TW201737889A - Cellulose granules and method for producing same, and cleaning composition including said granules - Google Patents

Abstract

The present invention provides granules that impart a moderate scrubbing feeling during use and that pose little risk of negatively affecting the environment even if the granules flow into rivers or seas after washing and rinsing. Specifically, the present invention provides cellulose granules that include powdered cellulose and a water-soluble polymer, the powdered cellulose 1) having an average value of the maximum aspect ratio of 1.5-3, and 2) having an average maximum diameter of 80 [mu]m or less, the content of water-soluble polymer being 1-100 parts by mass per 100 parts by mass of powdered cellulose, and the average particle size being 100-1400 [mu]m.

Description

Cellulose particles, a method for producing the same, and a cleaning composition containing the same

FIELD OF THE INVENTION This invention relates to cellulose granules and methods of making same. Moreover, the present invention also relates to a composition containing the particles.

Background of the Invention In recent years, in order to remove aging keratinocytes and the like, moderate stimulation of the skin is promoted to promote metabolism, and physical washing is difficult to remove dirt (excess keratin) and dirt in the pores in order to wash off general skin detergents. Scrubbing, etc., the scrub cleaner is provided with a cosmetic lotion such as a rinse-type facial cleanser, a bath soap, a solid soap, or the like, a massage cream, and the like. These scrub cleaners have a moderate feeling of use (sand feel) with particle cleaning when cleaning the skin, and there is a strong demand.

The particles (sand particles) contained in the scrub detergent may be about 50 to 1000 μm composed of a plant endocarp or a seed or a pulverized material of a seed core, a synthetic resin polymer such as a nylon powder or a polyethylene powder. particle.

PRIOR ART DOCUMENT PATENT DOCUMENT Patent Document 1: Japanese Laid-Open Patent Publication No. Hei No. Hei 10-226621

DISCLOSURE OF THE INVENTION PROBLEM TO BE SOLVED BY THE INVENTION In recent years, after the abrasive particles which have been washed out after use have been poured into rivers or oceans, they are not decomposed and accumulate in nature, and there is a concern that environmental effects are adversely affected. The endocarp or seed of a plant or the pulverized material of a seed nucleus is a natural product that is environmentally friendly, but the shape of the smashed object is distorted, and the slipperiness of the particle cannot be said to be good, and there is a sharp part. Injury to the skin and other doubts.

Accordingly, it is an object of the present invention to provide a granule which is capable of imparting a moderate feeling of matte when used, and which has a problem of adversely affecting the environment even if it flows into a river or a sea after washing and rinsing.

Means for Solving the Problem In view of the current situation, the present inventors have actively evaluated the materials, manufacturing methods, characteristics, and the like of the particles to be used, and found that particles containing powdered cellulose and water-soluble polymers are very suitable and are reviewed repeatedly. The present invention has been completed.

The present invention includes, for example, the subject matter described in the following items. Item 1. A cellulose granule comprising powdered cellulose and a water-soluble polymer; wherein the powdered cellulose is the following powdered cellulose: 1) the average aspect ratio of the maximum aspect ratio is 1.5 to 3, and 2) the average maximum diameter is 80 μm or less; the content of the water-soluble polymer is from 1 to 100 parts by mass based on 100 parts by mass of the powdered cellulose; and the average particle diameter of the cellulose particles is from 100 to 1400 μm. Item 2. The cellulose particle according to Item 1, wherein the water-soluble polymer is polyvinyl alcohol or a modified substance thereof. Item 3. The cellulose particle according to Item 2, wherein the degree of saponification of the polyvinyl alcohol or the modified substance thereof is from 80 to 99%. Item 4. The cellulose particles according to any one of items 1 to 3, which have an average circularity of from 80 to 90. Item 5. The cellulose granule according to any one of items 1 to 4, which has a 10% displacement compressive strength of 1 MPa or more. The cellulose granule according to any one of items 1 to 5, which further comprises a pharmaceutical agent. Item 7. A method for producing a cellulose granule according to any one of items 1 to 6, which comprises the steps of: (B) a water-soluble polymer in which powdered cellulose has been dispersed (Comparative) The step of drying the aqueous solution of polyvinyl alcohol or its modified substance. Item 8. The method according to Item 7, which further comprises the following steps before the step (B): (A) heating and stirring the powdered cellulose, the water-soluble polymer and water to obtain a water-soluble high dispersion of the powdered cellulose. The step of a molecular aqueous solution. Item 9. The method according to Item 7 or 8, wherein the step (B) is a step of drying and granulating the water-soluble polymer aqueous solution in which the powdered cellulose has been dispersed by heating and stirring to evaporate the water. Item 10. A cleaning composition comprising the cellulose particles of any one of items 1 to 6.

EFFECT OF THE INVENTION The cellulose granules of the present invention can give a moderate feeling of matte when used, and have little doubt that the flow into the river or the sea adversely affects the environment after washing and rinsing. Further, the cellulose particles of the present invention are preferably in a state in which the storage stability is high when blended in an oil-based or water-based composition, and a moderate smooth feeling can be maintained for a long period of time.

Form for Carrying Out the Invention The cellulose particles of the present invention are particles containing powdered cellulose and a water-soluble polymer.

[Powdered Cellulose] The powdered cellulose contained in the cellulose particles of the present invention may be a known powdered cellulose, and for example, powdered cellulose such as cotton linters, pulp, or recycled fibers may be used.

The above powdered cellulose has a maximum aspect ratio of powdered cellulose having an average enthalpy of 1.5 to 3 and an average maximum diameter of 80 μm or less. By using the above powdered cellulose as a raw material of the cellulose particles of the present invention, the cellulose particles of the present invention having moderate strength and feeling of use can be obtained. The powdered cellulose having a maximum aspect ratio of an average enthalpy of more than 3 or an average maximum diameter of more than 80 μm is longer or larger in terms of cellulose fibers, so cellulose fibers obtained by using the powdered cellulose may have cellulose fibers. Run out of the surface of the particle, and the shape is distorted. Further, even if the warp-shaped cellulose particles are used as the frosted particles, the touch (feeling feeling) is soft and soft, and a frosty feeling cannot be obtained. The average aspect ratio of the above powdered cellulose is preferably 1.5 to 2.5. Further, the average maximum diameter of the above powdered cellulose is preferably from 10 to 80 μm, and preferably from 10 to 50 μm. Further, the method of measuring the average 値 and the average maximum diameter of the maximum aspect ratio will be described later.

The above powdered cellulose preferably has an average particle diameter of 10 to 60 μm and preferably 10 to 50 μm. When the average particle diameter is 60 μm or less, the cellulose fibers on the surface of the obtained particles can be suppressed from fluffing, and the matte particles can exhibit good graininess and feeling of use. Further, since the particles are dense, when the particles are blended in an oil-based or water-based oil composition, an appropriate smoothness can be maintained for a longer period of time. Further, the method of measuring the average particle diameter will be described later.

As the particle shape of the above powdered cellulose, fibrous or spherical powdered cellulose or the like can be used. The average roundness of the above powdered cellulose is preferably from 70 to 95, and preferably from 80 to 95. By making the average circularity 70 or more, the number of long-fibrous cellulose particles is reduced, and the surface of the obtained particles becomes smooth, and particles having a good feeling of use can be formed. In addition, the method of measuring the average circularity will be described later.

Further, the powdered cellulose can be mechanically dispersed and pulverized. By this treatment, the average 値, average maximum diameter, average particle diameter, and the like of the maximum aspect ratio of the powdered cellulose can be adjusted.

The apparatus for performing the above dispersion or pulverization treatment may, for example, be a dry pulverizer (for example, a hammer mill, a corner pulverizer, a jet mill, etc.) or a wet pulverizer (for example, a bead mill, a disc mill, a high pressure). Homogenizer).

[Water-Soluble Polymer] The water-soluble polymer contained in the cellulose particles of the present invention may, for example, be hydroxypropylcellulose, hydroxypropylmethylcellulose, polyvinyl alcohol, polyvinylpyrrolidone, polyethylene glycol, or Such modified substances and the like. One type of the water-soluble polymer or two or more types may be used in combination. In which the powdered cellulose can be fastened and bonded, and the storage stability in the aqueous solution of the prepared cellulose particles, the oil-water liquid (the composition of the aqueous component and the oil component; in particular, the oil-type composition in water) is improved. Moreover, it is preferable to be a biodegradable water-soluble polymer, and particularly preferably polyvinyl alcohol or a modified substance thereof, in view of a small load on the environment after washing and flowing off.

The average degree of polymerization of the above polyvinyl alcohol or its modified material is preferably from 100 to 3,000, and preferably from 300 to 2,600. When a polyvinyl alcohol having a higher average degree of polymerization or a modified product thereof is used, the strength is increased, and the mechanical properties of the obtained cellulose particles are also preferably improved. On the other hand, when polyvinyl alcohol having a low average degree of polymerization or a modified product thereof has high heat fusibility and high water solubility, it is difficult to maintain stable particle strength when the obtained cellulose particles are blended in an aqueous or water-based oil composition. By using polyvinyl alcohol or a modified product having an average degree of polymerization within the above range, cellulose particles which can maintain a moderate scrub feel for a long period of time can be obtained. Further, the average degree of polymerization was calculated from the molecular weight measured by the GPC method.

The degree of saponification of the above polyvinyl alcohol or its modified substance is preferably from 80 to 99 mol%, and is preferably from 90 to 99 mol%, more preferably from 95 to 99 mol%. When the degree of saponification is less than 80 mol%, when the obtained cellulose particles are blended in a water-based or water-in-oil composition with the frosted particles, they are easily soluble in water and difficult to maintain particle shape and strength, so that it is impossible to maintain the shape and strength of the particles. The long-term stable existence. By using polyvinyl alcohol having a degree of saponification within the above range or a modified substance thereof, cellulose particles which can maintain a moderate feeling of smoothness for a long period of time can be obtained.

Examples of the polyvinyl alcohol (PVA) modified product include an anion-modified PVA derivative and a cationically modified PVA derivative. The anion-modified PVA derivative may, for example, be a carboxylic acid-modified PVA, an undecylenic acid-modified PVA, a sulfonic acid-modified PVA or the like. The cationically modified PVA derivative can be exemplified by ammonium modified PVA, hydrazine modified PVA, amine modified PVA, and the like.

An anionically modified PVA derivative, for example, a carboxylic acid-modified PVA, can be produced by introducing a compound having a carboxyl group into polyvinyl alcohol by a conventionally known method. Examples of the compound having a carboxyl group include fumaric acid, maleic acid, itaconic acid, anhydrous maleic acid, phthalic anhydride, trimellitic anhydride, acrylic acid, and the like. Further, the sulfonic acid-modified PVA can be produced by introducing a compound having a sulfonic acid group into polyvinyl alcohol by a conventionally known method. Examples of the compound having a sulfonic acid group include ethylenesulfonic acid, allylsulfonic acid, methallylsulfonic acid, 2-propenylamine-2-methylpropanesulfonic acid, p-sulfonic acid benzaldehyde, and the like. Wait.

The total content (ratio) of the powdered cellulose and the water-soluble polymer in the cellulose particles of the present invention is preferably from 60 to 100% by mass, and preferably from 80 to 100% by mass. By setting the total amount to 60% by mass or more, it is possible to balance the appropriate matte feel and excellent environmental suitability.

Further, the content ratio of the powdered cellulose to the water-soluble polymer in the cellulose particles of the present invention is 1 to 100 parts by mass based on 100 parts by mass of the powdered cellulose and the water-soluble polymer. The water-soluble polymer is preferably 2 to 80 parts by mass, and preferably 3 to 70 parts by mass, more preferably 4 to 60 parts by mass, and more preferably 5 to 50 parts by mass, based on 100 parts by mass of the powdered cellulose.

The cellulose particles preferably have a configuration in which powdered cellulose is bonded to each other via a water-soluble polymer.

The material constituting the cellulose particles of the present invention may be a material other than powdered cellulose or a water-soluble polymer (referred to as "other components"). Other ingredients may, for example, be generally used for film coating agents (for example, hydroxypropylmethylcellulose phthalate, hydroxypropylmethylcellulose acetate succinate, carboxymethylethylcellulose, ethylcellulose). , ethyl cellulose aqueous dispersion, aminoalkyl methacrylate copolymer E, methacrylic acid copolymer L, methacrylic acid copolymer S, methacrylic acid copolymer LD, aminoalkyl methacrylic acid Ester copolymer RS, hardened oil, etc.), surfactant (such as sucrose fatty acid ester, polyoxyethylene polyoxypropylene glycol, polysorbate, sodium lauryl sulfate, etc.), excipients (such as corn starch, potato starch, Rice starch, powdered sugar, lactose, D-mannitol, trehalose, crystalline cellulose, sodium carboxymethylcellulose, etc.), disintegrating agents (such as low-substituted hydroxypropyl cellulose, carboxymethyl cellulose calcium, and A component of a preparation such as sodium carboxymethylcellulose or partially gelatinized starch.

Further, the cellulose particles of the present invention may also contain a pharmaceutical agent. At this time, the cellulose particles of the present invention can exert an effect from a drug. Examples of the agent include a moisturizer, a touch modifier, a reductant, an oxidizing agent, a preservative, an antibacterial agent, a chelating agent, a pH adjuster, a UV absorber, a whitening agent, a vitamin and a derivative thereof, an anti-inflammatory drug, and an anti-inflammatory agent. , hair growth agent, blood circulation agent, stimulant, hormone, anti-wrinkle agent, anti-aging agent, firming agent, cold feeling agent, temperature sensitive agent, wound healing promoter, excitatory mitigator, analgesic, cell activator , plants, animals, microbial extracts, antipruritic agents, keratin separation, dissolution agents, sweating agents, cooling agents, astringents, anti-inflammatory analgesics, antifungals, antihistamines, sleeping sedatives, Ningshen, Antihypertensive agent, blood pressure diuretic, antibiotic, anesthetic, antibacterial substance, antiepileptic agent, coronary vasodilator, crude drug, moisturizer, antipruritic agent, keratin softening separating agent, ultraviolet shielding agent, antiseptic and bactericide, antioxidant Wait. The method of causing the cellulose particles to contain the agents may, for example, be a method of immersing the cellulose particles in a solvent solution in which a drug is dissolved in a suitable solvent (for example, water, alcohol, etc.), and coating the drug solution in the cellulose particles (for example, using a spray) The method of coating). The cellulose granules may also be dried after dipping or coating.

The cellulose particles of the present invention can be produced, for example, by drying an aqueous solution of a water-soluble polymer (hereinafter referred to as a "powdered cellulose dispersion") in which a powdered cellulose is dispersed.

The powdered cellulose dispersion can be produced, for example, by heating and mixing powdered cellulose such as cotton linters, pulp, and recycled fibers, and polyvinyl alcohol with water. Thereby, a slurry dispersion in which cellulose particles are dispersed in polyvinyl alcohol water is produced. The powdered cellulose used has a maximum aspect ratio of powdered cellulose having an average enthalpy of 1.5 to 3 and an average maximum diameter of 80 μm or less.

Heating and mixing can be carried out, for example, by mechanical treatment. The mechanical treatment can be carried out by a known method, for example, by a reaction vessel equipped with a stirrer, a Banbury mixer, a kneader, a uniaxial extruder, a twin-screw extruder, or the like. The powdered cellulose dispersion preferably contains, for example, 5 to 50% of a solid component (total of powdered cellulose and water-soluble polymer), and preferably contains 20 to 50%.

When the solid content concentration is high, the load can be completed when the evaporation is dry in the drying step. However, if the solid content is too high, the dispersion loses fluidity and is difficult to be uniformly mixed. Therefore, it is preferable to be a solid component in flowability. Dispersion was carried out in the amount.

Further drying can be carried out by allowing the cellulose powder dispersion to stand or heating under stirring to evaporate water. In particular, it is preferred to carry out drying under agitation and mixing to impart roundness (i.e., granulation) to the chamfering, and to produce dense and high-strength cellulose particles. The agitation mixing in the drying step can be carried out, for example, by using a jacketed kneader or a multi-shaft dryer or the like. After drying, the cellulose particles preferably have a water content of less than 2%.

Further, the obtained cellulose particles can be directly used in the present invention, and can be pulverized as needed. For example, the pulverization treatment can be performed by a dry pulverizer (for example, a hammer mill, a corner pulverizer, a jet mill, or the like), and the granule breaking particles (pulverized product) can be obtained by a classification treatment (for example, air classification, sieve classification). The pulverized material can also be suitably used as the cellulose granule of the present invention.

The cellulose particles of the present invention preferably have an average circularity of from 80 to 90. By having an average circularity of 80 or more, it is possible to suitably obtain a shape in which the particle shape is not warped and has a smooth feeling of use.

The cellulose particles of the present invention have an average particle diameter of from 100 to 1400 μm, and preferably from 150 to 800 μm. If the average particle diameter is less than 100 μm, it may be difficult to feel the graininess when used as a sanding agent. When the particle diameter is more than 1400 μm, the graininess is too strong at the time of use and the skin irritation is unfavorable.

The 10% displacement compressive strength of the cellulose particles of the present invention is preferably 1 MPa or more, and preferably 2 to 15 MPa. When the 10% displacement compressive strength is less than 1 MPa, the particle strength tends to be low, and there is a tendency that the graininess of moderate hardness is not felt.

Further, among the shape factors of the powdered cellulose and the cellulose particles, the average circularity, the average maximum diameter, the average minimum diameter, and the maximum aspect ratio are determined by an image analysis type particle size distribution measuring apparatus (for example, MicrotracBEL). MicrotracPartAn SI) determination. Other image analysis type particle size distribution measuring devices measured by the same principle (moving image analysis method) can also be used. The shape coefficients are described below.

Roundness: indicates the representative index of how close the projection image is to the circle (circle equivalent diameter/circumference diameter). Circle equivalent diameter: diameter of the circle having the same area as the particle projection image. Average diameter of the maximum aspect ratio of the circle with the same circumference: the average maximum diameter of the maximum aspect ratio calculated by the minimum diameter/maximum diameter: the largest diameter of the two parallel lines of the entrapped particle image (maximum diameter) Average mean diameter of the mean: the average of the smallest diameter (minimum diameter) of the two parallel lines of the particle, and the maximum and minimum diameters here are also called the maximum Frette path and the minimum Frey Trail.

Further, the average particle diameter of the cellulose particles was sieved by a Ro-tap type sieve oscillating machine (for example, a sifter type A), and a 30 g sample was sieved for 15 minutes using a JIS standard sieve (Z8801-1987). The particle size distribution was measured, and the particle size at which 50% by weight was accumulated was taken as the average particle diameter. In addition, the number of repetitions is set to 3, and the average 値 is taken.

In addition, the 10% displacement compressive strength of the cellulose particles is subjected to a load on the granulated particles (cellulose particles) by a micro compression tester (for example, a micro compression tester MCT-510 manufactured by Shimadzu Corporation) to measure the particle shape by 10%. The enthalpy of compression strength at the time of displacement.

The present invention also encompasses a cleaning composition comprising the cellulose particles of the present invention. The cleaning composition is suitable for washing the composition of the skin (skin-washing composition). More specifically, it can be applied to, for example, facial cleansers, bath soaps, bath shampoos, shower gels, hand soaps, shampoos, dishwashing detergents, liquid detergent lotions, and the like. Further, the cleaning composition is preferably a water-based composition or an oil-based composition in water.

In addition to the cellulose granules, the cleaning composition may contain any component (substrate, carrier, active ingredient, etc.) generally used insofar as it does not impair the effects of the present invention in accordance with the use and purpose of the composition. Such components may, for example, be surfactants, oils, tackifiers, humectants, wetting agents, colorants, preservatives, tactile sensitizers, perfumes, anti-inflammatory agents, bactericides, ultraviolet absorbers, antioxidants, condensation Agents such as agents, whitening agents, anti-inflammatory agents, water, alcohols, and the like.

The content of the cellulose particles in the cleaning composition is, for example, 0.5 to 30% by mass, 1 to 20% by mass, or 2 to 10% by mass.

EXAMPLES Hereinafter, the present invention will be described in detail by way of examples. In addition, the average roundness, the average maximum diameter, the average minimum diameter, and the maximum aspect ratio of the following powdered cellulose and cellulose particles were determined by using an image-analyzed particle size distribution measuring apparatus (Microtrac Part An SI manufactured by MicrotracBEL Co., Ltd.). Determination. Further, the average particle diameter of the cellulose particles was measured by a Ro-tap sieve shaker (manufactured by Hirohisa Kogyo Co., Ltd., shaker type A) and sieved with a JIS standard sieve (Z8801-1987) for 15 minutes. The particle size distribution was measured, and a particle size of 50% by weight was accumulated as an average particle diameter. In addition, the 10% displacement compressive strength of the cellulose particles was determined by applying a load to the cellulose particles using a micro compression tester MCT-510 manufactured by Shimadzu Corporation to measure the compressive strength at the time of 10% displacement of the particle particle shape.

[Example 1] 100 parts by mass of powdered cellulose "KC FLOCK W-400" (manufactured by Nippon Paper Co., Ltd., average 値2.1 of maximum aspect ratio, average maximum diameter of 35 μm), and 20 parts by mass of polyvinyl alcohol "PVA124" (( Kuraray, saponification degree 99%, average polymerization degree 2400) and 300 parts by mass of water were put into the table kneading machine "PBV-06S" (manufactured by the company) and stirred at 90 ° C for 1 hour to produce There is a powdered cellulose dispersed slurry dispersion.

Next, the slurry dispersion was stirred in the above-mentioned table kneading machine while heating with a jacket to 98 ° C to evaporate water to prepare cellulose particles.

The obtained cellulose particles had an average particle diameter of 550 μm and an average circularity of 87. Further, the obtained cellulose particles have a 10% displacement compressive strength of up to 9.5 MPa, and have sufficient strength in the case of frosted particles.

Further, five male testers evaluated the tactile sensation of the above cellulose particles in five stages on the basis of the following criteria, with an average of five points, and the slipperiness was smooth and moderately irritated to the skin. In addition, the evaluation of the tactile sensation of the following cellulose particles was also used.

<Evaluation Criteria for Tactile Properties of Cellulose Particles> 5 points: Slippery and strongly felt grainy.

4 points: It is slippery and feels grainy.

3 points: Feel the grain but not strong.

2 points: Feel the grain but weak.

1 point: I don't feel grainy.

[Example 2] In addition to replacing the powdered cellulose "KC FLOCK W-400" with "KC FLOCK W-100" (manufactured by Nippon Paper Co., Ltd., the average aspect ratio of 最大2.8, the average maximum diameter of 62 μm), In the same manner as in Example 1, cellulose particles having an average particle diameter of 680 μm were produced. The cellulose particles have an average circularity of 82 and a 10% displacement compressive strength of up to 5.0 MPa, which is sufficient strength for the abrasive particles.

Further, five male testers evaluated the tactile sensation of the above cellulose particles in five stages, with an average of 4 points, which was smooth and smooth and gave moderate stimulation to the skin.

[Example 3] An average of the same manner as in Example 1 was carried out except that the amount of polyvinyl alcohol "PVA124" (Kuraray, saponification degree: 99%, average polymerization degree: 2,400) was 10 parts by mass. Cellulose particles having a particle size of 260 μm. The cellulose particles have an average circularity of 88, and the 10% displacement compressive strength is as high as 12.6 MPa, which is sufficient strength for the abrasive particles. Further, five male testers evaluated the tactile sensation of the above cellulose particles in five stages, with an average of five points, which was smooth and smooth, and gave moderate stimulation to the skin.

[Example 4] The water in the slurry-like dispersion was evaporated without using a table kneading machine, and the mixture was allowed to stand to dry to evaporate the water, and the recovered dry solids was subjected to a high-speed pulverizer "Rotor Speed Mill pulverisette 14" ( Cellulose particles having an average particle diameter of 300 μm were produced in the same manner as in Example 1 except that the pulverization treatment was carried out by FRITSCH JAPAN (manufacturing). The cellulose particles have an average circularity of 84 and a 10% displacement compressive strength of up to 1.4 MPa, which is sufficient strength for the frosted particles.

Further, five male testers evaluated the tactile sensation of the above cellulose particles in five stages, with an average of 4 points, which was smooth and smooth and gave moderate stimulation to the skin.

[Example 5] The same as in Example 1 except that the polyvinyl alcohol "PVA124" was changed to "AH-26" (manufactured by Nippon Synthetic Chemical Industry Co., Ltd., saponification degree: 97 to 99%, average polymerization degree: 2600). Cellulose particles having an average particle diameter of 260 μm were produced in the same manner. The cellulose particles have an average circularity of 88, 10% compressive strength of up to 10 MPa, and have sufficient strength in the case of frosted particles.

Further, five male testers evaluated the tactile sensation of the above cellulose particles in five stages, with an average of five points, which was smooth and smooth, and gave moderate stimulation to the skin.

[Example 6] A pseudo-fresh detergent was prepared by blending 5 parts by mass of the cellulose particles obtained in Example 1 with respect to 100 parts by mass of a commercially available detergent (with no added abrasive). Five male testers evaluated the feeling of use of the pseudo-scrub detergent as an average of 5 points, and a smooth and good graininess was felt in the detergent.

Further, five male testers evaluated the feeling of use of the above-mentioned quasi-frost detergent after leaving it at 60 ° C for 6 months in an average of 5 points, and felt good graininess without any sensation. In addition, the evaluation criteria of the following scrub detergents were also used. Moreover, the commercially available detergents (without added scrub) used below are all the same.

<Evaluation criteria for the feeling of use of the scrub detergent> 5 points: It has a slippery property and can strongly feel the graininess. 4 points: It is slippery and feels grainy. 3 points: Feel the grain but not strong. 2 points: Feel the grain but weak. 1 point: I don't feel grainy.

[Example 7] A pseudo-fresh detergent was prepared by blending 5 parts by mass of the cellulose particles obtained in Example 2 with respect to 100 parts by mass of a commercially available detergent (no addition of a sanding agent). Five male testers evaluated the feeling of use of the pseudo-scrub detergent as an average of 4 points, and a smooth and good graininess was felt in the detergent.

Further, five male testers evaluated the feeling of use of the above-mentioned pseudo-scrub detergent at 60 ° C for 6 months, and averaged 4 points, and felt good graininess without any feeling of discomfort.

[Example 8] A pseudo-fresh detergent was prepared by blending 5 parts by mass of the cellulose particles obtained in Example 3 with respect to 100 parts by mass of a commercially available detergent (no addition of a sanding agent). Five male testers evaluated the feeling of use of the pseudo-scrub detergent as an average of 5 points, and a smooth and good graininess was felt in the detergent.

Further, five male testers evaluated the feeling of use of the above-mentioned quasi-frost detergent after leaving it at 60 ° C for 6 months in an average of 5 points, and felt good graininess without any sensation.

[Example 9] A pseudo-fresh detergent was prepared by blending 5 parts by mass of the cellulose particles obtained in Example 4 with respect to 100 parts by mass of a commercially available detergent (no addition of a sanding agent). Five male testers evaluated the feeling of use of the pseudo-scrub detergent as an average of 4 points, and a smooth and good graininess was felt in the detergent.

Further, five male testers evaluated the feeling of use of the above-mentioned pseudo-scrub detergent at 60 ° C for 6 months, and averaged 4 points, and felt good graininess without any feeling of discomfort.

[Example 10] A pseudo-fresh detergent was prepared by blending 5 parts by mass of the cellulose particles obtained in Example 5 with respect to 100 parts by mass of a commercially available detergent (no addition of a sanding agent). Five male testers evaluated the feeling of use of the pseudo-scrub detergent as an average of 5 points, and a smooth and good graininess was felt in the detergent.

Further, five male testers evaluated the feeling of use of the above-mentioned quasi-frost detergent after leaving it at 60 ° C for 6 months in an average of 5 points, and felt good graininess without any sensation.

[Example 11] An average particle was produced in the same manner as in Example 1 except that "PVA224" (manufactured by Kuraray: saponification degree: 86 to 89%, average polymerization degree: 2400) was used instead of polyvinyl alcohol "PVA124". Cellulose particles having a diameter of 350 μm. The cellulose particles have an average circularity of 84 and a 10% compressive strength of up to 4.0 MPa, which is sufficient strength for the abrasive particles.

Further, five male testers evaluated the tactile sensation of the above cellulose particles in five stages, with an average of five points, which was smooth and smooth, and gave moderate stimulation to the skin.

Then, a detergent was prepared in the same manner as in Example 6 using the above cellulose particles. Five male testers evaluated the feeling of use of the pseudo-scrub detergent as a five-stage evaluation with an average of 5 points, and a smooth and good graininess was felt in the detergent.

Moreover, the five-stage evaluation was performed similarly to the feeling of use of the pseudo-frost cleaner after being left at 60 ° C for 6 months, with an average of 3 points. Although it was guessed that a diachronic change occurred in the detergent, it was still felt. Grainy.

[Example 12] An average of the same manner as in Example 1 was carried out except that the amount of polyvinyl alcohol "PVA124" (Kuraray, saponification degree: 99%, average polymerization degree: 2,400) was 100 parts by mass. Cellulose particles having a particle size of 700 μm. The cellulose particles have an average circularity of 80 and a 10% displacement compressive strength of up to 14.5 MPa, which is sufficient strength for the abrasive particles.

Further, five male testers evaluated the tactile sensation of the above cellulose particles in five stages, with an average of 4 points, and the slipperiness was smooth and moderately irritated to the skin.

Further, a detergent was prepared in the same manner as in Example 6 using the above cellulose particles. Five male testers evaluated the feeling of use of the pseudo-scrub detergent as a five-stage evaluation with an average of 4 points, and a smooth and good graininess was felt in the detergent.

In addition, the five-stage evaluation was carried out in the same manner as the feeling of use of the pseudo-frosting detergent after leaving it at 60 ° C for 6 months, and an average of 4 points was obtained, and a good graininess was felt without any feeling of discomfort.

[Comparative Example 1] The powder cellulose "KC FLOCK W-400" was changed to "KC FLOCK W-50" (manufactured by Nippon Paper Co., Ltd., the average aspect ratio of the maximum 値3.5, the average maximum diameter of 94 μm, and the average minimum diameter of 27 μm) Further, cellulose particles having an average particle diameter of 460 μm were produced in the same manner as in Example 1. The cellulose particles had an average circularity of 75, and the cellulose fibers protruded from the surface of the particles and fluffed, and the slipperiness was poor, and the 10% compressive strength was also low, being 0.8 MPa. Five male testers evaluated the tactile sensation of the cellulose particles in five stages, with an average of 2 points, and no graininess was felt with the frosted particles.

Then, a detergent was prepared in the same manner as in Example 6 using the above cellulose particles. Five male testers evaluated the feeling of use of the pseudo-scrub detergent as a five-stage evaluation, and on average, two points, a smooth graininess was not felt in the detergent, and the feeling of use was insufficient.

Further, the feeling of use of the pseudo-frost cleaner after standing at 60 ° C for 6 months was similarly evaluated in five stages, and on average, two points were not observed, and a good graininess was not felt.

[Comparative Example 2] The same procedure as in Example 1 was carried out except that the powdered cellulose "KC FLOCK W-400" was changed to "cotton pulp" (average 値 4.0 of the maximum aspect ratio and an average maximum diameter of 105 μm). Cellulose particles having an average particle diameter of 250 μm were obtained. The cellulose particles have an average circularity of 70, and the cellulose fibers protrude from the surface of the particles (particles) and are fluffy, have poor slipperiness, and have a low compressive strength of 10%, which is 0.6. The feeling of the cellulose particles by the five male testers. A 5-stage evaluation was performed with an average of 2 points, and the graininess was not felt by the frosted particles.

Then, a detergent was prepared in the same manner as in Example 6 using the above cellulose particles. Five male testers evaluated the feeling of use of the pseudo-sanding detergent in five stages, with an average of two points, and the smooth graininess was not felt and the feeling of use was insufficient.

Further, the feeling of use of the pseudo-frost cleaner after standing at 60 ° C for 6 months was evaluated in the same manner in five stages, and the average was two points, and it was not possible to change the graininess.

[Example 13] An average particle was produced in the same manner as in Example 1 except that "PVA505" (manufactured by Kuraray: saponification degree: 73 to 75%, average polymerization degree: 2000) was used instead of polyvinyl alcohol "PVA124". Cellulose particles having a diameter of 250 μm. The cellulose particles had an average circularity of 85 and a 10% compressive strength of 2.0 MPa. Five male testers evaluated the tactile sensation of the prepared cellulose granules in five stages, with an average of 5 points, which was smooth and smooth and gave moderate stimulation to the skin.

Further, a detergent was prepared in the same manner as in Example 6 using the above cellulose particles. Five male testers evaluated the feeling of use of the pseudo-scrub detergent as a five-stage evaluation with an average of 5 points, and a smooth and good graininess was felt in the detergent.

However, the five-stage evaluation was performed in the same manner as the feeling of use of the above-mentioned quasi-smooth detergent at 60 ° C for 6 months, and an average of 1 minute indicates that the particle shape could not be maintained.

From this, it is understood that the degree of saponification of the polyvinyl alcohol used affects the stability of the cellulose particles.

[Comparative Example 4] 100 parts by mass of powdered cellulose "KC FLOCK W-400" (manufactured by Nippon Paper Co., Ltd., average 値2.1 of maximum aspect ratio, average maximum diameter of 35 μm), and 30 parts by mass of hydroxyethylcellulose "HEC" (Sumitomo Seiki Co., Ltd.) and 300 parts by mass of water were put into a table kneading machine "PBV-06S" (manufactured by the company), and stirred and mixed for 1 hour to obtain a powdery cellulose dispersed slurry. Dispersion.

The water in the slurry dispersion was evaporated without using a table kneading machine, and the mixture was allowed to stand to dry to evaporate the water, and the recovered dry solids were subjected to a high-speed pulverizer "Rotor Speed Mill pulverisette 14" (FRITSCH JAPAN) In the same manner as in Example 1, except that the pulverization treatment was carried out, the granules were not obtained, and the granules could not be obtained.

[Comparative Example 5] 100 parts by mass of powdered cellulose "KC FLOCK W-400" (manufactured by Nippon Paper Co., Ltd., average 値2.1 of maximum aspect ratio, average maximum diameter: 35 μm), and 150 parts by mass of polyvinyl alcohol "PVA124" (( Kuraray, saponification degree 99%, average polymerization degree 2400) and 100 parts by mass of water were put into the table kneading machine "PBV-06S" (made by the company) and stirred for 1 hour to obtain the existing powder fiber. a dispersible slurry dispersion.

Next, the slurry dispersion was stirred in the above-mentioned table kneading machine, and the water was evaporated to 98 ° C with a jacket to evaporate the water to obtain a dry solid, which was a plate-like particle, which was poor in slipperiness and did not have a moderate touch.

[Example 14] 100 parts by mass of powdered cellulose "cotton pulp" (average 値 4.0 of maximum aspect ratio, average maximum diameter of 105 μm) was dispersed in 300 parts by mass of water, and the obtained product was dispersed at a high pressure. The treatment apparatus (NIRO-SOAVI TYPE NS100IL2K, 150 MPa) was subjected to one treatment to obtain a powdered cellulose dispersion. The powdered cellulose dispersion in the powdered cellulose dispersion had an average aspect ratio of 2.5 and an average maximum diameter of 48 μm.

The powdered cellulose dispersion (100 parts by mass in terms of powdered cellulose) and 20 parts by mass of polyvinyl alcohol "PVA124" (Kuraray, saponification degree 99%, average degree of polymerization 2400) were used in accordance with Example 1. Cellulose particles having an average particle diameter of 320 μm were produced in the same manner.

The cellulose particles have an average circularity of 81 and a 10% displacement compressive strength of up to 11.0 MPa. In addition, five male testers evaluated the tactile sensation of the cellulose granules in five stages, with an average of 4 points, which was smooth and smooth and gave moderate stimulation to the skin.

Further, a detergent was prepared in the same manner as in Example 6 using the above cellulose particles. Five male testers evaluated the feeling of use of the pseudo-scrub detergent as a five-stage evaluation with an average of 4 points, and a smooth and good graininess was felt in the detergent.

In addition, the five-stage evaluation was carried out in the same manner as the feeling of use of the pseudo-frosting detergent after leaving it at 60 ° C for 6 months, and an average of 4 points was obtained, and a good graininess was felt without any feeling of discomfort.

no

Claims (10)

a cellulose granule comprising powdered cellulose and a water-soluble polymer; wherein the powdered cellulose is the following powdered cellulose: 1) the average aspect ratio of the maximum aspect ratio is 1.5 to 3, and 2) the average maximum diameter is less than 80 μm; The content of the water-soluble polymer is from 1 to 100 parts by mass based on 100 parts by mass of the powdered cellulose; and the average particle diameter of the cellulose particles is from 100 to 1400 μm. The cellulose particle of claim 1, wherein the water soluble polymer is polyvinyl alcohol or a modified substance thereof. The cellulose granule according to claim 2, wherein the degree of saponification of the polyvinyl alcohol or the modified substance thereof is from 80 to 99%. The cellulose particles according to any one of claims 1 to 3, which have an average circularity of from 80 to 90. The cellulose particles according to any one of claims 1 to 4, which have a 10% displacement compressive strength of 1 MPa or more. The cellulose granule according to any one of claims 1 to 5, which further contains a pharmaceutical agent. A method for producing a cellulose granule according to any one of claims 1 to 6, which comprises the steps of: (B) drying a water-soluble polymer aqueous solution in which powdered cellulose has been dispersed; . The method of claim 7, which further comprises the following steps before the step (B): (A) heating and stirring the powdered cellulose, the water-soluble polymer and water to obtain a water-soluble polymer aqueous solution in which the powdered cellulose has been dispersed. The steps. The method of claim 7 or 8, wherein the step (B) is a step of drying and granulating the water-soluble polymer aqueous solution in which the powdered cellulose has been dispersed by heating and stirring to evaporate the water. A cleaning composition comprising the cellulose particles of any one of claims 1 to 6.