JP2012067147A - Endothermic material and production method for endothermic material - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an easily obtainable material excellent in endothermic property, because, in conventional endothermic materials, endothermic fibers are produced as kneaded/adhered fiber threads produced by adding, kneading and adhering an infrared absorber in the stage of spinning, so, it is required to produce and stock a large amount of kneaded/adhered fiber threads so as to be able to correspond to orders received and thus such method is unsuitable for a small lot production of the endothermic fiber, and to provide a production method for the endothermic materials.SOLUTION: There is provided an endothermic material provided by dyeing treatment with C. I. Acid Green 1 of an iron-containing dye or C. I. Pigment Green 8 of an iron-containing pigment at a treating concentration of ≥0.5% o.w.f.

Description

  The present invention relates to an endothermic material capable of absorbing natural light and a method for producing the same.

  Conventionally, various so-called endothermic materials have been proposed, such as those in which conductive ceramic fine particles are contained in the core of a fiber in order to obtain heat retention effects and shortening drying time by imparting heat absorption properties to textile products. (For example, refer to Patent Document 1).

  However, in the one described in Patent Document 1, since the infrared absorbent is kneaded and adhered at the spinning stage and manufactured using the kneaded / attached fiber yarn, a large amount of kneaded / attached fiber yarn is produced. Therefore, there is a problem that it is not suitable for small-lot production.

  Further, by improving the infrared absorption ability by performing a dyeing process on the fiber, a fiber provided with a function to effectively prevent the radiography by an infrared camera or the like and a method for dyeing the fiber have also been proposed ( For example, see Patent Document 2).

  However, the high infrared absorption ability that can be required for preventing the radiographic imaging as required in Patent Document 2 is somewhat related to the endothermic property, but the endothermic property from natural light depends on the specific redness. In addition to the ability to absorb external light, it is also possible to absorb light of other wavelengths. In other words, in order to effectively obtain endothermic properties, it is desirable to absorb light of a wide wavelength region as long as the purpose is not impaired, rather than light of a specific wavelength. For this reason, it is not always possible to say that the high infrared absorption capability disclosed in Patent Document 2 directly leads to high heat absorption.

JP 2000-96346 A Japanese Patent Application No. 2009-299249

  The present invention is based on the above-mentioned background and focuses on obtaining reliable endothermic properties, and can provide a material having excellent endothermic properties that can be easily obtained and a method for producing the material. The intended purpose.

  In order to achieve such an object, the present invention takes the following measures.

  That is, the endothermic material and the method for producing the endothermic material according to the present invention are characterized by being dyed at a treatment concentration of 0.5% owf or more with a colorant in which iron is coordinated in the molecule. To do.

  Here, the “endothermic material” is a concept including various materials in addition to fibers and films.

  In addition, the “colorant in which iron is coordinated in the molecule” is not limited to dyes and pigments as long as it can color the above materials, and is a concept including a wide variety of compounds. .

  In addition, the endothermic material and the method for producing the endothermic material according to the present invention are dyed at a treatment concentration of 1.5% o.w.f or more with a colorant in which iron is coordinated in the molecule.

  In the endothermic material according to the present invention, the colorant in which iron is coordinated in the molecule is an iron-containing dye.

  In the present invention, the iron metal-containing dye is C.I. Acid Green 1.

  On the other hand, in the endothermic material according to the present invention, the colorant in which iron is coordinated in the molecule is an iron-containing pigment.

  In the present invention, the iron-containing pigment is C.I. Pigment Green 8.

The endothermic material according to the present invention has a coordinate L ^* value of 50 or more in L ^* a ^* b ^* color difference notation.

  Furthermore, the endothermic material according to the present invention is obtained by dyeing a fiber material.

  ADVANTAGE OF THE INVENTION According to this invention, it becomes possible to provide the manufacturing method of the material excellent in the endothermic material which can be obtained easily, and the said endothermic material.

The figure which shows the result of the experiment 1 which concerns on the Example of this invention as a table | surface and a graph. The figure which shows the result of the said experiment 2 as a table | surface and a graph. The figure which shows the result of the experiment 3 as a table | surface and a graph. The figure which shows the result of the experiment 4 as a table | surface and a graph. The figure which shows the result of the experiment 5 as a table | surface and a graph. The figure which shows the result of the experiment 6 as a table | surface and a graph. The figure which shows the result of the experiment 7 as a table | surface and a graph. The figure which shows the result of the experiment 8 as a table | surface and a graph. The figure which shows the result of the experiment 9 as a table | surface and a graph. The figure which shows the result of the experiment 10 as a table | surface and a graph. The figure which shows the result of the experiment 11 as a table | surface and a graph. The figure which shows the result of the experiment 12 as a table | surface and a graph. The figure which shows the result of the experiment 13 as a table | surface and a graph. The figure which shows the result of the experiment 14 as a table | surface and a graph. The figure which shows the result of the experiment 15 as a table | surface and a graph. The figure which shows the result of the experiment 16 as a table | surface and a graph. The figure which shows the result of the experiment 17 as a table | surface and a graph. The figure which shows the result of the experiment 18 as a table | surface and a graph. The figure which shows the result of the experiment 19 as a table | surface and a graph. The figure which shows the result of the experiment 20 as a table | surface and a graph. The figure which shows the result of the experiment 21 as a table | surface and a graph. The figure which shows the result of the experiment 22-1 as a table | surface and a graph. The figure which shows the result of the experiment 22-2 as a table | surface and a graph. The figure which shows the result of the same experiment 23-1 as a table | surface and a graph. The figure which shows the result of the same experiment 23-2 as a table | surface and a graph.

  Hereinafter, an embodiment of the present invention will be described.

  In order to achieve such an object, the present invention takes the following measures.

  That is, the endothermic material and the method for producing the endothermic material according to the present embodiment are characterized by being dyed with a colorant having iron coordinated in the molecule at a treatment concentration of 0.5% owf or more. It is what.

  It is the first time that the inventors of the present application have such an endothermic effect, in other words, a heat retention effect, in other words, a heat retention effect, and an effect of shortening the drying time after wetting the material. The present invention has been achieved by discovery.

  And if this is the case, the temperature difference from the control product is 2.0 ° C or more 10 minutes after irradiation in the functional material evaluation test method “Light Absorption Insulation / Temperature Test” by the Japan Spinning Inspection Association. The endothermic effect until 1 ° C. or higher is observed 1 minute after the light is turned off can be obtained easily and reliably.

  Further, in order to obtain a higher endothermic effect, the endothermic material and the method for producing the endothermic material are dyed at a treatment concentration of 1.5% owf or more with a colorant in which iron is coordinated in the molecule. It is desirable. When the treatment concentration is increased to around 2.00% o.w.f., a higher endothermic effect can be obtained.

In the case of a colored hue obtained at a processing density of about 0.50 to 1.00% owf, the coordinate L * value in L ^* a ^* b ^* color difference notation (CIELAB) can be increased, and further dyeing can be performed. Various colors can be developed by processing.

  The endothermic material according to the present invention is characterized in that the colorant in which iron is coordinated in the molecule is an iron-containing dye. Specifically, the iron metal-containing dye is desirably C.I. Acid Green 1.

  On the other hand, in the endothermic material according to the present invention, the colorant in which iron is coordinated in the molecule is preferably an iron metal-containing pigment.

  In the present invention, the iron-containing pigment is preferably C.I. Pigment Green 8.

The endothermic material according to the present invention is characterized in that the coordinate L ^* value in L ^* a ^* b ^* color difference notation is 50 or more. If this is the case, various color developments are possible by performing dyeing. In order to make it possible to develop a wide variety of colors, it is possible to add an acid dye, more specifically, a chrome-containing dye or a non-metal-containing acid dye, and dye it with an iron-containing dye. Since the hue of the visible portion can be adjusted by the combination with the dye, the color range is widened in dyeing, and green, blue, beige and red colors can also be dyed.

  The chromium-containing dye is CIAcid Yellow 17, CIAcid Yellow 116, CIAcid Yellow127, CIAcid Yellow 129, CIAcid Yellow 155, CIAcid Yellow 220, CIAcid Yellow 232, CIAcid Yellow 235, CIAcid Orange 86, CIAcid Orange 87, CIAcidOrange 88, CIAcid Orange 140, CIAcid Orange 162, CIAcid Orange 166, CIAcid Red 211, CIAcid Red 215, CIAcid Red 251, CIAcid Red 256, CIAcid Red 315, CI Acid Red 399, CIAcid Red 407, CIAcid Violet 75, CIAcid Blue 127: 1, CIAcid Blue 171, CIAcid Blue 193, CIAcid Blue 229, CIAcid Blue 317, CIAcid Blue 335, CIAcid Brown 19 , CIAcid Brown 28, CIAcid Brown 45, CIAcid Brown 224, CIAcid Brown 283, CIAcid Brown 298, CIAcid Brown 413, IsolanYellow NHF-S (trade name: manufactured by Dystar Japan Co., Ltd.), Isolan Red NHF -S (product name: manufactured by Dystar Japan Co., Ltd.) and Isolan Blue NHF-S (product name: manufactured by Dystar Japan Co., Ltd.) It preferred to use a dye selected one even without.

  The non-metal-containing acid dyes are CIAcid Yellow 79, CIAcid Orange 67, CIAcid Orange 95, CIAcid Red 52, CIAcid Red 111, CIAcid Red 138, CIAcid Violet 48, CIAcid Violet 97, CIAcid Blue 18, CIAcid Blue 205, CIAcid Blue 221, Kayanol Brilliant Flavine FL CONC (trade name: Nippon Kayaku Co., Ltd.), Kayanol Milling Yellow 5GW (trade name: Nippon Kayaku Co., Ltd.), Inolar Milling Red MNW It is preferable to use at least one dye selected from (trade name: manufactured by Inoue Chemical Co., Ltd.) and Lanaset Blue 2R (trade name: manufactured by Huntsman Japan Co., Ltd.).

  Furthermore, the endothermic material according to the present invention is preferably a material obtained by dyeing a fiber material. If this is the case, the endothermic property can be imparted only by dyeing the fiber material, so if the dyeing process is performed simultaneously with the dyeing to obtain the desired color for the required amount of the fiber material, the required amount The endothermic material can be easily obtained. As a result, it is possible to manufacture an endothermic material from a small lot while avoiding preparing a large amount of endothermic fibers in advance.

  Specifically, as a fiber material, in addition to nylon 6, nylon 66, and wool surge, polyester, silk, cotton, hemp, fiber materials blended with them, and other existing fiber materials are also effective. Can be applied to.

  In addition, the specific configuration of each part is not limited to the above embodiment, and various modifications can be made without departing from the spirit of the present invention.

  Examples of the present invention will be described in detail below, but the present invention is not limited to the examples.

  The treated fabric that has been dyed with the iron-containing dye CIAcid Green 1 or the iron-containing pigment CIPigment Green 8 has excellent heat retention and drying time reduction effects when exposed to natural light such as sunlight. Has been discovered by the present inventors.

  In this embodiment, the endothermic effect is proved by the functional material evaluation test method “light absorption heat retention / temperature measurement test” by the Japan Spinning Inspection Association.

<1. Creation of Examples and Comparative Examples>
Each Example and Comparative Example provided in Experiments 1 to 23-2 according to the present example shown in Tables 1 to 3 were prepared as follows.

<Experiment 1>
Preparation of Example 1: Trade name CIAcid Green 1 (Yamada Chemical Co., Ltd.) 0.50% owf, ammonium acetate 2.00% owf, refining detergent Emar 40 (Kao product) 1.00% owf, tap water added, Nylon 6 jersey cloth (color dyed product) was added as a treated product to prepare a treatment solution having a bath ratio of 1:60. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. After maintaining 10 minutes, 90% acetic acid was added by 0.25% owf after 10 minutes, and 90% acetic acid was added by 0.25% owf after 10 minutes, and exhaustion was promoted. The object to be processed thus obtained was named Example 1 according to this example.

  Preparation of Comparative Example 1: Telon Yellow RLN micro (CIAcid Yellow 230 / Dystar) 0.15% owf and Alizarine Direct Blue A2G conc. (CIAcid Blue 40 / Yamada Chemical Industries) 0.10% owf (Total 0.25% owf), ammonium acetate 2.00% owf, refined detergent Emar 40 (Kao product) to 1.00% owf, tap water added, and nylon 6 jersey cloth (color dyed product) as a treatment object. Thus, a treatment liquid having a bath ratio of 1:60 was prepared. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. 90% acetic acid was added at 0.25% o.w.f after 10 minutes while maintaining 100 ° C, and 90% acetic acid was added at 0.25% o.w.f after another 10 minutes to encourage exhaustion. As shown in Table 1, the object to be processed thus obtained has the same color as that of Example 1. Therefore, in the present Example, the said to-be-processed object was made into the comparative example 1 which is a normal processed cloth of a comparative sample.

<Experiment 2>
Preparation of Example 2: CIAcid Green 1 (Yamada Chemical Industries Co., Ltd.) was added to 1.00% owf, 90% acetic acid 1.00% owf, refined cleaning agent Emar 40 (Kao product) to 1.00% owf, tap water was added, and the material to be treated Nylon 6 jersey cloth (color dyed product) was added to prepare a treatment solution having a bath ratio of 1:60. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. After maintaining 10 minutes, 90% acetic acid was added by 0.25% owf after 10 minutes, and 90% acetic acid was added by 0.25% owf after 10 minutes, and exhaustion was promoted. The object to be processed thus obtained was named Example 2 according to this example.

  Preparation of Comparative Example 2: Telon Yellow RLN micro (CIAcid Yellow 230 / Dystar) 0.29% owf and Alizarine Direct Blue A2G conc. (CIAcid Blue 40 / Yamada Chemical) 0.21% owf (Total 0.50% owf), ammonium acetate 2.00% owf, scouring detergent Emar 40 (Kao product) 1.00% owf, tap water added, nylon 6 jersey cloth (color dyed product) as a treatment object Thus, a treatment liquid having a bath ratio of 1:60 was prepared. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. 90% acetic acid was added at 0.25% o.w.f after 10 minutes while maintaining 100 ° C, and 90% acetic acid was added at 0.25% o.w.f after another 10 minutes to encourage exhaustion. As shown in Table 1, the object to be processed thus obtained has the same color as in Example 2. Therefore, in the present Example, the said to-be-processed object was made into the comparative example 2 which is a normal processed cloth of a comparative control sample.

<Experiment 3>
Preparation of Example 3: CIAcid Green 1 (Yamada Chemical Industries Co., Ltd.) was added to 2.00% owf, 90% acetic acid 1.00% owf, tap water was added, and nylon 6 jersey cloth (color dye company product) was added as the object to be treated. A treatment liquid having a bath ratio of 1:60 was prepared. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. 90% acetic acid was added at 0.50% owf after 10 minutes while maintaining the temperature at 100 ° C., and 90% acetic acid was added at 0.50% owf after 10 minutes, and exhaustion was promoted. The object to be processed thus obtained was defined as Example 3 according to this example.

  Preparation of Comparative Example 3: Telon Yellow RLN micro (CIAcid Yellow 230 / Dystar) 0.58% owf and Alizarine Direct Blue A2G conc. (CIAcid Blue 40 / Yamada Chemical Industries) 0.42% owf (Total 1.00% owf), 90% acetic acid 1.00% owf, refined cleaning agent Emar 40 (Kao product) to 1.00% owf, tap water, and a nylon 6 jersey cloth (color dyed product) as the treatment object Thus, a treatment liquid having a bath ratio of 1:60 was prepared. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. 90% acetic acid was added at 0.25% o.w.f after 10 minutes while maintaining 100 ° C, and 90% acetic acid was added at 0.25% o.w.f after another 10 minutes to encourage exhaustion. As shown in Table 1, the object to be processed thus obtained has the same color as that of Example 3 above. Therefore, in the present Example, the said to-be-processed object was made into the comparative example 3 which is a normal processed cloth of a comparative control sample.

<Experiment 4>
Preparation of Example 4: CIAcid Green 1 (Yamada Chemical Industries Co., Ltd.) was added to 4.00% owf, 90% acetic acid 1.50% owf, tap water was added, and nylon 6 jersey cloth (color dye company product) was added as the object to be treated. A treatment liquid having a bath ratio of 1:60 was prepared. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. 90% acetic acid was added at 0.50% owf after 10 minutes while maintaining the temperature at 100 ° C., and 90% acetic acid was added at 0.50% owf after 10 minutes, and exhaustion was promoted. The object to be processed thus obtained was named Example 4 according to this example.

  Preparation of Comparative Example 4: Telon Yellow RLN micro (CIAcid Yellow 230 / Dyster product) carried out in Process 2 of Experiment 3 was 0.58% owf and Alizarine Direct Blue A2G conc. (CIAcid Blue 40 / Yamada Chemical Industries) ) With 0.42% owf (total 1.00% owf) gives the same color as in Example 4 above. Therefore, in the present Example, the said to-be-processed object was set as the comparative example 4 which is a normal process cloth of a comparative control sample.

<Experiment 5>
Preparation of Example 5: CIAcid Green 1 (Yamada Chemical Industries Co., Ltd.) was added to 6.00% owf, 90% acetic acid 2.00% owf, tap water was added, and nylon 6 jersey cloth (color dye company product) was added as the object to be treated. A treatment liquid having a bath ratio of 1:60 was prepared. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. 90% acetic acid was added at 0.50% owf after 10 minutes while maintaining the temperature at 100 ° C., and 90% acetic acid was added at 0.50% owf after 10 minutes, and exhaustion was promoted. The object to be processed thus obtained was named Example 5 according to this example.

  Preparation of Comparative Example 5: Telon Yellow RLN micro (CIAcid Yellow 230 / Dyster product) carried out in Process 2 of Experiment 3 was 0.58% owf and Alizarine Direct Blue A2G conc. (CIAcid Blue 40 / Yamada Chemical Industries) ) With 0.42% owf (total 1.00% owf) gives the same color as in Example 5 above. Therefore, in the present Example, the said to-be-processed object was set as the comparative example 5 which is a normal process cloth of a comparative control sample.

<Experiment 6>
The object to be treated was nylon 66 jersey cloth (color dyed product), and dyeing treatment was performed in the same manner as in Experiment 1 to prepare Example 6 and Comparative Example 6.

<Experiment 7>
The object to be treated was nylon 66 jersey cloth (color dyed product), and dyeing treatment was performed in the same manner as in Experiment 2 to prepare Example 7 and Comparative Example 7.

<Experiment 8>
The object to be treated was nylon 66 jersey cloth (color dyed product), and dyeing treatment was performed in the same manner as in Experiment 3 to prepare Example 8 and Comparative Example 8.

<Experiment 9>
Preparation of Example 9: CIAcid Green 1 (Yamada Chemical Co., Ltd.) 0.50% owf, ammonium acetate 2.00% owf, refining detergent Emar 40 (Kao product) 1.00% owf, tap water is added, and the material to be treated A wool surge cloth (color dyed product) was added as a treatment solution with a bath ratio of 1:60. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. After maintaining 10 minutes, 90% acetic acid was added by 0.25% owf after 10 minutes, and 90% acetic acid was added by 0.25% owf after 10 minutes, and exhaustion was promoted. The object to be processed thus obtained was named Example 9 according to this example.

  Preparation of Comparative Example 9: Acid Light Yellow 2G 90% (CI Acid Yellow 17 / Yamada Chemical Industries) is 0.30% owf and Alizarine Direct Blue A2G conc. (CI Acid Blue 40 / Yamada Chemical Industries) is 0.125% owf (Total 0.425% owf), 2.00% owf ammonium acetate, 1.00% owf refined detergent Emar 40 (Kao), tap water, and nylon 6 jersey cloth (color dyed company) To prepare a treatment solution having a bath ratio of 1:60. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. 90% acetic acid was added at 0.25% o.w.f after 10 minutes while maintaining 100 ° C, and 90% acetic acid was added at 0.25% o.w.f after another 10 minutes to encourage exhaustion. As shown in Table 1, the object to be processed thus obtained has the same color as in Example 9. Therefore, in the present Example, the said to-be-processed object was set as the comparative example 9 which is a normal processed cloth of a comparative sample.

<Experiment 10>
Preparation of Example 10: CIAcid Green 1 (Yamada Chemical Industries Co., Ltd.) was added to 1.00% owf, 90% acetic acid 1.00% owf, refined cleaning agent Emar 40 (Kao product) to 1.00% owf, tap water was added, and the material to be treated A wool surge cloth (color dyed product) was added as a treatment solution with a bath ratio of 1:60. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. After maintaining 10 minutes, 90% acetic acid was added by 0.25% owf after 10 minutes, and 90% acetic acid was added by 0.25% owf after 10 minutes, and exhaustion was promoted. The object to be processed thus obtained was named Example 10 according to this example.

  Preparation of Comparative Example 10: Acid Light Yellow 2G 90% (CI Acid Yellow 17 / Yamada Chemical Industries) is 0.60% owf and Alizarine Direct Blue A2G conc. (CIAcid Blue 40 / Yamada Chemical Industries) is 0.25% owf (Total 0.85% owf), tap water is added to 90% acetic acid 1.00% owf, and wool surge cloth (color dyed product) is added as an object to be treated. Created. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. 90% acetic acid was added at 0.25% o.w.f after 10 minutes while maintaining 100 ° C, and 90% acetic acid was added at 0.25% o.w.f after another 10 minutes to encourage exhaustion. As shown in Table 1, the object to be processed thus obtained has the same color as in Example 10. Therefore, in the present Example, the said to-be-processed object was set to the comparative example 10 which is a normal processed cloth of a comparative sample.

<Experiment 11>
Preparation of Example 11: CIAcid Green 1 (Yamada Chemical Co., Ltd.) is added to 2.00% owf, 90% acetic acid 1.50% owf, tap water is added, and wool surge cloth (color dye company product) is added as an object to be treated. A treatment solution having a bath ratio of 1:60 was prepared. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. After maintaining 10 minutes, 90% acetic acid was added by 0.25% owf after 10 minutes, and 90% acetic acid was added by 0.25% owf after 10 minutes, and exhaustion was promoted. The object to be processed thus obtained was named Example 11 according to this example.

  Preparation of Comparative Example 11: Acid Light Yellow 2G 90% (CI Acid Yellow 17 / Yamada Chemical Industries) is 1.20% owf and Alizarine Direct Blue A2G conc. (CI Acid Blue 40 / Yamada Chemical Industries) is 0.50% owf (Total 1.70% owf), 90% acetic acid 1.50% owf, tap water, wool wool cloth (color dyed product) as the treatment object, bath solution 1:60 treatment liquid Created. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. 90% acetic acid was added at 0.25% o.w.f after 10 minutes while maintaining 100 ° C, and 90% acetic acid was added at 0.25% o.w.f after another 10 minutes to encourage exhaustion. As shown in Table 1, the object to be processed thus obtained has the same color as that of Example 11. Therefore, in the present Example, the said to-be-processed object was set as the comparative example 11 which is a normal processed cloth of a comparative sample.

<Experiment 12>
Preparation of Example 12: CIAcid Green 1 (Yamada Chemical Industries Co., Ltd.) is added to 4.00% owf, 90% acetic acid 2.00% owf, tap water is added, and wool surge cloth (color dye company product) is added as an object to be treated. A treatment solution having a bath ratio of 1:60 was prepared. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. 90% acetic acid was added at 0.50% owf after 10 minutes while maintaining 100 ° C., and further 90% acetic acid was added at 0.50% owf after 10 minutes to encourage exhaustion. The object to be processed thus obtained was named Example 12 according to this example.

  <Creation of Comparative Example 12> Acid Light Yellow 2G 90% (CI Acid Yellow 17 / Yamada Chemical Industries) is 1.80% owf and Alizarine Direct Blue A2G conc. (CI Acid Blue 40 / Yamada Chemical Industries) is 0.75% Formulated with owf (Total 2.55% owf), 90% acetic acid 2.00% owf, tap water, Woolsurge cloth (color dyed product) as a treatment object, and a treatment solution with a bath ratio of 1:60 It was created. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. 90% acetic acid was added at 0.50% o.w.f after 10 minutes while maintaining the temperature at 100 ° C., and 90% acetic acid was added at 0.50% o.w.f. after another 10 minutes to promote exhaustion. As shown in Table 1, the object to be processed thus obtained has the same color as in Example 12 above. Therefore, in the present Example, the said to-be-processed object was set as the comparative example 12 which is a normal processed cloth of a comparative control sample.

<Experiment 13>
Preparation of Example 13: CIAcid Green 1 (Yamada Chemical Co., Ltd.) is added to 5.00% owf, 90% acetic acid 2.00% owf, tap water is added, and wool surge cloth (color dye company product) is added as an object to be treated. A treatment solution having a bath ratio of 1:60 was prepared. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. 90% acetic acid was added at 0.50% owf after 10 minutes while maintaining the temperature at 100 ° C., and 90% acetic acid was added at 0.50% owf after 10 minutes, and exhaustion was promoted. The object to be processed thus obtained was named Example 12 according to this example.

  Preparation of Comparative Example 13: Acid Light Yellow 2G 90% (CI Acid Yellow 17 / Yamada Chemical Industries) is 2.40% owf and Alizarine Direct Blue A2G conc. (CI Acid Blue 40 / Yamada Chemical Industries) is 1.00% owf (Total 3.40% owf), 90% acetic acid 2.00% owf, tap water, Woolsurge cloth (color dyed product) as a treatment object, and a treatment solution with a bath ratio of 1:60 Created. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. 90% acetic acid was added at 0.50% o.w.f after 10 minutes while maintaining the temperature at 100 ° C., and 90% acetic acid was added at 0.50% o.w.f. after another 10 minutes to promote exhaustion. The object to be treated thus obtained exhibited the same green color as the object to be treated obtained in the above-mentioned treatment 1, and was used as a normal processed cloth of a comparative control sample. As shown in Table 1, the object to be processed thus obtained has the same color as in Example 13. Therefore, in the present Example, the said to-be-processed object was set as the comparative example 13 which is a normal processed cloth of a comparative control sample.

<Experiment 14>
Preparation of Example 14: CIAcid Green 1 (Yamada Chemical Co., Ltd.) is added to 6.00% owf, 90% acetic acid 3.00% owf, tap water is added, and a wool surge cloth (color dye company product) is added as an object to be treated. A treatment solution having a bath ratio of 1:60 was prepared. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. 90% acetic acid was added at 0.50% owf after 10 minutes while maintaining the temperature at 100 ° C., and 90% acetic acid was added at 0.50% owf after 10 minutes, and exhaustion was promoted. The object to be processed thus obtained was named Example 14 according to this example.

  Preparation of Comparative Example 14: Acid Light Yellow 2G 90% (CI Acid Yellow 17 / Yamada Chemical Industries) is 3.00% owf and Alizarine Direct Blue A2G conc. (CI Acid Blue 40 / Yamada Chemical Industries) is 1.25% owf (Total 4.25% owf), tap water is added to 90% acetic acid 3.00% owf, wool surge cloth (color dyed company product) is added as the object to be treated, and a treatment solution with a bath ratio of 1:60 is added. Created. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. 90% acetic acid was added at 0.50% o.w.f after 10 minutes while maintaining the temperature at 100 ° C., and 90% acetic acid was added at 0.50% o.w.f. after another 10 minutes to promote exhaustion. As shown in Table 1, the object to be processed thus obtained has the same color as in Example 14. Therefore, in the present Example, the said to-be-processed object was made into the comparative example 14 which is a normal processed cloth of a comparative control sample.

<Experiment 15>
Preparation of Example 15: CIAcid Green 1 (Yamada Chemical Industries Co., Ltd.) was added to 7.00% owf, 90% acetic acid 3.00% owf, tap water was added, and a wool surge cloth (color dyed product) was added as an object to be treated. A treatment solution having a bath ratio of 1:60 was prepared. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. 90% acetic acid was added at 0.50% owf after 10 minutes while maintaining the temperature at 100 ° C., and 90% acetic acid was added at 0.50% owf after 10 minutes, and exhaustion was promoted. The object to be processed thus obtained was named Example 15 according to this example.

  Preparation of Comparative Example 15: Acid Light Yellow 2G 90% (CI Acid Yellow 17 / Yamada Chemical Industries) is 3.60% owf and Alizarine Direct Blue A2G conc. (CI Acid Blue 40 / Yamada Chemical Industries) is 1.50% owf (Total 5.10% owf), tap water is added to 90% acetic acid 3.00% owf, and wool surge cloth (color dyed product) is added as an object to be treated. Created. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. 90% acetic acid was added at 0.50% o.w.f after 10 minutes while maintaining the temperature at 100 ° C., and 90% acetic acid was added at 0.50% o.w.f. after another 10 minutes to promote exhaustion. As shown in Table 1, the object to be processed thus obtained has the same color as in Example 15. Therefore, in the present Example, the said to-be-processed object was made into the comparative example 15 which is a normal processed cloth of a comparative sample.

<Experiment 16>
Preparation of Example 16: Pigment Green 8 Conch (Chempro Exports / India product), Demol RN (Kitahiro Chemical product), and polyvinylpyrrolidone were dispersed in water at a weight ratio of 1: 1: 1. Using the above dispersion, add Pigment Green 8 component 0.50% owf, 90% acetic acid 0.50% owf, sodium acetate 0.50% owf and tap water, and put nylon 6 jersey (color dyed product) as the object to be treated. Thus, a treatment liquid having a bath ratio of 1:60 was prepared. The temperature was increased from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 60 minutes. The object to be processed thus obtained was named Example 16 according to this example.

  Preparation of Comparative Example 16: 0.15% owf of Telon Yellow RLN micro (CIAcid Yellow 230 / Dystar) and 0.10% owf of Alizarine Direct Blue A2G conc. (CIAcid Blue 40 / Yamada Chemical) (Total 0.25% owf), ammonium acetate 2.00% owf, refined detergent Emar 40 (Kao product) to 1.00% owf, tap water added, and nylon 6 jersey cloth (color dyed product) as a treatment object. Thus, a treatment liquid having a bath ratio of 1:60 was prepared. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. 90% acetic acid was added at 0.25% o.w.f after 10 minutes while maintaining 100 ° C, and 90% acetic acid was added at 0.25% o.w.f after another 10 minutes to encourage exhaustion. As shown in Table 1, the object to be processed thus obtained has the same color as in Example 16. Therefore, in the present Example, the said to-be-processed object was set as the comparative example 16 which is a normal process cloth of a comparative control sample.

<Experiment 17>
Preparation of Example 17: Pigment Green 8 Conch (Chempro Exports / India product), Demol RN (Kitahiro Chemical product), and polyvinylpyrrolidone were dispersed in water at a weight ratio of 1: 1: 1. Using the above dispersion, add Pigment Green 8 component to 1.00% owf, 90% acetic acid 0.50% owf, sodium acetate 0.50% owf and tap water, and put nylon 66 jersey (color dye company product) as the object to be treated. A treatment liquid having a bath ratio of 1:60 was prepared. The temperature was increased from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 60 minutes. The object to be processed thus obtained was named Example 17 according to this example.

  Preparation of Comparative Example 17: Telon Yellow RLN micro (CIAcid Yellow 230 / Dystar) 0.29% owf and Alizarine Direct Blue A2G conc. (CIAcid Blue 40 / Yamada Chemical Industries) 0.21% owf (Total 0.50% owf), ammonium acetate 2.00% owf, scouring detergent Emar 40 (Kao product) 1.00% owf, tap water added, nylon 66 jersey cloth (color dyed product) as the treatment object Thus, a treatment liquid having a bath ratio of 1:60 was prepared. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. 90% acetic acid was added at 0.25% o.w.f after 10 minutes while maintaining 100 ° C, and 90% acetic acid was added at 0.25% o.w.f after another 10 minutes to encourage exhaustion. As shown in Table 1, the object to be processed thus obtained has the same color as in Example 17. Therefore, in the present Example, the said to-be-processed object was set as the comparative example 17 which is a normal processed cloth of a comparative control sample.

<Experiment 18>
Preparation of Example 18: Pigment Green 8 Conch (Chempro Exports / India product), Demol RN (Kitahiro Chemical product), and polyvinylpyrrolidone were dispersed in water at a weight ratio of 1: 1: 1. Using the above dispersion, add Pigment Green 8 component to 1.00% owf, 90% acetic acid 0.50% owf, sodium acetate 0.50% owf, tap water, and put a wool surge cloth (color dyed product) as the object to be treated. A treatment liquid having a bath ratio of 1:60 was prepared. The temperature was increased from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 60 minutes. The object to be processed thus obtained was named Example 18 according to this example.

  Preparation of Comparative Example 18: Acid Light Yellow 2G 90% (CI Acid Yellow 17 / Yamada Chemical Industries) is 0.60% owf and Alizarine Direct Blue A2G conc. (CIAcid Blue 40 / Yamada Chemical Industries) is 0.25% owf (Total 0.85% owf), tap water is added to 90% acetic acid 1.00% owf, and wool surge cloth (color dyed product) is added as an object to be treated. Created. The temperature was raised from 40 ° C. to 100 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 100 ° C. for 50 minutes. 90% acetic acid was added at 0.25% o.w.f after 10 minutes while maintaining 100 ° C, and 90% acetic acid was added at 0.25% o.w.f after another 10 minutes to encourage exhaustion. As shown in Table 1, the object to be processed thus obtained has the same color as that of Example 18. Therefore, in the present Example, the said to-be-processed object was set as the comparative example 18 which is a normal process cloth of a comparative control sample.

＜実験１９＞
実施例１９の作成：鉄含金顔料C.I.Pigment Green 8を用い、明るい茶色の色相を得る「別浴処理」を行なった。Pigment Green 8コンク（Chempro Exports／India品）、デモールRN（北広ケミカル品）、ポリビニルピロリドンを、重量比1：1：1の比率で水中に分散させた。上記分散液にリオゲンPLFリキッド（クラリアント品）1.00%o.w.f.、メイサンFLS（明成化学品）0.4g/L、テキスポートBO48（日華化学品）1.0g/Lに、水道水を加え、被処理物を入れて浴比1：20の処理液を作成した。40℃から95℃まで1℃／分の速度で昇温し、95℃×30分の常圧処理を行った。尚、Pigment Green 8の濃度は0.80%o.w.f.、被処理物はナイロン66ジャージー布(色染社品)とした。しかる後、染料として、Telon Orange M-GSN（ダイスター品）1.30%o.w.f.、染色助剤としてメイサンFLS（明成化学品）0.6g/L、リオゲンKSE（クラリアント品）1.00%o.w.f.、90%酢酸3.00%o.w.f.に、水道水を加え、浴比1：20の処理液を作成した。上記処理１で得られる被処理物を入れ、40℃から95℃まで1℃／分の速度で昇温し、95℃×30分の常圧染色処理を行った。これにより得られた被処理物を、本実施例に係る実施例１９とした。

<Experiment 19>
Preparation of Example 19: Using an iron metal-containing pigment CIPigment Green 8, “separate bath treatment” was performed to obtain a light brown hue. Pigment Green 8 Conch (Chempro Exports / India product), Demol RN (Kitahiro Chemical product), and polyvinylpyrrolidone were dispersed in water at a weight ratio of 1: 1: 1. To the above dispersion, tap water is added to Liogen PLF Liquid (Clariant) 1.00% owf, Meisan FLS (Meisei Chemical) 0.4g / L, Textport BO48 (Nikka Chemical) 1.0g / L, A treatment solution with a bath ratio of 1:20 was prepared. The temperature was increased from 40 ° C. to 95 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 95 ° C. for 30 minutes. The concentration of Pigment Green 8 was 0.80% owf, and the object to be treated was nylon 66 jersey cloth (color dyed product). After that, Telon Orange M-GSN (Dyster product) 1.30% owf as dye, Meisan FLS (Meisei Chemical) 0.6g / L as dyeing assistant, Liogen KSE (Clariant product) 1.00% owf, 90% acetic acid 3.00% Tap water was added to owf to prepare a treatment solution with a bath ratio of 1:20. The object to be treated obtained in the above treatment 1 was put in, heated from 40 ° C. to 95 ° C. at a rate of 1 ° C./minute, and subjected to atmospheric dyeing treatment at 95 ° C. × 30 minutes. The object to be processed thus obtained was named Example 19 according to this example.

  Preparation of Comparative Example 19: Dyeing to obtain a light brown hue without using iron metal pigment C.I. Pigment Green 8 was performed. As dyes, Supranol Yellow 4GL <CIAcid Yellow 79> (Dyster product) 0.25% owf, Lanaset Blue 2R (Ciba SC product) 0.20% owf, Telon Orange M-GSN (Dyster product) 1.30% owf, Meishan FLS (Meisei Chemical Co., Ltd.) 0.6g / L, Liogen KSE (Clariant product) 1.00% owf, 90% acetic acid 3.00% owf as a dyeing aid, tap water, and the treatment object are added to a bath ratio of 1:20 A processing solution was prepared. The temperature was raised from 40 ° C. to 95 ° C. at a rate of 1 ° C./minute, and atmospheric pressure dyeing treatment was performed at 95 ° C. for 30 minutes. The object to be treated was nylon 66 jersey cloth (color dyed product). As shown in Table 2, the object to be processed thus obtained has the same color as in Example 19. Therefore, in the present Example, the said to-be-processed object was set as the comparative example 19 which is a normal processed cloth of a comparative control sample.

<Experiment 20>
Preparation of Example 20: Using the iron metal-containing pigment CIPigment Green 8, “same bath treatment” was performed to obtain a dark red hue. Pigment Green 8 Conch (Chempro Exports / India product), Demol RN (Kitahiro Chemical product), and polyvinylpyrrolidone were dispersed in water at a weight ratio of 1: 1: 1. In the above dispersion, Kayanol Milling Red BW (Nippon Kayaku) 1.30% owf as a dye, Meisan FLS (Meisei Chemical) 0.6g / L as a dyeing assistant, Riogen KSE (Clariant) 1.00% owf, 90% acetic acid 3.00 Tap water was added to% owf, and an object to be treated was added to prepare a treatment liquid having a bath ratio of 1:20. The temperature was raised from 40 ° C. to 95 ° C. at a rate of 1 ° C./minute, and atmospheric pressure dyeing treatment was performed at 95 ° C. for 30 minutes. The concentration of Pigment Green 8 was 0.80% owf, and the object to be treated was nylon 66 jersey cloth (color dyed product). The object to be processed thus obtained was named Example 20 according to this example.

  Preparation of Comparative Example 20: Dyeing to obtain a dark red hue without using iron-containing pigment C.I. Pigment Green 8 was performed. As a dye, Supranol Yellow 4GL <CIAcid Yellow 79> (Dyster product) 0.25% owf, Lanase Blue 2R (Ciba SC product) 0.20% owf, Kayanol Milling Red BW (Nippon Kayaku) 1.30% owf, Meishan FLS (Meisei Chemical Co., Ltd.) 0.6g / L, Liogen KSE (Clariant product) 1.00% owf, 90% acetic acid 3.00% owf as a dyeing aid, tap water, and the treatment object are added to a bath ratio of 1:20 A processing solution was prepared. The temperature was raised from 40 ° C. to 95 ° C. at a rate of 1 ° C./minute, and atmospheric pressure dyeing treatment was performed at 95 ° C. for 30 minutes. The object to be treated was nylon 66 jersey cloth (color dyed product). As shown in Table 2, the object to be processed thus obtained has the same color as in Example 20. Therefore, in the present Example, the said to-be-processed object was set as the comparative example 20 which is a normal process cloth of a comparative control sample.

<Experiment 21>
Preparation of Example 21: Using an iron metal-containing pigment CIPigment Green 8, “separate bath treatment” for obtaining a dark blue hue was performed. Pigment Green 8 Conch (Chempro Exports / India product), Demol RN (Kitahiro Chemical product), and polyvinylpyrrolidone were dispersed in water at a weight ratio of 1: 1: 1. To the above dispersion, tap water is added to Liogen PLF Liquid (Clariant) 1.00% owf, Meisan FLS (Meisei Chemical) 0.4g / L, Textport BO48 (Nikka Chemical) 1.0g / L, A treatment solution with a bath ratio of 1:20 was prepared. The temperature was increased from 40 ° C. to 95 ° C. at a rate of 1 ° C./min, and normal pressure treatment was performed at 95 ° C. for 30 minutes. The concentration of Pigment Green 8 was 0.80% owf, and the object to be treated was nylon 66 jersey cloth (color dyed product). After that, as dye, Lanaset Blue 2R (Dystar) 2.00% owf, as dyeing aid Meisan FLS (Meisei Chemical) 0.6g / L, Ryogen KSE (Clariant) 1.00% owf, 90% acetic acid 3.00% owf Then, tap water was added to prepare a treatment solution with a bath ratio of 1:20. The object to be treated obtained in the above treatment 1 was put in, heated from 40 ° C. to 95 ° C. at a rate of 1 ° C./minute, and subjected to atmospheric dyeing treatment at 95 ° C. × 30 minutes. An object to be processed thus obtained was named Example 21 according to this example.

  Preparation of Comparative Example 21: Dyeing to obtain a dark blue hue without using iron-containing pigment C.I. Pigment Green 8 was performed. Supranol Yellow 4GL (CIAcid Yellow 79) (Dyster product) 0.25% owf and Lanaset Blue 2R (Ciba SC product) 2.20% owf are blended as dyes, and Meisan FLS (Meisei Chemical) 0.6 as a dyeing assistant. Tap water was added to g / L, Liogen KSE (Clariant product) 1.00% owf, 90% acetic acid 3.00% owf, and a treatment solution with a bath ratio of 1:20 was prepared by adding an object to be treated. The temperature was raised from 40 ° C. to 95 ° C. at a rate of 1 ° C./minute, and atmospheric pressure dyeing treatment was performed at 95 ° C. for 30 minutes. The object to be treated was nylon 66 jersey cloth (color dyed product). As shown in Table 2, the object to be processed thus obtained has the same color as in Example 21. Therefore, in the present Example, the said to-be-processed object was set as the comparative example 21 which is a normal process cloth of a comparative control sample.

＜実験２２―１＞
実施例２２―１の作成：鉄含金顔料C.I.Pigment Green 8を用い、明るい茶色の色相を得る「別浴処理」を行なった。Pigment Green 8コンク（Chempro Exports／India品）、デモールRN（北広ケミカル品）、ポリビニルピロリドンを、重量比1：1：1の比率で水中に分散させた。上記分散液にキャリアジンCD-W（日成化成品）3.0%o.w.f.、90%酢酸0.2g/L、酢酸ナトリウム0.2g/Lを加え、被処理物を入れて浴比1：20で120℃×30分の加圧処理を行った。尚、Pigment Green 8の濃度は1.50%o.w.f.、被処理物はカチオン可染ポリエステル地(CDP)とした。しかる後、染料として、Nichilon Golden Yellow GL〈C.I.Basic Yellow 28〉（日成化成品）4.0 %o.w.f.、染色助剤としてアボランUL75（バイエル品）1.0 g/L、更に90%酢酸0.2 g/L、酢酸ナトリウム0.2g/L を加え、浴比1：20で110℃×30分の加圧染色処理を行った。これにより得られた被処理物を、本実施例に係る実施例２２―１とした。

<Experiment 22-1>
Preparation of Example 22-1: “Separate bath treatment” was performed to obtain a light brown hue using iron metal pigment CIPigment Green 8. Pigment Green 8 Conch (Chempro Exports / India product), Demol RN (Kitahiro Chemical product), and polyvinylpyrrolidone were dispersed in water at a weight ratio of 1: 1: 1. Carrier Gin CD-W (Nissei Kasei) 3.0% owf, 90% acetic acid 0.2g / L, sodium acetate 0.2g / L is added to the above dispersion, and the object to be treated is placed at 120 ° C with a bath ratio of 1:20. A pressure treatment for × 30 minutes was performed. The concentration of Pigment Green 8 was 1.50% owf, and the material to be treated was cationic dyeable polyester (CDP). After that, Nichilon Golden Yellow GL <CIBasic Yellow 28> (Nissei Kasei) 4.0% owf as a dye, Aboran UL75 (Bayer product) 1.0 g / L as a dyeing assistant, 0.2% / L 90% acetic acid, acetic acid Sodium 0.2 g / L was added, and pressure dyeing treatment was performed at 110 ° C. for 30 minutes at a bath ratio of 1:20. The to-be-processed object obtained by this was set as Example 22-1 which concerns on a present Example.

  Preparation of Comparative Example 22-1: Dyeing to obtain a light brown hue without using iron-containing pigment C.I. Pigment Green 8 was performed. Three types of dyes are included: Kayacryl Yellow 3RL-ED (Nippon Kayaku) 0.171% owf, Kayacryl Blue BG-ED (Nippon Kayaku) 0.036% owf, CDPN Red GL-ID (Nissei Kasei) 0.0196% owf. Desperon 100AW-N (Takamatsu Yushi) 1.00% owf as dyeing aid, 90% acetic acid 0.2g / L, sodium acetate 0.2g / L are added, and the object to be treated is put at 110 ° C at a bath ratio of 1:20. The pressure dyeing process for 30 minutes was performed. In addition, the to-be-processed object was made into the cation dyeable polyester base (CDP). After that, in a separate bath, Nichilon Golden Yellow GL <CIBasic Yellow 28> (Nissei Kasei) 4.00% owf as a dye, Aboran UL75 (Bayer product) 1.0 g / L as a dyeing assistant, and 90% acetic acid 0.2 g / L and sodium acetate 0.2 g / L were added, and the above-mentioned to-be-dyed material was added, and pressure dyeing treatment was performed at 110 ° C. for 30 minutes at a bath ratio of 1:20. As shown in Table 3, the object to be processed thus obtained has the same color as that of Example 22-1 above. Therefore, in this example, the object to be treated was Comparative Example 22-1 which is a normal processed cloth of a comparative sample.

<Experiment 22-2>
Production of Example 22-2: “Same bath treatment” was performed using iron metal pigment CIPigment Green 8 to obtain a light brown hue. Pigment Green 8 Conch (Chempro Exports / India product), Demol RN (Kitahiro Chemical product), and polyvinylpyrrolidone were dispersed in water at a weight ratio of 1: 1: 1. In the above dispersion, Nichilon Golden Yellow GL <CIBasic Yellow 28> (Nissei Kasei) 4.0% owf as a dye, Aboran UL75 (Bayer product) 1.0 g / L as a dyeing assistant, Carrier Gin CD-W (as a carrier agent) Nissei Chemicals) 3.0% owf, 90% acetic acid 0.2g / L, sodium acetate 0.2g / L, add the object to be treated, and pressurize at 120 ° C for 30 minutes at a bath ratio of 1:20 It was. The concentration of Pigment Green 8 was 1.5% owf, and the object to be treated was a cationic dyeable polyester fabric (CDP). The to-be-processed object obtained by this was made into Example 22-2 which concerns on a present Example.

  Preparation of Comparative Example 22-2: The same thing as Comparative Example 22-1 described above was designated as Comparative Example 22-2.

<Experiment 23-1>
Preparation of Example 23-1: “Separate bath treatment” was performed to obtain a dark red hue using iron metal pigment CIPigment Green 8. The dye was Nichilon Red RS (Nissei Kasei) 4.00% owf, and dyeing was carried out in the same manner as in Example 22-1. The to-be-processed object obtained by this was made into Example 23-1 which concerns on a present Example.

  Preparation of Comparative Example 23-1: Dyeing to obtain a dark red hue without using iron metal pigment C.I. Pigment Green 8 was performed. The dye used for the dyed product was Nichilon Red RS (Nissei Kasei) 4.00% o.w.f. Other dyeings were carried out in the same manner as in Comparative Example 22-1. As shown in Table 3, the object to be processed thus obtained has the same color as that of Example 23-1. Therefore, in this example, the object to be treated was Comparative Example 23-1, which is a normal processed cloth of a comparative sample.

<Experiment 23-2>
Preparation of Example 23-2: Using the iron metal-containing pigment CIPigment Green 8, “same bath treatment” for obtaining a dark red hue was performed. The dye used for the article to be dyed was Nichilon Red RS (Nissei Kasei) 4.00% owf, and dyeing was performed in the same manner as in Experiment 22-2. The object to be processed thus obtained was named Example 23-2 according to the present example.

  Preparation of Comparative Example 23-2: The same thing as Comparative Example 23-1 described above was used as Comparative Example 23-2.

＜２．温度測定試験＞
上記のように作成した各実施例並びに各比較例に係る処理布並びに通常加工布について、各々10cm×15cmに採取し、裏面中央部に熱電対温度センサーを設置し、試料表面に照射距離30cmの位置からレフランプ(Panasonic製写真用レフランプPRF-500WB)を照射し、温度変化を1分毎に測定した。測定は、照射10分間と消灯後10分間の20分間とし、試験環境は20±2℃、50±5％RHとした。試料を入れ替え、再度測定を行い、平均値を試験結果とした。
＜３．１ 実験１ないし１８に係る実験結果＞
表１に示した実験１ないし１８の各温度測定試験結果を、図１ないし図１８に示す。財団法人日本紡績検査協会の「光吸収保温性／温度測定試験」では、対照品との温度差が、照射10分後に2.0℃以上、消灯1分後に1.0℃以上認められることを、評価の目安としている。

<2. Temperature measurement test>
For each of the treated cloths and normal cloths according to each of the examples and comparative examples prepared as described above, each sample was taken at 10 cm × 15 cm, a thermocouple temperature sensor was installed in the center of the back surface, and the irradiation distance was 30 cm on the sample surface. A reflex lamp (Panasonic photographic reflex lamp PRF-500WB) was irradiated from the position, and the temperature change was measured every minute. Measurement was carried out for 20 minutes, 10 minutes after irradiation and 10 minutes after extinction, and the test environment was 20 ± 2 ° C. and 50 ± 5% RH. The sample was replaced and measured again, and the average value was taken as the test result.
<3.1 Results of Experiments 1 to 18>
The results of each temperature measurement test in Experiments 1 to 18 shown in Table 1 are shown in FIGS. In the “Light Absorption Thermal Insulation / Temperature Measurement Test” of the Japan Spinning Inspection Association, the standard for evaluation is that the temperature difference from the control product is 2.0 ° C or higher 10 minutes after irradiation and 1.0 ° C or higher 1 minute after turning off the light. It is said.

  From the results of Experiments 1 to 15, Nylon 6 and Nylon 66 jersey fabric treated with CIAcid Green 1 or wool surge fabric was compared with the same fiber dyed in green using acid dye. Good endothermic effect was observed in Acid Green 1 treatment. When the treatment concentration was increased to around 2.00% o.w.f., the best endothermic effect was obtained. Champion data in this experiment was Experiment 11: Wool Surge C.I. Acid Green 1 [2.00% o.w.f.], and a temperature difference from the control product was observed at 4.0 ° C. 10 minutes after irradiation and 2.9 ° C. 1 minute after extinguishing. However, even if the treatment concentration was further increased, the effect was not improved to the same extent as 2.00% o.w.f. If the color of the treated cloth is a high-lightness color such as a CIELAB coordinate L * value of around 60, various color developments are possible, so a treatment density of 0.50 to 1.00% o.w.f. seems to be practical.

  In addition, from the results of Experiments 16 to 18, good endothermic effects could be confirmed in nylon 6 and nylon 66 jersey cloth and wool surge cloth treated with iron metal pigment C.I. Pigment Green 8.

  In particular, the measurement result obtained in this test is an endothermic effect in a temperature range close to human body temperature, and can be said to be effective.

<3.2 Experimental Results for Experiments 19 to 21>
Each temperature measurement test result of Experiments 19 to 21 shown in Table 2 is shown in FIGS. As described above, the evaluation is that the temperature difference from the control product is 2.0 ° C. or more after 10 minutes of irradiation and 1.0 ° C. or more after 1 minute of light is turned off.

  From the results of Experiments 19 to 21, it can be said that various colors can be developed by using nylon 66 jersey cloth and iron-containing face C.I. Pigment Green 8 in combination with 0.80% o.w.f. treatment and acid dye. This iron-containing pigment CIPigment Green 8 treatment and dyeing treatment are colored in the same or different baths, and the same hue is developed only by dyeing treatment without using the iron-containing pigment CIPigment Green 8 As a result, the endothermic effect of the iron metal pigment CIPigment Green 8 treatment was confirmed. This means that the same effect can be expected with materials such as nylon 6 and wool.

  This endothermic heat treatment is an endothermic effect in a temperature range close to a human body temperature, and can be developed in various colors, and can be carried out in the same bath as the dyeing process.

<3.3 Experimental Results for Experiments 22 and 23>
Each temperature measurement test result of Experiments 22 to 23 shown in Table 3 is shown in FIGS. In these experiments as well, the temperature difference from the control product is 2.0 ° C. or higher 10 minutes after irradiation and 1.0 ° C. or higher 1 minute after extinguishing the light, as a guideline for evaluation.

  From the results of Experiments 22 to 23, in the polyester material obtained by treating the iron-containing pigment CIPigment Green 8 at a concentration of 1.50% owf, the treatment with the iron-containing pigment CIPigment Green 8 and the dyeing treatment can be performed in the same bath or in a separate bath. Compared to the case where the color was developed with the iron-containing pigment CIPigment Green 8 and the case where the same hue was developed without using the iron-containing pigment CIPigment Green 8, the endothermic effect of the treatment with the iron-containing pigment CIPigment Green 8 was compared. Was recognized.

  This heat absorption effect is an endothermic effect in a temperature range close to human body temperature, can be developed in various colors, can be carried out in the same bath as the dyeing process, and is further blended with polyester, nylon, wool, etc. It can be said to be a practical process at low cost because it is an effective process for materials.

<4. Conclusion>
Nylon 6, nylon 66, wool treated with iron-containing dye CIAcid Green 1 or iron-containing pigment CIPigment Green 8, defined as “colorant with iron coordinated in the molecule” according to the present invention When investigated as in this example, such a good endothermic effect was observed. These have an endothermic effect in a temperature range close to human body temperature. Considering that this example dyes fabric as an example, the results of the above examples demonstrate that the present invention is effective in the textile field. In particular, when the treatment concentration was increased to around 2.00% owf, the best endothermic effect was obtained. However, even if the treatment concentration was further increased, the effect was not improved to the same extent as 2.00% owf.

On the other hand, in the case of a colored hue obtained at a processing density of about 0.50 to 1.00% owf, various color developments are possible by performing further dyeing with a CIELAB coordinate L * value of around 60 and high brightness. Further, it was found that the treatment can be carried out in the same bath as the dyeing treatment, and a practical treatment can be realized at a low cost.
<Supplement>
The CIELAB coordinate values in this experiment are based on the `` L * a * b * color system (JIS Z 8729) '' that displays colors numerically, with lightness of `` L * '' and chromaticity of `` a * "," B * ". “L *” indicates a white direction as it is closer to 100, and a black direction as it is closer to 0. “A *” indicates the red direction as plus (+) and the green direction as minus (−). “B *” indicates a blue direction as plus (+) or yellow direction minus (−). The measurement was performed using a color spectrophotometer (SF-600plus) manufactured by datacolor and numerical software (CHROMA CALC).

  For the samples obtained in this test, select the color chart symbol of the closest color from JIS L 0808 Standard Processing Concentration Table No. 1 (1/1 of the standard density) and No. 3 (1/6 of the standard density), and CIELAB coordinates Values are measured and shown below for reference.

  The present invention can be used as an endothermic material capable of storing heat by absorbing light and a method for producing the endothermic material.

Claims (10)

  An endothermic material characterized in that it is dyed at a treatment concentration of 0.5% o.w.f or more with a colorant in which iron is coordinated in the molecule.   The endothermic material according to claim 1, wherein the endothermic material is dyed at a treatment concentration of 1.5% o.w.f or more with a colorant in which iron is coordinated in the molecule.   The endothermic material according to claim 1 or 2, wherein the colorant in which iron is coordinated in the molecule is an iron metal-containing dye. The endothermic material according to claim 3, wherein the iron-containing dye is C.I.Acid Green 1.   The endothermic material according to claim 1 or 2, wherein the colorant in which iron is coordinated in the molecule is an iron metal-containing pigment. The endothermic material according to claim 5, wherein the iron-containing pigment is C.I. Pigment Green 8. The endothermic material according to claim 1, 2, 3, 4, 5 or 6, wherein the coordinate L ^* value in L ^* a ^* b ^* color difference notation is 50 or more.   The endothermic material according to claim 1, 2, 3, 4, 5, 6 or 7, wherein the fiber material is dyed.   A method for producing an endothermic material, comprising a dyeing step of dyeing at a treatment concentration of 0.5% o.w.f or more with a colorant having iron coordinated in a molecule.   A method for producing an endothermic material, comprising a dyeing step of dyeing at a treatment concentration of 1.5% o.w.f or more with a colorant having iron coordinated in a molecule.

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