JPS6228838B2 - - Google Patents

Description

[Detailed description of the invention]

The present invention relates to a method for producing artificial soiled cloth useful for measuring the detergency of detergents. Since cleaning is a complex interfacial phenomenon between dirt, fibers (cloth), and detergent, it is ideal to use naturally soiled cloth that has been actually worn by humans to evaluate the cleaning power of detergents, and in fact, JIS The collar scale method is used to evaluate cleaning power. However, the properties and composition of dirt on natural dirt cloth vary depending on the individual wearer and other factors, and the state of dirt adhesion also changes. I regret that I cannot always maintain the same soiled cloth conditions when doing this. Therefore, the development of artificial soiled cloth that exhibits cleaning behavior similar to natural soiled cloth and that can guarantee reproducibility in terms of soil properties, composition, and adhesion state is a matter of research and development of detergents. It can also be said to be extremely important from the perspective of researching cleaning theory. By the way, the conventional methods for preparing artificially soiled cloth include the method of applying a paste-like mixture of inorganic dirt components and organic dirt components to the cloth (dry method), and the method of applying a paste mixture of inorganic dirt components and organic dirt components to the cloth. A method is known in which a mixture of the above is dispersed in an organic solvent such as carbon tetrachloride or perchloroethylene, and a cloth is immersed in the mixture (organic solvent-based wet method). In this case, the inorganic stain components include clay (Kanto loam), dust, iron oxide, carbon black, etc., and the organic stain components include a mixture of fatty acids, triglycerides, cholesterol esters, cholesterol, squalene, liquid paraffin, etc. is used. However, the dry method described above not only requires time and skill to prepare the artificially soiled cloth, but also requires the weight ratio of organic soil components to inorganic soil components to be equal to that of natural soils (approximately 80/20). If it is approximated, it has the disadvantage that it becomes extremely difficult to prepare artificially soiled cloth. On the other hand, the wet method mentioned above can use a dirt bath, so
It has the advantage that an artificially soiled cloth can be easily prepared, and the weight ratio of organic soil components to inorganic soil components can be made similar to that of natural soils. However, artificial soil fabrics prepared by this method are not similar to natural soil fabrics in that organic solvents are used. This is because natural dirt is presumed to adhere to fibers (cloth) in the form of sweat, that is, an emulsion or suspension using water as a dispersion medium.
Therefore, in order to easily prepare artificial soiled cloth that closely resembles natural soiled cloth, a wet method using water as a dispersion medium instead of an organic solvent (aqueous wet method) is recommended. The current water-based wet method had a fatal flaw in that protein stains could not be used. In other words, since natural dirt always contains nitrogen-containing compounds (proteins), in order to obtain an artificially soiled cloth that closely resembles natural soiled cloth, it is necessary to combine the above-mentioned organic soil components and inorganic soils. It is desirable to incorporate proteins into the mixture of ingredients. However, it has been extremely difficult to stably disperse protein-containing mixtures in both organic solvents and water. The present invention aims to solve the above-mentioned problems in the prior art, and has developed an artificial dirt whose cleaning behavior closely resembles that of natural dirt and is dispersible in water. It is an object of the present invention to provide a method for producing artificial soiled cloth by a wet method. Therefore, the artificial dirt for measuring detergency used in the present invention consists of the following four components (A) to (D), in which the amount of component (A) is 3 to 12 wt%, and the amount of component (B) is 3 to 12 wt%. The amount of is 10~75wt
%, the amount of component (C) is 20-40wt%, the amount of component (D) is 0.1
It is in the range of ~1.0wt%. (A) water-soluble protein, (B) organic component having the following composition, (i) oleic acid and/or linoleic acid,
25-65wt% (ii) Cholesterol ester of oleic acid and/or linoleic acid, 10-30wt% (iii) Triglyceride of oleic acid and/or linoleic acid, 15-40wt% (iv) Squalene, 1-8wt% (v ) Liquid paraffin, 1 to 8 wt% (vi) Cholesterol, 1 to 8 wt% (C) Soil containing 60 wt% or more of soil particles with a particle size of 2 μm or less, (D) Carbon black, in the above artificial dirt , gelatin is preferred as the water-soluble protein that is component (A), and components (i), (ii), and (iii) in component (B) are oleic acid, oleic cholesterol ester, and oleic triglyceride, respectively. is preferred. In addition, as component (C), soil mainly composed of crystalline clay minerals,
Among these, soil that has been dried to a constant weight at a temperature of 80 to 300°C is preferred. In order to produce artificially soiled cloth using the wet method, it is first necessary to prepare a stable aqueous dispersion containing artificial soils, that is, a soil bath. If they are dispersed, it is difficult to obtain a dirt bath in which each dirt component is uniformly dispersed. Therefore, in the present invention, component (A) is first dissolved in hot water to form a solution, and then component (D) is added to this solution.
A dirt bath is prepared by adding components (C) in this order and uniformly dispersing each component, and then adding component (B) and uniformly dispersing them. In this case, the dirt in the dirt bath consists of the four components (A) to (D) mentioned above, (A),
Each of the components (B), (C) and (D) is 3 to 30% of the dirt content.
12wt%, 10~75wt%, 20~40wt% and 0.1~
Occupies 1.0wt. The amount of dirt in the dirt bath may range from 10 to 100 g per 1 water. If you soak a cloth in the dirt bath prepared in the above procedure, pull it out, and dry it, the reflectance will be 30-50%.
You can get artificial dirt cloth. Dipping the cloth into the dirt bath, pulling it up, and drying the cloth can be carried out by the methods employed in conventional wet methods, but in the present invention, the cloth taken out from the dirt bath is It is desirable to immediately pass the dirt between two rubber rolls that are in contact with each other to evenly adhere the dirt to the cloth before drying, and drying should be done at a temperature range of 90 to 150 degrees Celsius for about 15 minutes to 3 hours. is preferred. As is clear from the above explanation, according to the present invention, artificial dirt containing nitrogen-containing compounds (proteins) like natural dirt can be mixed into an emulsion using water as a dispersion medium like natural dirt. It can also be applied to fabrics in the form of suspensions. Therefore,
Since the cleaning behavior of the artificially soiled cloth produced by the method of the present invention is very similar to that of the natural soiled cloth, the cleaning power of various detergents evaluated using this artificially soiled cloth is It has the advantage of being able to be seen as a detergent for dirt. Example An artificial soiled cloth of the present invention was prepared in the following manner. Kaolinite, a crystalline mineral, is used for inorganic stains.
200% clay whose main ingredient is vermiculite etc.
After drying at ℃ for 37 hours, it was ground to an average particle size of 1 μm and used. 3.5 g of gelatin was added to 950 c.c. of water, the gelatin was dissolved at about 40° C., and then 0.25 g of carbon black was added. After that, we developed a powerful emulsifying and dispersing machine called Polytron (Switzerland).
Carbon black was dispersed in water using KINEMATICA (manufactured by KINEMATICA). Next, 14.9 g of inorganic dirt was added and dispersed with a polytron, and 31.35 g of organic dirt was further added and emulsified and dispersed with a polytron to create a stable dirt bath. A 10 cm x 20 cm designated clean cloth (cotton cloth No. 60 designated by Yuka Kyokai) was immersed in this dirt bath, and the water was squeezed out using two rubber rolls to equalize the amount of dirt attached. This soiled cloth was dried at 105° C. for 430 minutes, and then both sides of the soiled cloth were rubbed 25 times on each side. This was cut into 5 cm x 5 cm pieces with a reflectance in the range of 42±2% and used as a dirty cloth. The soil composition of the artificially soiled cloth thus prepared is shown in Table 1, and the composition comparison with natural soil is shown in Table 2.

【table】

[Table] As is clear from Table 2, the soil composition in the artificially soiled cloth of the present invention is similar to the natural soil composition, including inorganic soil, organic soil, and protein soil. Furthermore, when observing the state of adhesion of dirt using an optical microscope and a scanning microscope, the state of adhesion of dirt was similar to that of natural dirt. Next, various cleaning experiments were carried out using the above-mentioned artificially soiled cloth and natural collar cloth. Cleaning method: The cleaning device is USTesting's Terg-O-
Using Tometer, 10 pieces of artificial dirty cloth and 60 per piece
Add 3 pieces of Sebam cloth with mg of organic dirt attached,
Washing was carried out using a knitted cloth at a bath ratio of 30 times at 120 rpm. 900 ml of washing solution was used, and rinsing was performed for 1 minute. Cleaning power evaluation method Cleaning power (%) = (K/S of dirty cloth - K/S of washed cloth) / (K of dirty cloth
/S - K/S of clean cloth) x 100 K/S = (1-R) ² /2R...[Kubelkar-
Munk's formula] First, in order to clarify the relationship between builder concentration and cleaning power, we used cleaning solutions with different builder concentrations [liquid temperature 25°C, hardness 3°DH, linear alkylbenzene sulfonic acid sodium compliant with JIS K-3377] (LAS) containing 0.02%], each of the above soiled cloths was washed. Three types of builders were used: sodium tripolyphosphate (STPP), sodium pyrophosphate (TSPP), and soda carbonate (Ash). Table 3 shows the relationship between builder concentration and detergency.

Shown as relative values in [Table].
Next, to investigate the relationship between cleaning temperature and cleaning power,
Each of the above soiled cloths was washed at different washing temperatures. In this case, the cleaning solution is LAS at 250ppm,
A cleaning solution with a hardness of 3° DH containing 150 ppm of TSPP and 240 ppm of sodium silicate was used. Display the results -
4.

[Table] Shown as relative values.
In addition, we investigated the relationship between the amount of protease-containing detergents and their cleaning power. Sodium α-olefin sulfonate (average molecular weight 339.5)
300ppm, TSPP 210ppm, sodium silicate
A proteolytic enzyme was added to a cleaning solution containing 240 ppm, at a temperature of 25° C. and a hardness of 3° DH to prepare cleaning solutions with different amounts, and these were used to wash the above-mentioned dirty cloth. For comparison, EMPA116 (blood, milk, Indian ink), which is commonly used as an artificial dirt cloth, was also subjected to a cleaning test. The results are shown in Table-5.

[Table] Shows the relative values when .
The above results indicate that the artificially soiled cloth of the present invention is similar to natural soils in terms of soil composition and adhesion state.

Claims (1)

[Scope of Claims] 1 (A) water-soluble protein, (B) an organic component having the following composition, (i) oleic acid and/or linoleic acid,
25-65wt% (ii) Cholesterol ester of oleic acid and/or linoleic acid, 10-30wt% (iii) Triglyceride of oleic acid and/or linoleic acid, 15-40wt% (iv) Squalene, 1-8wt% (v ) Liquid paraffin, 1 to 8 wt% (vi) Cholesterol, 1 to 8 wt% (C) Soil containing 60 wt% or more of soil particles with a particle size of 2 μm or less, (D) Carbon black, (A) to ( shown above) Consisting of four components (D), the amount of component (A) is 3 to 12 wt%, the amount of component (B) is 10 to 75 wt%, the amount of component (C) is 20 to 40 wt%, and the amount of component (D) is is 0.1~1.0wt%
A dirt bath containing artificial dirt in the range of 10 to 100 g per water is prepared according to the following procedure, and a cloth is immersed in this dirt bath, then taken out and dried. Method of manufacturing 30-50% artificial dirt cloth. [Silence bath preparation procedure] First, add component (D) to a solution of component (A) in warm water and disperse it uniformly, then add component (C) and uniformly disperse it, then add component (B). ) Add ingredients and disperse evenly. 2. The cloth taken up from the dirt bath is immediately passed through two adjacent rubber rolls to uniformly adhere dirt to the cloth, and then dried. A method for manufacturing artificial dirt cloth. 3. The method for producing artificial soiled cloth according to claim 1, characterized in that the cloth is dried at a temperature of 90 to 150°C for 15 minutes to 3 hours.