U.S. patent application number 12/097780 was filed with the patent office on 2009-07-09 for fibre modified by application of an organosiliconate agent, a fibre modifying agent comprising an organosilikonate and a method of modifying a fibre with said agent.
This patent application is currently assigned to KAO CORPORATION. Invention is credited to Seiichi Miyanaga, Keigo Suzuki.
Application Number | 20090176094 12/097780 |
Document ID | / |
Family ID | 38067707 |
Filed Date | 2009-07-09 |
United States Patent
Application |
20090176094 |
Kind Code |
A1 |
Suzuki; Keigo ; et
al. |
July 9, 2009 |
Fibre Modified By Application Of An Organosiliconate Agent, A Fibre
Modifying Agent Comprising An Organosilikonate and A Method of
Modifying A Fibre With Said Agent
Abstract
The present invention relates to a fiber modifying method
including step (i) of contacting an organosiliconate with fiber and
step (ii) of polymerizing the organosiliconate, a modified fiber
modified by this method and a fiber modifying agent containing an
organosiliconate and water.
Inventors: |
Suzuki; Keigo; (Wakayama,
JP) ; Miyanaga; Seiichi; (Tokyo, JP) |
Correspondence
Address: |
OBLON, SPIVAK, MCCLELLAND MAIER & NEUSTADT, P.C.
1940 DUKE STREET
ALEXANDRIA
VA
22314
US
|
Assignee: |
KAO CORPORATION
Chuo-ku, Tokyo
JP
|
Family ID: |
38067707 |
Appl. No.: |
12/097780 |
Filed: |
December 26, 2006 |
PCT Filed: |
December 26, 2006 |
PCT NO: |
PCT/JP2006/326335 |
371 Date: |
June 17, 2008 |
Current U.S.
Class: |
428/391 ;
427/387; 556/400 |
Current CPC
Class: |
C07F 7/0836 20130101;
D06M 15/643 20130101; D21H 11/20 20130101; D21C 9/002 20130101;
D06M 13/513 20130101; Y10T 428/2962 20150115 |
Class at
Publication: |
428/391 ;
427/387; 556/400 |
International
Class: |
D06M 15/643 20060101
D06M015/643; D02G 3/36 20060101 D02G003/36; D06M 13/513 20060101
D06M013/513 |
Foreign Application Data
Date |
Code |
Application Number |
Dec 28, 2005 |
JP |
2005-379643 |
Claims
1. A method of modifying fiber, comprising the following steps (i)
and (ii): (i) contacting an organosiliconate with fiber, and (ii)
polymerizing the organosiliconate.
2. The method according to claim 1, wherein the organosiliconate is
an organosiliconate represented by formula (1):
R.sup.1.sub.p--Si(OM.sup.+).sub.q(OH).sub.4pq (1) wherein R.sup.1
represents a C1 to C6 linear or branched alkyl group or a phenyl
group, M represents a group capable of forming a monovalent cation,
p represents an integer of 1 or 2, and q represents a number in the
range of 0.1 to (4-p).
3. The method according to claim 1, wherein the organosiliconate
comprises a monoalkylsiliconate represented by formula (2) and a
dialkylsiliconate represented by the following formula (3):
R.sup.1Si(OM.sup.+).sub.n(OH).sub.3n (2)
R.sup.1.sub.2Si(OM.sup.+).sub.m(OH).sub.2m (3) wherein R.sup.1
represents a C1 to C6 linear or branched alkyl group or a phenyl
group, M represents a group capable of forming a monovalent cation,
a plurality of R.sup.1 and M may be the same as or different from
one another, n is a number of 0.1 to 3, and m is a number of 0.1 to
2.
4. The method according to claim 1, wherein, in step (i), the
organosiliconate is contacted in an aqueous solution thereof with
fiber.
5. The method according to claim 1, wherein, in step (i), the
organosiliconate is contacted with fiber in the presence of a
surfactant.
6. The method according to claim 1, wherein, in step (ii),
polymerization of the organosiliconate is carried out at 60.degree.
C. or more.
7. The method according to claim 1, which further comprises step
(iii) of washing the modified fiber after step (ii).
8. A modified fiber modified by the method according to claim
1.
9. The modified fiber according to claim 8, wherein the fiber is an
organic fiber.
10. The modified fiber according to claim 8, wherein the surface of
a single fiber is coated thereon with a polymer of the
organosiliconate to a thickness not greater than 1/10 as large as
the diameter of the single fiber.
11. The modified fiber according to claim 8, wherein a polymer of
the organosiliconate is contained in the inside of the single
fiber.
12. A fiber-modifying agent comprising an organosiliconate.
13. The fiber-modifying agent according to claim 12, which further
comprises a surfactant.
Description
FIELD OF THE INVENTION
[0001] The present invention relates to a fiber modifying method
for suitably improving the feel and strength of natural fibers such
as cotton, wool and silk, semisynthetic fibers and regenerated
fibers such as acetate and rayon, pulp and its processed paper, and
nonwoven fabrics, modified fiber having improved feel and strength,
and a fiber modifying agent.
BACKGROUND OF THE INVENTION
[0002] Natural fibers such as cotton, wool, silk and hemp, and pulp
derived from wood are fibrous organic natural polymers derived from
plants and animals and have been used as materials for clothing,
fabrics, paper etc. since ancient times. These natural fibers have
preferable characteristics respectively, and for further improving
these characteristics, various fiber treatment techniques have been
developed.
[0003] For example, softener treatment with an organic cationic
compound is carried out very commonly nowadays to improve the feel
of cotton clothing after washing thereby making it more pliant and
soft or to allow wool clothing originally hardly washable with
water to be washed readily even in the home.
[0004] As a modification method of conferring a drying promoting
effect on fiber, a method of processing cellulose fiber which
includes treating cellulose fiber with an alkali metal hydroxide,
washing the fiber with water, and treating them with a hydrophobic
treating agent such as a resin treating agent, a hydrophobilizing
crosslinking agent or a hydrophobilizing agent is disclosed in JP-A
2003-342875. Further, JP-A 2005-89882 discloses a method of
treating fiber which includes spraying objective fiber with a
water-absorbing, quick-drying property-conferring composition
containing a copolymer consisting of specific monomers including
silicone-containing monomers and an organic solvent and then
evaporating the solvent.
[0005] As a method of modifying paper more toughly, a method of
applying/curing a composition based on an alkoxysilane condensate
is disclosed in JP-A 2002-61094.
SUMMARY OF THE INVENTION
[0006] The present invention provides a fiber modifying method
including the following steps (i) and (ii), a modified fiber
modified by this method, and a fiber modifying agent containing an
organosiliconate and water.
Step (i): step of contacting an organosiliconate with fiber. Step
(ii): step of polymerizing the organosiliconate.
DETAILED DESCRIPTION OF THE INVENTION
[0007] In the prior arts, an organic cationic compound is adsorbed
onto the surface of fiber to bring about softness and a fiber
shrinkage preventing effect at the time of washing, however, the
organic compound is washed away and eliminated in next washing,
thus failing to permanently keep its softening effect.
[0008] In any of the above-described conventional methods of
conferring a drying-promoting effect, the surface of fiber is
significantly hydrophobilized thus seriously lowering moisture
absorptivity/water absorptivity that are the most promising
properties of natural fibers and also deteriorating the original
feel of the fiber, to cause a problem of significantly
deteriorating their comfortable feel upon wearing and use. That is,
it is impossible in the state of arts to confer a drying-promoting
effect on natural fibers while the original moisture absorptivity
and feel of the natural fibers are maintained.
[0009] The method of applying/curing a liquid composition based on
an alkoxysilane condensate is a technique in which the whole of a
paper product as an aggregate of single fiber is strongly condensed
and solidified with a silicon compound, and paper can be formed as
filler into a resin molded product, but the processed product thus
obtained has a problem of deterioration in the original pliability
and moisture absorptivity of paper.
[0010] As described above, a method of suitably improving the
softness, quick-drying property and toughness of natural fibers
while maintaining the feel, moisture absorption/water absorption
functions, inherent in the fiber, has never known up to now.
[0011] The present invention provides a novel fiber modifying
method capable of conferring softness, quick-drying property and
toughness on fiber while maintaining advantages inherent therein, a
fiber modifying agent, and suitably modified fiber.
[0012] According to the present invention, the quick-drying
property, softness and/or toughness can be conferred on fiber,
while the original properties of the fiber are maintained.
[Organosiliconate]
[0013] The organosiliconate in the present invention refers to an
organosilicate compound having at least one hydrocarbon group on a
silicon atom, and at least one siliconate group [--SiOM.sup.+
wherein M.sup.+ is a group capable of forming a monovalent
cation].
[0014] The organosiliconate may be a partial condensation product
(dimer, trimer, tetramer etc.) and is preferably a tetramer or less
for easy permeation into single fiber, more preferably a dimer or
less, even more preferably a monomer.
[0015] The organosiliconate is preferably an organosiliconate
represented by the following formula (1):
R.sup.1.sub.p--Si(OM.sup.+).sub.q(OH).sub.4pq (1)
wherein R.sup.1 represents a C1 to C6 linear or branched alkyl
group or a phenyl group, M represents a group capable of forming a
monovalent cation, p represents an integer of 1 or 2, and q
represents a number in the range of 0.1 to (4-p).
[0016] R.sup.1 is preferably a C1 to C6 alkyl group. Preferable
examples include an alkyl group such as a methyl group, ethyl
group, n-propyl group, isopropyl group, butyl group, isobutyl group
and t-butyl group, and a phenyl group. For improving the softness
of fiber, the number of carbon atoms is preferably in a broad
range. R.sup.1 is more preferably a methyl group or a phenyl group,
more preferably a methyl group, for improving the drying rate of
fiber. For improving the toughness of fiber, R.sup.1 is more
preferably a methyl group.
[0017] M includes alkali metals such as lithium, sodium, potassium,
rubidium and cesium, an ammonium group, and a phosphonium group,
and is preferably an alkali metal such as lithium, sodium or
potassium, or an ammonium group, more preferably sodium or an
ammonium group.
[0018] The number of M's per silicon atom, that is, q, is
preferably 0.5 or more, more preferably 1 or more, from the
viewpoint of the water solubility of the organosiliconate. Every
hydroxyl group may be in the form of 0 Mt, and the value of 4-p-q
may be 0.
[0019] The organosiliconates may be used alone or may contain a
monoalkylsiliconate represented by the following formula (2)
(referred to hereinafter as monoalkylsiliconate (2)) and a
dialkylsiliconate represented by the following formula (3)
(referred to hereinafter as dialkylsiliconate (3)):
R.sup.1Si(OM.sup.+).sub.n(OH).sub.3n (2)
R.sup.1.sub.2Si(OM.sup.+).sub.m(OH).sub.2m (3)
wherein R.sup.1 and M have the same meanings as defined above, a
plurality of R.sup.1's and M's may be the same or different, n is a
number of 0.1 to 3, and m is a number of 0.1 to 2.
[0020] In the formulae (2) and (3), the organosiliconates having
the same R.sup.1 and M may be used, or the organosiliconates having
different R.sup.1 and M may be used.
[0021] R.sup.1 and M are preferably those in the formula (1).
Preferable examples of the monoalkylsiliconate include lithium
methylsiliconate, sodium methylsiliconate, potassium
methylsiliconate, sodium ethylsiliconate, and sodium
propylsiliconate, among which sodium methylsiliconate is more
preferable. Preferable examples of the dialkylsiliconate include
sodium dimethylsiliconate, sodium diethylsiliconate, and sodium
methylethylsiliconate, among which sodium dimethylsiliconate is
more preferable.
[0022] The mixing ratio of the monoalkylsiliconate (2) to the
dialkylsiliconate (3) (i.e., monoalkylsiliconate
(2)/dialkylsiliconate (3) ratio by weight) is preferably in the
range of 95/5 to 0 /100, more preferably in the range of 95/5 to
5/95.
[0023] For improving the drying rate of fiber, the mixing ratio is
more preferably in the range of 95/5 to 30/70, even more preferably
90/10 to 50/50, further more preferably 90/10 to 70/30.
[0024] For improving the softness of fiber, the mixing ratio is
more preferably in the range of 70/30 to 0/100, even more
preferably 50/50 to 0/100, further more preferably 30/70 to
0/100.
[0025] For improving the toughness of fiber, the mixing ratio is
more preferably in the range of 95/5 to 30/70, even more preferably
95/5 to 50/50, further more preferably 95/5 to 70/30.
[0026] Each of n and m is preferably 0.5 or more, more preferably 1
or more. For further improving the water absorption and moisture
absorption of fiber, n is preferably 0.5 to 1.5, more preferably
0.5 to 1.2, and m is preferably 0.5 to 2.0, more preferably 0.5 to
1.5.
[Fiber]
[0027] The fiber to which the present invention is applicable are
preferably organic fibers. The organic fibers include plant-derived
water-swelling fibers such as cotton, hemp, pulp, paper mulberry,
mitsumata (a paper bush, Edgeworthia Chrysantha), kenaf, cotton
linter etc.; water-swelling fibers, regenerated or semisynthetic,
such as acetate and rayon, and animal water-swelling fibers such as
wool fibers and silk, including fibers made of animal hair of
sheep, camel, llama, alpaca etc.
[0028] As these fibers, single fiber may be subjected as such to
the modifying method of the present invention, or fiber in the form
of fabric, cloth, yarn, or primary or secondary fabrication
products such as clothing, string, rope, paper or pulp nonwoven
fabric may be subjected to the fiber modifying method of the
present invention.
[0029] Preferable fiber used in the present invention include
cotton, hemp, pulp, acetate, rayon, wool fiber, or primary or
secondary fabrication products thereof, and more preferable fiber
include cotton, pulp, acetate, rayon or primary or secondary
fabrication products thereof.
[Fiber-Treating Agent]
[0030] The fiber-modifying agent of the present invention contains
an organosiliconate and water. The content of the organosiliconate
in the fiber-modifying agent of the present invention is preferably
0.1% by weight or more, more preferably 2% by weight or more or is
preferably 82% by weight or less, more preferably 58% by weight or
less.
[0031] The fiber-treating agent of the present invention preferably
contains a surfactant for improving the permeation of the
organosiliconate into the inside of single fiber. As the
surfactant, it is possible to employ any of a nonionic surfactant,
an anionic surfactant, a cationic surfactant and an amphoteric
surfactant.
[0032] The surfactant is preferably a nonionic surfactant having a
hydrophile-lipophile balance (HLB) value of 9 to 15, particularly
11 to 14. The HLB is a value calculated according to the Griffin
method.
[0033] Preferable examples of the nonionic surfactant include
polyoxyalkylene alkyl ether, polyoxyalkylene alkenyl ether, higher
fatty acid sucrose ester, polyglycerin fatty acid ester, higher
fatty acid mono- or diethanol amide, polyoxyethylene hardened
castor oil, polyoxyethylene sorbitan fatty acid ester,
polyoxyethylene sorbitol fatty acid ester, alkyl saccharide-based
surfactants, alkylamine oxide, alkylamide amine oxide etc. Among
these, polyoxyalkylene alkyl ether and polyoxyethylene hardened
castor oil are preferable, and polyoxyethylene alkyl ether is even
more preferable.
[0034] The content of the surfactant in the fiber modifying agent
of the present invention is preferably 0.1 to 20% by weight, more
preferably 0.5 to 15.degree. by weight, even more preferably 1 to
10% by weight, from the viewpoint of emulsification upon mixing and
promotion of hydrolysis.
[Method of Modifying Fiber]
[0035] The method of modifying fiber according to the present
invention includes the steps (i) and (ii) and preferably further
includes the step (iii) of washing fiber after the step (ii).
[0036] Hereinafter, each step is described in detail.
<Step (i)>
[0037] The organosiliconate is contacted with fiber, preferably by
contacting the organosiliconate in an aqueous solution with fiber,
more preferably by contacting it with fiber in the presence of a
surfactant. The specific method of contacting the organosiliconate
with fiber includes a method of applying an aqueous
organosiliconate solution onto fiber, a method of spraying fiber
with an aqueous organosiliconate solution, a method of dipping
fiber in an aqueous organosiliconate solution, etc. The fiber to be
treated may be either wet or dry.
[0038] The concentration of the organosiliconate in the aqueous
organosiliconate solution is preferably 0.01% by weight or more,
more preferably 0.05% by weight or more, even more preferably 0.2%
by weight or more. For expecting an accumulative effect, the
aqueous organosiliconate solution may be used at low concentration.
For expecting an outstanding effect by conducting the treatment
once, it is effective to use the aqueous organosiliconate solution
at high concentration. The concentration of the organosiliconate is
preferably 15% by weight or less, more preferably 10% by weight or
less.
[0039] The weight of the organosiliconate based on the weight of
fiber is preferably 0.5% by weight or more, more preferably 1% by
weight or more, to exhibit the effect of the invention. The weight
is preferably 50% by weight or less, more preferably 25% by weight
or less.
[0040] The time of contacting the organosiliconate with fiber may
be a few seconds, preferably 1 minute or more, more preferably 30
minutes or more, even more preferably 1 hour or more. The contact
time is preferably within 24 hours, more preferably within 12
hours. By dipping for 30 minutes or more, a significant improvement
in the drying rate of fiber and toughness is recognized.
[0041] The temperature at which the organosiliconate is contacted
with fiber is not particularly limited.
<Step (ii)>
[0042] Polymerization of the organosiliconate can be carried out by
drying fiber which have been contacted with the organosiliconate.
Specifically, indoor drying, outdoor drying, hot-air drying and
press heating can be mentioned. The drying temperature is not
particularly limited, but drying can be carried out preferably in
the range of 0 to 150.degree. C. By drying at 50.degree. C. or
less, the water absorption of fiber after treatment can be kept
high. By drying at a temperature of 50.degree. C. or more, more
preferably 60.degree. C. or more, the drying time can be reduced
and the softness and toughness of fiber can be effectively
increased.
[0043] Organosilicate can be also polymerized by neutralizing the
aqueous solution of the organosilicate contained in fiber with an
acid and adjusting the pH to 12 or less. The pH is preferably 11.5
or less, more preferably 11 or less, even more preferably 9 or
less. Although there is no lower limit to the pH, the pH is
preferably 1 or more, more preferably 5 or more. The acid used in
neutralization is not particularly limited, and an inorganic acid
such as hydrochloric acid, sulfuric acid, nitric acid and
phosphoric acid and an organic acid such as oxalic acid, citric
acid and acetic acid are preferably used.
<Step (iii)>
[0044] After the step (ii), the step (iii) of washing fiber is
preferably carried out whereby an excess of the polymerized product
can be removed and the original feel of fiber can be maintained. In
washing, water can be used, and in this case, a surfactant may be
contained in water.
[Modified Fiber]
[0045] The fiber modified by the modifying method of the present
invention contain a polymer of the organosiliconate on the surface
of single fiber and/or the inside of single fiber. The presence of
the organosiliconate polymer can be confirmed by detecting silicon
on the surface of single fiber and/or in the inside of single
fiber, upon analysis of a section of fiber by an energy dispersive
X-ray spectroscope (EDS).
[0046] Modified fiber containing single fiber coated thereon with a
polymer of the organosiliconate in a thickness of not greater than
1/10 relative to the diameter of single fiber are preferable from
the viewpoint of maintaining characteristics inherent in the
fiber.
BRIEF DESCRIPTION OF THE DRAWINGS
[0047] FIG. 1 is an SEM photograph of a section of a modified cloth
obtained in Example 39;
[0048] FIG. 2 is a silicon mapping photograph of a section of a
modified cloth obtained in Example 39;
[0049] FIG. 3 is an STEM photograph of a section of a modified
cloth obtained in Example 39;
[0050] FIG. 4 is a photograph showing a result of qualitative
analysis of spots 1 and 2 in FIG. 3;
[0051] FIG. 5 is an SEM photograph of a section of a modified cloth
obtained in Example 40;
[0052] FIG. 6 is a silicon mapping photograph of a section of a
modified cloth obtained in Example 40;
[0053] FIG. 7 is an STEM photograph of a section of a modified
cloth obtained in Example 40;
[0054] FIG. 8 is a photograph showing a result of qualitative
analysis of spots 1 and 2 in FIG. 7;
[0055] FIG. 9 is an SEM photograph of a section of a modified cloth
obtained in Example 41;
[0056] FIG. 10 is a silicon mapping photograph of a section of a
modified cloth obtained in Example 41; and
[0057] FIG. 11 is a photograph showing a result of qualitative
analysis of spots 1 and 2 in FIG. 9.
EXAMPLES
[0058] The present invention is described in more detail by
reference to the Examples below. The Examples are mere illustrative
of the present invention and not intended to limit the present
invention.
[0059] In the Examples below, "%" is by weight unless otherwise
specified. Materials used in the following examples were obtained
or prepared as follows:
[0060] Sodium Methylsiliconate
[0061] Sodium methylsiliconate (NS-1, with 33% nonvolatile
component when dried at 105.degree. C. for 3 hours, manufactured by
Osaki Kogyo Co., Ltd.). The Na/Si ratio is 1.0. The sodium
methylsiliconate is hereinafter referred to simply as
methylsiliconate.
[0062] Sodium dimethylsiliconate
[0063] 327 g of 27.5% aqueous sodium hydroxide solution was
introduced into a 1000-mL three-neck flask, and then 222 g
dimethyldimethoxysilane (LS-1370 manufactured by Shin-Etsu Chemical
Co., Ltd.; hereinafter, dimethyldimethoxysilane refers to this
commercial product) was added thereto, and the mixture was stirred
for about 24 hours while a nitrogen gas was allowed to flow into it
whereby a colorless and transparent aqueous solution was obtained.
The resulting aqueous solution was lyophilized to give 226 g sodium
dimethylsiliconate as white solid. The Na/Si ratio was 1.5. The
sodium dimethylsiliconate is referred to hereinafter as
dimethylsiliconate.
Example 1
(1) Preparation of Modifying Agent
[0064] 17.4 g methylsiliconate was mixed with 165.5 g water and
then stirred for 5 minutes to give an aqueous uniform solution
thereby preparing 182.9 g modifying agent. The composition of the
resulting modifying agent is shown in Table 1.
(2) Pretreatment of Cotton Towels
[0065] Cotton towels (T. W220, white, manufactured by Takei Towel
Co., Ltd.) were washed repeatedly 10 times with a commercially
available clothing detergent (Liquid Attack, manufactured by Kao
Corporation) in an automatic washing machine (Hitachi Automatic
Washing Machine KW-5026 "Shizuka Gozen") (37 g detergent, 57 L tap
water was used, washing for 5 minutes.fwdarw.rinsing once with
running water.fwdarw.spin drying for 3 minutes). After spin drying
in the final round of treatment was finished, the towels were hung
and air-dried in a room to give pretreated towels. The weight of
each of the pretreated towels was 70 g.
(3) Modification of the Cotton Towels
[0066] The pretreated cotton towel (69.7 g) was dipped in 182.9 g
modifying agent for 60 minutes and then dried at room temperature
(20.degree. C.). The amount of the organosiliconate relative to the
cotton towel was 25%. The dried cotton towel was washed with a
clothing detergent (Liquid Attack, manufactured by Kao Corporation)
(washing conditions: 30 g detergent, 45 L tap water was used,
washing for 5 minutes.fwdarw.rinsing once with running
water.fwdarw.spin drying for 3 minutes) and then air-dried in a
room to give a modified towel. The increase in the weight of the
cotton towel after modification was 12.3%.
(4) Evaluation of Quick-Drying Property and Water Absorption
[0067] The obtained modified cotton towels were evaluated for
quick-drying property and water absorption in the following method.
The results are shown in Table 1.
<Method of Evaluation of Quick-Drying Property>
[0068] The towels for evaluation were washed in an automatic
washing machine (Hitachi Automatic Washing Machine KW-5026 "Shizuka
Gozen") (30 g detergent, 45 L tap water was used, washing for 5
minutes.fwdarw.rinsing once with running water.fwdarw.spin drying
for 3 minutes), and after spin drying was finished, the towels were
hung and air-dried at a constant temperature/humidity of 20.degree.
C. under 65% RH until their weight became constant. The water
content (%) with time was determined according to the following
equation (I). The time in which the water content became 10% after
initiation of drying was used as an indicator of quick-drying
property.
Water content (%)={weight (g) of towel just after spin
drying-weight (g) of towel reaching a constant weight}/weight (g)
of towel reaching a constant weight.times.100 (I)
<Method of Evaluation of Water Absorption (Bireck
Method)>
[0069] A plain-weave portion of the towel was cut into a
rectangular strip with a dimension of 2 cm.times.25 cm, and this
strip cloth was suspended in the vertical direction by fixing its
upper edge, and after the lower edge, 1 cm, was dipped in water at
20.degree. C., the height of water absorbed was observed with time
(1 minute, 3 minutes, 5 minutes and 10 minutes) with the naked eye
and recorded in the unit of cm. This measurement was carried out in
a room at constant temperature/humidity (20.degree. C./65% RH).
Examples 2 to 8
[0070] Methylsiliconate, dimethylsiliconate, and water were used to
produce modifying agents having the compositions shown in Table 1
in the same manner as in Example 1. Cotton towels were modified in
the same manner as in Example 1 except that these modifying agents
were used, and the resulting modified cotton towels were evaluated
for quick-drying property and water absorption in the same manner
as in Example 1. The results are shown in Table 1.
Examples 9 to 12
[0071] Modifying agents with the compositions shown in Table 1 were
prepared in the same manner as in Example 1, and 1 cotton towel
pretreated in the same manner as in Example 1 was dipped in each of
the modifying agents for about 15 minutes, then 6 N hydrochloric
acid (Wako Pure Chemical Industries, Ltd.) was added dropwise
thereto until the pH of the modifying agent became 7, and the towel
was spin-dried. The towel in a wet state was washed with a clothing
detergent (Liquid Attack, manufactured by Kao Corporation) under
the same conditions as in Example 1 and air-dried in a room to give
a modified towel. The resulting modified cotton towel was evaluated
for quick-drying property and water absorption in the same manner
as in Example 1. The results are shown in Table 1.
Comparative Example 1
[0072] A cotton towel pretreated in the same manner as in Example
1, which had not been modified with the modifying agent, was
evaluated for quick-drying property and water absorption in the
same manner as in Example 1. The results are shown in Table 1.
TABLE-US-00001 TABLE 1 Example 1 2 3 4 5 6 7 8 Modifying
Methylsiliconate (g) 17.4 12.0 8.5 5.2 0.0 2.4 1.2 0.2 agent
Dimethylsiliconate (g) 0.0 5.1 8.5 12.1 17.2 5.7 2.8 0.5 Water (g)
165.5 154.7 149.4 145.8 137.8 138.8 136.9 134.7 Weight (g) of
modifying agent 182.9 171.8 166.5 163.0 155.1 146.9 141.0 135.4
Formulation of Organosiliconate (%) 9.5 10.0 10.3 10.6 11.1 5.5 2.9
0.5 the modifying Water (%) 90.5 90.0 89.7 89.4 88.9 94.5 97.1 99.5
agent Methyisiliconate/dimethylsiliconate 10/0 7/3 5/5 3/7 0/10 3/7
3/7 3/7 (weight ratio) Modifying Drying temperature (.degree. C.)
20 20 20 20 20 20 20 20 method Neutralization -- -- -- -- -- -- --
-- Modified fiber Kind Cotton Cotton Cotton Cotton Cotton Cotton
cotton Cotton towel towel towel towel towel towel towel towel Fiber
weight (g) 69.7 68.4 68.3 69.0 68.9 67.6 67.6 67.2 Modification
amount (% owf*.sup.1) 25.0 25.0 25.0 25.0 25.0 12.0 6.0 1.0
increase (%) of weight 12.3 15.1 14.2 12.2 3.4 5.9 3.7 1.4 after
modification Evaluation of Water content [%] just after spin-drying
67.8 54.2 62.6 56.0 63.1 62.6 74.3 90.4 quick-drying Drying time
[hours]for reduction to 10% 6.1 4.7 4.7 4.0 4.7 5.2 6.7 7.3
property Evaluation Water absorption [cm] (after 1 minute) 1.2 2.1
2.1 3.2 5.8 3.8 4.1 5.5 result of Water absorption [cm] (after 3
minutes) 2.2 4.2 4.2 5.0 9.2 6.8 7.8 8.3 water Water absorption
[cm] (after 5 minutes) 3.9 7.0 5.9 6.2 10.5 8.6 9.2 9.8 absorption
Water absorption [cm] (after 10 minutes) 4.4 8.3 7.1 7.5 12.8 8.9
10.9 11.7 Comparative Example example 9 10 11 12 1 Modifying
Methylsiliconate (g) 12.0 8.6 5.2 0.0 No modifica- agent
Dimethylsiliconate (g) 5.2 8.6 12.0 17.3 tion Water (g) 1017.9
1012.9 1007.7 1000.0 Weight (g) of modifying agent 1035.1 1030.1
1024.9 1017.3 Formulation of Organosiliconate (%) 1.7 1.7 1.7 1.7
the modifying Water (%) 98.3 98.3 98.3 98.3 agent
Methyisiliconate/dimethylsiliconate 7/3 5/5 3/7 0/10 (weight ratio)
Modifying Drying temperature (.degree. C.) -- -- -- -- method
Neutralization Neutraliza- Neutraliza- Neutraliza- Neutraliza- tion
tion tion tion Modified fiber Kind cotton cotton cotton cotton
cotton towel towel towel towel towel Fiber weight (g) 68.7 68.9
68.7 69.1 68.9 Modification amount (% owf*.sup.1) 25.0 25.0 25.0
25.0 -- increase (%) of weight 1.6 1.6 1.5 1.2 -- after
modification Evaluation of Water content [%] just after spin-drying
86.9 90.4 76.7 77.9 92.0 quick-drying Drying time [hours]for
reduction to 10% 6.0 6.0 4.0 4.0 7.5 property Evaluation Water
absorption [cm] (after 1 minute) 5.5 5.4 5.0 5.1 5.9 result of
Water absorption [cm] (after 3 minutes) 8.3 8.5 8.3 8.7 9.0 water
Water absorption [cm] (after 5 minutes) 9.4 9.6 9.2 9.8 10.7
absorption Water absorption [cm] (after 10 minutes) 12.4 12.5 12.5
12.7 13.0 *.sup.1% owf refers to the percentage by weight of the
siliconate in the solution relative to the fiber (this applies also
to Tables below).
[0073] As is evident from Table 1, the towels modified by the fiber
modifying method of the present invention showed lower water
contents upon spin drying after washing than the controls which
were not subjected to the modification treatment of the present
invention and have reduced the drying time required for reduction
to a water content of 10%. When methylsiliconate and
dimethylsiliconate are simultaneously used, particularly when the
proportion of dimethylsiliconate is higher, not only a reduction in
the time required for attaining a water content of 10% but also
excellent water absorption could be achieved.
Examples 13 to 22
[0074] Methylsiliconate, dimethylsiliconate, and water were used to
prepare modifying agents having the compositions shown in Table 2
in the same manner as in Example 1. Cotton towels were modified
with these modifying agents in the same manner as in Example 1 to
give modified cotton towels. However, the step (ii) was carried out
by drying at 20.degree. C. in Examples 13 to 16, and the
polymerization step (ii) was carried out by drying at 80.degree. C.
in Examples 17 to 22. The resulting modified cotton towels were
evaluated for their softness by the following method. The results
are shown in Table 2.
<Method of Evaluation of Softness>
[0075] The towels were washed once with a commercial clothing
detergent (Liquid Attack, manufactured by Kao Corporation) in an
automatic washing machine (Hitachi Automatic Washing Machine
KW-5026 "ShizukaGozen") (37 gdetergent, 57 L tapwater was used,
washing for 5 minutes.fwdarw.rinsing once with running
water.fwdarw.spin drying for 3 minutes). The washed towels were
air-dried in a room and left for 1 day in a room at constant
temperature/humidity (20.degree. C./65% RH). Thereafter, the towels
were evaluated sensorially three times for softness to the touch by
a panel of 5 persons, and the average softness was determined.
Point -3: The treated towel is evidently harder than the unmodified
towel. Point -2: The treated towel is a little harder than the
unmodified towel. Point -1: The treated towel is slightly harder
than the unmodified towel. Point 0: The treated towel is not
different in hardness from the unmodified towel. Point 1: The
treated towel is slightly softer than the unmodified towel. Point
2: The treated towel is a little softer than the untreated towel.
Point 3: The treated towel is evidently softer than the unmodified
towel.
Examples 23 to 24
[0076] Methylsiliconate, dimethylsiliconate, and water were used to
prepare modifying agents having the compositions shown in Table 2
in the same manner as in Example 1. Cotton towels were modified
with these modifying agents in the same manner as in Example 9 to
give modified towels. The final pH upon neutralization after
dipping was 7. The resulting modified cotton towels were evaluated
for their softness in the same manner as in Example 13. The results
are shown in Table 2.
Comparative Example 2
[0077] Cotton towels pretreated in the same manner as in Example 1,
which had not been modified with the modifying agent, were
evaluated for softness in the same manner as in Example 13. The
results are shown in Table 2.
TABLE-US-00002 TABLE 2 Example 13 14 15 16 17 18 19 Modifying
Methylsiliconate (g) 8.5 5.2 0.0 2.4 12.1 8.6 5.2 agent
Dimethylsiliconate (g) 8.5 12.1 17.2 5.7 5.2 8.6 12.1 Water (g)
149.4 145.8 137.8 138.8 156.2 150.7 146.0 Weight (g) of the
modifying agent 166.5 163.0 155.1 146.9 173.5 167.9 163.3
Formulation of Organosiliconate (%) 10.3 10.6 11.1 5.5 10.0 10.3
10.6 the modifying Water (%) 89.7 89.4 88.9 94.5 90.0 89.7 89.4
agent Methylsiliconate/dimethylsiliconate (%) 5/5 3/7 0/10 3/7 7/3
5/5 3/7 (weight ratio) Modifying method Drying temperature
(.degree. C.) 20 20 20 20 80 80 80 Neutralization -- -- -- -- -- --
-- Modified fiber Kind Cotton Cotton Cotton Cotton Cotton Cotton
Cotton towel towel towel towel towel towel towel Fiber weight (g)
68.3 69.0 68.9 67.6 69.1 68.9 69.2 Modification amount (% owf) 25
25 25 12 25 25 25 Increase (%) of weight 14.2 12.2 3.4 5.9 3.7 5.5
7.1 after modification Evaluation result of softness 1.2 2.0 1.8
1.6 1.6 2.6 3.0 Comparative Example example 20 21 22 23 24 2
Modifying Methylsiliconate (g) 0.0 2.4 1.2 5.2 0.0 No modifi- agent
Dimethylsiliconate (g) 17.4 5.7 2.8 12.0 17.3 cation Water (g)
138.8 138.7 136.4 1007.7 1000.0 Weight (g) of the modifying agent
156.2 146.8 140.4 1024.9 1017.3 Formulation of Organosiliconate (%)
11.1 5.5 2.9 1.7 1.7 the modifying Water (%) 88.9 94.5 97.1 98.3
98.3 agent Methylsiliconate/dimethylsiliconate (%) 0/10 3/7 3/7 3/7
0/10 (weight ratio) Modifying method Drying temperature (.degree.
C.) 80 80 80 -- -- Neutralization -- -- -- Neutral- Neutral-
ization ization Modified fiber Kind Cotton Cotton Cotton Cotton
Cotton Cotton towel towel towel towel towel towel Fiber weight (g)
69.4 67.5 67.3 68.7 69.1 68.9 Modification amount (% owf) 25 12 6
25 25 -- Increase (%) of weight 6.4 4.0 2.8 1.5 1.2 -- after
modification Evaluation result of softness 3.0 2.6 0.6 1.0 1.0
0.0
[0078] As is evident from Table 2, the towels modified by the
modification method of the present invention became so soft to the
touch as to be sufficiently recognizable as compared with the
unmodified towels. The modifying method involving polymerization at
80.degree. C. could confer higher softness.
Examples 25 to 31
[0079] Methylsiliconate, dimethylsiliconate, polyoxyethylene lauryl
ether (Emulgen 108 manufactured by Kao Corporation; the average
number of ethylene oxides added, 6; HLB 12.1) and water were used
to prepare modifying agents having the compositions shown in Table
3 in the same manner as in Example 1. A wool sweater (ram crew neck
sweater, gray, manufactured by UNIQLO) silk, rayon tow, hemp,
acetate tow (all of which are commercially available), crystalline
cellulose powder (manufactured by MERCK) and Laubholz bleached
kraft pulp (LBKP) were dipped in each of these modifying agents for
60 minutes and then dried at 80.degree. C. for 12 hours, and
thereafter, the respective fiber were washed in the same manner as
in Example 1 to give modified fiber. The respective modified fiber,
as compared with their corresponding unmodified fiber as the
control, were evaluated for softness in the same manner as in
Example 13. The results are shown in Table 3.
Example 32
[0080] 5.3 g paper obtained by the following production method was
dipped for 30 seconds in 124.5 g modifying agent with the
composition shown in Table 3, then raised, air-dried at room
temperature for 10 minutes, and dried at 105.degree. C. for 2
minutes. The increase in the weight of the paper after modification
was 12.5%. The resulting paper after modification, as compared with
untreated paper as control, was evaluated for softness in the same
manner as in Example 13. The results are shown in Table 3.
<Method of Producing the Paper>
[0081] Laubholz bleached kraft pulp (abbreviated hereinafter as
LBKP) was dissociated and beaten at room temperature to give 2.2%
LBKP slurry. The Canadian standard freeness of the slurry was 420
ml. 2.2% LBKP slurry was weighed out such that the basis weight of
a sheet after paper making became 85 g/m.sup.2 on an oven-dry
weight basis. The slurry was diluted to a pulp density of 0.5% with
water and used to produce paper with a 150-mesh wire in a
rectangular TAPPI paper making machine, followed by coating to give
wet paper. The wet paper after paper making was pressed at 3.5
kg/cm.sup.2 for 5 minutes with a pressing machine and then dried at
105.degree. C. for 2 minutes with a drum dryer. The water content
of the dried paper was regulated for 1 day under the conditions of
23.degree. C. and 50% humidity.
TABLE-US-00003 TABLE 3 Example 25 26 27 28 29 30 31 32 Modifying
Methylsiliconate (g) 25.7 0.3 0.6 0.6 5.5 3.0 13.3 4.0 agent
Dimethylsiliconate (g) 60.0 0.8 1.4 1.5 12.9 7.0 31.0 9.2 Emulgen
108 (g) 17.1 0.0 0.0 0.0 0.0 0.0 0.0 0.0 Water (g) 723.7 6.9 9.2
9.3 302.7 110.5 374.4 111.3 Weight of modifying agent (g) 826.5 8.0
11.2 11.4 321.1 120.5 418.7 124.5 Formulation of the
Organosiliconate (%) 10.4 13.4 18.4 18.4 5.7 8.3 10.6 10.6
modifying agent Emulgen 108 (%) 2.4 0.0 0.0 0.0 0.0 0.0 0.0 0.0
Water (%) 87.6 86.6 81.6 81.6 94.3 91.7 89.4 89.4
Methylsiliconate/dimethylsiliconate 3/7 3/7 3/7 3/7 3/7 3/7 3/6 3/7
(weight ratio) Drying temperature (.degree. C.) 20 80 80 80 80 80
80 105 Modified fiber kind Wool Silk Rayon Hemp Acetate Cellulose
Pulp Paper sweater tow tow Fiber weight (g) 342.7 4.3 8.2 8.4 73.6
40.0 177.3 5.3 modification amount (% owf) 25.0 25.0 25.0 25.0 25.0
25.0 25.0 25.0 Increase in weight 7.5 10.0 7.5 8.8 5.4 5.7 4.5 12.5
after modification (%) Evaluation result of softness 1.6 0.6 1.2
0.6 1.4 1.6 2.4 2.6
[0082] As is evident from Table 3, the fiber modified by the
modification treatment of the present invention became so soft to
the touch as to be sufficiently recognizable as compared with the
corresponding unmodified fiber.
Examples 33 to 36
[0083] Methylsiliconate, dimethylsiliconate, and water were used to
prepare modifying agents having the compositions shown in Table 4
in the same manner as in Example 1. Five cotton towels were
modified with these modifying agents in the same manner as in
Example 17. The resulting modified towels were evaluated for
prevention of removal of down by the following method. The results
are shown in Table 4.
<Method of Evaluating Prevention of Removal of Down>
[0084] The 5 towels were dried for 3 hours in a tumbler-type drying
machine (dehumidification-type electric clothing drying machine
NH-D502, manufactured by Matsushita Electric Industrial Co., Ltd.),
and this drying for 3 hours was repeated 10 times. From the amount
of down remaining on a filter of the drying machine, the degree of
down removal was determined according to the following
equation:
Degree of down removal (%)=amount of down remaining on a filter of
the drying machine/weight of the towels before drying.times.100
Comparative Example 3
[0085] Cotton towels pretreated in the same manner as in Example 1,
which had not been modified with the modifying agent, were
evaluated for prevention of down removal in the same manner as in
Example 33. The results are shown in Table 4.
TABLE-US-00004 TABLE 4 Exampel Comparative 33 34 35 36 example 3
Modifying Methylsiliconate (g) 86.7 61.0 14.6 2.4 No modifica-
agent Dimethylsiliconate (g) 0.0 26.1 6.3 1.0 tion Water (g) 823.1
787.6 716.9 690.6 Weight of modifying agent (g) 909.8 874.7 737.7
694.0 Formulation of the Organosiliconate (%) 9.5 10.0 2.8 0.5
modifying agent Water (%) 90.5 90.0 97.2 99.5
Methylsiliconate/dimethylsiliconate 10/0 7/3 7/3 7/3 (weight ratio)
Drying temperature (.degree. C.) 80 80 80 80 Modified fiber Kind
Cotton Cotton Cotton Cotton Cotton towel towel towel towel towel
Fiber weight (g) 346.9 348.3 347.5 343.5 68.9 Modification amount
(% owf) 25.0 25.0 6.0 1.0 -- Increase (%) in weight 4.7 5.2 2.2 1.5
-- after modification Evaluation result of Degree of down removal
(%) 0.21 0.17 0.20 0.23 0.28 prevention of down removal
[0086] As is evident from Table 4, the modified towels of the
present invention indicated that removal of down can be controlled
sufficiently recognizably with less release of down in processing
in the drying machine than the unmodified towels.
Examples 37 and 38
[0087] Methylsiliconate, dimethylsiliconate, polyoxyethylene lauryl
ether (Emulgen 108 manufactured by Kao Corporation) and water were
used to prepare modifying agents having the compositions shown in
Table 5 in the same manner as in Example 1. A wool jersey (wool
jersey knit cloth (manufactured by Yato Shoten) cut in a size of
2.0 cm in width.times.2.0 cm in length) was dipped in each of the
modifying agents for 60 minutes and then dried at 80.degree. C. for
12 hours to give a modified wood jersey for evaluation. This wool
jersey was evaluated for wear resistance in the following method.
The results are shown in Table 5.
<Method of Evaluating Wear Resistance>
[0088] The wool jersey cut in a size of 1.3 cm in width and 19.5 cm
in length was wound around a rotating portion of an Acron wear
testing machine (for JIS tire rubber) and examined in a wear test
under a loading of 4.5 kg at an inclined angle of 5.degree. on a
truck wheel A36-P5-V, 3000 revolutions, at a rate of 75 rpm, and
damage to the portion of the cloth contacting with a whetstone was
evaluated under the following criteria:
.circle-w/dot.: Frayed spots (fiber cutting) are less than 10.
.largecircle.: Frayed spots (fiber cutting) are 10 or more and less
than 50%. x: Frayed spots (fiber cutting) are 50% or more.
Comparative Example 4
[0089] A wool jersey not modified with the modifying agent of the
present invention was evaluated for wear resistance in the same
manner as in Example 37. The results are shown in Table 5.
TABLE-US-00005 TABLE 5 Example Example Comparative 37 38 example 4
Modifying Methyl 3.1 2.1 No agent siliconate (g) modifi- Dimethyl-
0.0 0.9 cation siliconate (g) Emulgen 108 (g) 0.6 0.6 Water (g)
29.2 26.7 Weight of modifying agent (g) 32.9 30.2 Formulation of
Organo- 9.4 9.8 the modifying siliconate (%) agent Emulgen 108 (%)
1.9 2.0 Water (%) 88.8 88.3 Methylsiliconate/dimethyl- 10/0 7/3
siliconate (weight ratio) Drying temperature (.degree. C.) 20 20
Modified Kind Wool Wool Wool fiber jersey jersey jersey Fiber
weight (g) 12.3 11.8 12.2 Modification 25.0 25.0 -- amount (% owf)
Increase in 4.1 8.1 -- weight after modification (%) Evaluation
Wear test .largecircle. .circleincircle. X result of wear (visual
check) resistance
[0090] As is evident from the results in Table 5, the modified
fiber of the present invention, as compared with the unmodified
fiber, have improved wear resistance to a whetstone, to exhibit
increased toughness.
Example 39
[0091] Methylsiliconate and water were used to prepare modifying
agents having the compositions shown in Table 6 in the same manner
as in Example 1. A cotton broad cloth pretreated in the following
manner was dipped in each of the modifying agents and dried at
80.degree. C. and then washed in the same manner as in Example 1 to
give a modified cloth. The resulting modified cloth was subjected
to plane analysis of silicon in a section of the single fiber
(SEM-EDS observation) by the following method. An SEM photograph of
a section of this modified cloth is shown in FIG. 1, and its
silicon mapping is shown in FIG. 2. The modified cloth was also
subjected to element analysis of a section of the single fiber
(STEM-EDS observation) by the following method. An STEM photograph
of a section of this modified cloth is shown in FIG. 3, and the
results of qualitative analysis of the inside (spot 1) of single
fiber and the gap (spot 2) between single fiber are shown in FIG.
4.
[0092] In FIGS. 1 and 2, it was observed that silicon is
distributed mainly on the surface of single fiber of cotton. In
FIGS. 3 and 4, it was observed that silicon is present in the
inside of single fiber in the qualitative analysis of the inside
(spot 1) of single fiber and the gap (spot 2) between single
fiber.
<Method of Pretreatment of Cotton Broad Cloth>
[0093] 1.5 kg cotton broad cloth (manufactured by Yato Shoten) was
washed 5 times with a commercial detergent ("Attack" manufactured
by Kao Corporation) in an automatic washing machine (type NW-6BZ,
Hitachi, Ltd.) (detergent concentration of 0.0667%, 54 L tap water,
water temperature of 20.degree. C., washing for 9
minutes.fwdarw.rinsing once with stationary water.fwdarw.spin
drying for 1 minute), then washed with water (rinsing with running
water for 15 minutes.fwdarw.spin drying for 5 minutes) in a
two-bath washing machine (VH-360S1 manufactured by Toshiba
Corporation) and then air-dried. This cloth was cut into a piece of
15 cm.times.25 cm to give a pretreated cloth.
<Plane Analysis of Silicon in Single-Fiber Section (SEM-EDS
Observation)>
[0094] The fiber was embedded in epoxy resin, then hardened and cut
into a section with a microtome (ULTRACUT UTR manufactured by
LEICA) and made electrically conductive by deposition with Pt--Pd.
This fiber section was observed under a field emission scanning
electron microscope (FE-SEM: S4800, manufactured by Hitachi, Ltd.,
accelerating voltage of 15 kV, probe current High, focus mode HR,
condenser lens 3, aperture 1). The plane analysis of silicon was
carried out with an energy dispersive X-ray spectroscope (EDS)
(EMAX ENERGY EX-350 manufactured by Horiba, Ltd., mapping
measurement time 1500 seconds, process time 5).
<Qualitative Analysis of Single-Fiber Section (STEM-EDS
Observation)>
[0095] The fiber was embedded in epoxy resin, then hardened and cut
into a thin section of 200 nm in thickness with a microtome
(ULTRACUT UTR manufactured by LEICA). This fiber section was
observed under a field emission scanning electron microscope
(FE-SEM: S4800, manufactured by Hitachi, Ltd., accelerating voltage
of 30 kV, probe current High, focus mode HR, condenser lens 3,
aperture 1).
[0096] Qualitative analysis was carried out with an energy
dispersive X-ray spectroscope (EDS) (EMAX ENERGY EX-350
manufactured by Horiba, Ltd., qualitative analysis, loading time 60
seconds, process time 6), to determine the presence of silicon in
each spot.
Example 40
[0097] Methylsiliconate, dimethylsiliconate and water were used to
prepare modifying agents having the compositions shown in Table 6
in the same manner as in Example 1. A cloth was modified with each
of these modifying agents in the same manner as in Example 39 to
give a modified cloth. The resulting modified cloth was examined
for plane analysis of silicon in a section of the single fiber
(SEM-EDS observation) and for qualitative analysis of a section of
the single fiber (STEM-EDS observation) in the same manner as in
Example 39. An SEM photograph of a section of this modified cloth
is shown in FIG. 5, and its silicon mapping is shown in FIG. 6. An
STEM photograph of a section of this modified cloth is shown in
FIG. 7, and the results of qualitative analysis of the inside (spot
1) of single fiber and the gap (spot 2) between single fiber are
shown in FIG. 8.
[0098] In FIGS. 5 and 6, it was observed that silicon is
distributed mainly on the surface of single fiber of cotton and is
also present in the inside of single fiber. From FIGS. 7 and 8, it
was confirmed that silicon is present in the inside of single
fiber, but silicon is not present in the gap between single
fiber.
Example 41
[0099] Methylsiliconate, dimethylsiliconate, polyoxyethylene lauryl
ether (Emulgen 108 manufactured by Kao Corporation) and water were
used to prepare modifying agents having the compositions shown in
Table 6 in the same manner as in Example 1. A wool jersey cloth
(wool jersey knit cloth (manufactured by Yato Shoten) cut in a size
of 2.0 cm.times.2.0 cm) was dipped in each of the modifying agents
for 60 minutes, then dried at 20.degree. C. and then washed in the
same manner as in Example 1 to give a modified cloth. The resulting
modified cloth was subjected to plane analysis of silicon in a
section of single fiber (SEM-EDS observation) in the same manner as
in Example 39. An SEM photograph of a section of this modified
cloth is shown in FIG. 9, and its silicon mapping is shown in FIG.
10. In FIGS. 9 and 10, it was observed that silicon is thinly and
uniformly distributed mainly on the surface of single fiber of the
wool jersey cloth and is also present in the inside of single
fiber. The results of qualitative analysis of the inside (spot 1)
of single fiber and the gap (spot 2) between single fiber in the
same visual field as in SEM-EDS observation are shown in FIG.
11.
TABLE-US-00006 Example 39 40 41 Modifying Methyl- 1.3 0.4 0.9 agent
siliconate (g) Dimethyl- 0.0 1.0 2.1 siliconate (g) Water (g) 12.7
11.7 25.3 Emulgen 108 (g) 0.0 0.0 0.6 Weight of the modifying agent
(g) 14.0 13.1 28.9 Formulation of Organo- 9.5 10.6 10.4 the
modifying siliconate (%) agent Emulgen 108 (%) 0.0 0.0 2.1 Water
(%) 90.5 89.4 87.6 Methylsiliconate/dimethyl- 10/0 3/7 3/7
siliconate (weight ratio) Drying temperature (.degree. C.) 80 80 20
Modified Kind cotton cotton wool fiber broad broad jersey cloth
cloth Fiber amount (g) 5.3 5.5 12.0 Modification 25 25 25 amount (%
owf) Increase in 8.4 7.2 8.6 weight after modification (%)
[0100] It is evident from the above that the modified fiber of the
invention includes silicon inside, not in gap among single fiber.
This causes no fixing among single fiber, but free movement of the
fiber.
* * * * *