MICROSPHERICAL PARTICLE

Abstract

An object of the present invention is to provide microsphere particles containing powdered cellulose, which have an excellent massage effect, a high cleansing effect, and excellent dispersibility. A microspherical particle comprising powdered cellulose meets the following condition of (A) or (B): (A) an average particle diameter of less than 50 m, and a sphericity of 0.1 or more to 1.0 or less; or (B) the microspherical particle has an average particle diameter of 50 to 100 and a sphericity of 0.1 or more to less than 0.7.

Claims

1. A microspherical particle comprising powdered cellulose, the microspherical particle having the following (A) or (B): (A) an average particle diameter of less than 50 m, and a sphericity of 0.1 to 1.0; or (B) an average particle diameter of 50 to 100 m, and a sphericity of 0.1 or more to less than 0.7.

2. The microspherical particle according to claim 1, wherein the microspherical particle has an average particle diameter of 5 or more to 70 m or less, and an average polymerization degree of 50 to 2,000.

3. A cleaning composition comprising the microspherical particle according to claim 1.

4. A cosmetic composition comprising the microspherical particle according to claim 1.

5. A cleaning composition comprising the microspherical particle according to claim 2.

6. A cosmetic composition comprising the microspherical particle according to claim 2.

Description

EXAMPLES

[0079] The present invention will be described in detail below by way of examples; however, the present invention is not limited by the following examples.

Example 1-1 (Microspherical Particle 1)

[0080] Powdered cellulose W-06MG (manufactured by Nippon Paper Industries Ltd., mean particle size 6 m, average degree of polymerization 150, apparent specific gravity 0.34 g/ml) in an amount of 500 g was charged into a mixer, and water was adequately added and they were mixed by stirring. This wetted powder was charged into a centrifugal tumbling granulator CF-360N (manufactured by Freund Corp.) and granulation was performed with spraying water appropriately during 100 minutes. The generated particles were fluidized and dried, thus obtaining microspherical particles having an average particle diameter of 50 a sphericity of 0.68, a dry hardness of less than 20 g/mm.sup.2, and an apparent specific gravity of 0.38 g/ml.

Example 1-2 (Microspherical Particle 2)

[0081] Microspherical particles having an average particle diameter of 24 m, a sphericity of 0.65, a dry hardness of less than 20 g/mm.sup.2, and an apparent specific gravity of 0.80 g/ml were obtained in the same manner as that in Example 1-1 except that the time for granulation was increased.

Example 1-3 (Microspherical Particle 3)

[0082] Microspherical particles having an average particle diameter of 32 m, a sphericity of 0.60, a dry hardness of less than 20 g/mm.sup.2, and an apparent specific gravity of 0.63 g/ml were obtained in the same manner as that in Example 1-1 except that the amount of spraying water was increased.

Comparative Example 1

[0083] Polyethylene beads (product name: Microscrub 35PC, manufactured by Prospector Corp.) having an average particle diameter of 350 m and a sphericity of 0.38 was used instead of the microspherical particles containing the powdered cellulose.

Example 2-1 (Microspherical Particle 4)

[0084] Powdered cellulose W-06MG (manufactured by Nippon Paper Industries Ltd., mean particle size 6 m, average degree of polymerization 150, apparent specific gravity 0.34 g/ml) in an amount of 500 g was charged into a mixer, and water was adequately added and they were mixed by stirring. This wetted powder was charged into a centrifugal tumbling granulator CF-360N (manufactured by Freund Corp.) and granulation was performed with spraying water appropriately during 100 minutes. The generated particles were fluidized and dried, thus obtaining microspherical particles having an average particle diameter of 62 m, a sphericity of 0.69, a dry hardness of less than 20 g/mm.sup.2, and an apparent specific gravity of 0.51 g/ml.

Example 2-2 (Microspherical Particle 5)

[0085] Powdered cellulose W-400M (manufactured by Nippon Paper Industries Ltd., mean particle size 24 m, average degree of polymerization 140, apparent specific gravity 0.48 g/ml) in an amount of 500 g was charged into a mixer, and water was adequately added and they were mixed by stirring. This wetted powder was charged into a centrifugal tumbling granulator CF-360N (manufactured by Freund Corp.) and granulation was performed with spraying water appropriately during 100 minutes. The generated particles were fluidized and dried, thus obtaining microspherical particles having an average particle diameter of 88 m, a sphericity of 0.69, a dry hardness of less than 20 g/mm.sup.2, and an apparent specific gravity of 0.74 g/ml.

Example 2-3 (Microspherical Particle 6)

[0086] Microspherical particles having an average particle diameter of 58 a sphericity of 0.70, a dry hardness of less than 20 g/mm.sup.2, and an apparent specific gravity of 0.66 g/ml were obtained in the same manner as that in Example 2-1 except that the amount of spraying water was decreased.

Comparative Example 2

[0087] As another cellulose type of a microspherical particle, cellulose beads (VIVAPURCS100S, manufactured by J. Rettenmaier & Sohne), having an average particle diameter 170 dry hardness 84 g/mm.sup.2, were used.

[0088] <Evaluation of Microspherical Particle>

[0089] <Average Particle Diameter>

[0090] A laser diffraction/scattering particle size distribution measurement device (Microtrac MT3300EX, manufactured by MicrotracBEL Corp.) was used. A measurement was performed with a sample in an amount of 0.2 g, which was added to ethanol used as a dispersion medium in the measurement, thus determining a particle diameter at a cumulative volume of 50% (the average particle diameter).

[0091] <Measurement of Sphericity>

[0092] Image data of the microspherical particle as an observation object was acquired using an optical microscope (product name: Digital Microscope VHX-600, manufactured by Keyence Corp.) and image analysis was performed using Image Hyper II (manufactured by Digimo Co., Ltd.). The sphericity was determined from the formula: sphericity =A/B, where A was an area of the microspherical particle determined by the image analysis, and B was an area of an imaginary perfect sphere which is determined by calculation assuming that the diameter of which is the maximum major axis diameter of the microspherical particle.

[0093] <Measurement of Dry Hardness>

[0094] A dry hardness (g/mm.sup.2) was determined by measuring a peak value of a crushing strength of one microspherical particle using a particle granule hardness meter (product name: GRANO, manufactured by Okada Seiko Co., Ltd.) and calculating an average value of 20 particles.

[0095] <Cleaning Composition>

[0096] <Cleaning Composition, Evaluation of Massage (Body)>

[0097] To 95 g of a commercially available body cleanser (product name: Dove body wash G, manufactured by Unilever Japan K.K.), 5 g of the microspherical particles of Examples 1-1 to 1-3 and 2-1 to 2-3, the polyethylene beads of Comparative Example 1, or a cellulose type microspherical particle (product name: VIVAPURCS100S, manufactured by J. Rettenmaier & Sohne) of Comparative Example 2 were each added and mixed by stirring, thus preparing each mixture liquid. After the mixture liquids thus obtained were left to stand for 5 hours, 5 g of each mixture liquid was applied to the cheeks of five subjects and then the applied part was rubbed 20 times by the palm. Then, feeling of rubbing was evaluated according to the following indexes. The evaluation was indicated with the average value of the five subjects. [0098] A: Tactile sensation with massage feeling was given. [0099] B: Tactile sensation with weak massage feeling was given. [0100] C: No tactile sensation with no massage feeling was given.

[0101] Results of each body cleaning composition including Examples 1-1 to 1-3 or the polyethylene beads of Comparative Example 1 are shown in Table 1. Further, results of each cleaning composition including Examples 2-1 to 2-3 or a cellulose type microspherical particle of Comparative Example 2 are shown in Table 2.

[0102] Note that, in Tables 1-3 shown below, the symbol of - indicates non-measurement or measurement inability.

[0103] <Cleaning Composition, Evaluation of Massage (Scalp)>

[0104] To 95 g of a commercially available body cleanser (product name: Merit, manufactured by Kao Corp.), 5 g of the microspherical particles of Examples 1-1 to 1-3 and 2-1 to 2-3, the polyethylene beads of Comparative Example 1, or cellulose type microspherical particles (product name: VIVAPURCS100S, manufactured by J. Rettenmaier & Sohne) of Comparative Example 2 were each added and mixed by stirring, thus preparing each mixture liquid. After the mixture liquids thus obtained were left to stand for 5 hours, 0.5 g of each mixture liquid was applied to a scalp of five subjects and then the applied part was rubbed 10 times by a finger. Then, feeling of rubbing was evaluated according to the following indexes. The evaluation was indicated with the average value of the five subjects. [0105] A: Tactile sensation with massage feeling was given. [0106] B: Tactile sensation with weak massage feeling was given. [0107] C: No tactile sensation with no massage feeling was given.

[0108] Results of each body cleaning composition including Examples 1-1 to 1-3 or the polyethylene beads of Comparative Example 1 are shown in Table 1. Further, results of each cleaning composition including Examples 2-1 to 2-3 or cellulose type microspherical particles of Comparative Example 2 are shown in Table 2.

[0109] <Cleaning Composition, Evaluation of Massage (Inside Mouth)>

[0110] To 95 g of a commercially available toothpaste (product name: Guard Hello Standing Tube, manufactured by Kao Corp.), 5 g of the microspherical particles of Examples 1-1 to 1-3 and 2-1 to 2-3, the polyethylene beads of Comparative Example 1, or cellulose type microspherical particles (product name: VIVAPURCS100S, manufactured by J. Rettenmaier & Sohne) of Comparative Example 2 were each added and mixed by stirring, thus preparing each mixture liquid. After the mixture liquids thus obtained were left to stand for 5 hours, five subjects each took 1 g of each mixture liquid by a finger and applied to inside of the mouth and the gums, and then the applied part was rubbed 10 times. Then, feeling of rubbing was evaluated according to the following indexes. The evaluation was indicated with the average value of the five subjects.

[0111] A: Tactile sensation with massage feeling was given.

[0112] B: Tactile sensation with weak massage feeling was given.

[0113] C: No tactile sensation with no massage feeling was given.

[0114] Results of each body cleaning composition including Examples 1-1 to 1-3 or the polyethylene beads of Comparative Example 1 are shown in Table 1. Further, results of each cleaning composition including Examples 2-1 to 2-3 or a cellulose type microspherical particle of Comparative Example 2 are shown in Table 2.

[0115] <Cleaning Composition, Evaluation of Cleaning Performance (Body)>

[0116] To 95 g of a commercially available body soap (product name: Biore uRf, manufactured by Kao Corp.), 5 g of the microspherical particles of Examples 1-1 to 1-3 and 2-1 to 2-3 were each added, thus preparing each cleaning liquid. An area measuring 22 cm on the left palm of each panelist was uniformly painted with a blue oily marking pen (Hi-Mackee Care, manufactured by Zebra Co., Ltd.). Subsequently, 5 g of the above cleaning liquids were each applied to the painted part to clean by rubbing 100 times with both palms. After washed with water and dried, the palm was observed with 20x magnification using a microscope (VH-7000, manufactured by Keyence Corp.) to evaluate a removal degree (the cleaning performance) of the blue marking. Results are shown in Table 1.

[0117] A+: Cleaning performance was very good. Most of blue color was removed.

[0118] A: The blue color was so removed that cleaning performance was realized.

[0119] B: Cleaning performance was observed, but blue color faintly remained.

[0120] C: Cleaning performance was observed and blue color remained.

[0121] <Cleaning Composition, Evaluation of Dispersibility>

[0122] An amount of 100 g each of the cleaning liquids, which were prepared as described above, was placed in a screw-top glass bottle (250 ml). After the lid was put, the bottle was shaken up and down ten times. After the bottle was left to stand for 1 hours, the lid was opened and the liquid was stirred again with a glass stir bar, and then dispersibility was evaluated according to the following manners.

[0123] A: There was no resistance at the time of stirring at the bottom part of the screw-top glass bottle, and the dispersibility of the microspherical particles was excellent.

[0124] B: A little resistance was felt at the time of stirring at the bottom part of the screw-top glass bottle. Some sediment of the microspherical particles was felt; however, it was solved by the re-stirring.

[0125] C: Resistance was felt at the bottom part of the screw-top glass bottle. It was not solved by the re-stirring.

TABLE-US-00001 TABLE 1 Evaluation of Microspherical Particle 1-3 (Cleaning Composition) Microspherical Particle Average Inside Type of Material of Particle Dry Body Scalp Mouth Microspherical Microspherical Diameter Hardness Massage Evaluation Evaluation of Massage Massage Particle Particle (m) Sphericity (g/mm.sup.2) Effect of Cleaning Dispersibility Effect Effect Microspherical W-06MG 50 0.68 less than A A+ A A A Particle 1 20 (Example 1-1) Microspherica1 W-06MG 24 0.65 less than B A+ A B A Particle 2 20 (Example 1-2) Microspherical W-06MG 32 0.60 less than A A A B A Particle 3 20 (Example 1-3) Polyethylene Beads 350 0.38 A A A (Comparative Example 1)

TABLE-US-00002 TABLE 2 Evaluation of Microspherical Particle 4-6 (Cleaning Composition) Microspherical Particle Average Inside Type of Material of Particle Dry Body Scalp Mouth Microspherical Microspherical Diameter Hardness Massage Evaluation Evaluation of Massage Massage Particle Particle (m) Sphericity (g/mm.sup.2) Effect of Cleaning Dispersibility Effect Effect Microspherical W-06MG 62 0.69 less than A A+ A A A Particle 4 20 (Example 2-1) Microspherical W-400M 88 0.69 less than A A+ B A A Particle 5 20 (Example 2-2) Microspherical W-06MG 58 0.70 less than A A+ A B A Particle 6 20 (Example 2-3) VIVAPUR CS100S Cellulose 170 84 A B-C B B B-C (Comparative Example 2) Polyethylene Beads 350 0.38 A A A A A (Comparative Example 1)

[0126] <Cosmetic Composition>

[0127] <Cream>

[0128] To 10 g of commercial moisturizing cosmetic (product name: NIVEA Cream c, manufactured by Nivea Kao Corp.), 2 g of the microspherical particles of Example 2-2 (Microspherical Particle 5), Example 2-6 (Microspherical Particle 6), Example 1-3 (Microspherical Particle 3), or Example 1-2 (Microspherical Particle 2), as mentioned above, were each added and stirred well to prepare a mixture liquid, thereby obtaining each cream agent.

[0129] <Solid Stick>

[0130] To a surface for use of a commercial moisturizing cosmetics in the form of a solid stick (product name: Menturm medical use stick, manufactured by Omi Brothers Corp.), 2 g of the microspherical particles of Examples 2-2 (Microspherical Particle 5), Example 2-6 (Microspherical Particle 6), Example 1-3 (Microspherical Particle 3) or Example 1-2 (Microspherical Particle 2), as mentioned above, were each uniformly attached, thereby obtaining each solid stick agent.

[0131] <Milky Lotion>

[0132] To 10 g of a commercial moisturizing cosmetic (product name: Grandane Luxage Lift Moisture Emulsion, manufactured by Kose Corp.), 2 g of the microspherical particles of Example 2-2 (Microspherical Particle 5), Example 2-6 (Microspherical Particle 6), Example 1-3 (Microspherical Particle 3) or Example 1-2 (Microspherical Particle 2), mentioned above, were each added and stirred well to prepare a mixture liquid, thereby obtaining each milky lotion agent.

[0133] <Oil>

[0134] To 10 g of a commercial moisturizing cosmetic (product name: Johnson Baby Oil, manufactured by Johnson & Johnson Corp.), 3 g of the microspherical particles of Examples 2-2 (Microspherical Particle 5), Example 2-6 (Microspherical Particle 6), Example 1-3 (Microspherical Particle 3) or Example 1-2 (Microspherical Particle 2), mentioned above, were each added and stirred well to prepare a mixture liquid, thereby obtaining each oil agent.

[0135] <Gel>

[0136] To 10 g of a commercial moisturizing cosmetic (product name: Chifure Wet and Soft Gel, manufactured by Chifure Corp.), 2 g of the microspherical particles of Example 2-2 (Microspherical Particle 5), Example 2-6 (Microspherical Particle 6), Example 1-3 (Microspherical Particle 3), or Example 1-2 (Microspherical Particle 2), mentioned above, were each added and stirred well to prepare a mixture liquid, thereby obtaining each gel agent.

[0137] <Cosmetic Composition, Evaluation of Massage (Body)>

[0138] Each cosmetic composition of the cream, the solid stick, the milky lotion, the oil, or the gel was applied at an appropriate amount on the brachium and elbow of five subjects by lightly stroking. Then, feeling of application was evaluated according the following indexes. The evaluation was indicated with the average value of the five subjects. Evaluation results are shown in Table 3. [0139] A: Tactile sensation with massage feeling was given. [0140] B: Tactile sensation with weak massage feeling was given. [0141] C: No tactile sensation with no massage feeling was given.

[0142] Note that when two evaluation indexes are tied with the symbol of -, it means that its evaluation is at the middle of these two indexes. For example, when an evaluation is between A and B, it is described as A-B.

[0143] <Cosmetic Composition, Evaluation of Wiping Off Feeling>

[0144] Furthermore, a coated surface was wiped off once with a tissue (product name: Scottie, manufactured by NIPPON PAPER CRECIA Corp.). Then, feeling of wiping off was evaluated according the following indexes. The evaluation was indicated with the average value of five subjects. Evaluation results are shown in Table 3. [0145] A: There was no or less feeling of friction at the time of wiping off. [0146] B: There was a little friction feeling at the time of the wiping off. [0147] C: There is strong friction feeling at the time of the wiping off, which causes pain.

[0148] <Cosmetic Composition, Evaluations of Massage (Face) and Wiping Off Feeling>

[0149] The massage feeling and wiping off feeling were evaluated in the same manner as described above, by using each cosmetic composition of the cream, the solid stick, the milky lotion, the oil, or the gel which were prepared as described above, except that it was evaluated at cheek and T-zone, which is the part from forehead to nose, of five subjects. Those were shown in Table 3 in the average value of the five subjects in the same manner as above. Evaluation results are shown in Table 3.

TABLE-US-00003 TABLE 3 Evaluation of Cosmetic Composition Body Face Microspherical Particle Wiping Wiping Type of Microspherical Average Particle Form of Massage off Massage Off Particle Diameter (m) Sphericity Cosmetices Effect Feeling Effect Feeling Microspherical Particle 5 88 0.69 Cream A A-B A A-B Microspherical Particle 6 58 0.70 A-B A-B A-B A-B Microspherical Particle 3 32 0.60 A-B A-B A-B A-B Microspherical Particle 2 24 0.65 A-B A-B A-B A-B Microspherical Particle 5 88 0.69 Solid A A-B A A-B Microspherical Particle 6 58 0.70 Stick A-B A-B A-B A-B Microspherical Particle 3 32 0.60 A-B A-B A-B A-B Microspherical Particle 2 24 0.65 A-B A-B A-B A-B Microspherical Particle 5 88 0.69 Milky A-B A-B A-B A-B Microspherical Particle 6 58 0.70 Lotion A-B B A-B B Microspherical Particle 3 32 0.60 A-B B A-B B Microspherical Particle 2 24 0.65 A-B B A-B B Microspherical Particle 5 88 0.69 Oil A A-B A A-B Microspherical Particle 6 58 0.70 A-B B A-B B Microspherical Particle 3 32 0.60 A-B B A-B B Microspherical Particle 2 24 0.65 A-B B A-B B Microspherical Particle 5 88 0.69 Gel A A-B A A-B Microspherical Particle 6 58 0.70 A-B B A-B B Microspherical Particle 3 32 0.60 A-B B A-B B Microspherical Particle 2 24 0.65 A-B B A-B B

[0150] Additional advantages and modifications will readily occur to those skilled in the art. Therefore, the invention in its broader aspects is not limited to the specific details and representative embodiments shown and described herein. Accordingly, various modifications may be made without departing from the spirit or scope of the general inventive concept as defined by the appended claims and their equivalents.