JP2002277374A - Pigment for coloring mixture solution for testing wet tensile strength - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a pigment for a coloring mixture solution for a wet tensile strength test having solubility to all the coloring mixture solutions for the wet tensile strength test specified in revised JIS K 6768:1999, and having no surface active action in itself, and provide the coloring mixture solution for the wet tensile strength test containing the pigment. SOLUTION: The pigment for the coloring mixture solution for the wet tensile strength test comprises the pigment soluble in water, ethylene glycol monoethyl ether, formamide and methanol, having substantially no surface active action, and having stability with the lapse of time in surface tension of the mixture solution when dissolved in one kind selected from the solvents hereinbefore or in a mixed solution comprising two to four kinds selected therefrom. The coloring mixture solution for the wet tensile strength test in which the pigment is dissolved, and a kit using the mixture solution are provided also in the present invention.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a dye for a coloring mixture for a wetting tension test used for coloring a mixture for a wetting tension test used for measuring a wetting tension, and a wetting tension test for dissolving the dye. The present invention relates to a coloring mixture and a kit comprising the coloring mixture.

[0002]

2. Description of the Related Art Wetting tension is one measure of the ability of a plastic film to hold inks, coatings, adhesives, and the like. The test method of the wetting tension was specified in "Method of Wetting Test for Polyethylene and Polypropylene Films" of Japanese Industrial Standard JIS K 6768,
In 1980, the International Organization for Standardization (ISO)
8296: Revised significantly based on 1987 (JIS K 676
8: 1999). That is, in the conventional JIS K 6768, a method using a standard solution consisting of a mixed solution having a surface tension in the range of 30.0 to 56.0 mN / m, prepared using two kinds of reagents, formamide and ethylene glycol monoethyl ether, is used for polyethylene. The method was limited to the wet tension test method for polypropylene film and polypropylene film. Is 58.0 ~ 73.0
Addition of mixtures in the range of mN / m has been extended to test methods applicable to plastic films and sheets in general (22.6-73.0 mN / m).

According to JIS K 6768: 1999, the principle of the wetting tension is as follows: "A series of mixed liquids having a gradually increasing surface tension is dropped on the surface of a plastic film until the surface of the plastic film is wetted. Wetting of the test surface The tension can be approximated by the surface tension of the mixed solution. "

A specific test method of the wetting tension specified in JIS K 6768: 1999 is as follows. That is, the test liquid mixture in which the wetting tensions are different in order is dropped and applied to the surface of the plastic film test piece, and the wetness is determined in the state of the center of the liquid film after 2 seconds, and the test piece is determined. The value of the surface tension of the liquid mixture determined to be able to wet the surface of the sample accurately in 2 seconds is defined as the wet tension of the test piece.

In this wet tension test, the amount of the test mixture to be applied (the thickness of the liquid film applied to the test piece) is
The amount of the coating solution must be appropriate because it has a significant effect on the accuracy of the test, and when applied to the surface of the test piece, an excess or deficiency in the amount of the coating solution causes a measurement error. However, since the test mixture itself is colorless, if it is used as it is, it is difficult to visually determine whether the amount of the coating solution is appropriate. For this reason, in JIS K 6768 before the revision, a colored mixture of Victoria Pure Bull-BO, a highly colored dye, added to the test mixture at a concentration of 0.03% or less, and used as the wet tension standard solution However, JIS K 6768: 1999 stipulates only the composition of the mixture for the wetting tension test, and does not specify a dye.

[0006] Then, when a conventionally used pigment (Victoria Pure Blue BO) was dissolved in methanol and water, formamide and a mixture thereof added by the amendment, several problems occurred. That is, the conventional dye has particularly poor solubility in water, the surface tension of a mixed solution containing water is extremely low, and it is extremely difficult to prepare a test mixed solution having an intended wetting tension. The problem is that the measured value of the wetting tension is not constant because the surface tension of the sample changes over time.

Further, even in the method specified in JIS K 6768 before the amendment, the wet tension standard solution in which the dye is dissolved has a problem that the mixed solution is easily discolored depending on storage conditions.

[0008]

DISCLOSURE OF THE INVENTION The present invention has been made in view of the above situation, and has been made in accordance with the revised JIS K 6768: 1.
A dye for a wetting tension test coloring mixture and a wetting tension test coloring mixture containing the dye, having solubility in all of the wetting tension test mixtures specified in 999, and having no surfactant activity per se. The purpose is to provide.

[0009]

According to the present invention, there is provided a compound having a solubility in water, ethylene glycol monoethyl ether, formamide and methanol, having substantially no surfactant activity per se, and selected from the above-mentioned solvents. One or two to four
A coloring matter for a coloring mixture for a wetting tension test, comprising a coloring matter having stability over time of the surface tension of the mixture when dissolved in the kind of the mixture. The invention of ".

[0010] The present invention also relates to a compound selected from the above-mentioned solvents which has solubility in water, ethylene glycol monoethyl ether, formamide and methanol, has substantially no surfactant activity per se, and Or, when dissolved in a mixture of two to four kinds, a dye having surface tension stability over time of the mixed solution, and a solution of the mixed solution, for a wetting tension test having stability over time of surface tension. Colored mixture. "
Invention.

[0011] The present invention further relates to a compound selected from the group consisting of "soluble in water, ethylene glycol monoethyl ether, formamide and methanol, having substantially no surfactant activity per se, and one selected from the above-mentioned solvents. Or, when dissolved in a mixture of 2 to 4 types, a dye having stability with time of the surface tension of the mixture and a solution of the mixture, and a plurality of solutions having different wetting tensions from each other. , A colored mixed liquid kit for a wetting tension test having stability over time of surface tension. "

Further, the present invention relates to CIAcid Blue 27,
A dye selected from CIAcid Blue 43, Food Green No. 3 (Fast Green FCF) or Food Blue No. 1 (Brilliant Blue FCF) and one or two to four selected from water, ethylene glycol monoethyl ether, formamide and methanol
A solution with a mixture of seeds having a wetting tension of about 22 mN /
A colored mixture liquid kit for a wetting tension test having a stability with time of surface tension, comprising a plurality of solutions, each showing a different numerical value in the range of m to about 73 mN / m. The invention of ".

That is, the present inventors have revised JIS K 6768: 199.
As a result of intensive studies in search of a dye suitable for being added to the mixture for wetting tension test used in 9, it was found that a dye having specific properties was suitable for this purpose, and the present invention was completed. Reached.

The dyes for the colored mixture for the wetting tension test according to the present invention include water, ethylene glycol monoethyl ether, formamide, methanol and mixtures thereof used for measuring the wetting tension in the revised JIS K 6768: 1999. It has the solubility of being able to dissolve the required concentration in the liquid, and specifically, has a practically sufficient solubility in the mixed solution,
Specifically, those having a solubility of 0.01 w / vol% or more are mentioned.

It is preferable that the dye has substantially no surfactant activity. When the dye is dissolved in one or a mixture of two to four selected from the above-mentioned solvents, the dye is mixed. It is preferable to use a dye having a stability with time such that the surface tension of the liquid hardly changes for at least 1 to 3 months. Further, in consideration of ease of use and the like, the color of the dye itself does not change even after storage for at least 1 to 3 months (has color stability over time), and is in a solution state dissolved in the mixed solution. It is preferable that the color change is hardly observed for 1 to 3 months even if stored. Further, a blue type is preferable because the wetting tension can be easily measured.

Examples of the dye satisfying the above requirements include anthraquinone acid dye and triphenylmethane dye.

Specific examples of anthraquinone dyes include:
For example, CIAcid Blue 27 represented by the following structural formula,

[0018]

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Alternatively, CIAcid Blue represented by the following structural formula
43 and the like.

[0020]

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Specific examples of the triphenylmethane dye include, for example, a blue food dye, specifically, for example, Food Green No. 3 (Fast Green FCF) represented by the following structural formula:

[0022]

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Alternatively, there may be mentioned Food Blue No. 1 (Brilliant Blue FCF) represented by the following structural formula.

[0024]

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The colored mixture for the wetting tension test according to the present invention is a mixture of one or two or four selected from water, ethylene glycol monoethyl ether, formamide and methanol, as defined in JIS K 6768: 1999. The liquid (wetting tension test mixture: Table 1) is a solution in which the dye for the coloring mixture for wetting tension test according to the present invention is dissolved at a predetermined concentration, and the mixture is colored. The dissolution method and the like are not particularly limited.

[0026]

[Table 1] Table 1

The concentration of the dye for the coloring mixture for wetting tension test in the coloring mixture for wetting tension test is determined by dissolving the dye in the mixture for the wetting tension test. What is necessary is just to be colored to the extent that the excess or deficiency state is easily understood. Usually 0.01 to 1.10 w / vol%, preferably 0.01 to 0.05 w
/ vol%.
Taking into account the fact that it was defined as 03 w / vol%, it is more preferably 0.03 w / vol%.

The coloring mixture kit for a wetting tension test according to the present invention comprises a solution obtained by dissolving the dye for a wetting tension test coloring mixture according to the present invention in the above wetting tension test mixture. And a plurality of solutions having different wetting tensions from each other. JISK 6768: 1999 stipulates 36 kinds of liquid mixtures for wetting tension test, but the kit may be composed of colored mixtures of all 36 kinds of liquid mixtures for wetting tension test. Good and one with the wetting tension to be measured and / or wetting tension in the vicinity
It may be composed of colored mixture of up to 36 kinds of mixture for wetting tension test. These solutions have a surface tension stability over time of at least 1 to 3 months.

As a specific embodiment of the coloring mixture kit for wetting tension test according to the present invention, CIAcid Blue 27, CIAcid Blue 43, Edible Green No. 3 (Fast Green FCF) or Edible Blue No. 1 (Brilliant
Blue FCF) or the like, comprising a coloring mixture for a wetting tension test in which a dye for a coloring mixture for a wetting tension test according to the present invention is dissolved, wherein the wetting tension is about 22 mN / m to about 73 mN / m.
It is composed of a plurality of types of solutions having different numerical values within the range of mN / m. JIS K 6768: 1999 stipulates 36 kinds of liquid mixtures for wetting tension test within the range of about 22 mN / m to about 73 mN / m.
It may be composed of a colored mixture of all 36 kinds of mixture for wetting tension test, and may have a wetting tension to be measured and / or a wetting tension in the vicinity thereof of 1 to 3.
It may be composed of a colored mixed liquid of six kinds of mixed liquids for a wetting tension test. These solutions have a surface tension stability over time of at least 1 to 3 months.

Hereinafter, the present invention will be described in more detail with reference to Examples, but the present invention is not limited thereto.

[0031]

EXAMPLES Example 1 (1) Preparation of Colored Liquid Mixture for Wetting Tension Test JIS K 6768: 1999 (“Plastic-Film and Sheet-Wet Tension Testing Method”, published on October 31, 1999,
Printing, published by the Japan Standards Association), CIAcid Blue was added to nine kinds of wet tension test mixtures as shown in Table 1.
27 was prepared so that each was dissolved at 0.03 (w / vol)% to obtain a colored mixed solution for a wetting tension test. In addition, the solvent used for the mixture for the wetting tension test used was a standard specified in JIS K 6869: 1999. (2) Measurement of surface tension The colored mixture for wetting tension test prepared in (1) was placed in a brown bottle and stored at room temperature or 37 ° C for 1 to 3 months, respectively.
The surface tension of the colored mixture for the wetting tension test at the start, at the time of storage for 1 month, and at the time of storage for 3 months was measured using a Du-Nouy surface tensiometer (Kyowa Interface Chemical Co., Ltd., CBVP-Z type, set temperature 23 ± 0.2 ℃)
It measured using.

(3) Results The results are shown in Table 2.

[0033]

[Table 2] Table 2

As is evident from the results in Table 2, the mixture according to the present invention, CIAcid Blue 27, was added to the wetting tension test mixture.
Was dissolved in all of the tested mixtures (mixtures for wetting tension test added in JIS K 6768: 1999: 22.6, 27.3, 58.0, 63.0, 70.0, 7
3.0 mN / m, and the conventionally specified mixture for wet tension test: both 30.0, 31.0 and 37.0 mN / m), either at room temperature or at 37 ° C for 1 month to 3 months. Even when stored for a month, the surface tension hardly changed, and good aging stability was observed. CIAcid Blue 27 has good solubility in all of the wetting tension test mixtures used, and the wetting tension test coloring mixture in which the dye was dissolved shows almost no discoloration of the solution due to long-term storage. I couldn't.

Example 2 A colored mixture for a wetting tension test was prepared in the same manner as in Example 1 except that CIAcid Blue 43 was used instead of CIAcid Blue 27, and the surface tension was measured in the same manner as in Example 1. did. Table 3 shows the results.

[0036]

[Table 3] Table 3

As is clear from the results in Table 3, CIAcid B
The coloring mixture for wetting tension test in which lue 43 was dissolved was also stored at room temperature for all the wetting tension test mixtures tested.
Regardless of the storage at 7 ° C., even after storage for 1 to 3 months, the surface tension hardly changed, and good day-to-day stability was observed. CIAcid Blue 43 has good solubility in any of the wetting tension test mixtures used, and the wetting tension test coloring mixture in which the dye was dissolved shows almost no discoloration of the solution due to long-term storage. I couldn't.

Example 3 A colored mixture for a wetting tension test was prepared in the same manner as in Example 1 except that Edible Green No. 3 was used instead of CIAcid Blue 27, and the surface tension was measured in the same manner as in Example 1. It was measured. Table 4 shows the results.

[0039]

[Table 4] Table 4

As is clear from the results in Table 4, edible green 3
No. (Fast Green FCF) was dissolved, and the surface tension hardly changed even when stored at room temperature or at 37 ° C for 1 to 3 months. Stability over time was observed. In addition, edible green No. 3 (Fast G
reen FCF) has good solubility in any of the wetting tension test mixtures used, and the wetting tension test coloring mixture in which the dye was dissolved shows almost no discoloration of the solution due to long-term storage. Was.

Example 4 A colored mixture for a wetting tension test was prepared in the same manner as in Example 1 except that Food Blue No. 1 was used instead of CIAcid Blue 27, and the surface tension was measured in the same manner as in Example 1. It was measured. Table 5 shows the results.

[0042]

[Table 5] Table 5

As is clear from the results in Table 5, edible blue 1
No. (Brilliant Blue FCF) was dissolved in the colored mixture for wetting tension test, either at room temperature or at 37 ° C.
Even if stored for one to three months, the surface tension hardly changes,
Good inter-day stability was observed. In addition, Food Blue No. 1 (Br
illiant Blue FCF) has good solubility in any of the wetting tension test mixtures used, and the wetting tension test coloring mixture in which the dye was dissolved does not show any discoloration of the solution due to long-term storage. Was.

Comparative Example 1 (1) Preparation of Colored Liquid Mixture for Wetting Tension Test JIS K 6768: 1999 (“Plastic-Film and Sheet-Wet Tension Test Method”, published October 31, 1999,
In accordance with the printing, published by the Japan Standards Association), Victoria Pure Blue BO was dissolved in each of the five kinds of wet tension test mixtures as shown in Table 5 so as to be 0.03 (w / vol)%. This was prepared and used as a colored mixed solution for a wetting tension test. (2) Measurement of surface tension The surface tension of the coloring mixture for wetting tension test prepared in (1) was measured using a Du-Nouy surface tensiometer (manufactured by Kyowa Interface Chemical Co., Ltd., CBVP-
(Z type, set temperature 23 ± 0.2 ° C).

(3) Results The results are shown in Table 6.

Table 6

As is clear from the results in Table 6, JIS 6768:
When Victoria Pure Blue, a conventionally used dye, is dissolved in the coloring mixture for wetting tension test (wetting tension: 22.6, 58.0, 63.0, 73.0 mN / m) added in 1999, It can be seen that the surface tension decreases.
Furthermore, the measured value changed with time during the measurement of the surface tension. In addition, we have added a wet tension measuring solution (ethylene glycol monomethyl ether) with a wetting tension measuring solution (ethylene glycol monomethyl ether) of 30.0 and 37.0 mN / m which has been conventionally specified (JIS K 6768).
When pure blue is dissolved, the surface tension of the solution does not match the theoretical value. In other words, Victoria Pure Blue BO is not preferable as a dye for a coloring mixture for a wetting tension test. I understand.

[0048]

As is apparent from the above description, the present invention relates to a dye for a coloring mixture for a wetting tension test having solubility in a mixture for a wetting tension test specified in the revised JIS K 6768, and the dye. It is intended to provide a kit for a wetting tension test comprising a coloring mixture for wetting tension test using a coloring mixture for a wetting tension test using the coloring matter for a wetting tension test according to the present invention. , Revised JIS K 6768
This makes it possible to accurately and more easily measure the wetting tension according to the above-mentioned rules.

Claims (8)

[Claims] 1. One or two to four solvents selected from the above-mentioned solvents, having solubility in water, ethylene glycol monoethyl ether, formamide and methanol, having substantially no surfactant activity per se. A dye for a colored mixed solution for a wetting tension test, comprising a dye having stability over time of the surface tension of the mixed solution when dissolved in the mixed solution. 2. The ink composition further has color stability over time.
The dye according to claim 1. 3. The dye according to claim 1, wherein the dye is blue. 4. The dye according to claim 3, wherein the dye is an anthraquinone acid dye or a triphenylmethane dye. 5. An anthraquinone-based acid dye is CI Acid Blu
e27, CIAcid Blue 43, whose triphenylmethane pigment is food green No. 3 (Fast Green FCF) or food blue 1
No. (Brilliant Blue FCF). 6. A solvent which is soluble in water, ethylene glycol monoethyl ether, formamide and methanol, has substantially no surfactant activity per se, and one or two to four selected from the above-mentioned solvents. A colored mixture for a wetting tension test having a temporal stability of surface tension, comprising a dye having a temporal stability of the surface tension of the mixed liquid when dissolved in the mixed liquid of the above. 7. A solvent which is soluble in water, ethylene glycol monoethyl ether, formamide and methanol, has substantially no surfactant activity per se, and one or two to four selected from the above-mentioned solvents. When dissolved in a mixed solution of the above, a dye having a surface tension stability of the mixed solution over time, and a solution of the mixed solution, comprising a plurality of types of solutions having different wetting tensions from each other. Colored liquid mixture kit for wetting tension test with stability over time. 8. CIAcid Blue 27, CIAcid Blue 43, Food Green No. 3 (Fast GreenFCF) or Food Blue No. 1 (Brill
iant Blue FCF), and a solution of a mixture of one or two to four selected from water, ethylene glycol monoethyl ether, formamide and methanol, having a wetting tension of about 22 mN / m to A colored mixed liquid kit for a wetting tension test, comprising a plurality of solutions exhibiting different numerical values within a range of about 73 mN / m and having stability over time of surface tension.