JPH02264080A - Aromatic fiber structure and production thereof - Google Patents

Abstract

PURPOSE:To obtain an aromatic fiber structure of high durability and persistence by mixing perfume-containing microcapsules and a resin binder at a specific weight ratio and fixing them in the fiber structure. CONSTITUTION:Perfume-containing microcapsules using a formalin resin such as urea-formalin resin, melamine resin as a capsule wall material and a resin binder such as a silicone resin, preferably an organopolysiloxane are mixed at a weight ratio of 2/1 to 1/5 to prepare an emulsion. A fiber structure, especially a structure containing extremely fine fibers less than 0.7 denier/single fiber and having a void volume of less than 80%, (such as yarns, woven, knitted and nonwoven fabrics) is dipped or printed with the emulsion to fix the microcapsules in the gaps or spaces in the fiber structure whereby said perfume- containing microcapsules of 1 to 50% particle sizes are obtained containing in an amount of 0.3 to 7% owf.

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to an aromatic fiber structure, and more specifically, the present invention relates to an aromatic fiber structure, and more specifically, to a woven or knitted fabric, microcapsules containing a fragrance are attached to a woven or knitted fabric to impart a durable fragrance. knitting.

This article relates to clothing and its manufacturing method.

[Conventional technology]

Conventionally, various developments have been made regarding fragrant fiber structures such as clothing, and many of them have been on the market.

However, most of these products are simply sprayed with fragrant substances such as perfumes at the time of finishing, or applied with a binder or glue, or are applied in an open atmosphere system, or are placed inside a packaging bag during packaging. This was done by enclosing aromatic paper in the paper, or by using eight pieces of paper as aromatic paper, and transferring the scent to woven and knitted fabrics and clothing.

However, it goes without saying that the fragrance of the clothing obtained as described above is poor, and the fragrance is only 1.
The fragrance completely disappeared after washing several times, and the product value was extremely low. Furthermore, the fragrance quickly evaporates when it comes into contact with the outside air while being worn, and some products have even been able to maintain their fragrance for only a few hours after use. In addition, in cases where the scent of aromatic paper is transferred to clothing in a packaging bag, the strength of the fragrance varies depending on the time elapsed after the bag is sealed, and as a result, the fragrance does not become pleasant and the product itself may be defective. There were times when it happened.

Aiming to solve these problems, aromatic substances are applied to fiber structures in a closed system encapsulated in microcapsules,
Attempts have been made to destroy the microcapsules by stress applied to the fiber structure during use, converting it into an open system and emitting fragrance.

For example, a method of applying microcapsules containing an odorant and a sizing agent containing a melamine resin to a textile product (Br', 140
No. 1143); No. 4 microcapsules containing fragrances
A method of attaching microcapsules containing fragrance to a male using a capsule transfer agent mainly consisting of a cationic biological substance such as ammonium salt, or a nonionic biological substance such as sorbitan ester (Japanese Patent Application Laid-Open No. 52-31200). Method for obtaining fragrant towel fabric by applying a mixture of acrylic resin and acrylic resin (JP-A-58-4886'l;-) Fragrance microcapsules coated with glue wall film, thermoplastic substance, and thickener A method for obtaining a printed article that emits an aroma by printing a printing paste consisting of
JP-A-53-19200); A method for obtaining a scented printed material that emits an aroma by heat-transferring a binder layer consisting of a microcapsule of a fragrance, a pigment, a polymeric resin, etc. to an object to be transferred (JP-A-53-1) %885): etc. have been proposed.

[Problem to be solved by the invention]

However, as shown in these conventional proposals, j11
In the method of applying microcapsules to a knitted fabric using a glue or a resin binder, drying or low-temperature heating alone inevitably results in poor adhesion and poor washing durability. In addition, if heat fixation is performed at high temperature after drying, the adhesiveness will improve, but
There are drawbacks such as deterioration of the fragrance due to high temperatures, destruction of microcapsules due to vaporization of the fragrance, and hardening of the texture due to penetration of the resin into the woven or knitted system. In particular, in the case of thin woven or knitted fabrics, such as stockings, the constituent yarns thereof are composed of nylon filaments with smooth surfaces, and it is therefore extremely difficult to sufficiently adhere the microcapsules thereto. Therefore, if a large amount of binder is applied with the sole intention of increasing the amount of adhesion, the texture will become rough and the product value will be lost. In addition, JP-A-53-10 (i
As disclosed in Japanese Patent Application No. 885, not only is it not possible to impart a sufficiently durable fragrance even when the fragrance is applied by thermal transfer printing, but the fragrance usually evaporates and deteriorates at temperatures above 150°C. There is a problem in that there are only a limited number of fragrances that can withstand heat transfer.

Additionally, a significant problem with many of these prior art techniques is that many of the substances applied to the glue or binder, especially nitrogen-containing organic compounds, have inherent unpleasant odors that can ruin the aroma. be.

Therefore, an object of the present invention is to provide an aromatic fiber structure that has a long-lasting and preferable fragrance and whose basic physical properties such as texture and color fastness are not impaired.

[Means to solve the problem]

In order to achieve the above object, the present invention provides a fiber structure to which fragrance-containing microcapsules are attached, in which the microcapsules and the resin binder are provided in a ratio (weight ratio) of 2:1 to 1:5. And the amount of both of these is the amount of adhesion! The composition is such that it occupies 0.3 to 7.0% of the fiber structure tilit.

Preferable methods for manufacturing this aromatic fiber structure include dipping, padding, spray coating, or printing a treatment agent in which a fragrance-containing microcapsule and a resin binder are mixed into a fiber structure that has been previously subjected to water-repellent treatment. There is a method of assigning it by

In addition, non-woven fabrics or woven or knitted fabrics impregnated with polyurethane elastomer, synthetic leather with a grain layer formed thereon by a wet or dry process, non-woven fabrics made of ultrafine fibers, or brushed m-knit fabrics impregnated with polyurethane elastomer. After-buffed suede so-called synthetic leather, thick and long (preferably tapered tips) prickly hair and thin and short fluff are flocked to the base fabric and fixed with latex adhesive, fur-like fabric, pile yarn based. For fiber structures such as carpets that are adhesively fixed to cloth with latex, there are two methods:
It can also be applied by mixing it into the polyurethane elastomer, silver surface solution, latex, or the like.

Furthermore, fibrillation described below! Single yarn denier obtained from lit composite fiber, preferably 0.7 denier or less
If a fibrous structure containing 11 fibers is used, the fragrance-containing microcapsules can be firmly held by simply trapping them in the fiber gaps of the fibrous structure without using the binder.

FIGS. 1 (1) to (11) are cross-sectional views showing examples of fibrillated composite fibers used in a preferred embodiment of the present invention. In these figures, A, B indicate different fiber components.

Moreover, FIGS. 2 and 3 are photographs (magnification: 500 times) showing the shape of the fibers of a plain cotton fabric to which microcapsules are attached.

The fiber structures referred to in the present invention include yarns, cords, knitted fabrics, nonwoven fabrics, raised blankets, leather and fur, and secondary products thereof, such as coats, kimono suits, uniforms, sweaters,
Outer clothing such as skirts, slacks, cardigans, sportswear, dress shirts, casual wear, pajamas, and shorts.

Underwear such as lingerie, foundation, and sanitary clothing, hosiery such as stockings and socks, futon lining,
Bedding items such as sheets, duvet covers, and blankets, accessories such as gloves, ties, scarves, shawls, and eyeglass cleaners, curtains, carpets, and wall coverings.

Includes upholstery fabrics, upholstery, automobile interior materials, etc.

From the viewpoint of water repellent treatment, it is more advantageous for these materials to have a larger basis weight. As the constituent fibers, any of natural fibers, synthetic fibers with no regenerated fibers, or mixed yarns such as single-spun yarns, mixed fibers, etc., may be used. In addition, from the relationship with binder adhesion, fibers with unevenness, such as cotton,
Porous fibers having macrovoids or fibers having affinity with the binder are advantageous. Particularly preferably,
Ultrafine synthetic fibers with a single yarn denier of 0.7 denier or less, for example, JP-A-57-117647 and JP-A-60-21
Fibrillation described in Publication No. 5869! ! The application of composite fibers is of great advantage. Here, "fibril"
refers to fine-grained fibers that are bundled in large numbers to form fiber bundles.For example, fibers with a composite structure consisting of multiple components (composite fibers) can be divided into each component, or alkali or It can be easily obtained by dissolving it in acids, solvents, etc. and removing easily decomposed components.

The fibrillated composite am in the present invention refers to two or more polymers selected from, for example, various polyesters, various polyamides, polyethylene, and polypropylene, particularly polyamides and polyesters, in which one component is the other in the cross section of a single filament. It refers to a shape that does not completely enclose the components of 1lt-filament and is joined along the longitudinal direction of the 1lt-filament. Specifically, the cross section is as shown in Figure 1 (
Side-by-side type composite fiber as shown in 1), same figure (2)
～(3) A side-by-side warping type composite fiber,
A composite fiber consisting of a component having a radial shape as shown in (4) to (8) and another component having a shape that complements the radiating portion, and a composite fiber that has a radial shape as shown in (9) to (10) of the same. another component having a shape with a 7-shaped recess that complements the radiating portion and faces toward the center; and a component that has the radial shape and has a 7-shaped recess that complements the recess. Examples include conjugate fibers made of the same components and side-by-side fully turned conjugate fibers with hollow portions as shown in (11).

Examples of polyamides include nylon 4. nylon 6,
Nylon 7, Nylon ll, Nylon 12, Nylon 6
6. Nylon 610. Examples include polymethaxylene adipamide, polyparaxylylene decanamide, polybiscyclohexylmethanedecanamide, and copolyamides containing these components.

Examples of polyester include polyethylene terephthalate, polytetramethylene terephthalate, polyethyleneoxybenzoate, and poly1,4-dimethylcyclohexane terephthalate.

Examples include polyvivalolactone and copolyesters containing these components.

The ratio of both polyamide/polyester components is usually within the range of 0.05 to 0.95. Further, in FIG. 1, it is preferable that A is polyamide and B is polyester, but the invention is not necessarily limited to this.

However, in order to achieve sufficient trapping of microcapsules, it is preferable that the fibrillated composite fiber has a single filament fineness of 0.7 denier or less, particularly 0.5 denier or less after fibrillation.

Here, "fibrillation" means that, for example, when a fibrillated composite fiber has a cross section as shown in Figure 1 (3), the joint of each component is divided, and the three segment yarns of one component and the other For example, when this composite fiber has a cross section as shown in Figure 1 (6), it is divided in the same way and becomes a cross-shaped fibril. This means that five fibrils are formed, consisting of one component's segment threads having a cross section of , and the other component's four segment threads having a fan-shaped cross section. Furthermore, even if the fibrillated composite fiber has any other cross-sectional shape, its fibrillated state is
This can be easily inferred based on the above description.

The fibrillated composite filament as described above can also be used as a crimped yarn or a latent crimped yarn. Among them, a latent crimped yarn is preferable, and the composite filament is heated-heat-set as described above. After being untwisted to form a crimped yarn, it can be further heat-set again under substantial tension to form a latent crimped yarn.

Furthermore, the fibrillated composite fibers can be used alone or in combination with other fibers to form a fiber structure.

There are no particular limitations on the other fibers, and any suitable synthetic filament yarn can be used, with polyester yarn being particularly suitable.
Among these, single yarn fineness of 1.5 denier or less is preferable! ,
Polyester yarns of 0 denier or less are most preferred,
Furthermore, natural fibers or recycled fibers can also be used. In textiles, fibrillated composite filaments are typically used in the weft yarns, and yarns containing conventional synthetic fibers, natural fibers, or recycled fibers are used in the warp yarns.

The above-mentioned fibrillation can be carried out by applying physical force using known methods, or by chemical methods such as swelling of the polymer component.

There is also a known method for obtaining ultrafine fibers by dissolving and removing certain components of composite fibers (Japanese Patent Publication No. 7723/1983).

The gap between the ultrafine fibers is preferably 20 μm or less, and it is particularly preferable that the cross section of each ultrafine fiber is not circular but angular. Due to such narrow gaps and the angular cross-section of the ultrafine fibers, the microcapsules are firmly held in the fibrous structure, especially without the need for a separate glue or binder. For this reason, the porosity of the fiber structure containing ultrafine fibers is 80% or less, especially 5%.
It is preferably 0% or less. Note that the porosity here refers to the weight (g) of the fiber structure x 100/vertical length (cm
) x Width (cm) x Thickness (cm) x Specific gravity (g/cm)
). In addition, this ultra-fine fiber has a
Preferably, the content is at least 30% by weight.

The composition of the fragrance-encapsulated microcapsules used in the present invention is not particularly limited as long as they can be broken by appropriate friction and emit a fragrance, and the microencapsulation method itself is known. From the viewpoint of sustained release of odorants and mechanical strength of the microcapsules, the wall material is preferably an organic polymer, such as polyurethane or urea-formalin resin.

Examples include, but are not limited to, cyclodextrin. However, it is preferable that the wall material is made of urea-formalin or melamine-formalin resin, and low-formalin microcapsules are particularly preferable.

The size of microcapsules is usually an average particle size of 1 to 50
.mu., preferably 5 to 20 .mu., particularly particles in which most of the particle size distribution falls within the range of 5 to 20 .mu. When the wall material is urea-formalin resin, the particle size is 2 to 50μ, preferably 5 to 20μ, and the wall thickness is 0.1 to 20μ.
μ is preferably about 0.5 to 4 μ, and when the wall material is melamine-formalin resin, the particle size is 5 to 50 μ.
The thickness of the wall is preferably about 5-20μ, preferably about 0.2-30μ, and preferably about 0.5-6μ.

The odorants as used in the present invention refer to natural fragrances, synthetic fragrances, and liquid or powder compounds that generate fragrances, either singly or as a mixture. Examples of natural fragrances include animal fragrances such as musk, civet, castoreum, and ambergris. , botanical fragrances include lemon oil, rose oil, citronella oil, sandalwood oil, and peppermint oil.

Cinnamon oil etc. In addition, as a synthetic fragrance, α-
There is a fragrance consisting of pinene, limonene, geraniol, linalool, lavandulol, nerolidol, etc.

This odorant is preferably 5 to 99% by weight, particularly preferably 50 to 95% by weight based on the total weight of the microcapsule.
Contained.

The silicone-based resin binder, which is most preferably used as a binder in the present invention, has a coating effect and plays a role as an adhesive between the microcapsules and the woven or knitted fabric, and has particularly good dispersibility in water. A silicone-based aqueous emulsion type that can be easily diluted with water is preferred, for example, one containing organopolysiloxane as a main component and emulsified with an emulsifier. This hardens by removing water and forms a rubber-like film that has the characteristics of silicone rubber.
It has a durable adhesive effect.

This organopolysiloxane emulsion is more preferably a low temperature reaction type organopolysiloxane prepolymer emulsion. The low temperature reaction type organopolysiloxane prepolymer emulsion mentioned here is:
For example, for every 100 parts of an organopolysiloxane and its derivatives having a small number (2 in each molecule) of hydroxyl groups bonded to silicon atoms, 0.0 parts of a reaction product of an aminofunctional silane or its hydrolyzate and an acid anhydride. 1 to 10 parts by weight and 1 to 5 parts by weight of colloidal silica
0f [1 to 60 parts by weight of a homogeneous dispersion of the entire organopolysiloxane and 0.01 to 0.01 to 60 parts by weight of a curing catalyst.
An aqueous silicone emulsion comprising 10 parts by weight, 0.3 to 20 parts by weight of an anionic emulsifier, and 25 to 600 parts by weight of water can be mentioned.

Furthermore, as the binder applicable to the present invention, an emulsion of a blocked isocyanate prepolymer having low temperature reactivity can be used together with a metal salt of a fatty acid. This low-temperature-reactive blocked isocyanate prepolymer includes sodium bisulfite, acetylacetone, ethyl acetoacetate, diethyl malonate, etc., which react with isocyanate groups to create temporarily stable compounds, which are then thermally dissociated by heat treatment. A prepolymer obtained by polymerizing an acrylic or methacrylic compound and a modified acrylic or methacrylic compound such as silicone-modified or fluorine-modified compound. can be mentioned.

Further, the metal salt of fatty acid is a catalyst that promotes the dissociation of blocked isocyanate, and examples thereof include zinc octylate, zirconium octylate, zinc laurate, and zinc stearate.

Furthermore, as this binder, an emulsion of an acrylic or methacrylic compound obtained by emulsion polymerization of a monomer containing one or more vinyl groups can also be used. Such emulsions include, for example, acrylic acid, methacrylic acid, methyl acrylate, methyl methacrylate, ethyl acrylate, ethyl methacrylate. It is an emulsion of emulsion polymers such as butyl acrylate, butyl methacrylate, acrylonitrile, acrylamide, N-methylol acrylamide, 2-hydroxyethyl acrylate, 2-hydroxybutyl acrylate, etc.

Furthermore, polyalkylene emulsions, emulsions of polyester resins made of polyhydric alcohols and polybasic acids, or polyurethane emulsions made of diisocyanates and polyols can also be used as binders.

This polyalkylene is polyethylene.

Polypropylene, etc., and polyhydric alcohols,
Ethylene glycol, l,4-butanediol, 1,6
Examples of polybasic acids include phthalic acid, adipic acid, maleic acid, trimetic acid, and terephthalic acid. Further, diisocyanates include hexamethylene diisocyanate, xylene diisocyanate, tolylene diisocyanate, 4.4°-diphenylmethane diisocyanate, 1,5-naphthalene diisocyanate, etc., and polyols include polyethylene adipate, polypropylene adipate, polybutylene adipate, etc. , polyethylene phthalate.

polyethylene glycol, polypropylene glycol,
Examples include polyethylene propylene glycol, and a polyurethane resin emulsion made of these forms a water-insoluble resin by drying.

Further, it is desirable that the binder contains a pressure buffer. Pressure AM agents include emulsions containing polyorganic carboxylic acids such as polyacrylic acid or acrylic acid and acrylate copolymers, compounds that form salts with alkaline substances such as ammonia and soda ash, polyacrylic acid sodium salts, Neutralized products of organic polycarboxylic acids such as polyacrylic acid ammonium salts and polyacrylic acid amino salts, or neutralized products of copolymers of acrylic acid and acrylates, polyalkylene glycols such as polyethylene glycol and polypropylene glycol, and polyethylene glycols. These are compounds selected from polyalkylene glycols such as glycol and polypropylene glycol whose ends are substituted with alkyl groups C, H□+1 [wherein n is an integer of 1 to 25], polyvinylpyrrolidone, and the like.

As mentioned above, microcapsules containing odorants (
It is added to a treatment solution consisting of the emulsion and preferably a pressure buffer and applied to the fiber structure. It is preferable to adjust the ash with sodium bicarbonate, ammonia, etc.

When this application is carried out by the padding method, spray method, or immersion deliquification method, the microcapsules containing the odorant are
-10% by weight, preferably 0.2-5.0% by weight, and 0.1-2Of[wt%] preferably 0.2-5.0% by weight of the emulsilone.
5 to 5.0% by weight, and preferably around 5% by weight of a pressure-resistant buffer, with a pickup rate of 10 to 2.
00%, preferably 40 to 150% by weight, by budding, spraying, dipping and dehydration. Particularly when using the blocked isocyanate prepolymer emulsion, it is desirable to use the fatty acid metal salt in an amount of 0.5 to 30% by weight, preferably 5 to 15% by weight, based on the blocked isocyanate.

Furthermore, when printing and coating methods are used, 0.1 to 10% by weight of microcapsules containing odorants, preferably 0.2 to 5.0% by weight, and 1 to 95% by weight of the emulsion, preferably 5 to 5% by weight. An aqueous solution or emulsion containing 95% by weight and around 5% by weight of a pressure buffer,
In the case of printing, the viscosity is 2000 to 8000 cps (
BM type viscometer (20℃), viscosity a for coating
oo.

It is preferable to adjust the amount to 16,000 cps.

In any case, the binder is 0.0% of the microcapsule.
It is applied 5 to 5 times, preferably 1 to 3 times (weight ratio), and exhibits a sufficient adhesive effect. If the amount is less than 0.5 times, the coating effect will be poor, while if it is more than 5 times the amount, the amount of microcapsules attached will hardly change. Depending on the type of resin, the problem of off-odor may occur, which is undesirable.

The amount of both of these substances usually accounts for 0.3 to 7.0%, preferably 0.5 to 5.0%, of the weight of the woven or knitted fabric in the area to which they are attached. In other words, since microcapsules are sufficiently attached to woven or knitted fabrics when the binder is applied in the above ratio, if the amount of both of these substances attached is less than the above 0.3%, the strength of the fragrance will be reduced. On the other hand, if it exceeds 7.0%, the texture of the woven or knitted fabric will be affected, and the fragrance sometimes emitted may become too strong, so both are unsuitable. . In other words, a product that satisfies all the requirements of having a favorable scent dispersion effect, a suitable texture and flexibility, and also having appropriate durability and not being interfered with by foreign odors, is suitable for the above-mentioned adhesion. It's the amount.

It is preferable to apply this binder to a final product such as clothing that does not undergo any post-processing, and the product may be immersed in a treatment liquid bath containing the binder, and then dehydrated and dried in a manner that does not impair the texture.

In addition, when the fiber structure to be treated contains the ultrafine fibers, the binder as described above is not used.
Microcapsules can be applied to a fibrous structure by dispersing the microcapsules in a liquid dispersion medium, preferably water, and impregnating the fibrous structure containing ultrafine fibers with this dispersion. However, in order to further increase the durability of the microcapsules so that they do not fall off during washing or the like, the microcapsule dispersion may further contain a sizing agent, a binder as described above, and the like. A glue like this,
It is not necessary to use a large amount of the binder; for example, about 0.1 to 2% by weight based on the dispersion is sufficient. In addition, from the viewpoint of further increasing the durability against repeated washing, an organic polymer binder is preferable to a sizing agent, and examples thereof include polyurethane elastomers, silicone resins, polyacrylic resins, polyurethane urea elastomers, and the like.

After applying the emulsion to the fiber structure in this manner, it is dried at a temperature below 150° C. to fix the microcapsules on the surface of the 11 fibers. An example of dry geography is drying at a temperature of 60 to 150"C, preferably 80 to 130"C for 10 seconds to 30 minutes, preferably 30 seconds to 10 minutes, or drying at a temperature of 80 to 150"C, preferably 100 to 13"C.
Heat treatment may be performed at 0° C. for 10 seconds to 10 minutes, preferably 30 seconds to 5 minutes.

In addition, softener, texture control agent, dye fixing agent.

There is no particular problem with the effects of the present invention even if ordinary finishing agents such as reactive resins, reduced resins, catalysts, etc. are used in combination. There is no problem even if the following are used in combination.

By the above-described treatment, a durable fragrance can be imparted to the fibrous structure without impairing its texture. However, in order to suppress a change in hue of the area to which the treatment liquid is applied, such as when a nearly colorless treatment liquid is used, it is desirable to perform a water repellent treatment prior to the above treatment. Furthermore, the water-repellent treatment prevents the microcapsules and the binder from penetrating into the fibrous structure, so that the hardening of the texture of the fibrous structure is suppressed and a decrease in strength is also suppressed.

The water repellent may be any compound that can impart any desired water repellency to the fiber structure, such as wax-based natural waxes and their derivatives such as Carteva wax and Candelilla wax, synthetic waxes such as higher fatty acids and higher Emulsions of solid esters made of alcohol, emulsions of silicone-based dimethylpolysiloxane and its derivatives,
Examples include emulsions of polyolefins such as polyethylene and polypropylene, emulsions of cationic quaternary amine compounds, etc., and emulsions of synthetic resins such as polyamides and polyacrylics alone or as copolymers.

In addition, for this water repellent treatment, for example, a water repellent alone or two or more may be used in an amount of 0.1 to 10% by weight, preferably 0.5 to 5% by weight.
The aqueous solution or emulsion consisting of
After padding in quantity%, the temperature is 80-190℃, preferably 120℃.
A method of drying at ~170°C is exemplified.

〔Effect of the invention〕

The present invention has the following effects due to the configuration described above.

First, since the fragrance-containing microcapsules are attached to a fibrous structure, such as clothing, the capsules are gradually broken during wear or due to intentional friction, releasing a suitable fragrance. Therefore, the fragrance does not emanate and disappear all at once, but has sufficient sustainability.

In addition, by adding a resin binder to the microcapsules in an appropriate ratio, the adhesive strength and adhesion properties are significantly improved, and the desired amount of adhesion and good fragrance durability are achieved.

The manufacturing method does not require complicated processing steps, and by applying a treatment agent containing a mixture of microcapsules and a resin binder in an appropriate ratio and performing heat treatment, the fiber structure of woven or knitted fabrics or clothing can be improved. It is possible to impart a durable fragrance to objects without impairing their original texture.

That is, by selecting the microcapsules, binder, pressure buffer, processing temperature, etc. as in the present invention, there is less destruction of the microcapsules during the processing process, and the destruction of the microcapsules occurs only when the fibrous structure is used (worn). This will allow the aroma to be sufficiently released. In particular, when a silicone-based binder is used, the problem of aroma interference due to the binder's off-flavor does not occur.

In addition, the adhesion of microcapsules to fiber structures is good, but this does not impair the texture, especially if water-repellent treatment is performed prior to fragrance treatment, the texture, hue, strength, etc. can suppress the decline in

In addition, in view of the fact that conventional fiber structures containing ultrafine fibers either lacked durability significantly, or had rough and hard texture after achieving durability, the fiber structures with fragrance of the present invention ,
The effects of the present invention are remarkable because durability is imparted without impairing the feel and there is no problem of binder odor.

Hereinafter, the present invention will be explained in detail based on examples.

Example 1 The following 10 types of dyed woven products and clothing were subjected to water-repellent treatment according to a standard method (water-repellent softener: mainly composed of methylhydrodiene polysiloxane). In addition, 10 g/l of microcapsules containing fragrance of urea resin (jasmine scent, average particle size 8 μm, M thickness 1 μm) was added to 10 g/i (or 20 g/i Mixed thoroughly.

Next, the emulsion containing the microcapsules was printed, immersed, or padded onto a woven or knitted fabric, followed by centrifugal dehydration, drying, and a moist heat treatment of 120 to 130" C1. In this way, the fragranced microcapsules were attached. The woven and knitted fabrics and garments are then sent to a drying and final setting process to form aromatic woven and knitted fabrics or aromatic clothing layers.

■ Cotton Ne40/-2 interlock ■ Cotton Ne
40/2 single jersey ■ Sweater knitted with mNe18/4 colored yarn ■ Cardigan knitted with Ne18/4 colored yarn made of 50% cotton and 50% absorbent porous acrylic ■ Ne40 made of 65% polyester and 35% rayon
122 x 79/inch) twill weave ■ 50% polyester
Dobby weave of 50% cotton Ne45 (120x76/inch) ■Mixed yarn of normally spun U-section filament and high-speed spun round-section filament False twisted yarn 75 d y'36, f
Black-dyed fabric with pear-skinned Georgette on the outside and satin on the back (2
20 x 87/inch) ■ Aibetsu double layer 14 momme (60.2 g, /rIi) ■ Plain fabric using No. 48 wool twin yarn 0 Silk de Chine fabric 12 momme (51.6 g/ff1) Next, from the above woven and knitted fabric ■ After tailoring a sports training bar, a sports shirt from ■, a dress shirt from ■ and ■, formal wear from ■, a tie from ■ and ■, and a scarf from [phase], dry cleaning durability and texture were tested.

In addition, the dry cleaning resistance test was conducted according to JISLO21.
It was carried out according to the 7401 method and expressed as the number of times until the fragrance disappeared. In addition, the fragrance was evaluated by 10 people on a 5-point scale (0 points are given for those emitting the optimal fragrance, +1 points are given above and below for those that are too strong, and -1 points are given for those that are too weak).
-2) and the average score was taken as the evaluation score. Regarding the texture, 10 people also found it to be good and slightly poor.

0 for each item that you felt was inferior. -1. -2 and the average score was taken as the evaluation score.

Looking at these results, it becomes clear that the fragranced clothing according to the present invention has achieved the original purpose, that is, it has a durable, pleasant scent and a good texture. Dew.

Example 2 Knit and dye the following two types of stockings.

After the fixing process was completed, the process was carried out in the same manner as in Example 1.

Test item; ■Pantyhose leg part; 15d/3f kennel thread Panty toe part; 30d/8f woolly thread ■Pantyhose (support type) Leg part: (20X13X18DCY)X13d/
Part of 3f raw silk panties: (20X30POY)X30d/8f
Woolly yarn tow part: 13d/3f raw silk X30d/8f woolly yarn % o w f [Sanyo Kasei Kogyo ■] Buffer; Ultra MT [Mitejima Kagaku Kogyo ■] The washing resistance test was conducted according to the JIS L0217103 method, and was expressed as the number of times until the fragrance disappeared.

In addition, the fragrance was evaluated by 10 people on a 5-point scale (0 points are given for those emitting the optimal fragrance, +1 and +2 are given for those that are too strong above and below that, and -1 and -2 are given for those that are too weak). ), and the average score was used as the evaluation score. Regarding texture, the same <10 people checked only those items that they felt were particularly poor, and expressed in the number of checks.

Looking at these results, it becomes clear that the aromatic stockings according to the present invention have achieved the original purpose, that is, they have a durable, pleasant scent and a good texture. Dew.

Furthermore, the test method that is the basis for the numerical values in the examples listed below is as follows.

(1) Tear strength JIS L-10%D method (2) Washing JIS L-0217103 method (3) Dry cleaning JIS L-0217401 method (4) Fragrance Scored based on the criteria shown below for 10 testers. It is shown as the average value of the evaluation.

5: Optimal fragrance 4: A little less 3: About half of it 2: A little bit 1: Almost none 0: None 5) Discoloration/Sl! At one time /S = (1-R)' /2R (R: maximum absorption wavelength of spectrophotometer) ○: K/S! 4 degree change 3% or less Δ: 〃 3-10% A plain cotton fabric with a weft count of 60, a thread density of 88 strands/inch, and a basis weight of 70 g/m was obtained.

To this plain woven fabric, 31i amount % of Viclon 29 (cationic softener made by Ipposha Yushi Kogyoki) and light silicone R-167 were added.
(Silicone-based softener manufactured by Kyoeisha Yushi Kogyo ■) 11% by weight of an aqueous treatment liquid was padded at a pick-up rate of 70%, and then dried at 130° C. for 1 minute. After that, particle size 5 to 15μ (average 1
1% by weight of an aqueous dispersion containing 46% by weight of microcapsules with a wall material of urea-formalin resin of 0μ), and KM- of an organopolysiloxane prepolymer emulsion.
After padding with an aqueous treatment solution containing 3% by weight of 2002T (manufactured by Shin-Etsu Chemical) at a pickup rate of 70%, drying was performed at 120° C. for 2 minutes.

Table 3 shows the physical properties and fragrance durability of the obtained plain cotton fabric.

Example 4 The same cotton plain fabric as that used in Example N3 was used, and the particle size was 5 to 15 μm (average
Pick up an aqueous treatment liquid consisting of 1% by weight of an aqueous dispersion containing 46% by weight of microcapsules whose walls are made of urea-formalin resin (Oμ) and 3% by weight of Boccoat R3020 (acrylic emulsion manufactured by Dainippon Ink ■). After padding at a rate of 70%, drying was performed at 120° C. for 2 minutes.

Table 3 shows the physical properties and fragrance durability of the obtained plain cotton fabric.

Comparative Example 1 Using the sample obtained in Example 3, the sample was further heated at 150°C.
Heat fixation was performed for 3 minutes at .

Table 3 shows the physical properties and fragrance durability of the obtained plain cotton fabric.

Table 3 Example 5 A warp silk spinning machine 140 which was refined, bleached and printed using a commonly known method. Thread density: 114 threads/inch using count double yarn, thread density: 89 threads/inch using 66 count single thread from weft silk spinning, weight: 82 g
/m" Fuji silk plain fabric was obtained.

This plain woven fabric was padded with an aqueous treatment solution containing 5% by weight of Silicolane ES-10 (Ipposha Yushi Kogyo A+* silicone softener) at a pickup rate of 80%, and then dried at 130° C. for 1 minute.

After that, sandalwood oil (synthetic blended fragrance manufactured by Takasago International Corporation) 89
1 mm% of an aqueous dispersion containing 48% by weight of microcapsules having a particle size of 4 to 14μ (average 9.5μ) as a wall material of urea-formalin resin, and organopolysiloxane prepolymer emulsion KM-20027.
Viscosity: 6800 cps (BM type viscometer Printing was carried out using a 120-mesh flat screen using printing paste (20°C), and then dried at 130°C for 1 minute.

Table 4 shows the physical properties and fragrance durability of the obtained Fuji net.

Example 6 The same Fuji net used in Example 5 was used to produce urea containing 89% by weight of sandalwood oil (synthetic blended fragrance manufactured by Takasago International Corporation) and having a particle size of 4 to 14 μm (average 9.5 μm). - 1% by weight of an aqueous dispersion containing 48% by weight of microcapsules whose walls are formalin resin, and Rikenzor A-105
(Acrylic ester binder manufactured by Miki Riken Kogyo)
5% by weight and 94% by weight of the same emulsion glue used in Example 5, with a viscosity of 7200 cps (BM
Using printing paste (type viscometer 20℃),! After printing with a 20 mesh flat screen, 130
Dry at ℃ for 1 minute.

Table 4 shows the physical properties and fragrance durability of the obtained Fuji net.

Comparative Example 2 Using the sample obtained in Example 5, the sample was further heated at 150°C.
Heat fixation was performed for 3 minutes at .

Table 4 shows the physical properties and fragrance durability of the obtained Fuji net.

Table 4 Example 7 A sweater cardigan and skirt were knitted and sewn using a cotton/acrylic blend ratio of 5G 150:36 yarn that had been scoured, bleached, and dyed by a commonly known method. .

After this sweater was immersed for 30 seconds in an aqueous treatment solution consisting of 1% by weight of Silicolan ES-10 (silicon softener made by Ippo Sha Yushiko 1! Masu) and 2% by weight of Yodozol PR400 (polyethylene emulsion made by Kanebo N5Ce). , centrifugally dehydrated to a pick-up rate of 95%, and incubated at 80°C for 20
Drying was performed for minutes. Thereafter, an aqueous dispersion containing 52% by weight of microcapsules having a wall material of melamine-formalin resin with a particle size of 12 to 18μ (average 15μ) containing 90% by weight of a lemon-lime fragrance (manufactured by Takasago International Corporation, synthetic blended fragrance) 1) Emulsion of siloxane prepolymer KM-20021,-1 (Shin-Etsu Chemical @ J Dehydrate in a dehydrator, prepare the mold, and dry at 95℃ in an open dryer.
Drying was performed for 0 minutes. Table 5 shows the durability of the scent of the sweaters, cardigans and skirts obtained.

Table 5 Example 8 Scoured, bleached, mercerized and dyed by a commonly known method, warp 60, yarn density 90/inch, weft 60,
A plain cotton fabric with a thread density of 88 threads/inch and a basis weight of 70 g/m' was obtained. This plain weave contains 47% by weight of microcapsules whose wall material is a urea-formalin resin with a particle size of 5 to 15μ (average 10μ) containing 92% by weight of Fragrance 5H3037 (vendor synthetic fragrance manufactured by Takasago International Corporation). The aqueous dispersions were (A) 0.2% by weight, (B) 1.
0 wt%, (C) 3.0 wt%, and organoborisiloxane gorebolimer emulsion KM2002L-1
((manufactured by Etsu Kagaku)) An aqueous buffer consisting of the following components: (A) 94.8% by weight, (B) 9
Using a printing paste containing 4% by weight and 92% by weight of (C), printing was carried out using a 120-mesh flat screen, followed by drying at 130"C for 1 minute.

Table 6 shows the physical properties and fragrance durability of the obtained plain cotton fabric. Furthermore, the shapes of the fibers of each cotton plain fabric to which microcapsules are attached are shown in FIGS. 2(A), 2(B), and 2(C).

Comparative Example 3 The same cotton plain fabric as that used in Example 8 was used, and the particle size was 5 to 15 μm (average 10 μm) containing 92% by weight of fragrance 5H3037 (vendor-based synthetic fragrance manufactured by Takasago International Corporation). 1% by weight of an aqueous dispersion containing 47% by weight of microcapsules whose wall material is urea-formalin resin, 5% by weight of binder LE-25 (acrylic binder manufactured by Hayashi Kagaku Kogyo ■), and fine gum HE (Daiichi Kogyo ■).
Printing was carried out using a 120 mesh flat screen using a printing paste with a viscosity of 5800 cps (BM type viscometer at 20°C) containing 94!1% by weight of an aqueous paste consisting of 5% by weight of carboxymethylcellulose (manufactured by Carboxymethyl Cellulose), and then printing at 130°C. It was dried for 1 minute.

Table 6 shows the physical properties and fragrance durability of the obtained plain cotton fabric.
Moreover, the shape of the fibers of the cotton plain fabric after processing is shown in FIG.

Table 6 Example 9 A melamine formalin resin with a particle size of 8 to 18 μm (average 12 μm) containing a musk type fragrance (synthetic fragrance manufactured by Takasago International Co., Ltd.) 88 weight 9 I was added to the Fuji silk plain fabric used in Example 5. Microcapsule 52 with wall material! 1.5% by weight of an aqueous dispersion containing i%, 3% by weight of KM-20027 (Shin-Etsu Chemical side type) of an emulsion of organopolysiloxane prepolymer, and end groups of polyethylene glycol with a molecular weight of 22,000. After padding with an aqueous treatment solution consisting of 10% by weight of a buffer consisting of 5% by weight of an alkyl group substituted substance of Ct 7 Hs h and each component at a pickup rate of 80%, drying was performed at 120°C for 2 minutes. .

Table 7 shows the physical properties and fragrance durability of the obtained Fuji silk.

Comparative Example 4 The same Fuji silk as that used in Example 9 was used, and 88% by weight of musk type fragrance (synthetic fragrance manufactured by Takasago International Co., Ltd.)
1.5% by weight of an aqueous dispersion containing 52% by weight of microcapsules whose walls are made of melamine-formalin resin with a particle size of 8 to 18μ (average 12μ), and Boncourt R-13.
6 (acrylic binder manufactured by Dainippon Ink ■) at a pick-up rate of 80%, the pad was dried for 2 minutes at 120°C.

Table 7 shows the physical properties and fragrance durability of the obtained Fuji silk.

Comparative Example 5 Using the sample obtained in Comparative Example 4, 150"
Heat treatment was performed at C for 3 minutes.

Table 7 shows the physical properties and fragrance durability of the obtained Fujigumi.

Table 7 This plain woven fabric was subjected to the same treatment as in Example 8.

Table 8 shows the physical properties and fragrance durability of the obtained plain woven fabric.

Table 8 Example 10 A yarn with a warp of 60 and a yarn density of % threads/inch, which was scoured, bleached, mercerized, heat set, and dyed by a commonly known method.
Weft count 60, thread density 72 threads/inch, basis weight 82 g/m”
A blended plain woven fabric consisting of 75% cotton and 25% polyester was obtained.

Implementation @ 11 Scoured, bleached, mercerized, and dyed using commonly known methods, warp count 40, yarn density 90 threads/inch, weft count 40,
Thread density 75/inch, basis weight 108g/m! A plain cotton fabric was obtained. This plain weave is used for fragrance BA9185 (
Each aqueous dispersion containing 93% by weight of microcapsules (A) 48% by weight of microcapsules with a particle diameter of 7 to 16μ (average 12μ) and melamine-formalin resin wall material containing 93% by weight of citrus-based synthetic fragrance (manufactured by Takasago Perfumery Co., Ltd.) %, (B) 0.5% by weight, (C) 2. (lffiffi!%, and 5% by weight of Hielaston on M-2076 (blocked isocyanate emulsion of natural polysaccharides manufactured by Daiichi Kogyo Seiyaku ■) and Elastron Catalyst 32 (metal salt of fatty acids manufactured by Daiichi Kogyo Seiyaku Co., Ltd.) (A) 94.3% by weight, (B) 94% by weight, (C
) After adjusting the pH of the printing paste containing 9Z511i to 9 with baking soda, printing was performed using a 120 mesh flat screen, and heat treatment was performed at 120°C for 1 minute and at 130°C for 2 minutes and 30 seconds.

The physical properties and fragrance durability of the obtained plain cotton fabric were evaluated using the same plain cotton fabric as that used in Comparative Example 6 and Example 11.
Water containing 48% by weight of microcapsules whose wall material is melamine-formalin resin with a particle size of 7 to 16μ (average 12μ) containing 93% of Fragrance BA-9185 (citrus synthetic fragrance manufactured by Takasago International Corporation) The dispersion liquid was divided into (A) α, 2% by weight, (B) 0.5% by weight, and (C
) ZO melon weight, and 5% by weight of Elastron M-2076 (natural polysaccharide blocked isocyanate emulsion manufactured by Dai-Kogyo Seiyaku) and Elastron Catalyst 32
(Dai-Kogyo Seiyaku side-type fatty acid metal salt catalyst) 0.5% by weight
and Fine Gum HE (carboxymethyl cellulose, manufactured by Daiichi Kogyo Seiyaku ■) in an amount of 5% by weight.
) 94.3% by weight, (B) 94.0% by weight, (C) IJ
After adjusting the printing paste with L5% by weight to pH 9 with baking soda! Printing was performed using a 20-mesh flat screen and dried at 120° C. for 1 minute.

Table 9 shows the physical properties and fragrance durability of the obtained plain cotton fabric.

Comparative Example 7 Using the same cotton plain fabric as that used in Example 11,
An aqueous dispersion containing 93% by weight of Fragrance BA9185 (citrus-based synthetic fragrance manufactured by Takasago International Corporation) and 48% by weight of microcapsules whose walls are made of melamine-formalin resin with a particle size of 7 to 16 μm (average 12 μm). (A) 0.2% by weight, (B) 0.5% by weight, (C) Z
(A) 94.81% by weight, (A) 94.81% by weight, 5% by weight of Boncoat R3020 (acrylic binder manufactured by Dainippon Ink ■), and 5% by weight of polyacrylic acid sodium salt with a molecular weight of 720,000. B) 94.5% by weight, (C) 93.0! A printing paste consisting of 1J1% was printed using a 120 mesh flat screen and dried at 120°C for 1 minute.

The physical properties and fragrance durability of the obtained plain cotton fabric are shown in Table 9. Example 12: Uses warp silk spun 140 count double yarn, scouring, bleaching, mercerizing, and dyeing using commonly known methods, yarn density: 114. / inch, weft silk spinning 66 count single yarn, thread density 89 / inch,
A Fuji silk plain fabric with a basis weight of 62 g/m' was obtained.

This plain woven fabric is made of fragrance BA7985 (jasmine-based synthetic fragrance manufactured by Takasago Fragrance Industry @) containing 91% by weight of particle size 5.
1% by weight of an aqueous dispersion containing 46% by weight of microcapsules whose wall material is urea-formalin manure consisting of ~15μ (average 10μ), and Elastron M-1039B (fluorine-modified acrylic manufactured by Daiichi Kogyo Seiyaku ■). Blocked isocyanate emulsion) 51flL% and Elastron Catalyst 32 (fatty acid metal salt catalyst manufactured by Daiichi Kogyo Seiyaku ■)
0.5% by weight and a molecular weight of 22,000 polyethylene glycol with terminal groups of C, H□ alkyl group substitution product 5! l
An aqueous treatment solution consisting of 5% by weight of each component was adjusted to pH 9 with baking soda, and a pickup rate of 60% was obtained.
After padding at 120°C for 2 minutes,
Heat treatment was performed at ℃ for 2 minutes.

The physical properties and fragrance durability of the obtained Fuji silk were evaluated in Comparative Example 8. The same Fuji silk as that used in Example 12 was used, and fragrance BA-7985 (jasmine-based synthetic fragrance manufactured by Takasago International Co., Ltd.) 91i amount 1% by weight of an aqueous dispersion containing 46% by weight of microcapsules whose wall material is urea-formalin resin with a particle size of 5 to 15μ (average lOμ) including
, and 5% by weight of Boncoat R-510 (acrylic binder manufactured by Dainippon Ink ■), and 5% by weight of a buffer consisting of 5% by weight of an alkyl group substituted product of polyethylene glycol having a molecular weight of 22,000 and an end group of C1211M. The aqueous treatment liquid was padded at a pickup rate of 70%, dried at 120°C for 2 minutes, and heat treated at 130°C for 2 minutes.

The physical properties and fragrance durability of the obtained Fuji silk are shown in Table 1θ.Example 13 The plain cotton fabric used in Example 11 was used as Fragrance BA798.
5 (Jasmine-based synthetic fragrance manufactured by Takasago Fragrance Industry Co., Ltd.) 913℃
Microcapsules with a wall material of urea-formalin resin having a particle size of 5 to 15 μm (average 10 μm) including
Each aqueous dispersion containing 6% by weight (A) 0.2% by weight
, (B) 1.0% by weight, (C) &0% by weight, and 5% by weight of Yodozol A-1209 (jl [Spun NSC@H acrylic emulsion binder) and 5% by weight of polyacrylic acid sodium salt with a molecular weight of 720,000. An aqueous buffer consisting of (A) 94.8% by weight, (B) 94% by weight, and (C), respectively.
92 Comparative Example 9 Using the same cotton plain fabric as that used in Example 13,
Fragrance BA-7985 (jasmine-based synthetic fragrance manufactured by Takasago Fragrance Industry Co., Ltd.) Containing 91% by weight, particle size 5-15μ (
An aqueous dispersion containing 4.6% by weight of microcapsules whose walls are made of urea-formalin resin with an average of lOμ) (A) 0.2wt 11%, (B) 1rLJ 1%,
(C)&0% by weight and U Yodozol A-1209 (Kanebo NS CIm 1')') Lux Mulsion Binder) 5% by weight and Fine Gum HE (Carboxymethyl cellulose manufactured by Daiichi Kogyo ■) 5% by weight. (A) 94.8% by weight, (B) 94.0% by weight, respectively.
(C) After printing with a printing paste consisting of 9λ0% by weight using a 120 mesh flat screen, at 130°C.
and dried for 1 minute.

The physical properties and fragrance durability of the obtained cotton plain fabric are shown in Table 11. Example 14 The Fuji silk plain fabric used in Example 5 was treated with particles containing 89% by weight of sandalwood oil (synthetic fragrance manufactured by Takasago International Corporation). Diameter 4~14μ
2% by weight of an aqueous dispersion containing 48% by weight of microcapsules whose walls are made of urea-formalin resin (average 9.5μ), and Superflex E-2000 (polyurethane emulsion manufactured by Daiichi Kogyo Seiyaku ■) 5 % by weight, and the terminal group of polyethylene glycol with a molecular weight of 22,000 is C.
An aqueous treatment solution consisting of 8% by weight of a buffer consisting of 5% by weight of an alkyl group substituted product of r t H*s was padded at a pick-up rate of 70%, and dried at 120°C for 2 minutes. After that, heat treatment was performed at 130° C. for 1 minute.

Table 12 shows the physical properties and fragrance durability of the obtained blind silk.

Comparative Example IO Four microcapsules were made using the same Fuji silk as that used in Example 14 and had a wall material of urea-formalin resin containing 89% by weight of sandalwood oil (synthetic fragrance manufactured by Takasago International Corporation).
After padding with an aqueous treatment liquid consisting of 2% by weight of an aqueous dispersion containing 8% by weight and 5% by weight of Superflex E-2000 (polyurethane emulsion manufactured by Daiichi Kogyo Seiyaku ■) at a pickup rate of 70%, the mixture was heated at 120°C. Drying was performed for 2 minutes, and then heat treatment was performed at 130° C. for 1 minute.

Table 12 shows the physical properties and fragrance durability of the obtained Fujigumi.

Table 12 Example 15 Scouring, bleaching, and printing were carried out using a commonly known method.4
0 count, thread density 90 threads/inch, weft count 40, thread density 7
A plain cotton fabric with 5 pieces/inch and a basis weight of 108 g/m'' was obtained.

This plain woven fabric contains 91% by weight of fragrance BA7985 (jasmine-based synthetic fragrance manufactured by Takasago International Corporation) and 46% by weight of microcapsules whose wall material is a urea-formalin resin with a particle size of 5 to 15μ (average 10μ). Aqueous dispersion (A) 0, 2% by weight, (B) 1.01%, respectively
i amount%, (C)&0% by weight, and Hyotosole PE-40
(A
), 94.8% by weight of (B), and 92% by weight of (C) was printed using a 120 mesh flat screen, and then dried at 130'C for 1 minute.

Table 13 shows the physical properties and fragrance durability of the obtained plain cotton fabric.

Table 13 Example 16 Using the Fuji silk plain fabric used in the above-mentioned Example N5, byakudan-mae (
2 weights of an aqueous dispersion containing 48% by weight of microcapsules made of urea-formalin resin with a particle size of 4 to 14μ (average 9.5μ) and having a wall material of urea-formalin resin containing 89% by weight of synthetic fragrance manufactured by Takasago Fragrance Industry (aJ). %, and Finetex ES675
'(Polyester emulsion manufactured by Dainippon Ink ■) 5f
[Pickup rate of an aqueous treatment liquid consisting of 1% J and 8% by weight of a buffer consisting of 5% by weight of an alkyl group substituted product of polyethylene glycol with a molecular ff of 122,000 and an end group of 01□Hs s. 120 after padding at 70%
Drying was performed at 130° C. for 2 minutes, and heat treatment was performed at 130° C. for 1 minute.

Table 14 shows the physical properties and fragrance durability of the obtained Fuji silk. becomes 2/2
A twill fabric (density diameter x weft = 110 x 9 G pieces/inch) was prepared.

An aqueous solution (30°C) containing 1% by weight of benzyl alcohol 1011j1914 and emulsifier Sanmol BK Conc (manufactured by NICCA Chemical Industry ■) was pad-nipped onto the above fabric (squeezing ratio 5ort amount 94), and then left at room temperature for 10 minutes. did. Next, the nip alone was repeated 5 times, washed with warm water at 70° C. for about 2 minutes, and dried.

The weft of the fabric is fibrillated and has a thickness of approximately 0.1 to 0.2 d.
The single yarn fineness is , and the fabric density is 170 x 100 threads/inch (the number of weft threads as raw threads).

This woven fabric was heat set at 190°C and dyed to obtain a fiber structure used in the present invention.

Microcapsules with a diameter of about 5 to 10 microns were prepared, which were made of 20% by weight of urea-formalin resin as a wall material and 80% by weight of fragrance oil. Then, 1% by weight of the microcapsules and the urethane elastic material Elastron F-29 were added to the water.
(manufactured by Daiichi Kogyo Seiyaku ■) A dispersion containing 0.5% Ii was pad-nipped onto the fiber structure, and the pick-up rate was 6.
It was dried at 0f [% by weight] and 120°C.

The product obtained in this way was washed repeatedly in accordance with JIS L-1042 and tested for fragrance durability.
The scent was clearly recognized even after washing twice. For comparison, when a polyester knit containing no fibrillated composite fibers was processed in the same manner, a scent was observed after one wash, but almost no scent was observed after two washes.

Example 18 Using a fibrillated composite fiber yarn of 40 d/25 f, an interlock knitted fabric (wale/course=50/6 Q) was knitted using a 40-gauge circular knitting machine.

20 wt% benzyl alcohol and 20 wt% emulsifier
An aqueous solution (30° C.) containing the above was pad-nipped onto the knitted fabric (squeezing ratio: 100% by weight). And again, the above pad -
After nipping, the knitted fabric was immersed in hot water at 80° C. for 20 minutes in a relaxed state to shrink the knitted fabric and remove benzyl alcohol, and then dried. The area shrinkage rate of knitted fabric is 6
It was 0% by weight.

A 0.5% by weight dispersion of the same microcapsules as in Example 17 in water (without binder resin) was placed in a pan, and the bottom surface of a stainless steel roller with fine grooves cut into it was placed in the dispersion. The microcapsule dispersion liquid was applied to the knitted fabric by dipping and nipping the knitted fabric between a roller and a rubber roller disposed above the knitted fabric, followed by continuous drying at 100°C.

When the durability of the fragrance was tested in the same manner as in Example 17, it was found to be 5.
The scent was clearly recognized after washing twice. For comparison, a similar test was conducted using a polyester knit made of 40 d/25 f fibers that are not fibrillated composite fibers, and almost no scent was observed after one wash.

Example 19 The following dyed yarn was subjected to water repellent treatment using the water repellent softener of Example 1 according to a conventional method. Further, 2 g/It of the fragrance-containing microcapsules of Example 1 and 5 g/I of the silicone-based aqueous emulsion were mixed. Next, the thread was immersed in the emulsion so that the amount of microcapsules attached was 0.45%, and then dried at 90°C for 20 minutes and dry heat treated at 130°C for 30 seconds. The hand-knitted woolen yarn or handicraft yarn to which the fragrance-containing microcapsules were attached in this way was sent to a final setting process according to a conventional method, and was made into an aromatic hand-knitted woolen yarn or handicraft yarn.

■ Hand-knitted yarn made from 12th and 4th wool ■ 18th wool
Hand-knitted wool yarn made from No. 4 Shiko ■ Hand-knitted yarn made from 18 No. 4-ko yarn made of 50% wool and 50% porous acrylic ■ Handicraft yarn made from 16's/3 cotton ■ 50% cotton and 50% porous acrylic Craft yarn made of 16's/3 of cotton ■ Lace thread made of 50's/3 of cotton These were tested for washing durability in accordance with the JISL0217 1% method and texture in the same manner as in Example 1. did. The results are shown in Table 15. The results show that the aromatic hand-knitted wool yarn or handicraft yarn of the present invention has achieved the original purpose, that is, it has a durable, pleasant scent and a good texture. It will become clear that they have.

Example 20 The following five types of dyed fabrics were subjected to water repellency treatment and aroma microcapsule adhesion treatment in the same manner as in Example 1, and then dried and finish-set according to a conventional method to obtain aromatic fabrics.

■ 75 d/36 f polyester yarn round cross section on the back, 75 d/36 f round cross section on the front, 28 gauge 2 bar fancy knitted fabric using three types of polyester yarn: triangular cross section and cationic dyeable ■ 75 d on the back /36f round cross section polyester thread,
French back brushed fabric using 3 types of polyester threads with round cross section of 75d/36f on the front, triangular cross section and cationic dyeable ■ 75d/36f round cross section polyester thread on the back and middle, round cross section and cationic dyeable on the front Velor fabric using two types of polyester yarn ■ 50 d/24 f round cross section PB on the back and middle
Two types of T-processed yarn and round cross-section polyester yarn 50 d/24 f, a highly stretchable twill fabric using 75 d/36 f round cross-section polyester yarn on the front ■ Round cross-section polyester yarn 75 d/36 f and insert yarn 3. No. 60 polyester/IT blend yarn. A car seat was made from Raschel knitted lace with the real twisted yarn, a car seat was made from the above woven and knitted fabrics (1), (2) and (2), a side material was made from (2), and a seat cover was made from -0 and (2), and then their washing durability and texture were tested.

The washing resistance test was conducted according to the JIS L0217103 method, and the number of times until the fragrance disappeared was as follows: Example 21 Fineness: 1. Using a 6-nylon staple with a θ denier and a fiber length of 51 m, a web was created with a card and a cross wrapper, and this web was needle punched,
A three-dimensional nonwoven fabric having a weight of 15 g/nf, a thickness of 1.0 l, and an apparent density of 0.15 g/ai was obtained.

A 16% dimethylformamide solution of polyurethane lastomer was added to this nonwoven fabric at an impregnation rate of approximately 50% per weight of the nonwoven fabric.
After impregnating it to a concentration of 0%, it was immersed in a 40° C. coagulation bath [water dimethylformamide = 80:20 (weight ratio)] to coagulate. Next, the substrate was immersed in warm water at 60° C. for 2 hours to remove the solvent, and then dried with hot air at 120° C. to obtain a base material filled with polyurethane lastomer.

The substrate thus obtained had a weight of 280 g/ad.

Next, on the surface of this base material, a particle system of 5 to 10μ (average 8μ 400 g/d of a solution prepared by adding and mixing microcapsules whose walls are made of urea-formalin resin ° in an amount of 6% based on the solid content of the polyurethane elastomer, and then in a coagulation bath at 40 °C [water dimethylformamide = 80:2G (weight ratio)] after immersion for 30 minutes, 60
After soaking in warm water at 100°C for 2 hours and rinsing thoroughly,
The product was dried with hot air to obtain synthetic leather with a silver surface.

According to the present invention, it is possible to produce aromatic, silver-faced synthetic leather without requiring any special measures in each process such as the coagulation process, and the resulting synthetic leather has mechanical properties, For example, in terms of bending resistance, there is no inferiority compared to a product that does not contain aromatic microcapsules.

[Brief explanation of drawings]

FIG. 1 is a cross-sectional view showing a composite fiber used in an example of the present invention, and FIGS. 2 and 3 are photographs showing the shape of the fiber to which microcapsules are attached (50x magnification). ). Man. Diagram of different fiber components

Claims (5)

[Claims] (1) Fragrance-filled microcapsules are fixed to the fiber structure by a resin binder, and the weight ratio of the microcapsules to the resin binder is 2:1 to 1:5, and the amount of both of them adhered to the attached part. 0.3 of the fiber structure weight
Aromatic fiber structures account for ~7.0%. (2) The aromatic fiber structure according to claim 1, wherein the microcapsules have a wall material made of a formalin-based resin selected from urea-formalin resin and melamine-formalin resin. (3) Claim 1 wherein the resin binder is a silicone resin.
The aromatic fiber structure described. (4) Contains fibers with a single yarn denier of 0.7 denier or less,
An aromatic fiber structure characterized in that microcapsules containing an odorant and having an average diameter of 1 to 50 microns are retained in the fiber gaps of the fiber structure having a porosity of 80% or less. (5) After applying a treatment liquid consisting of microcapsules containing odorants and an emulsion of a low-temperature-reactive organopolysiloxane prepolymer to at least a portion of the fiber structure, drying at a temperature of less than 150°C . A method for producing an aromatic fiber structure, which comprises fixing the microcapsules to the surface of fibers.