JPH01280080A - Method for durable aromatic treatment - Google Patents

Abstract

PURPOSE:To obtain an aromatic fiber rich in persistence with durability by applying a treating liquid containing microcapsules enclosing an aromatic substance therein and low-temperature reactive type organopolysiloxane prepolymer to part of a fiber structure. CONSTITUTION:A treating liquid consisting of microcapsules enclosing an aromatic substance therein and having urea formalin resin as a wall agent and a low-temperature reactive type organopolysiloxane prepolymer is applied to at least part of a fiber structure, which is then dried at (150 deg.C to adhere the above-mentioned microcapsules to the fiber surface and afford the aimed soft aromatic fiber rich in durability in washing. Furthermore, water repellent treatment can be carried out before the aromatic treatment to suppress deterioration in feeling, hue and tenacity.

Description

DETAILED DESCRIPTION OF THE INVENTION (Industrial Field of Application) The present invention relates to a method for treating fibrous structures with good durability.

(Prior Art) Various methods have been used to impart fragrance to fiber structures.

For example, a method of applying microcapsules containing an odorant and a sizing agent to a textile product (Japanese Unexamined Patent Publication No. 49-19197), applying a mixture of microcapsules containing a fragrance and an acrylic resin to obtain an fragrant towel fabric. Method, (Unexamined Japanese Patent Publication No. 1983-
4886) A method for obtaining a printed article that emits a fragrance by printing an Ikkyo dye paste consisting of microcapsules of a fragrance coated with a paste wall film, a thermoplastic substance, and a thickener.

(Japanese Patent Publication No. 53-47440, Japanese Patent Application Publication No. 53-49200)
A method for obtaining an aromatic printed material that emits an aroma by thermally transferring a binder layer consisting of microcapsules of a fragrance, a dye, a polymer resin, etc.
6885) Also, a method of applying porous powder adsorbing odorants together with a water-soluble glue (Japanese Unexamined Patent Publication No. 48-36483)
A method of applying a mixture of a fragrance adsorbed to polyamide resin and silica gel, a resin binder, an organic solvent, and a rubber monomer. (Unexamined Japanese Patent Publication No. 53-52561) A method of mixing a powdered fragrance in which a fragrance is adsorbed on fine silica powder with a pigment, and printing cloth with this aromatic pigment.
53408) Furthermore, there is a method of heat-sealing an interlining to a textile material by applying a mixture of a fragrance and a textile adhesive to one side of the interlining, (JP-A-49-119000) using a printing paste mixed with a fragrance and a pigment. A method of printing on cloth and then applying a coating agent containing a mixture of perfume and resin liquid,
112283) Method for obtaining fragrant terry cloth by mixing fragrance powder into pigment resin and printing on terry cloth, (JP-A-58-87382) After immersing textile products in a processing bath containing fragrance and fragrance retaining agent. Deliquified, dried and made into 1 ta of scented fiber
There is a method for obtaining a J product (Japanese Patent Application Laid-Open No. 59-150171), and a method in which a fragrance is melt-spun into a fiber polymer (Japanese Patent Application Laid-open Nos. 48-93714 and 61-63716).

(Intelligence B that the invention seeks to solve) However, such conventional methods have various drawbacks. For example, in the method of applying fragrance microcapsules with a glue, the microcapsules are removed as the glue falls off during washing. It has the disadvantage of not being durable after washing and having a hard texture because it falls off. Furthermore, in the method of applying perfume microcapsules together with a resin binder, drying or low-temperature heating alone results in poor adhesion of the resin binder and poor washing durability. In addition, if heat fixation is performed at a high temperature after drying, the adhesion will improve, but the high temperature may cause deterioration of the fragrance, breakage of microcapsules due to vaporization of the fragrance, and the resin may become transparent, resulting in poor texture. The disadvantage is that it becomes hard.

Methods in which fragrance is adsorbed onto porous powder or resin and applied using a glue or resin binder provide sustained release, but the initial release of fragrance is low and the effect is inferior, as well as the release of fragrance during storage. However, the storage period is short, and the adsorbed fragrance tends to be detached from the resin during washing, resulting in poor washing durability.

Furthermore, the method of applying fragrance directly together with an adhesive, pigment, and resin binder has the disadvantage that the preservation of the fragrance is extremely poor and the washing durability is also poor.

In addition, although the method of melt-spinning fragrances into synthetic fiber polymers is durable, it may impair the basic physical properties of the yarn (strength, elongation, etc.), the compatibility of some fragrances may be poor, and some fragrances may have low boiling points. They cannot be used and have limited scents, and for those that undergo post-processing (dying, finishing), there are processing limitations and there are many types of scents that cannot be processed.

The purpose of the present invention is to apply various fragrances to various fiber structures with good durability, while maintaining basic physical properties such as texture and color fastness, in comparison to conventional fragrance processing methods. The objective is to establish a processing method that can be processed using various processing methods.

(Means for Solving the Problems) That is, the present invention provides at least a portion of a fiber structure with an emulsion of microcapsules containing formalin-based resin as a wall material and odorants, and a low-temperature-reactive organopolysiloxane prepolymer. After applying a treatment solution consisting of
It is characterized by drying at a temperature of less than 0° C. to fix the microcapsules to the fiber surface, and further, prior to such treatment, a tO water treatment is performed.

The microcapsules referred to in the present invention have a wall material of urea-formalin resin and a particle size of 2 to 50 μm, preferably 5 to 2 μm.
0μ Wall thickness is preferably 0.1 to 20μ C 0.5 to 4μ Or, the wall material is melamine-formalin resin and the particle size is 5μ
~50μ preferably 5-20μ, wall thickness 0.2-30μ
Preferably it is about 0.5 to 6μ.

The odorants referred to in the present invention are natural fragrances, synthetic fragrances, and liquid or powder compounds that generate fragrances, either singly or in mixtures.Natural fragrances include animal fragrances such as musk, civet,
Plant fragrances such as castoreum and ambergris include lemon oil, rose oil, citronella oil, sandalwood oil, peppermint oil, and cinnamon oil. In addition, synthetic fragrances include α-pinene, limonene, geraniol, linalool,
There are blended fragrances consisting of lavandulol, nerolidol, etc.

In the present invention, the low-temperature-reactive organopolysiloxane prepolymer emulsion refers to, for example, 100 parts by weight of an organopolysiloxane and its derivative having at least two hydroxyl groups bonded to a silicon atom in one molecule.
0.1 to 10 parts by weight of a reaction product of amine functional silane or its hydrolyzate and acid anhydride and 1 to 50 ffi of colloidal silica! 1 to 60 parts by weight of a homogeneous dispersion of ilt parts to the organopolysiloxane, 0.01 to 10 parts by weight of a curing catalyst, 0.3 to 20 parts by weight of an anionic emulsifier, and 25 to 600 parts by weight of water. Examples include aqueous emulsions of silicone comprising:

Microcapsules containing an odorant, as described above, are added to the low temperature reactive organopolysiloxane prepolymer emulsion and applied to the fibrous structure.

That is, when the application is carried out by a banding method, a spray method, or a mass removal method, the odorant is 5 to 99% by weight, preferably 50 to 99% by weight.
0.1-10% by weight of microcapsules containing 95% by weight, preferably 0.2-5.0% by weight, and 0.1% by weight of the organopolysiloxane prepolymer emulsion.
~20 heavy view% weight or 0.5~5. Apply an aqueous treatment solution containing O1i% to a pad, spray, or Tl at a pink-up rate of 10 to 200%, preferably 40 to 150% by weight.
? n. It is recommended to dehydrate.

Furthermore, when printing and coating methods are used, microcapsules containing 5 to 99% by weight of odorants, preferably 30 to 60% by weight, may be mixed with 0.05 to 20% by weight or preferably 0.
．． 1 to 5.0% by weight and preferably 1 to 99% by weight of the organopolysiloxane prepolymer emulsion.
An aqueous solution or emulsion containing ~99% by weight can be prepared as it is or with a thickener if necessary to a viscosity of 2000~20000.
It is preferable to increase the viscosity and print and coat it on cps (BM type viscometer at 20°C).

After applying the low-reactive organopolysiloxane prepolymer emulsion to the fibrous structure in this way, 15
Drying is carried out at a temperature below 0°C to make the microcapsules stick to the fiber surface. An example of drying treatment is a temperature of 60
~150℃, preferably 80~130℃ for 10 seconds ~ 30
Drying is preferably carried out for 30 seconds to IO minutes, or heat treatment is carried out after drying at a temperature of 80 to 150°C, preferably 100 to 130°C, for 10 seconds to IO minutes, preferably 30 seconds to 5 minutes.

By the above-described treatment, a durable fragrance can be imparted to the fibrous structure without impairing its texture. However, in order to suppress the 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 necessary to
It is desirable to perform a water treatment. Furthermore, as a result of the water treatment suppressing the penetration of the microcapsules and binder into the fibrous structure, hardening of the texture of the fibrous structure is suppressed, and a decrease in strength is also suppressed.

As such a water repellent, any t.

Any compound can be used as long as it can impart aqueous properties, such as wax-based natural waxes and their derivatives such as carnauba wax and candelilla wax, emulsions made of synthetic waxes such as solid esters of higher fatty acids and higher alcohols, silicone-based dimethyl Examples include emulsions of polysiloxane and its derivatives, emulsions of polyolefins such as polyethylene and polypropylene, emulsions of cationic quaternary amine compounds, emulsions of synthetic resins such as polyamides and polyacrylics alone or in copolymers, etc. It will be done.

In addition, in the tθ water treatment, for example, an aqueous solution or emulsion consisting of a to liquid agent alone or two or more of them in a concentration of 0.1 to 10% by weight, preferably 0.5 to 5.0ffl, is used at a big amplifier rate l.
After padding with O to 120% by weight, preferably 40 to 80% by weight, drying is carried out at a temperature of 80 to 190°C, preferably 120 to 170°C.

In addition, even if the above-mentioned In water agent is used in combination with a general finishing agent that does not harm the TA water properties of the pretreatment, such as a softener, a texture control agent, a dye fixing agent, a reactive resin, a condensation resin, and a catalyst, the present invention will still work. There is no particular problem with the effect.

Furthermore, even if 10% by weight or less of a pigment is used in combination during fragrance treatment, there is no particular problem with the effects of the present invention.

(Effects of the Invention) The aroma treatment method of the present invention can impart a durable aroma to a fiber structure without changing its original texture.

By selecting the microcapsules, binder, and processing temperature as in the present invention, there is less destruction of the microcapsules during the processing process, and the fiber structure can be used (when worn).
Only after that, the microcapsules are destroyed and the fragrance is fully released.

In addition, the adhesion of microcapsules to fiber structures is good, but this does not affect the texture, especially if water repellent treatment is performed prior to fragrance treatment, which will further improve the texture, hue, and texture.
The decrease in strength can be suppressed.

(Example) Next, the present invention will be explained in detail with reference to Examples, and the test method that is the basis for the numerical values in the Examples is as follows.

(1) Tear strength JIS L-1096D method (2)
Laundry JIS L-0217103 Method (3) Dry Cleaning JIS L-0217401 Method - Ning (4) Fragrance Represented as the average value of 10 testers evaluated using the following table.

5: Optimal scent 4: Slightly less 3: About half 2: Slightly present 1: Almost none 0: None (5) Discoloration K/S concentration K/S = (1-R
) 2/2R (R: maximum absorption wavelength of spectrophotometer) ○: Change in K/S concentration 3% or less Δ: 3 to 10% X: 10% or more Example 1 Scouring, bleaching, and A mercerized and printed plain cotton fabric having a warp count of 60, a thread density of 90 threads/inch, a weft thread count of 60, a thread density of 88 threads/inch, and a basis weight of 70 g/mz was obtained.

The plain woven fabric was coated with Viclon 29 (cationic fabric softener made by Ipposha Yushi Kogyo 0 Tori) 3x%, Light Silicone R-167 (
Silicone softener manufactured by Kyoeisha Yushi Kogyo), 1% by weight
After padding with an aqueous treatment solution containing 70% pink-up rate, drying was performed at 130° C. for 1 minute.

After that, Fragrance BA7985 (Takasago Fragrance Industry Co., Ltd.)
1% by weight of an aqueous dispersion containing 46% by weight of microcapsules made of urea-formalin resin with a particle size of 5 to 15μ (average 10μ) containing 91% by weight of jasmine-based synthetic fragrance (manufactured by @Jasmine) and organopolysiloxane. Prepolymer emulsion KM-20027 (manufactured by Shin-Etsu Chemical) triple loading%
After banding an aqueous treatment solution consisting of the following at a pickup rate of 70%, drying was performed at 120° C. for 2 minutes.

Table 1 shows the physical properties and fragrance durability of the obtained plain cotton fabric.

Example 2 The same cotton plain fabric as that used in Example 1 was used, and urea-formalin containing 91% by weight of fragrance BA7985 (jasmine fragrance manufactured by Takasago International Corporation NZ) with a particle size of 5 to 15μ (average lOμ) was used. The pick-up rate of an aqueous treatment liquid consisting of 1% by weight of an aqueous dispersion containing 1% by weight of 46 microcapsules with resin as a wall agent and 3% by weight of Bosocor 1-R3020 (manufactured by Dainippon Ink ■, acrylic emulsion) was 70%. After padding, it was dried at 120° C. for 2 minutes.

Table 1 shows the physical properties and fragrance durability of the obtained plain cotton fabric.

Comparative Example 1 The sample obtained in Comparative Example 1 was further heated at 150°C for 3
Fixation was performed by heating for a minute.

Table 1 shows the physical properties and fragrance durability of the obtained plain cotton fabric.

Example 3 A warp silk spun 140 count double yarn, yarn density of 114 threads/inch, a weft silk spun 6 which was scoured, bleached and printed using a commonly known method.
6th wheel thread used, thread density 89 threads/inch, weight 62 g/m
” Fujihimo plain woven fabric was obtained.

The V6 material was banded with an aqueous treatment solution containing 5% Silicoran B510 (silicon softener manufactured by Ipposha Yushi Kogyo 2) at a pink-up rate of 80%, and then dried at 130° C. for 1 minute.

After that, sandalwood oil (synthetic blended fragrance manufactured by Takasago Fragrance Industry 01) 8
Microcapsules 48 whose wall material is urea-formalin resin containing 9% by weight and having a particle size of 4 to 14 μm (average 9.5 μm)
An aqueous dispersion containing 1% by weight and an organopolysiloxane prepolymer emulsion of KM-20027 (
(manufactured by Shin-Etsu Chemical) 5% by weight and emulsion paste (printing paste prepared in the ratio of kerosene oil/water/polyethylene glycol distearate-50150/2)
A printing paste with a viscosity of 6,800 cps (BM type viscometer at 20° C.) made of 94 times a heavy prison was printed using a 120 mesh flat screen, and then dried at 130° C. for 1 minute.

Table 2 shows the physical properties and fragrance durability of the obtained Fujigumi.

Example 4 The same Fujigumi as used in Example 2 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 14μ (average 9.5μ). -48% by weight of microcapsules with formalin resin as a wall agent
1% by weight of an aqueous dispersion containing
The viscosity is 7200 cps ([
After printing with a 120-mesh flat screen using a printing paste using a 3M type viscometer (20°C), it was dried at 130°C for 1 minute.

Table 2 shows the physical properties and fragrance durability of the obtained Fujigumi.

Comparative Example 2 The sample obtained in Comparative Example 3 was further heated at 150°C for 3 days.
Fixation was performed by heating for a minute.

Table 2 shows the physical properties and fragrance durability of the Fuji silk obtained.

Example 5 Sweaters, cardigans, and skirts were knitted and sewn using a cotton/acrylic blend ratio of 50,150 and a yarn count of 36 that had been scoured, bleached, and dyed using commonly known methods.

The sweater was manufactured by Silicolan ES-10 (Ipposha Yushi Kogyo ■
Silicone softener) 1% by weight and Yodozol PE4
00 (Polyethylene emulsion manufactured by Shinebo N5cn) After being immersed in an aqueous treatment solution consisting of 2FFI 1% for 30 seconds, centrifugal dehydration to achieve a pick-up rate of 95%, and then centrifugal dehydration at 80°C for 2
Drying was performed for 0 minutes. After that, an aqueous dispersion containing 52% by weight of microcapsules containing 90% by weight of lemon-lime fragrance (manufactured by Takasago International Co., Ltd., synthetic blended fragrance) and having a particle size of 12 to 18 μm (average 15 μm) and made of melamine-formalin resin as a wall agent. The solution was immersed for 1 minute in an aqueous treatment solution consisting of 0.7% by weight and 2% by weight of organopolysiloxane prepolymer emulsion KM-2002L-1 (manufactured by Shin-Etsu Chemical U), and then centrifugally dehydrated to a pink amplifier rate of 80%. After dehydration in a machine, the mold was prepared and dried in an oven dryer at 95°C for 10 minutes.

Table 3 shows the durability of the fragrance of the obtained sweaters, cardigans, and skirts.

Table 1 Table 2

Claims (2)

[Claims] (1) After applying a treatment liquid to at least a portion of the fiber structure, the treatment liquid consists of microcapsules containing formalin-based resin as a wall material and containing odorants, and an emulsion of a low-temperature-reactive organopolysiloxane prepolymer, and then heated to a temperature of 150°C. 1. A durable fragrance treatment method, characterized in that the microcapsules are adhered to the surface of fibers by drying at a temperature of less than 100 mL. (2) A durable fragrance treatment method in which the treatment according to claim 1 is performed after water-repellent treatment is applied to a fibrous structure.