 is an IR spectrum of a cellulose fiber converted from of a cellulose diacetate fiber by the alkali treatment in Example 3.
  • Fig. 2 is an IR spectrum of the cellulose triacetate fibers of the fabric obtained by alkali treatment according to Example 3.
  • cellulose diacetate/cellulose triacetate fabrics used as a raw material in the present invention means any fabric in which cellulose diacetate is conjugated with cellulose triacetate alone or in combination with other types of fibers.
  • Rayon fibers which are artificial fibers with the same chemical structure as cellulose, are defined as regenerated cellulose fibers, in which 15% or fewer hydroxyl groups are substituted (Fibers Chemistry, Lewin Eli M. Pearce, Dekker p.914, 1985), and usually used in high-grade applications with favorable intrinsic brightness, specific gravity, and sense of touch.
  • Natural and regenerated cellulose fibers have the crystalline structures of cellulose I and II, respectively, while a mixed crystalline structure of cellulose II and IN is found in the cellulose fibers produced by saponification of cellulose diacetate, which are measured to have a crystallinity of 14 to 34% (by a gravimetric method) and a birefringence of 0.012 to 0.024.
  • Cellulose fibers obtained by the saponification of cellulose diacetate fibers are a kind of rayon fibers.
  • the cellulose fibers prepared from cellulose diacetate range from 1.48 to 1.51 gm/cm 3 in specific gravity, 1.2 to 2.5gf/de in tensile strength, 20 to 50% in ductility, and 12 to 13 % in moisture regain under standard conditions. These physical properties are similar to those of general rayon fibers.
  • the saponification of cellulose diacetate/cellulose triacetate fabrics is done with strong alkali, or with strong alkali and weak alkali in one bath or two baths.
  • alkali compounds useful in the saponification of the present invention include alkali metal hydroxides, such as sodium hydroxide, alkali earth metal hydroxides, such as calcium hydroxide, and alkali metal carbonates, such as sodium carbonate.
  • alkali compounds may be used independently or in combination with a saponification promoter.
  • a saponification promoter Well known are those which are based on phosphonium or quaternary ammonium.
  • Examples of commercially available saponification promoters include ⁇ EORATE ⁇ CB of Korea Fine
  • alkali is used as an aqueous solution and in the amount of 10 to 60 wt% of cellulose diacetate fibers.
  • the saponification to convert cellulose diacetate fibers to cellulose fibers is performed by dipping the conjugated fabrics in the aqueous alkaline solution at a temperature of 70 °C or higher, more preferably 70 °C to 130°C, for 1 to 120 minutes, once or twice.
  • the cellulose/cellulose triacetate fabrics produced by the selective saponification of the present invention is treated with a disperse dye, which is usually used in dyeing of polyester, cellulose diacetate, cellulose triacetate, the cellulose fibers converted from cellulose diacetate remain undyed.
  • a reactive dye can dye the converted cellulose fibers, but cannot dye the other fibers.
  • a weight loss of a sample is defined as a percentage of a value obtained by dividing a difference between sample weights before and after alkali treatment with the sample weight before alkali treatment.
  • Polyester-conjugated satin fabrics (warp 70d/20f, warp density 283 ply/inch, weft 200d/57f, weft density 88 ply/inch) comprising, as warps, cellulose triacetate fibers with a degree of acetyl substitution of 2.9 or higher and, as wefts, diacetate fibers with a degree of acetyl substitution of 2.5, were scoured and dried.
  • Into a liquid dyeing machine were charged the satin fabrics and water, along with
  • Example 1 The procedure of Example 1 was repeated except that the amount of NaOH was varied as described in Table 1 , below.
  • cellulose diacetate fibers are reduced in denier, but increased in strength and elongation when the cellulose diacetate fibers are converted to cellulose fibers.
  • cellulose triacetate fibers are not changed in their physical properties.

Abstract

Disclosed is a method for producing cellulose/cellulose triacetate fabrics. The method is characterized by the alkali treatment of a conjugated fabric comprising cellulose diacetate fibers with a degree of substitution of 2.0 to 2.75 and cellulose triacetate fibers with a degree of substitution of 2.75 or higher to convert the cellulose diacetate fibers into cellulose fibers.

Description

METHOD FOR PRODUCING CELLULOSE/CELLULOSE TRIACETATE
FABRICS
TECHNICAL FIELD
The present invention relates to a novel method for producing fabrics in which cellulose is conjugated with cellulose triacetate.
BACKGROUND ART
Cellulose acetate fibers, such as cellulose diacetate fibers and cellulose triacetate fibers, are deacetylated or saponified with alkali to form cellulose fibers. Generally cellulose diacetate fibers can be more easily saponified, in comparison with cellulose triacetate fibers.
DISCLOSURE OF THE INVENTION
The present inventors, in consideration of the above fact, have conducted extensive studies into the production of cellulose/cellulose triacetate conjugated fabrics, resulting in the finding that strong alkai alone or in combination with weak alkali 'can selectively saponify the cellulose diacetate in cellulose diacetate/cellulose triacetate conjugated fibers, and various color tones can be expressed on the resulting conjugated fabrics consisting of cellulose and celluose triacetate, which have different intrinsic dyeing characteristics from each other.
Therefore, it is an object of the present invention to provide a novel method for producing cellulose/cellulose triacetate fabrics.
Based on the present invention, the above object could be accomplished by a provision of a method for producing a cellulose/cellulose triacetate fabric, wherein a conjugated fabric comprising cellulose diacetate fibers with a degree of substitution of 2.0 to 2.75 and cellulose triacetate fibers with a degree of substitution of 2.75 or higher is treated with alkali to convert the cellulose diacetate to cellulose.
BRIEF DESCRIPTION OF THE DRAWINGS
The above and other objects, features and other advantages of the present invention will be more clearly understood from the following detailed description taken in conjunction with the accompanying drawings, in which:
Fig. 1 is an IR spectrum of a cellulose fiber converted from of a cellulose diacetate fiber by the alkali treatment in Example 3.
Fig. 2 is an IR spectrum of the cellulose triacetate fibers of the fabric obtained by alkali treatment according to Example 3.
BEST MODES FOR CARRYING OUT THE INVENTION
Before the present method for producing cellulose/cellulose triacetate fabrics is disclosed or described, it is to be understood that the terminology used therein is for the purpose of describing particular embodiments only and is not intended to be limiting. The term "cellulose diacetate/cellulose triacetate fabrics" used as a raw material in the present invention means any fabric in which cellulose diacetate is conjugated with cellulose triacetate alone or in combination with other types of fibers.
Rayon fibers, which are artificial fibers with the same chemical structure as cellulose, are defined as regenerated cellulose fibers, in which 15% or fewer hydroxyl groups are substituted (Fibers Chemistry, Lewin Eli M. Pearce, Dekker p.914, 1985), and usually used in high-grade applications with favorable intrinsic brightness, specific gravity, and sense of touch.
Upon saponification of cellulose diacetate with alkali, its acetyl groups are converted to hydroxyl groups with concomitant rearrangement of molecular chains from an amorphous form to a crystalline form by folding or packing. Natural and regenerated cellulose fibers have the crystalline structures of cellulose I and II, respectively, while a mixed crystalline structure of cellulose II and IN is found in the cellulose fibers produced by saponification of cellulose diacetate, which are measured to have a crystallinity of 14 to 34% (by a gravimetric method) and a birefringence of 0.012 to 0.024.
Cellulose fibers obtained by the saponification of cellulose diacetate fibers are a kind of rayon fibers. The cellulose fibers prepared from cellulose diacetate range from 1.48 to 1.51 gm/cm3 in specific gravity, 1.2 to 2.5gf/de in tensile strength, 20 to 50% in ductility, and 12 to 13 % in moisture regain under standard conditions. These physical properties are similar to those of general rayon fibers.
In accordance with the present invention, the saponification of cellulose diacetate/cellulose triacetate fabrics is done with strong alkali, or with strong alkali and weak alkali in one bath or two baths.
Examples of alkali compounds useful in the saponification of the present invention include alkali metal hydroxides, such as sodium hydroxide, alkali earth metal hydroxides, such as calcium hydroxide, and alkali metal carbonates, such as sodium carbonate. Such alkali compounds may be used independently or in combination with a saponification promoter. Well known are those which are based on phosphonium or quaternary ammonium. Examples of commercially available saponification promoters include ΝEORATE ΝCB of Korea Fine
Products, which is a phosphonium based saponification promoter; and KF ΝEORATE ΝA-40 of Korea Fine Products, DYK-1125 of IPPOSHA Co., Japan, DXY-10N of IPPOSHA Co., Japan, caserine PES of MEISEI CHEMICAL WORKS, LTD., Japan, caserine PEL of MEISEI CHEMICAL WORKS, LTD., Japan, caserine PEF of MEISEI CHEMICAL WORKS, LTD., Japan, and
SNOGEN PDS of Dae Young Chemical, Co., Korea, all being quaternary ammonium-based saponified promoter.
For use in saponification, alkali is used as an aqueous solution and in the amount of 10 to 60 wt% of cellulose diacetate fibers. The saponification to convert cellulose diacetate fibers to cellulose fibers is performed by dipping the conjugated fabrics in the aqueous alkaline solution at a temperature of 70 °C or higher, more preferably 70 °C to 130°C, for 1 to 120 minutes, once or twice.
When the cellulose/cellulose triacetate fabrics produced by the selective saponification of the present invention is treated with a disperse dye, which is usually used in dyeing of polyester, cellulose diacetate, cellulose triacetate, the cellulose fibers converted from cellulose diacetate remain undyed. On the other hand, a reactive dye can dye the converted cellulose fibers, but cannot dye the other fibers.
A better understanding of the present invention may be obtained in light of the following examples which are set forth to illustrate, but are not to be construed to limit the present invention.
In the following examples, a weight loss of a sample is defined as a percentage of a value obtained by dividing a difference between sample weights before and after alkali treatment with the sample weight before alkali treatment.
EXAMPLE 1
Polyester-conjugated satin fabrics (warp 70d/20f, warp density 283 ply/inch, weft 200d/57f, weft density 88 ply/inch) comprising, as warps, cellulose triacetate fibers with a degree of acetyl substitution of 2.9 or higher and, as wefts, diacetate fibers with a degree of acetyl substitution of 2.5, were scoured and dried. Into a liquid dyeing machine were charged the satin fabrics and water, along with
NaOH at an amount of 38 wt% based on diacetate, followed by temperature elevation from 30°C to 100°C at a rate of 2°C/min. After the maximum temperature was maintained for 30min, the temperature was allowed to decrease to 30°C at a rate of 2°C/min. Following the drainage of the liquid, the remaining alkali was removed by washing with water. Weight loss of the fabrics was measured to be 13.3%.
In the IR spectra of the resulting fabrics, obtained by use of IR spectroscopic analyzer (MAGNA 750, Nicolet, USA), a peak at 1760cm"1, corresponding to a cellulose carbonyl, disappeared from a portion which was initially cellulose diacetate, while the peak was found to remain in a portion which was initially cellulose triacetate. That is to say, there were obtained fabrics in which cellulose, cellulose triacetate and polyester were conjugated.
The weight loss percentages of the alkali-treated . fabrics were calculated and their cellulose fibers, along with untreated fabrics, were measured for physical properties. The results are given in Tables 2 and 3, below.
EXAMPLES 2 TO 5
The procedure of Example 1 was repeated except that the amount of NaOH was varied as described in Table 1 , below.
TABLE 1
Figure imgf000006_0001
TABLE 2
Figure imgf000006_0002
Figure imgf000007_0001
TABLE 3
Figure imgf000007_0002
As stated above, cellulose diacetate fibers are reduced in denier, but increased in strength and elongation when the cellulose diacetate fibers are converted to cellulose fibers. In Examples 1 to 3, it is confirmed that cellulose triacetate fibers are not changed in their physical properties. The fabrics obtained in Examples 4 and 5, whose weight loss was relatively high, were found to be reduced in the denier, strength and elongation of cellulose triacetate fibers, suggesting that saponification also occurred in the triacetate portion.
The present invention has been described in an illustrative manner, and it is to be understood that the terminology used is intended to be in the nature of description rather than of limitation. Many modifications and variations of the present invention are possible in light of the above teachings. Therefore, it is to be understood that within the scope of the appended claims, the invention may be practiced otherwise than as specifically described.

Claims

1. A method for producing a cellulose/cellulose triacetate fabric, wherein a conjugated fabric comprising cellulose diacetate fibers with a degree of substitution of 2.0 to 2.75 and cellulose triacetate fibers with a degree of substitution of 2.75 or higher is treated with alkali to convert the cellulose diacetate to cellulose.
2. The method as set forth in claim 1, wherein the conjugated fabric is treated with strong alkali, or a combination of strong alkali and weak alkali in one bath or two baths.
3. The method as set forth in claim 2, wherein the alkali is added in combination with a saponifying promoter.
4. The method as set forth in any one of claims 1 to 3, wherein the conjugated fabric further comprises a fiber different from cellulose diacetate and cellulose triacetate.
PCT/KR2001/002039 2001-03-21 2001-11-27 Method for producing cellulose/cellulose triacetate fabrics WO2002075029A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR2001/014489 2001-03-21
KR10-2001-0014489A KR100472827B1 (en) 2001-03-21 2001-03-21 Method for producing cellulous/cellulous triacetate fabric

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WO2002075029A1 true WO2002075029A1 (en) 2002-09-26

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1792635A1 (en) * 2004-08-30 2007-06-06 Kaneka Corporation Granulocyte adsorbent
EP2368915A1 (en) * 2010-03-26 2011-09-28 Taiwan Textile Research Institute Cellulose-based masterbatch with improved breaking elongation, application thereof and method for preparing the same
TWI399399B (en) * 2010-03-30 2013-06-21 Taiwan Textile Res Inst Cellulose masterbatch with network structure, application thereof and method for preparing the same

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KR100472831B1 (en) * 2001-03-21 2005-03-07 에스케이케미칼주식회사 Method for producing fabric of hollow rayon/rayon mixed fibers with different shrinkage
KR100406884B1 (en) * 2001-05-22 2003-11-21 에스케이케미칼주식회사 Method for producing fabric of cellulose mixed fibers with different shrinkages
KR100466878B1 (en) * 2001-09-13 2005-01-24 에스케이케미칼주식회사 Method of producing Cellulose conjugate fabrics having a different dyeing property

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JPH07216651A (en) * 1994-01-19 1995-08-15 Mitsubishi Rayon Co Ltd Acetate fiber and its production
JPH083820A (en) * 1994-06-17 1996-01-09 Mitsubishi Rayon Co Ltd Acetate conjugate fiber having latent crimp and manufacture thereof
JPH08158197A (en) * 1994-12-07 1996-06-18 Toyobo Co Ltd Production of stretchable cellulosic woven fabric
JPH09143819A (en) * 1995-11-21 1997-06-03 Mitsubishi Rayon Co Ltd Cellulose acetate conjugated fiber and its production

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KR100471004B1 (en) * 2000-03-27 2005-03-07 에스케이케미칼주식회사 Rayon fiber, fiber product, film and preparations thereof
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JPH07102419A (en) * 1993-10-04 1995-04-18 Mitsubishi Rayon Co Ltd Acetate composite fiber and its production method
JPH07216651A (en) * 1994-01-19 1995-08-15 Mitsubishi Rayon Co Ltd Acetate fiber and its production
JPH083820A (en) * 1994-06-17 1996-01-09 Mitsubishi Rayon Co Ltd Acetate conjugate fiber having latent crimp and manufacture thereof
JPH08158197A (en) * 1994-12-07 1996-06-18 Toyobo Co Ltd Production of stretchable cellulosic woven fabric
JPH09143819A (en) * 1995-11-21 1997-06-03 Mitsubishi Rayon Co Ltd Cellulose acetate conjugated fiber and its production

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1792635A1 (en) * 2004-08-30 2007-06-06 Kaneka Corporation Granulocyte adsorbent
EP1792635B1 (en) * 2004-08-30 2014-05-21 Kaneka Corporation Granulocyte adsorbent
EP2368915A1 (en) * 2010-03-26 2011-09-28 Taiwan Textile Research Institute Cellulose-based masterbatch with improved breaking elongation, application thereof and method for preparing the same
US8188164B2 (en) 2010-03-26 2012-05-29 Taiwan Textile Research Institute Cellulose-based masterbatch with improved breaking elongation, application thereof and method for preparing the same
US8372193B2 (en) 2010-03-26 2013-02-12 Taiwan Textile Research Institute Cellulose-based masterbatch with improved breaking elongation, application thereof and method for preparing the same
TWI393807B (en) * 2010-03-26 2013-04-21 Taiwan Textile Res Inst Cellulose masterbatch with improved breaking elongation, application thereof and method for preparing the same
TWI399399B (en) * 2010-03-30 2013-06-21 Taiwan Textile Res Inst Cellulose masterbatch with network structure, application thereof and method for preparing the same

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KR100472827B1 (en) 2005-03-07
KR20020074611A (en) 2002-10-04

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