JPH01292183A - Durable fragrance treatment - Google Patents

Abstract

PURPOSE:To obtain cloth having washing resistance and durable fragrance without damaging feeling, by treating a fibrous structure with a treating solution consisting of fragrant substance-containing microcapsule, organopolysiloxane prepolymer of low-temperature reaction type and pressure-resistant buffering agent. CONSTITUTION:At least part of fibrous structure is provided with a treating solution consisting of microcapsule which uses ureaformalin-based resin as a wall agent and contains a fragrant substance (e.g., natural or synthetic perfume), emulsion of an organopolysiloxane prepolymer of low-temperature reaction type and pressure-resistant buffering agent (e.g., emulsion containing polyacrylic acid, etc.) dried at <150 deg.C and the microcapsule is sealed to the surface of the cloth to give a fragrant fibrous structure having excellent washing durability and persistence without losing characteristic feeling of cloth.

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 Patent Application Laid-Open No. 19197-1987), applying a mixture of microcapsules containing a fragrance and an acrylic resin to obtain an fragrant towel fabric. Method, (JP-A-58-
4886) A method for obtaining a printed article that emits a fragrance by printing a printing 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 mixture of a fragrance adsorbed to a polyamide resin and a silica gel, a resin binder, an organic solvent, and a rubber monomer, (JP-A-53-52561) mixed with pigment,
A method of printing cloth with this aromatic pigment (Japanese Patent Application Laid-open No. 53
-53408) Furthermore, a method of heat-sealing an interlining to a fiber material by applying a mixture of a fragrance and a textile adhesive to one side of the interlining, (JP-A-49-119000) 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 fragrance and resin liquid (Japanese Patent Laid-Open No. 54
-112283) A method for obtaining fragrant toweling by mixing fragrance powder into pigment resin and printing on toweling (Japanese Patent Application Laid-open No. 58-87382) A textile product is immersed in a processing bath containing a fragrance and a fragrance retention agent. Method for obtaining numbered textile products by post-deliquification and drying (Japanese Unexamined Patent Publication No. 59-150171), etc.
There is a method in which a fragrance is melt-spun into a fiber polymer (JP-A-48-93714, JP-A-61-63716).

(Problem H to be Solved by the Invention) However, such conventional methods have various drawbacks. g4
For example, in the method of applying fragrance microcapsules with a glue, the microcapsules fall off when the glue falls off during washing, so the washing durability is poor (it also has a hard texture). In the method of applying it together with a resin binder, if only drying or low-temperature heating is used, the adhesiveness of the resin binder is poor and washing durability is poor.Furthermore, if heat fixation is performed at a high temperature after drying, the adhesiveness will improve, but
Disadvantages include deterioration of fragrance due to high temperatures, destruction of microcapsules due to vaporization of fragrance, and penetration of resin, resulting in a hard texture.

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, and to apply various fragrances to various fiber structures without impairing 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 the following processing methods.

(Means for Solving the Problems) That is, the present invention provides at least a portion of a fiber structure with microcapsules containing formalin-based resin as a wall material and odorants, and an emulsion of a low-temperature-reactive organopolysiloxane prepolymer. After applying a treatment liquid consisting of a pressure buffer and a pressure-resistant buffer, the microcapsules are dried at a temperature of less than 150° C. to fix the microcapsules to the fiber surface.

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 0.1-20μ Preferably 0.5-4μ 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, cibesoto,
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 mixed fragrances consisting of lavangerol, nerolidol, etc.

In the present invention, the low-temperature reaction type organopolysiloxane prepolymer emulsion is, for example, an organopolysiloxane having at least two silicon-bonded hydroxyl groups in one molecule and 100 parts by weight of its derivatives, and an aminofunxyternarsilane. Or a homogeneous dispersion of 0.1 to 10 parts by weight of a reaction product of a hydrolyzate thereof and an acid anhydride, 1 to 50 parts by weight of colloidal silica, and 1 to 60 parts by weight of organopolysiloxane, and a curing catalyst. 0.01 to 10 parts by weight and 0.43 parts by weight of anionic emulsifier
-20 parts by weight and 25-600 parts by weight of water.

The buffering agents used in the present invention 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, and polyacrylic acid. Neutralized products of organic polycarboxylic acids such as soda salts, polyacrylic acid ammonium salts, and polyacrylic acid amino salts, or neutralized products of copolymers of acrylic acid and acrylates, and polyalkylene glycols such as polyethylene glycol and polypropylene glycol. Or, the terminal of polyalkylene glycol such as polyethylene glycol, polypropylene glycol, etc. is alkyl group C, H□, l [in the formula, n is an integer of 1 to 25]
The compound is selected from compounds substituted with polyvinylpyrrolidone and polyvinylpyrrolidone.

As described above, the microcapsules containing the odorant are added to the treatment liquid consisting of the low-temperature-reactive organopolysiloxane prepolymer emulsion and the pressure-resistant buffering agent, and applied to the fiber structure.

That is, when the application is carried out by a puffing method, a spray method, or an immersion deliquification method, the odorant is 5 to 99% by weight, preferably 50 to 99% by weight.
0.1 to 1011 microcapsules containing 95% by weight
% preferably from 0.2 to 5.0% by weight and the organopolysiloxane prepolymer emulsion from 0.1 to 2% by weight.
0% by weight, preferably 0.5-5.0% by weight and pressure resistance m
It is preferable to use a pad, spray, or immerse/dehydrate an aqueous treatment solution consisting of about 5% by weight at a pick-up rate of 10 to 200%, preferably 40 to 150% by weight.

Furthermore, when printing and coating methods are used, microcapsules containing 5 to 99% by weight of odorants, preferably 50 to 95% by weight, can be used in an amount of 0.1 to 10% by weight, preferably 0.5% by weight.
2 to 5.0% by weight and 1 to 95% by weight of the organopolysiloxane prepolymer emulsion, preferably 5 to 95% by weight.
When printing an aqueous solution or emulsion containing 95% by weight and around 5% by weight of a pressure buffer, the viscosity is 2000~8.
000 cps (BM type viscometer at 20°C), and in the case of coating, it is preferable to adjust the viscosity to 8,000 to 16,000 cps.

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 fix the microcapsules to the fiber surface. An example of a drying process is a temperature of 60
-150°C, preferably 80-130°C for 10 seconds to 30
Drying is preferably carried out for 30 seconds to 10 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 10 minutes, preferably 30 seconds to 5 minutes.

Note that there is no particular problem with the effects of the present invention even if ordinary finishing agents such as softeners, texture control agents, dye fixing agents, reactive resins, condensation resins, catalysts, etc. are used in combination. Furthermore, even if 10% by weight or less of pigment is used in fragrance treatment,
There are no particular problems 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 impairing its original feel.

That is, microcapsules, binders, pressure buffers,
By selecting the processing temperature as in the present invention, pressure resistance with thickening properties can be achieved! 1 Since the street agent exhibits associative properties and is uniformly dispersed, there is little destruction of microcapsules during the processing process, and the microcapsules are destroyed only when the fiber structure is used (worn), and the fragrance is sufficiently released. .

Furthermore, the adhesion of the microcapsules to the fibrous structure is good, but this does not impair the texture.

(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) Washing JIS L-0217103 method (3) Dry IJ JIS L-021? 401
Method (4) Fragrance Represented as the average value of 10 testers evaluated based on the criteria shown below.

5: Optimal scent 4: Slightly less 3: About half 2: Slightly present! : Almost none, 0: None Example 1 Scoured, bleached, mercerized, and dyed by a commonly known method, warp 60, yarn density 90/inch, weft 60, yarn density 88/inch. A fine woven fabric with a basis weight of 70 g/m'' was obtained.The plain weave was coated with urea-formalin containing 92% by weight of Fragrance 5H3037 (vendor-based synthetic fragrance manufactured by Takasago International Corporation) and having a particle size of 5 to 15 μm (average lOμ). (A) 0.2% by weight and (B) 1.0% by weight of an aqueous dispersion containing 47% by weight of microcapsules with resin as a wall material, respectively.
% by weight, (C) 3.0% by weight, and organopolysiloxane prepolymer emulsion KM2002L-1 (
(A) 94.8% by weight, (B) 94% by weight, and (C) 92% by weight, respectively.
After printing with a 120 mesh flat screen using the printing paste consisting of % by weight, drying was performed at 130° C. for 1 minute.

The physical properties and fragrance durability of the obtained fine fabrics are shown in Table 1, and the shapes of the fibers of each fine fabric to which the microcapsules were attached are shown in FIGS. 1(A), (B), and (C).

Comparative Example 1 The same fine fabric as that used in Example 1 was used, and the particle size was 5 to 15μ (average lOμ) containing 92% by weight of fragrance 5H3037 (vendor synthetic fragrance manufactured by Takasago International Corporation). 1! An aqueous dispersion containing 47% by weight of microcapsules with urea-formalin resin as a wall agent! amount%
and 5% by weight of binder LE-25 (acrylic binder manufactured by Hayashi Kagaku Kogyo ■) and fine gum HE (Daiichi Kogyo ■)
A printing paste with a viscosity of 5,800 Cpa (BM type viscometer 20 @ C) consisting of 94% by weight of an aqueous paste consisting of 5% by weight (manufactured by Carboxymethyl Cellulose) was printed using a '120 mesh flat screen, and then heated at 130℃ for 1 minute. It was dried.

Table 1 shows the physical properties and fragrance durability of the obtained fine woven fabric, and FIG. 2 shows the shape of the fibers of the fine woven fabric after processing.

Example 2 Scoured, bleached, and printed using a commonly known method, using warp silk spun 140-count twin yarn, thread density 1.14 threads/inch, using weft silk-spun 66-count wheel thread, thread density 89 threads/inch. , weight 62
g/m" Fuji silk plain fabric was obtained.

The plain fabric is made of a particle size of 8 to 18 μm (average 12 μm) containing 88% by weight of musk type fragrance (synthetic fragrance manufactured by Takasago International Corporation).
1.5% by weight of an aqueous dispersion containing 52% by weight of microcapsules made of melamine/formalin resin as a wall material.
, and 3% by weight of emulsion of organopolysiloxane prepolymer KM-20027 (manufactured by Shin-Etsu Chemical ■), and 5% by weight of alkyl group substituted with terminal groups of polyethylene glycol having a molecular weight of 22,000 (ctv) Is%. An aqueous treatment solution containing 10% by weight of a buffering agent and each component was dried at 120° C. for 2 minutes after budding at a pink-up rate of 80%.

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

Comparative Example 2 The same Fuji silk as that used in Example 2 was used, and 88% by weight of musk type fragrance (synthetic fragrance manufactured by Takasago International Co., Ltd.)
5 microcapsules containing melamine/formalin resin with a particle size of 8 to 18 μm (average 12 μm) as a wall material.
2% by weight of an aqueous dispersion containing 1.5% by weight and Bonco)
R-136 (acrylic binder manufactured by Dainippon Ink) 3
The aqueous treatment solution consisting of % by weight was applied to a pad at a pickup rate of 80%, and then dried at 120° C. for 2 minutes.

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

Comparative Example 3 The sample obtained in Comparative Example 2 was further heated at 150°C for 3
Heat treatment was performed for minutes.

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

Example 3 The yarn was scoured, bleached, mercerized, heat-scented, and dyed by a commonly known method, with a warp of 60 and a thread density of 96 threads/inch.
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.

The plain woven fabric was subjected to the same treatment as in Example 1.

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

Table 1 Table 2 Table 3

[Brief explanation of the drawing]

Figures 1 and 2 are photographs showing the shape of the fibers of the fine fabric to which microcapsules are attached. (Magnification: 500x)

Claims (1)

[Claims] (1) At least a portion of the fiber structure is provided with a treatment liquid consisting of microcapsules containing formalin-based resin as a wall material and containing odorants, an emulsion of a low-temperature-reactive organopolysiloxane prepolymer, and a pressure-resistant buffer. After, 1
A durable fragrance treatment method, characterized in that the microcapsules are fixed to the fiber surface by drying at a temperature of less than 50°C.