JPH026672A - Persistent perfume-imparting treatment - Google Patents

Abstract

PURPOSE:To impart fibrous structure with persistent perfume by applying, on said fibrous structure, a treating liquid comprising perfume-including microcapsules, pressure-proof buffering agent and an emulsion from each specific acrylic or methacrylic compound, etc., followed by heat treatment. CONSTITUTION:Part of a fibrous structure is treated with a treating liquid comprising (1) perfume (e.g., natural or synthetic)-including microcapsules made of formaldehyde resin, (2) a pressure-proof buffering agent (e.g., polyacrylic acid or copolymer emulsion from acrylic acid and acrylate) and (3) an emulsion from acrylic or methacrylic compound, prepared by emulsion polymerization of a monomer containing one or more vinyl groups, polyalkylene polymer emulsion or emulsion of polyester resin from polyhydric alcohol and polybasic acid, followed by drying at <150 deg.C to firmly attach said microcapsules to the surface of the fiber, thus imparting said fibrous structure with perfume highly resistant to washing.

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 odorants and a sizing agent to textile products. (Unexamined Japanese Patent Publication No. 4919197) A method of obtaining fragrant towel fabric by applying a liquid mixture of microcapsules containing a fragrance and an acrylic resin. (Unexamined Japanese Patent Publication No. 58-4
886) 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 lAl1 material wall film, a thermoplastic substance, and a thickener.

(JP-A-53-47440, JP-A-5349200) A method for obtaining an aromatic printed product that emits an aroma by heat-transferring a binder layer consisting of microcapsules of a fragrance, a pigment, a polymer resin, etc. to a transfer target. (Unexamined Japanese Patent Publication No. 53-106
885>Also, a method of applying porous powder adsorbing odorants together with a water-soluble glue. (JP 48-36483) A method of applying a mixture of a mixture of a fragrance adsorbed to a polyamide resin and silica gel, a resin binder, an organic solvent, and a rubber monomer. (JP-A-5352561) A method in which a powdered fragrance in which a fragrance is adsorbed on silica-based fine powder is mixed with a pigment, and cloth is printed with this aromatic pigment. (Unexamined Japanese Patent Publication No. 53-534
08) Furthermore, a method in which a mixture of fragrance and fiber adhesive is applied to one side of the interlining and then heat-sealed to the fibers. (Unexamined Japanese Patent Publication No. 49-119000) A method of printing on cloth with a printing paste mixed with a fragrance and a pigment, and then applying a coating agent containing a mixture of a fragrance and a resin liquid. (Unexamined Japanese Patent Publication No. 54-112
283) Mix the fragrance powder into the pigment resin and make it into towel cloth!・How to obtain fragrant towel fabric. (Unexamined Japanese Patent Publication No. 5
8-87382) A method of obtaining a numbered textile product by immersing a textile product in a processing bath containing a fragrance and a fragrance retaining agent, followed by deliquification and drying. (Japanese Unexamined Patent Publication No. 59-150171) In addition, there is a method of melt-spinning a fragrance into a fiber polymer (Japanese Unexamined Patent Publication No. 48-1989).
-93714, JP-A-61-63716), etc.

(Problems to be Solved by the Invention) However, such conventional methods have various drawbacks. For example, in the method of applying perfume microcapsules using a glue, the microcapsules fall off when the glue falls off during washing, resulting in poor washing durability and a hard texture. 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 high temperature after drying, the adhesion will improve, but the high temperature will cause deterioration of the fragrance, breakage of the microcapsules due to vaporization of the fragrance, and penetration of the resin, resulting in a hard texture. There is a drawback.

Although the method of adsorbing fragrance on porous powder or resin and applying it using glue and resin binder has sustained release properties,
In addition to the lack of initial scent release and poor effectiveness, the release of scent occurs during storage and the storage period is short, and when washed, the adsorbed fragrances tend to detach from the resin, resulting in poor washing durability. There are drawbacks.

Furthermore, the method of directly applying fragrance along 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 includes microcapsules containing formalin-based resin as a wall material and containing odorants, a pressure-resistant buffering agent, and one or more microcapsules in at least a portion of a fiber structure. Applying a treatment liquid consisting of an emulsion of an acrylic or methacrylic compound obtained by emulsion polymerization of a monomer containing a vinyl group, and then drying at a temperature of less than 150°C to fix the microcapsules to the fiber surface; After applying a treatment liquid consisting of microcapsules containing formalin-based resin and odorants, a pressure-resistant buffer, and a polyalkylene polymer emulsion to at least a portion of the fiber structure, the temperature is lower than 150°C. drying to fix the microcapsules to the fiber surface, or at least a part of the fiber structure contains microcapsules containing formalin-based resin as a wall material and containing an odorant, a pressure-resistant buffering agent, and a multilayer structure. After applying a treatment liquid consisting of a polyester resin emulsion consisting of a hydric alcohol and a polybasic acid,
The microcapsules are fixed to the fiber surface by drying at a temperature of less than °C, and further, the microcapsules containing formalin-based resin as a wall material and containing an odor substance are added to at least a portion of the fiber structure, and the microcapsules are resistant to pressure. A durable fragrance characterized by applying a treatment liquid consisting of a buffer and an emulsion of a polyurethane resin consisting of a diisocyanate and a polyol, and then drying at a temperature of less than 150°C to fix the microcapsules to the fiber surface. This is a processing method. The microcapsules referred to in the present invention refer to microcapsules whose wall material is urea-
It is a formalin resin and has a particle size of 2 to 50μ, preferably 5
~20μ wall thickness 0.1-20μ preferably 065-4μ
Alternatively, the wall material is a melamine-formalin resin, the particle size is 5 to 50μ, preferably 5 to 20μ, and the wall thickness is 0.2 to 3.
It is about 0μ, preferably 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 mixed fragrances consisting of Lahangulol, nerolidol, etc.

In the present invention, the emulsion of an acrylic or methacrylic compound obtained by emulsion polymerization of a monomer containing one or more vinyl groups includes, for example, acrylic acid, methacrylic acid, methyl acrylate, methyl methacrylate, ethyl acrylate, ethyl Methacrylate, butyl acrylate, butyl methacrylate-1, acrylonitrile, acrylamide, N=methylol acrylamide,
It is an emulsion of emulsion polymers such as 2-hydroxyethyl acrylate and 2-hydroxybutyl acrylate.

Examples of polyalkylene include polyethylene and polypropylene, and examples of polyhydric alcohols include ethylene glycol, 1,4-bucundiol, 1,6 hexanediol, diethylene glycol, and trimethylolpropane.
Examples of polybasic acids include phthalic acid, adipic acid, maleic acid, trimetic acid, and terephthalic acid.

Furthermore, examples of the diisocyanate include hexamethylene diisocyanate, xylene diisocyanate, tolylene diisocyanate, 4-4゛ diphenylmethane diisocyanate 2-1-11-5 naphthalene diisocyanate, and examples of the polyol include polyethylene adipate, polypropylene diisocyanate, and polypropylene diisocyanate.・Polybutylene adipate, polyethylene phthalate, polyethylene glycol, polypropylene glycol, polyethylene propylene glycol, etc. are mentioned, and an emulsion of a polyurethane resin made of these can be dried to form a water-insoluble resin.

In the present invention, buffering agents include emulsions containing polyorganic carboxylic acids such as polyacrylic acid or oacrylic acid and acrylate copolymers, compounds that form salts with alkaline substances such as ammonia and soda ash, and polyacrylic acid and acrylate copolymers. Neutralized products of organic polycarboxylic acids such as sodium acrylate, ammonium polyacrylate, and amino salts of polyacrylic acid, or neutralized products of copolymers of acrylic acid and acrylate, and polypropylene glycol such as polyethylene glycol and polypropylene glycol. Selected from alkylene glycol, a compound in which the terminal end of polyalkylene glycol such as polyethylene glycol, polypropylene glycol, etc. is substituted with an argyl group C, lH2,,, (=10, where n is an integer from 1 to 25), and polyvinylpyrrolidone. It is a compound that is

The microcapsules containing the odorant as described above are added to the treatment solution consisting of the emulsion and pressure buffering agent as described above and applied to the fiber structure.

That is, when the application is carried out by a padding method, a spray method, or an immersion deliquification method, the odorant is 5 to 99% by weight, preferably 50 to 99% by weight.
0.1-10% by weight of microcapsules containing 95% by weight, preferably 0.2-5.0% by weight, and 0.1-20% by weight of each of the above emulsions, preferably 0.5-5.0% by weight.
An aqueous treatment solution containing about 5% by weight of a pressure buffer and a pressure buffering agent has a pink amplifier rate of 10 to 200%, preferably 40% by weight.
It is preferable to perform water weight, spraying, or soaking/dehydration at ~150% weight.

Further, when using a printing method or a coating method, microcapsules containing 5 to 99% by weight of an odorant, preferably 50 to 95% by weight, are used in an amount of 0.1 to 10Flit%, 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 around 5% by weight of pressure buffering agent, 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 each emulsion is applied to the fiber structure in this manner, it is dried at a temperature of less than 150"C to fix the microcapsules to the fiber surface. As an example of the drying treatment, the temperature is preferably 60 to 150C. Dry at 80-130°C for 10 seconds-30 minutes, preferably 30 seconds-10 minutes, or dry at a temperature of 80-150°C, preferably 100-130°C.
C. for 10 seconds to 10 minutes, preferably 30 seconds to 5 minutes.

In addition, even if ordinary finishing agents such as softeners, texture control agents, dye fink agents, reactive resins, condensation resins, catalysts, etc. are used in combination, the effects of the present invention will not be affected by the special number 2 problem. do not have. Furthermore, even when a pigment is used in combination with 10% by weight or less during aroma 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 impairing its original feel.

That is, microcapsules, binders, pressure buffers,
By selecting the processing temperature as in the present invention, the pressure-resistant buffering agent with thickening properties exhibits associative properties and is uniformly dispersed, so that there is less destruction of microcapsules during the processing process, and when the fiber structure is used (when worn). ), the microcapsules are destroyed and the fragrance is fully 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 (2) Washing (3) Dry chestnut -ning (4) Incense JIS L-1096D method JIS L-0217103 method JIS L-0217/401 method The following test was conducted for 10 testers. Based on the average score evaluated based on the criteria show.

5: Optimum fragrance 4: Slightly less 3: About half 2: Slightly present 1: Almost none 0: None Example 1 4o count scouring, bleaching, mercerizing, and dyeing using commonly known methods. A plain cotton fabric with a thread density of 90 threads/inch, a weft count of 40, a thread density of 75 threads/inch, and a basis weight of 108 g/m2 was obtained. The plain weave was coated with 46% by weight of microcapsules containing 91% by weight of Fragrance BA7985 (Takasago Fragrance Co., Ltd. Gradient Jasmine Synthetic Fragrance T4) and having a urea-formalin resin wall agent having a particle size of 5 to 15μ (average 10μ). The aqueous dispersion containing (A) 0.2% by weight, (B
) 1.0% by weight, (C) 3.0% by weight, and 5% by weight of theacrylic emulsion binder made by Yodozol A1209 (Kanebo r, + sc side'p) and 5% by weight of polyacrylic acid sodium salt with a molecular weight of 720,000. (A) 94.8% by weight and (B) 94% by weight (C
) After printing with a printing paste consisting of 92 layers using a 120 mesh flat screen,
Dry for a minute. Table 1 shows the physical properties and fragrance durability of the obtained plain cotton fabric.

Comparative Example 1 The same cotton handwoven fabric as that used in Example 1 was used, and particle size of 5 to 15 μm containing 91% by weight of fragrance BA7985 (jasmine-based synthetic fragrance manufactured by Takasago Fragrance Industry Co., Ltd. (→)) was used.
(A) 0.2% by weight, (B) 1% by weight, and (C) 3% by weight, respectively.
．． 0% by weight and Yotozo/l, AAl209 (spun NSC
An aqueous sizing agent consisting of 5 wt.
A) 94.8% by weight, (B) 94.0% by weight, (C) 9
A printing paste consisting of 2.0% by weight was printed using a 120 mesh flat screen and then dried at 130°C for 1 minute.

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

Table 1 Example 2 Scouring, bleaching, and printing using a commonly known method. Warp silk spinning 140 @ hand double yarn, yarn density 114/inch, weft silk spinning 66 count single yarn, yarn density 89 wood. /inch, basis weight 62
A Fuji silk plain fabric of g/m2 was obtained.

The plain fabric is coated with microcapsules containing 89% by weight of sandalwood oil (synthetic fragrance manufactured by Takasago International Co., Ltd.) and containing 48 microcapsules having a urea-formalin resin as a wall agent and having a particle size of 4 to 14 μm (average 9°5 μm). 2% by weight of an aqueous dispersion, 5% by weight of Superflex E-2000 (polyurethane emulsion manufactured by Daiichi Kogyo Seiyaku 0→), and polyethylene glycol with a molecular weight of 22,000 whose terminal groups are C17H: + 5 alkyl groups. An aqueous treatment solution consisting of 8% by weight of a buffer consisting of 5% by weight of substitutes and each component was banded at a pink-up rate of 70%, dried at 120°C for 2 minutes, and then heat-treated at 130°C for 1 minute. was carried out.

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

Comparative Example 2 Using the same Fuji silk as that used in Example 2, 48 microcapsules were made with a urea-formalin resin wall agent containing 89% by weight of sandalwood oil (synthetic fragrance manufactured by Takasago International Corporation).
An aqueous treatment solution consisting of 2% by weight of an aqueous dispersion containing Jyujukei and 5% by weight of Superflex E-2000 (polyurethane emulsion manufactured by Daiichi Kogyo Seiyaku ■) was treated with a pink amplifier rate of 7.
After padding at 0%, drying was performed at 120°C for 2 minutes, and then heat treatment was performed at 130°C for 1 minute.

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

Table 2 contains an aqueous dispersion containing 46% by weight of microcapsules made of urea-formalin resin with a particle size of 5 to 15μ (average 10μ) as a wall material, respectively (A) 0.2% and (B).
) 1.0% by weight, (C) 3.0% by weight, Yodozol PE400 (Kanebo NSC Tsukuda) polyethylene emulsion binder) 5% ffi and 5% by weight of polyacrylic acid sodium salt with a molecular weight of 720,000. Aqueous buffering agent (A) 94°8% by weight, (B) 94% by weight, (C)
After printing with a 92 weight printing paste using a 120 mesh flat screen, it was dried at 130° C. for 1 minute. Physical properties of the obtained plain cotton fabric and Example 3 Scouring, bleaching, and printing were carried out by a commonly known method.
Count, thread density 90 threads/inch, weft thread count 40, thread density 75
A plain cotton fabric with a fabric weight of 108 g/m2 was obtained.

The plain woven fabric was made into Fragrance BA7985 (Takasago Fragrance Industry Co., Ltd.).
91% by weight (jasmine-based synthetic fragrance made in Song Dynasty) Table 3 Example 4 Using warp silk spinning 140 count twin yarn, scouring, bleaching, and pudding 1- by a commonly known method, yarn density 114 threads/inch, Weft silk spinning using 66 count single yarn, thread density 89 threads/inch, area weight 62
A Fuji silk plain fabric of g/m2 was obtained.

The plain woven fabric contains 89% by weight of sandalwood oil (synthetic fragrance manufactured by Takasago International Co., Ltd.) and 48% by weight of microcapsules whose wall material is a urea-formalin resin having a particle size of 4 to 14μ (average 9°5μ). 2% by weight of an aqueous dispersion, 5% by weight of Finetenx ES675 (polyester emulsion manufactured by Dainippon Ink a@), and 5% by weight of an alkyl group substituted product of polyethylene glycol with a molecular weight of N22,000 whose terminal group is C17His. An aqueous treatment solution containing 8% by weight of a buffering agent was padded at a pink-up rate of 70%, dried at 120°C for 2 minutes, and then heat-treated at 130°C for 1 minute.

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

Table 4

Claims (4)

[Claims] (1) At least a portion of the fiber structure is obtained by emulsion polymerization of microcapsules containing formalin-based resin as a wall material and containing odorants, a pressure-resistant buffering agent, and a monomer containing one or more vinyl groups. After applying a treatment solution consisting of an emulsion of an acrylic or methacrylic compound,
A durable fragrance treatment method, characterized in that the microcapsules are fixed to the fiber surface by drying at a temperature below .degree. (2) After applying a treatment solution consisting of microcapsules containing formalin-based resin and odorants as a wall material, a pressure-resistant buffering agent, and a polyalkylene polymer emulsion to at least a portion of the fiber structure, the temperature is increased to 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. (3) At least a part of the fiber structure consists of microcapsules that use formalin-based resin as a wall material and encapsulate odorants, a pressure-resistant buffer, and an emulsion of polyester resin made of polyhydric alcohol and polybasic acid. A durable fragrance treatment method, which comprises applying a treatment liquid and then drying at a temperature of less than 150° C. to fix the microcapsules to the fiber surface. (4) 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, a pressure-resistant buffer, and an emulsion of polyurethane resin made of diisocyanate and polyol. After that, the microcapsules are dried at a temperature of less than 150° C. to fix the microcapsules to the fiber surface.