JPH10131054A - Fiber treating agent composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain the subject composition capable of imparting excellent feeling and shrink resistance to various kinds of fibers, especially animal fibers such as wool by compounding two kinds of specific organopolysiloxanes with colloidal silica, a condensation reaction catalyst, a nonionic surfactant, etc. SOLUTION: This composition is obtained by compounding (A) 100 pts.wt. of a mixture (weight ratio of 90:10 to 10:90) of two kinds of organopolysiloxanes (each of the compounds has a viscosity of at least 10cSt at 25 deg.C) of formula I and formula II [each of R is independently a 1-20C monovalent hydrocarbon group; R<1> is a divalent hydrocarbon group; R<2> and R<3> are each H or a monovalent hydrocarbon group; A is OH or a 1-5C alkoxy; as for B, at least one is a monovalent hydrocarbon group and others may be each OH or an alkoxy; (m) and (n) are each an integer of one or more; (a) is an integer of 0-5], (B) 1-50 pts.wt. of colloidal silica, (C) 0.1-20 pts.wt. of a condensation reaction catalyst, (D) 1-30 pts.wt. of a nonionic surfactant or a cationic surfactant and (E) an arbitrary amount of water.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

[0001] The present invention relates to a fiber treatment composition. More specifically, the present invention relates to an aqueous emulsion type fiber treatment composition capable of imparting excellent texture and shrink resistance to various fibers, particularly animal fibers represented by wool.

[0002]

2. Description of the Related Art Wool trousers, suits, sweaters, and the like have the disadvantage that when washed with water, the fibers become entangled with each other to form felt and shrink. Therefore, a wool product that can be easily washed at home and that does not shrink is desired. In order to respond to this, for example, it is known that wool fibers or wool products are treated with a urethane-based shrink-proofing agent. However, in this method, the texture becomes coarse and the wool inherent flexibility is impaired. There was a problem. Numerous studies have been made on silicone fiber treatment agents to improve such problems. For example, a reaction product of methoxy group-containing dimethylpolysiloxane, silica, aminopropyltriethoxysilane and maleic anhydride is used. An aqueous emulsion-type fiber treatment agent comprising an aminoethylaminopropyltrimethoxysilane and a tin catalyst has been proposed (see JP-A-3-152275). However, this fiber treating agent has a drawback that the shrink resistance is insufficient and the treated fiber becomes hard. The present inventors have previously proposed an aqueous emulsion type fiber treating agent comprising dimethylpolysiloxane containing hydroxyl-blocked amino groups at both ends of the molecular chain, colloidal silica, methyltrimethoxysilane, and a tin catalyst (JP-A-4-119).
No. 173). However, this fiber treating agent has a drawback in that the cross-linking reaction proceeds excessively, so that the smoothness of the treated fiber is low and the slimy feeling is poor.

[0003]

DISCLOSURE OF THE INVENTION The present inventors have made intensive studies to solve the above-mentioned disadvantages, and as a result, have reached the present invention.
That is, an object of the present invention is to provide a fiber treatment composition capable of imparting excellent texture and shrink resistance to various fibers, particularly animal fibers represented by wool.

[0004]

Means for Solving the Problems The present invention provides (A) and (a) a general formula:

Embedded image Wherein R is the same or different and is a monovalent hydrocarbon group having 1 to 20 carbon atoms, R ¹ is a divalent hydrocarbon group, and R ² and R ³ are a hydrogen atom or a monovalent hydrocarbon group. And A is a hydroxyl group or an alkoxy group having 1 to 5 carbon atoms. M and n are integers of 1 or more, and a is an integer of 0 to 5). An amino group-containing organopolysiloxane having at least 10 centistokes, and (b) a general formula:

Embedded image Wherein R is the same or different and is a monovalent hydrocarbon group having 1 to 20 carbon atoms, R ¹ is a divalent hydrocarbon group, and R ² and R ³ are a hydrogen atom or a monovalent hydrocarbon group. And B is a group selected from the group consisting of a monovalent hydrocarbon group, a hydroxyl group and an alkoxy group, at least one of which is a monovalent hydrocarbon group, and m and n are integers of 1 or more. And a is an integer of 0 to 5), and a mixture of amino group-containing organopolysiloxanes having a viscosity at 25 ° C. of at least 10 centistokes, provided that the mixture of components (a) and (b) The ratio is 90:10 to 10:90 by weight. １００ 100 parts by weight, (B) 1 to 50 parts by weight of colloidal silica, (C) 0.1 to 20 parts by weight of catalyst for condensation reaction, (D) 1 to 30 parts by weight of nonionic or cationic surfactant And (E) an arbitrary amount of water.

[0005]

DESCRIPTION OF THE PREFERRED EMBODIMENTS To explain this, the amino group-containing organopolysiloxane (a) constituting the component (A) imparts flexibility, smoothness, sliminess, lubricity and shrink resistance to fibers. It has the effect of doing. Further, the hydroxyl group or the alkoxy group at the terminal of the molecular chain reacts with the hydroxyl group on the surface of the colloidal silica of the component (B) to crosslink, and has an effect of improving the durability of these effects. This component has the general formula:

Embedded image It is represented by In the above formula, R is the same or different monovalent hydrocarbon group having 1 to 20 carbon atoms, and is a methyl group, an ethyl group, a propyl group, a butyl group, a pentyl group, a vinyl group,
Examples thereof include a 3,3,3-trifluoropropyl group, a phenyl group, an allyl group, and a cyclohexyl group. Of these, a methyl group is the most common, but a methyl group and another group can be combined. Further, it is not necessary that all Rs in one molecule be the same, but it is preferable that at least 50 mol% of Rs be a methyl group. R ¹ is a divalent hydrocarbon group, and an alkylene group such as a methylene group, an ethylene group, a propylene group, a butylene group, and an isobutylene group;
An alkylene arylene group such as a group represented by (CH ₂ ) ₂ —C ₆ H ₄ — is exemplified. Among these, an ethylene group or a propylene group is common. R ² and R ³ are a hydrogen atom or a monovalent hydrocarbon group. Examples of the monovalent hydrocarbon group include a methyl group, an ethyl group, a propyl group, a phenyl group, and a cyclohexyl group. A is a hydroxyl group or an alkoxy group having 1 to 5 carbon atoms, and examples of the alkoxy group include a methoxy group, an ethoxy group, a propoxy group, and a butoxy group. Among these, a hydroxyl group or a methoxy group is common. m and n are integers of 1 or more. a is an integer of 0 to 5, but 0 or 1 is generally used. The viscosity of this component at 25 ° C is at least 10
Centistokes, preferably 50 to 10,000
The range is 0 centistokes. This is because if it is less than 10 centistokes, it becomes impossible to impart flexibility, smoothness, compression recovery, wrinkle resistance and shrink resistance to the fiber. Such an amino group-containing organopolysiloxane of this component can be synthesized by a known method. For example, the formula: H ₂ N (CH ₂ ) ₃ Si (CH ₃ ) (OC
H ₃ ) _{2 The} dimethoxyaminosilane represented by ₂ or a hydrolytic condensate thereof and a cyclic siloxane such as octamethylcyclotetrasiloxane are subjected to an equilibration reaction in the presence of a basic catalyst to prepare a desired viscosity. It can be produced by neutralizing a basic catalyst using the same.

The component (b), which is another component constituting the component (A), is a component that is a feature of the present invention. This component provides the fiber with flexibility, smoothness,
In addition to having the function of imparting sliminess, lubricity and shrinkage resistance, the monovalent hydrocarbon group at the molecular chain terminal prevents the reaction with the component (B), and the crosslinked film formed by the components (A) and (B) forms By suppressing the hardening, it has the effect of maintaining a soft feel for a long time. This component has the general formula:

Embedded image It is represented by In the above formula, R, R ¹ , R ² , R ³ , m, n and a are the same as described above. B is a group selected from the group consisting of a monovalent hydrocarbon group, a hydroxyl group and an alkoxy group;
At least one of them must be a monovalent hydrocarbon group. Examples of the monovalent hydrocarbon group include a methyl group, an ethyl group, a propyl group, a phenyl group, and a cyclohexyl group. Examples of the alkoxy group include a methoxy group, an ethoxy group, a propoxy group, and a butoxy group. Among these, a methyl group, a hydroxyl group or a methoxy group is common. The viscosity of this component at 25 ° C. is at least 10 centistokes, preferably 50 to 10,000.
It is in the range of centistokes. This is because if it is less than 10 centistokes, it becomes impossible to impart flexibility, smoothness, compression recovery, wrinkle resistance and shrink resistance to the fiber. Such an amino group-containing organopolysiloxane of this component can be synthesized by a known method.
For example, the formula: H ₂ N (CH ₂ ) ₃ Si (CH ₃ ) (OC
Dimethoxyaminosilane represented by H ₃ ) ₂ or a hydrolytic condensate thereof, a cyclic siloxane such as octamethylcyclotetrasiloxane, and hexamethyldisiloxane were equilibrated in the presence of a basic catalyst to prepare a desired viscosity. Thereafter, it can be produced by neutralizing the basic catalyst with an acid.

[0007] In the component (A), the mixing ratio of the component (a) and the component (b) is 90:10 to 10:90 by weight, preferably 70:30 to 30:70. This is because if the ratio of component (a) exceeds 90, the texture of the treated fiber becomes hard, and if it is less than 10, the durability of the composition of the present invention to washing decreases.

[0008] The colloidal silica of the component (B) is formed by forming a strong organopolysiloxane film by cross-linking by condensation reaction of many hydroxyl groups present on the surface with alkoxy groups and hydroxyl groups in the component (A). It has the effect of imparting durability to shrink resistance, flexibility and smoothness. The colloidal silica used in the present invention is obtained by hydrolyzing tetraethyl silicate or sodium silicate in water containing a surfactant or the like to form a colloid, and has a particle size of about 4 to 20 μm. Such colloidal silica is generally commercially available as an aqueous dispersion having a silica concentration of 5 to 40% by weight, and among them, those which are stable in the presence of a nonionic surfactant or a cationic surfactant. Is preferred. Further, a material whose surface is covered with aluminum powder or the like can also be used. The blending amount of the component (B)
It is in the range of 1 to 50 parts by weight, preferably 10 to 25 parts by weight, per 100 parts by weight of the component (A). If the amount is less than 1 part by weight, a strong organopolysiloxane film will not be formed and the washing resistance will be poor.
If the amount is more than 0 parts by weight, the organopolysiloxane film is too hard and the texture of the fiber is reduced.

The catalyst for the condensation reaction of the component (C) is a catalyst for causing a cross-linking reaction between the component (A) and the component (B), and examples thereof include organometallic catalysts and amine catalysts containing no organic silicon. Examples of the organometallic catalyst include dibutyltin diacetate, dibutyltin dilaurate, dioctyltin dilaurate, dibutyltin dioctate, zinc naphthenate, cobalt naphthenate, zinc octylate, cobalt octylate, diisooctyl mercaptoacetate dioctylate, and naphthenic acid. Examples thereof include metal salts of organic acids such as zirconium, zirconium octylate, and tetrabutyl orthotitanate. Examples of the amine catalyst include diethanolamine and triethanolamine. Further, when this component is previously emulsified with a nonionic surfactant or a cationic surfactant to form an emulsion, it can be more uniformly dispersed in the composition of the present invention. The amount of the component (C) is 10
It is in the range of 0.1 to 20 parts by weight, preferably 0.5 to 15 parts by weight, based on 0 part by weight.

The nonionic surfactant or cationic surfactant of the component (D) is a component for emulsifying the component (A) or other components as required. This component includes polyoxyalkylene alkyl ethers, polyoxyalkylene alkyl phenol ethers, polyoxyalkylene alkyl esters, polyoxyalkylene sorbitan alkyl esters, sorbitan alkyl esters, aliphatic amine salts, quaternary ammonium salts, Examples thereof include alkylpyridinium salts, one or more of which can be used. The amount of the component (D) is 1 to 3 with respect to 100 parts by weight of the component (A).
The range is 0 parts by weight.

The water of the component (E) is the same as the component (A)
The component (D) is a component for emulsifying the component, and the amount thereof is not particularly limited as long as the component can be stabilized as an emulsion.

The composition of the present invention comprises the above components (A) to (E).
Component (F), and further represented by the general formula:

Embedded image It is preferable to add and blend the organosilane represented by the formula (1) or a partially hydrolyzed condensate thereof. This component reacts not only with a hydroxyl group or an alkoxy group, which is a terminal group of the component (A), to crosslink, but also with a hydroxyl group on the surface of the colloidal silica of the component (B), and also exists on the surface of wool or silk. It reacts with amino groups, carboxyl groups, or mercapto groups to impart durable shrink resistance, smoothness, and flexibility to fibers. In the above formula, R is the same as described above. R ⁴ is a monovalent hydrocarbon group having 1 to 5 carbon atoms,
Examples include a methyl group, an ethyl group, and a propyl group. Q is a monovalent organic group containing an amino group, an epoxy group, an acryloxy group or a methacryloxy group, or a group having 1 to 2 carbon atoms.
0 is a monovalent hydrocarbon group. The amino group-containing organic group has the formula:

Embedded image (Wherein, R ¹ , R ² , R ³ and a are the same as those described above), and a group represented by the formula: —CH ₂ CH ₂ CH ₂ NH ₂ or a formula represented by the following formula: a group represented by _{-CH 2 CH 2 CH 2 -NH-} CH 2 CH 2 NH 2 is illustrated. As the epoxy group-containing organic group,
formula:

Embedded image A group or a formula represented by:

Embedded image A group represented by is exemplified. The acryloxy group-containing organic group of the formula: a group represented by _{-CH 2 CH 2 CH 2 OOCCH =} CH 2 . Examples of the methacryloxy group-containing organic group,
Formula: a group represented by _{-CH 2 CH 2 CH 2 OOCC (} CH 3) = CH 2 can be exemplified. Examples of the monovalent hydrocarbon group having 1 to 20 carbon atoms include the same groups as those described above for R.
Among these, an amino group-containing organic group and an epoxy group-containing organic group are preferable. b is 0 or 1, but preferably 0. This partially hydrolyzed condensate of organosilane can be obtained by mixing the above-mentioned organosilane, water and a trace amount of acid or alkali and keeping the mixture at 50 to 70 ° C. The amount of the component (F) is (A)
It is in the range of 0.1 to 30 parts by weight, preferably 0.5 to 10 parts by weight, based on 100 parts by weight of the component. When the amount is less than 0.1 part by weight, the adhesion of the organopolysiloxane film to the fiber is reduced, and when the amount exceeds 30 parts by weight, the organopolysiloxane film becomes brittle, and in any case, the fiber is durable. This is because shrinkage resistance, flexibility, and smoothness cannot be imparted.

The composition of the present invention may further comprise, if necessary, an organopolysiloxane other than the component (A), an anti-wrinkle agent,
Thickeners, coloring agents, antiseptic / antifungal agents, rust inhibitors, etc. can be added and blended.

The composition of the present invention can be prepared, for example, by adding the amino group-containing organopolysiloxane (A) alone or (A)
The surfactant (D) and the water (E) are added to the amino group-containing organopolysiloxane of the component and the organosilane of the component (F) or the partially hydrolyzed condensate thereof to form an emulsion. )) Can be produced by adding the colloidal silica of the component and the condensation reaction catalyst of the component (C) which has been previously prepared in the form of an emulsion. At this time, it is better to age at room temperature for 10 to 20 days.

As a method of treating fibers with the composition of the present invention, there is a method of attaching the fibers to a fiber material by spraying, dipping, knife coating or the like. By leaving it at room temperature or drying by heat treatment after adhesion, a strong crosslinked film is formed on the fiber surface, and durable shrinkage resistance, flexibility, smoothness, wrinkle resistance and compression recovery can be imparted. . Further, the effect can be further enhanced by heat-treating the fiber treated with the composition of the present invention at a temperature of 110 to 160 ° C. for 3 to 10 minutes.

The fiber material to which the composition of the present invention is applied includes animal fibers having a scaly structure on the surface, such as wool, alpaca, mohair, and angora; natural fibers, such as silk, hemp, and cotton; and rayon, acetate. Examples of such fibers include recycled fibers; synthetic fibers such as polyester, polyamide, vinylon, polyacrylonitrile, polyethylene, polypropylene, and urethane; glass fibers, carbon fibers, and silicon carbide fibers. Among these, especially wool,
It is suitably applied to fibers having a scaly structure on the surface, such as alpaca, mohair, and angora. In terms of shape, top, cheese, skein, staple, filament, tow,
Examples include woven fabric, knitted fabric, non-woven fabric, hanging with resin-treated cloth, artificial leather, and the like, and particularly preferred are filament, tow, woven fabric, knitted fabric, and non-woven fabric.

The composition of the present invention as described above can form a strong crosslinked film on the surface of various fibers and impart durable shrink resistance and excellent texture to the fibers. For this reason, the fibers treated with the composition of the present invention have the advantages that they do not easily shrink even when washed with water, and that excellent texture is maintained.

[0018]

Next, the present invention will be described in detail with reference to examples.
In the examples, "parts" means parts by weight, and "%" means percent by weight. Viscosity is a measurement at 25 ° C.

[0019]

Embodiment 1 Formula:

Embedded image A polyoxyethylene (6 mol of ethylene oxide) lauryl ether 60 was added to 300 parts of an amino group-containing organopolysiloxane having a viscosity of 880 centistokes.
And 80 parts of water were added and uniformly stirred. This mixture is emulsified using a colloid mill type emulsifier, and then water 56
0 parts were added to prepare a uniform emulsion (emulsion A). As above, the average composition formula:

Embedded image An emulsion of an amino group-containing organopolysiloxane having a viscosity of 1,100 centistokes was prepared (emulsion B). The thus obtained emulsion A, emulsion B and colloidal silica [Snowtex AK (manufactured by Nissan Chemical Industries, Ltd., trade name: 80% water, 20% colloidal silica)] were blended as shown in Table 1. The amount was added and blended. Further, as a catalyst for the condensation reaction, zinc octoate (20 parts), polyoxyethylene (45 mol) nonylphenol ether (2.5 parts), dialkyl (coconut oil) dimethyl ammonium chloride (2.5 parts) were used.
5 parts and 2 parts of an emulsion of zinc octoate emulsified with 75 parts of water were added and blended to prepare a fiber treatment composition, which was kept at room temperature for 10 days. The fiber treatment composition thus obtained is diluted with water to a predetermined concentration (solid content).
And a wool of 45 cm × 45 cm 10 was prepared.
Three unstained 0% surge cloths for clothing were soaked for 30 seconds. Next, it was squeezed by adjusting the squeezing rate to 100% with a mangle roller, spread on a wire mesh, and dried at room temperature for 24 hours. This was further heat-treated at 130 ° C. for 5 minutes in a hot air circulating dryer, and then allowed to cool at room temperature. The treated cloth was marked at three locations in the vertical and horizontal directions at intervals of 30 cm, and washed five times under the following washing conditions. After washing and drying the treated cloth, the length between marks was measured, and the washing shrinkage (%) in the vertical and horizontal directions was calculated by the following equation.

(Equation 1) (Washing conditions: Bath ratio 1:50, temperature 40 ° C., time 15 minutes, weak alkaline detergent [Kao Corporation, trade name:
And then washed twice with water except that the detergent was removed. This cycle was one wash. In addition, the wrinkle prevention rate (Monsanto method) and the hand feeling before and after washing were measured by the wrinkle prevention rate (Monsanto method) and the feel by hand according to JIS L 1096 General Textile Test Method. The results are shown in Table 1. The fiber treated with the fiber treatment composition of the present invention has a very good hand and a small shrinkage ratio in washing with water. From this, the fiber treatment composition of the present invention is suitable as a treatment agent for 100% wool fabric. It has been found.

[0020]

Comparative Examples 1 to 5 In Example 1, emulsion A,
A fiber treating agent composition was prepared in the same manner as in Example 1, except that the amounts of the emulsion B and the colloidal silica were changed. Washing shrinkage, wrinkle prevention and texture of the obtained fiber treating agent composition were measured in the same manner as in Example 1, and the results are shown in Table 1.

[0021]

[Table 1]

[0022]

Embodiment 2 Formula:

Embedded image And 150 parts of an amino group-containing organopolysiloxane having a viscosity of 880 centistokes represented by the following formula:

Embedded image 150 parts of an amino group-containing polyorganosiloxane having a viscosity of 830 centistokes represented by the formula: H ₂ NC ₂ H
After uniformly mixing 5 parts of γ- (β-aminoethyl) aminopropyltrimethoxysilane represented by ₄ NHC ₃ H ₆ Si (OCH ₃ ) ₃ , polyoxyethylene (6 mol of ethylene oxide) lauryl ether was added thereto. 60 parts and 80 parts of water were added and uniformly stirred. This mixture was emulsified using a colloid mill-type emulsifier, and then 555 parts of water was added to prepare a uniform emulsion. Take 80 parts of this emulsion and add it to colloidal silica [Nissan Chemical Industries, Ltd.
, Trade name: Snowtex AK (water content 80%, colloidal silica 20%)]. Next, as a condensation reaction catalyst, zinc octoate emulsified with 20 parts of zinc octoate in 2.5 parts of polyoxyethylene (45 mol) nonylphenol ether, 2.5 parts of dialkyl (coconut oil) dimethyl ammonium chloride and 75 parts of water Was added and blended to prepare a fiber treatment composition. Washing shrinkage, wrinkle prevention and texture of the obtained fiber treatment composition were measured in the same manner as in Example 1. The results are shown in Table 2. The fiber treated with the fiber treatment composition of the present invention has a good texture, and the washing shrinkage is significantly smaller than that of the composition of the comparative example. It turned out to be suitable.

[0023]

Comparative Example 6 In Example 2, the formula:

Embedded image The amount of the amino group-containing organopolysiloxane having a viscosity of 880 centistokes represented by the formula is 300 parts, and the formula:

Embedded image A fiber treatment composition was prepared in the same manner as in Example 2 except that the amino group-containing polyorganosiloxane having a viscosity of 830 centistokes was not added. Washing shrinkage ratio, wrinkle prevention ratio and texture of the obtained fiber treating agent composition were measured in the same manner as in Example 2, and the results are shown in Table 2.

[0024]

Embodiment 3 Formula:

Embedded image And 150 parts of an amino group-containing organopolysiloxane having a viscosity of 880 centistokes represented by the following formula:

Embedded image 150 parts of an amino-containing polyorganosiloxane having a viscosity of 830 centistokes represented by the formula: CH ₂ ＣC
After uniformly mixing 5 parts of γ-methacryloxypropyltrimethoxysilane represented by (CH ₃ ) COOC ₃ H ₆ Si (OCH ₃ ) ₃ , 60 parts of polyoxyethylene (6 mol of ethylene oxide) lauryl ether was added thereto. And 80 parts of water were added and stirred uniformly. This mixture was emulsified using a colloid mill-type emulsifier, and then 555 parts of water was added to prepare a uniform emulsion. Take 80 parts of this emulsion and add colloidal silica [manufactured by Nissan Chemical Industries, Ltd.
Trade name: Snowtex AK (water 80%, colloidal silica 20%)] was blended. Next, as a condensation reaction catalyst, 20 parts of zinc octoate were mixed with 2.5 parts of polyoxyethylene (45 mol) nonylphenol ether 2.5.
, 2.5 parts of dialkyl (coconut oil) dimethylammonium chloride and 1 part of an emulsion of zinc octoate emulsified with 75 parts of water to prepare a fiber treatment composition. Washing shrinkage, wrinkle prevention and texture of the obtained fiber treatment composition were measured in the same manner as in Example 1. The results are shown in Table 2. The fiber treated with the fiber treatment composition of the present invention has a good texture, and the washing shrinkage is significantly smaller than that of the composition of the comparative example. It turned out to be suitable.

[0025]

Comparative Example 7 In Example 3, the formula:

Embedded image The amount of the amino group-containing organopolysiloxane having a viscosity of 880 centistokes represented by

Embedded image A fiber treatment composition was prepared in the same manner as in Example 3 except that the amino group-containing polyorganosiloxane having a viscosity of 830 centistokes was not added. Washing shrinkage, wrinkle prevention and texture of the obtained fiber treatment composition were measured in the same manner as in Example 3, and the results are shown in Table 2.

[0026]

[Table 2]

[0027]

Example 4 Octamethylcyclotetrasiloxane 39
0 parts and the formula: H ₂ NC ₂ H ₄ NHC ₃ H ₆ SiCH ₃ (OC
After uniformly stirring 10 parts of γ- (β-aminoethyl) aminopropylmethyldimethoxysilane represented by H ₃ ) ₂ , 50 parts of hexadecyltrimethylammonium chloride and 500 parts of water were added and uniformly mixed. .
This mixed solution was subjected to a pressure of 400 kg / c using a homogenizer.
The treatment was performed three times under the condition of m2. This was transferred to a four-necked flask, and a solution of 1.0 part of sodium hydroxide dissolved in 47.5 parts of water was added thereto, followed by polymerization at 80 ° C. for 8 hours. After the polymerization, 1.5 parts of acetic acid was added and the mixture was cooled.

Embedded image An emulsion of an amino group-containing organopolysiloxane having a viscosity of 2,600 centistokes was prepared (emulsion C). On the other hand, 388 parts of octamethylcyclotetrasiloxane, 2 parts of hexamethyldisiloxane, and γ- (β-aminoethyl) aminopropyl represented by the formula: H ₂ NC ₂ H ₄ NHC ₃ H ₆ SiCH ₃ (OCH ₃ ) ₂ After uniformly stirring 10 parts of methyldimethoxysilane, 50 parts of hexadecyltrimethylammonium chloride and 500 parts of water were added and uniformly mixed. This mixture was treated three times using a homogenizer at a pressure of 400 kg / cm 2. This was transferred to a four-necked flask, a solution of 1.0 part of sodium hydroxide dissolved in 47.5 parts of water was added, and the mixture was kept at 80 ° C. for 6 hours and then at 40 ° C. for 4 hours. Polymerized. After the polymerization, 1.5 parts of acetic acid was added and cooled,

Embedded image An emulsion of an amino group-containing polyorganosiloxane having a viscosity of 2,500 centistokes was prepared (emulsion D). After mixing 100 parts of the emulsion C and 100 parts of the emulsion D thus obtained, 2 parts of γ-glycidoxypropyltrimethoxysilane and colloidal silica [trade name: Snowtex BK, manufactured by Nissan Chemical Industries, Ltd.] (Water 80%, colloidal silica 20%)] 100 parts and the condensation reaction catalyst (gin octoate emulsion) used in Example 1 were added, and the mixture was kept at 50 ° C. for 10 days to prepare a fiber treatment composition. Was prepared. The fiber treatment composition thus obtained was diluted with water to prepare a treatment solution having a predetermined concentration (solid content). A sweater containing 85% wool and 15% acrylic was used for 30 seconds. Dipped. Next, the squeezing rate is 1
It was adjusted to 00%, squeezed, spread on a wire mesh, and dried at room temperature for 24 hours. This is further dried at 80 ° C. for 5
After heat treatment for minutes, the mixture was allowed to cool at room temperature. Markings at intervals of 30 cm were made at two places in the vertical direction of the height portion and the sleeve portion of this sweater, and the washing shrinkage was measured in the same manner as in Example 1. The change in texture before and after washing was measured by finger touch. Table 3 shows the results. The sweater treated with the fiber treatment composition of the present invention has a very good feel and the washing shrinkage is significantly smaller than the composition of the comparative example. From this, the fiber treatment composition of the present invention is a wool knitted fabric. It turned out to be suitable as a treating agent for use.

[0028]

Comparative Example 8 A fiber treating agent composition was prepared in the same manner as in Example 4 except that the blending amount of the emulsion C was changed to 200 parts and the emulsion D was not blended. Washing shrinkage and texture of the obtained fiber treatment composition were measured in the same manner as in Example 4, and the results are shown in Table 3.

[0029]

[Table 3]

[0030]

According to the present invention, the fiber treatment composition of the present invention comprises the above (A)
Component (E) or component (A) to component (F), and particularly because component (b) is contained, when this is applied to various fibers, the fiber has excellent texture and shrink resistance. It has the characteristic that it can be provided.

Claims (4)

[Claims] (A) (a) a general formula: Wherein R is the same or different and is a monovalent hydrocarbon group having 1 to 20 carbon atoms, R ¹ is a divalent hydrocarbon group, and R ² and R ³ are a hydrogen atom or a monovalent hydrocarbon group. And A is a hydroxyl group or an alkoxy group having 1 to 5 carbon atoms. M and n are integers of 1 or more, and a is an integer of 0 to 5). An amino-containing organopolysiloxane having at least 10 centistokes, and (b) a general formula: Wherein R is the same or different and is a monovalent hydrocarbon group having 1 to 20 carbon atoms, R ¹ is a divalent hydrocarbon group, and R ² and R ³ are a hydrogen atom or a monovalent hydrocarbon group. And B is a group selected from the group consisting of a monovalent hydrocarbon group, a hydroxyl group and an alkoxy group, at least one of which is a monovalent hydrocarbon group, and m and n are integers of 1 or more. And a is an integer of 0 to 5), and a mixture of amino group-containing organopolysiloxanes having a viscosity at 25 ° C. of at least 10 centistokes, provided that the mixture of components (a) and (b) The ratio is 90:10 to 10:90 by weight. １００ 100 parts by weight, (B) 1 to 50 parts by weight of colloidal silica, (C) 0.1 to 20 parts by weight of catalyst for condensation reaction, (D) 1 to 30 parts by weight of nonionic or cationic surfactant A fiber treating agent composition comprising: Part (A) and an arbitrary amount of (E) water. (A) (a) a general formula: Wherein R is the same or different and is a monovalent hydrocarbon group having 1 to 20 carbon atoms, R ¹ is a divalent hydrocarbon group, and R ² and R ³ are a hydrogen atom or a monovalent hydrocarbon group. And A is a hydroxyl group or an alkoxy group having 1 to 5 carbon atoms. M and n are integers of 1 or more, and a is an integer of 0 to 5). An amino group-containing organopolysiloxane having at least 10 centistokes, and (b) a general formula: Wherein R is the same or different and is a monovalent hydrocarbon group having 1 to 20 carbon atoms, R ¹ is a divalent hydrocarbon group, and R ² and R ³ are a hydrogen atom or a monovalent hydrocarbon group. And B is a group selected from the group consisting of a monovalent hydrocarbon group, a hydroxyl group and an alkoxy group, at least one of which is a monovalent hydrocarbon group, and m and n are integers of 1 or more. And a is an integer of 0 to 5), and a mixture of amino group-containing organopolysiloxanes having a viscosity at 25 ° C. of at least 10 centistokes, provided that the mixture of components (a) and (b) The ratio is 90:10 to 10:90 by weight. １００ 100 parts by weight, (B) 1 to 50 parts by weight of colloidal silica, (C) 0.1 to 20 parts by weight of catalyst for condensation reaction, (D) 1 to 30 parts by weight of nonionic or cationic surfactant Part, (E) optional amount of water and (F) general formula: Wherein R is the same or different monovalent hydrocarbon group having 1 to 20 carbon atoms, R ⁴ is a monovalent hydrocarbon group having 1 to 5 carbon atoms, and Q is an amino group or an epoxy group. , An acryloxy group or a methacryloxy group, a monovalent organic group or a monovalent hydrocarbon group having 1 to 20 carbon atoms, b is 0 or 1.) or an organosilane represented by the following formula: A fiber treating composition comprising 0.1 to 30 parts by weight. 3. The fiber treatment composition according to claim 2, wherein Q of component (F) is an epoxy group-containing organic group or an amino group-containing organic group. 4. The fiber treating agent composition according to claim 1, which is used for treating a fiber having a scaly structure.